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Sample records for synchrotron x-ray microdiffraction

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

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-12-01

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

  3. Indentation Size Effects in Single Crystal Copper as Revealed by Synchrotron X-ray Microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Feng, G.; Budiman, A. S.; Nix, W. D.; Tamura, N.; Patel, J. R.

    2007-11-19

    The indentation size effect (ISE) has been observed in numerous nanoindentation studies on crystalline materials; it is found that the hardness increases dramatically with decreasing indentation size - a 'smaller is stronger' phenomenon. Some have attributed the ISE to the existence of strain gradients and the geometrically necessary dislocations (GNDs). Since the GND density is directly related to the local lattice curvature, the Scanning X-ray Microdiffraction ({mu}SXRD) technique, which can quantitatively measure relative lattice rotations through the streaking of Laue diffractions, can used to study the strain gradients. The synchrotron {mu}SXRD technique we use - which was developed at the Advanced Light Source (ALS), Berkeley Lab - allows for probing the local plastic behavior of crystals with sub-micrometer resolution. Using this technique, we studied the local plasticity for indentations of different depths in a Cu single crystal. Broadening of Laue diffractions (streaking) was observed, showing local crystal lattice rotation due to the indentation-induced plastic deformation. A quantitative analysis of the streaking allows us to estimate the average GND density in the indentation plastic zones. The size dependence of the hardness, as found by nanoindentation, will be described, and its correlation to the observed lattice rotations will be discussed.

  4. Synchrotron X-ray Microdiffraction Analysis of Proton Irradiated Polycrystalline Diamond Films

    Science.gov (United States)

    Newton, R. I.; Davidson, J. L.; Ice, G. E.; Liu, W.

    2004-01-01

    X-ray microdiffraction is a non-destructive technique that allows for depth-resolved, strain measurements with sub-micron spatial resolution. These capabilities make this technique promising for understanding the mechanical properties of MicroElectroMechanical Systems (MEMS). This investigation examined the local strain induced by irradiating a polycrystalline diamond thin film with a dose of 2x10(exp 17) H(+)per square centimeter protons. Preliminary results indicate that a measurable strain, on the order of 10(exp -3), was introduced into the film near the End of Range (EOR) region of the protons.

  5. 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.

  6. Plastic deformation in Al (Cu) interconnects stressed by electromigration and studied by synchrotron polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Advanced Light Source; UCLA; Chen, Kai; Chen, Kai; Tamura, Nobumichi; Valek, Bryan C.; Tu, King-Ning

    2008-05-14

    We report here an in-depth synchrotron radiation based white beam X-ray microdiffraction study of plasticity in individual grains of an Al (Cu) interconnect during the early stage of electromigration. The study shows a rearrangement of the geometrically necessary dislocations (GND) in bamboo typed grains during that stage. We find that about 90percent of the GNDs are oriented so that their line direction is the closest to the current flow direction. In non-bamboo typed grains, the Laue peak positions shift, indicating that the grains rotate. An analysis in terms of force directions has been carried out and is consistent with observed electromigration induced grain rotation and bending.

  7. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-05-15

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

  10. Characterization of Local Strain around Through-Silicon Via Interconnects by Using X-ray Microdiffraction

    Science.gov (United States)

    Nakatsuka, Osamu; Kitada, Hideki; Kim, Youngsuk; Mizushima, Yoriko; Nakamura, Tomoji; Ohba, Takayuki; Zaima, Shigeaki

    2011-05-01

    We have demonstrated the characterization of the local strain structure in thinned Si layers for wafer-on-a-wafer (WOW) applications by using X-ray microdiffraction with a synchrotron radiation source. The microdiffraction reveals the fluctuation of strains in the thin Si layer around through-silicon via (TSV) interconnects with a sub-micrometer scale. We can separately estimated the in-plane and out-of-plane strain structures in the Si layer, and found that the anisotropic strain is induced in the Si layer between the TSV interconnects.

  11. Probing Phase Transformations and Microstructural Evolutions at the Small Scales: Synchrotron X-ray Microdiffraction for Advanced Applications in [Phase 3 Memory,] 3D IC (Integrated Circuits) and Solar PV (Photovoltaic) Devices

    Energy Technology Data Exchange (ETDEWEB)

    Radchenko, I. [Singapore Univ. of Technology and Design (SUTD) (Singapore); Tippabhotla, S. K. [Singapore Univ. of Technology and Design (SUTD) (Singapore); Tamura, N. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Budiman, A. S. [Singapore Univ. of Technology and Design (SUTD) (Singapore)

    2016-10-21

    Synchrotron x-ray microdiffraction (μXRD) allows characterization of a crystalline material in small, localized volumes. Phase composition, crystal orientation and strain can all be probed in few-second time scales. Crystalline changes over a large areas can be also probed in a reasonable amount of time with submicron spatial resolution. However, despite all the listed capabilities, μXRD is mostly used to study pure materials but its application in actual device characterization is rather limited. This article will explore the recent developments of the μXRD technique illustrated with its advanced applications in microelectronic devices and solar photovoltaic systems. Application of μXRD in microelectronics will be illustrated by studying stress and microstructure evolution in Cu TSV (through silicon via) during and after annealing. Here, the approach allowing study of the microstructural evolution in the solder joint of crystalline Si solar cells due to thermal cycling will be also demonstrated.

  12. X-ray powder microdiffraction for routine analysis of paintings

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Hradil, David; Grygar, Tomáš

    2005-01-01

    Roč. 20, č. 3 (2005), s. 224-229 ISSN 0885-7156 R&D Projects: GA MŠk(CZ) LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray microdiffraction * art work analysis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.483, year: 2005

  13. Lawrence Bragg, microdiffraction and X-ray lasers.

    Science.gov (United States)

    Spence, J C H

    2013-01-01

    We trace the historical development of W. L. Bragg's `law' and the key experimental observation which made it possible using polychromatic radiation at a time when neither X-ray wavelengths nor cell constants were known. This led, through his phasing and solving large mineral structures (without use of a computer), to work on metals, proteins, bubble rafts and his X-ray microscope. The relationship of this to early X-ray microdiffraction is outlined, followed by a brief review of electron microdiffraction methods, where electron-probe sizes smaller than one unit cell can be formed with an interesting `failure' of Bragg's law. We end with a review of recent femtosecond X-ray `snapshot' diffraction from protein nanocrystals, using an X-ray laser which generates pulses so short that they terminate before radiation damage can commence, yet subsequently destroy the sample. In this way, using short pulses instead of freezing, the nexus between dose, resolution and crystal size has been broken, opening the way to time-resolved diffraction without damage for a stream of identical particles.

  14. Application of white-beam X-ray microdiffraction for the study of mineralogical phase identification in ancient Egyptian pigments

    OpenAIRE

    Lynch, P.A.; Tamura, N.; Lau, D.; Madsen, I.; Liang, D.; Strohschnieder, M.; Stevenson, A.W.

    2007-01-01

    High-brightness synchrotron X-rays together with precision achromatic focusing optics on beamline 7.3.3 at the Advanced Light Source have been applied for Laue microdiffraction analysis of mineralogical phases in Egyptian pigments. Although this task is usually performed using monochromatic X-ray diffraction, the Laue technique was both faster and more reliable for the present sample. In this approach, white-beam diffraction patterns are collected as the sample is raster scanned across the in...

  15. X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Raman, S.; Sparks, C.J. Jr.

    1978-01-01

    An experimental set-up for x-ray fluorescence analysis with synchrotron radiation was built and installed at the Stanford Synchrotron Radiation Project. X-ray spectra were taken from numerous and varied samples in order to assess the potential of synchrotron radiation as an excitation source for multielement x-ray fluorescence analysis. For many applications, the synchrotron radiation technique is shown to be superior to other x-ray fluorescence methods, especially those employing electrons and protons as excitation sources

  16. High-Performance Parallel and Stream Processing of X-ray Microdiffraction Data on Multicores

    International Nuclear Information System (INIS)

    Bauer, Michael A; McIntyre, Stewart; Xie Yuzhen; Biem, Alain; Tamura, Nobumichi

    2012-01-01

    We present the design and implementation of a high-performance system for processing synchrotron X-ray microdiffraction (XRD) data in IBM InfoSphere Streams on multicore processors. We report on the parallel and stream processing techniques that we use to harvest the power of clusters of multicores to analyze hundreds of gigabytes of synchrotron XRD data in order to reveal the microtexture of polycrystalline materials. The timing to process one XRD image using one pipeline is about ten times faster than the best C program at present. With the support of InfoSphere Streams platform, our software is able to be scaled up to operate on clusters of multi-cores for processing multiple images concurrently. This system provides a high-performance processing kernel to achieve near real-time data analysis of image data from synchrotron experiments.

  17. Local layer structure of smectic liquid crystals by X-ray micro-diffraction

    CERN Document Server

    Takanishi, Y

    2003-01-01

    The local layer structure of smectic liquid crystal has been measured using time-resolved synchrotron X-ray micro-diffraction. Typical layer disorders observed in surface stabilized (anti-) ferroelectric liquid crystals, i.e. a stripe texture, a needed-like defect and a zigzag defect, are directly analyzed. The detailed analysis slows that the surface anchoring force due to the interaction between the liquid crystal molecule and the alignment thin film plays an important role to realize both the static and dynamic local layer structures. The layer structure of the circular domain observed in the liquid crystal of bent-shaped molecules found to depend on the applied electric field though the optical micrograph shows little difference. The frustrated, double and single layer structures of the bent-shaped molecule liquid crystal are determined depending on the terminal alkyl chain length. (author)

  18. Tensile strained germanium nanowires measured by photocurrent spectroscopy and X-ray microdiffraction.

    Science.gov (United States)

    Guilloy, Kevin; Pauc, Nicolas; Gassenq, Alban; Gentile, Pascal; Tardif, Samuel; Rieutord, François; Calvo, Vincent

    2015-04-08

    Applying tensile strain in a single germanium crystal is a very promising way to tune its bandstructure and turn it into a direct band gap semiconductor. In this work, we stress vapor-liquid-solid grown germanium nanowires along their [111] axis thanks to the strain tranfer from a silicon nitride thin film by a microfabrication process. We measure the Γ-LH direct band gap transition by photocurrent spectrometry and quantify associated strain by X-ray Laue microdiffraction on beamline BM32 at the European Synchrotron Radiation Facility. Nanowires exhibit up to 1.48% strain and an absorption threshold down to 0.73 eV, which is in good agreement with theoretical computations for the Γ-LH transition, showing that the nanowire geometry is an efficient way of applying tensile uniaxial stress along the [111] axis of a germanium crystal.

  19. Synchrotron X-ray magnetic scattering

    CERN Document Server

    Stirling, W G

    2003-01-01

    Research on magnetic materials constitutes an increasingly important part of the programmes of most major synchrotron radiation centres. The extremely high brilliance and small spot size of advanced synchrotron beamlines, combined with element-specific resonant effects at certain absorption edges, provide a powerful probe of magnetic structures and phase transitions, with excellent wavevector resolution. Over the last decade a variety of experimental techniques have been developed, exploiting these effects for the study of thin film, multilayer and bulk magnetic materials. In this paper the basic concepts of X-ray magnetic scattering will be introduced, followed by recent examples taken from work at Daresbury Laboratory (UK), the European Synchrotron Radiation Facility (Grenoble, France) and the National Synchrotron Light Source (Brookhaven National Laboratory, USA). Investigations of domain patterns in thin magnetic films employing X-ray resonant magnetic scattering (XRMS) will be described, followed by a se...

  20. Application of X-ray microdiffraction in non-destructive microanalysis of colour layers and microtraces

    Czech Academy of Sciences Publication Activity Database

    Grünwaldová, Veronika; Kotrlý, M.; Bezdička, Petr; Kotulanová, Eva; Hradil, David

    2006-01-01

    Roč. 13, č. 3 (2006), s. 152-153 ISSN 1210-8529 R&D Projects: GA MV RN20052005001 Institutional research plan: CEZ:AV0Z40320502 Keywords : X-ray powder microdiffraction * pigments * colour layers of artworks Subject RIV: CA - Inorganic Chemistry

  1. Scanning x-ray microdiffraction with submicron white beam for strain and orientation mapping in thin films

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, N.; MacDowell, A.A.; Spolenak, R.; Valek, B.C.; Bravman, J.C.; Brown, W.L.; Celestre, R.S.; Padmore, H.A.; Batterman, B.W.; Patel, J.R.

    2003-01-14

    Scanning X-ray Microdiffraction (m-SXRD) combines the use of high brilliance synchrotron sources with the latest achromatic X-ray focusing optics and fast large area 2D-detector technology. Using white beams or a combination of white and monochromatic beams, it allows for orientation and strain/stress mapping of polycrystalline thin films with submicron spatial resolution. The technique is described in detail as applied to the study of thin aluminium and copper blanket films and lines following electromigration testing and/or thermal cycling experiments. It is shown that there are significant orientation and strain/stress variations between grains and inside individual grains. A polycrystalline film when investigated at the granular (micron) level shows a highly mechanically inhomogeneous medium that allows insight into its mesoscopic properties. If the m-SXRD data are averaged over a macroscopic range, results show good agreement with direct macroscopic texture and stress measurements .

  2. Unraveling submicron-scale mechanical heterogeneity by three-dimensional X-ray microdiffraction

    Science.gov (United States)

    Li, Runguang; Xie, Qingge; Wang, Yan-Dong; Liu, Wenjun; Wang, Mingguang; Wu, Guilin; Li, Xiaowu; Zhang, Minghe; Lu, Zhaoping; Geng, Chang; Zhu, Ting

    2018-01-01

    Shear banding is a ubiquitous phenomenon of severe plastic deformation, and damage accumulation in shear bands often results in the catastrophic failure of a material. Despite extensive studies, the microscopic mechanisms of strain localization and deformation damage in shear bands remain elusive due to their spatial‑temporal complexities embedded in bulk materials. Here we conducted synchrotron-based X-ray microdiffraction (μXRD) experiments to map out the 3D lattice strain field with a submicron resolution around fatigue shear bands in a stainless steel. Both in situ and postmortem μXRD results revealed large lattice strain gradients at intersections of the primary and secondary shear bands. Such strain gradients resulted in severe mechanical heterogeneities across the fatigue shear bands, leading to reduced fatigue limits in the high-cycle regime. The ability to spatially quantify the localized strain gradients with submicron resolution through μXRD opens opportunities for understanding the microscopic mechanisms of damage and failure in bulk materials.

  3. Provenance study of Gothic paintings from North-East Slovakia by handheld x-ray fluorescence, microscopy and x-ray microdiffraction

    Czech Academy of Sciences Publication Activity Database

    Hradil, David; Hradilová, J.; Bezdička, Petr; Švarcová, Silvie

    2008-01-01

    Roč. 37, č. 4 (2008), s. 376-382 ISSN 0049-8246 R&D Projects: GA ČR(CZ) GA203/07/1324 Institutional research plan: CEZ:AV0Z40320502 Keywords : Gothic paintings * X-ray fluorescence * X-ray microdiffraction Subject RIV: CA - Inorganic Chemistry Impact factor: 1.390, year: 2008

  4. X-ray powder microdiffraction in the analysis of art works

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Bayerová, T.; Hradil, David

    2004-01-01

    Roč. 11, 1a (2004), s. 43 ISSN 1211-5894. [European Powder Diffraction Conference /9./. Prague, 02.09.2004-05.09.2004] R&D Projects: GA MŠk LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z4032918 Keywords : X-ray powder microdiffraction * pigments * colour layers of art works Subject RIV: CA - Inorganic Chemistry

  5. Fast X-ray microdiffraction techniques for studying irreversible transformations in materials.

    Science.gov (United States)

    Kelly, Stephen T; Trenkle, Jonathan C; Koerner, Lucas J; Barron, Sara C; Walker, Nöel; Pouliquen, Philippe O; Tate, Mark W; Gruner, Sol M; Dufresne, Eric M; Weihs, Timothy P; Hufnagel, Todd C

    2011-05-01

    A pair of techniques have been developed for performing time-resolved X-ray microdiffraction on irreversible phase transformations. In one technique capillary optics are used to focus a high-flux broad-spectrum X-ray beam to a 60 µm spot size and a fast pixel array detector is used to achieve temporal resolution of 55 µs. In the second technique the X-rays are focused with Kirkpatrick-Baez mirrors to achieve a spatial resolution better than 10 µm and a fast shutter is used to provide temporal resolution better than 20 µs while recording the diffraction pattern on a (relatively slow) X-ray CCD camera. Example data from experiments are presented where these techniques are used to study self-propagating high-temperature synthesis reactions in metal laminate foils.

  6. Techniques for materials research with synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Bowen, D.K.

    1983-01-01

    A brief introductory survey is presented of the properties and generation of synchrotron radiation and the main techniques developed so far for its application to materials problems. Headings are:synchrotron radiation; X-ray techniques in synchrotron radiation (powder diffraction; X-ray scattering; EXAFS (Extended X-ray Absorption Fine Structure); X-ray fluorescent analysis; microradiography; white radiation topography; double crystal topography); future developments. (U.K.)

  7. Synchrotron radiation X-ray microfluorescence techniques

    Indian Academy of Sciences (India)

    Synchrotron X-ray imaging systems with fluorescence techniques was developed for biomedical researches in Brazilian Synchrotron Laboratory. An X-ray fluorescence microtomography system was implemented to analyse human prostate and breast samples and an X-ray microfluorescence system was implemented to ...

  8. Synchrotron radiation X-ray microfluorescence techniques and ...

    Indian Academy of Sciences (India)

    Synchrotron X-ray imaging systems with fluorescence techniques was developed for biomedical researches in Brazilian Synchrotron Laboratory. An X-ray fluorescence microtomography system was implemented to analyse human prostate and breast samples and an X-ray microfluorescence system was implemented to ...

  9. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Cernik, R.J.

    1996-01-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school

  10. Glancing angle synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cernik, R.J. [Daresbury Lab., Warrington, WA (United States)

    1996-09-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school.

  11. Advanced Nanoscale Characterization of Cement Based Materials Using X-Ray Synchrotron Radiation: A Review

    KAUST Repository

    Chae, Sejung R.

    2013-05-22

    We report various synchrotron radiation laboratory based techniques used to characterize cement based materials in nanometer scale. High resolution X-ray transmission imaging combined with a rotational axis allows for rendering of samples in three dimensions revealing volumetric details. Scanning transmission X-ray microscope combines high spatial resolution imaging with high spectral resolution of the incident beam to reveal X-ray absorption near edge structure variations in the material nanostructure. Microdiffraction scans the surface of a sample to map its high order reflection or crystallographic variations with a micron-sized incident beam. High pressure X-ray diffraction measures compressibility of pure phase materials. Unique results of studies using the above tools are discussed-a study of pores, connectivity, and morphology of a 2,000 year old concrete using nanotomography; detection of localized and varying silicate chain depolymerization in Al-substituted tobermorite, and quantification of monosulfate distribution in tricalcium aluminate hydration using scanning transmission X-ray microscopy; detection and mapping of hydration products in high volume fly ash paste using microdiffraction; and determination of mechanical properties of various AFm phases using high pressure X-ray diffraction. © 2013 The Author(s).

  12. An automatic analysis of strain-depth profile in X-ray microdiffraction

    International Nuclear Information System (INIS)

    Lagomarsino, S.; Giannini, C.; Guagliardi, A.; Cedola, A.; Scarinci, F.; Aruta, C.

    2004-01-01

    The increased demanding of high spatial resolution analysis for local strain/stress measurements gave an impulse for developing new X-ray microdiffraction technique. In particular spatial resolution of the order of 100-300 nm can be recently obtained using an X-ray waveguides as optical element. However, the great number of datasets which must be acquired and analyzed to probe the full field of strain variations renders the high-resolution technique not suitable for systematic analysis. In this communication, we present a data treatment procedure for an automatic analysis of microdiffraction profiles measured with X-ray waveguide to obtain quantitative information about local strain variations. The presented procedure allows to extract a depth-dependent strain profile directly from the measured data to be used as initial guess for calculating the diffraction profile by means of the dynamical theory in the Takagi-Taupin recursive formalism. Then a Monte Carlo fitting data refinement is applied to optimize the strain profile

  13. 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

  14. A Superbend X-Ray Microdiffraction Beamline at the Advanced Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, N.; Kunz, M.; Chen, K.; Celestre, R.S.; MacDowell, A.A.; Warwick, T.

    2009-03-10

    Beamline 12.3.2 at the Advanced Light Source is a newly commissioned beamline dedicated to x-ray microdiffraction. It operates in both monochromatic and polychromatic radiation mode. The facility uses a superconducting bending magnet source to deliver an X-ray spectrum ranging from 5 to 22 keV. The beam is focused down to {approx} 1 um size at the sample position using a pair of elliptically bent Kirkpatrick-Baez mirrors enclosed in a vacuum box. The sample placed on high precision stages can be raster-scanned under the microbeam while a diffraction pattern is taken at each step. The arrays of diffraction patterns are then analyzed to derive distribution maps of phases, strain/stress and/or plastic deformation inside the sample.

  15. Optoelectronic Picosecond Detection of Synchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Durbin, Stephen M. [Purdue Univ., West Lafayette, IN (United States)

    2017-08-04

    The goal of this research program was to develop a detector that would measure x-ray time profiles with picosecond resolution. This was specifically aimed for use at x-ray synchrotrons, where x-ray pulse profiles have Gaussian time spreads of 50-100 ps (FWHM), so the successful development of such a detector with picosecond resolution would permit x-ray synchrotron studies to break through the pulse width barrier. That is, synchrotron time-resolved studies are currently limited to pump-probe studies that cannot reveal dynamics faster than ~50 ps, whereas the proposed detector would push this into the physically important 1 ps domain. The results of this research effort, described in detail below, are twofold: 1) the original plan to rely on converting electronic signals from a semiconductor sensor into an optical signal proved to be insufficient for generating signals with the necessary time resolution and sensitivity to be widely applicable; and 2) an all-optical method was discovered whereby the x-rays are directly absorbed in an optoelectronic material, lithium tantalate, which can then be probed by laser pulses with the desired picosecond sensitivity for detection of synchrotron x-rays. This research program has also produced new fundamental understanding of the interaction of x-rays and optical lasers in materials that has now created a viable path for true picosecond detection of synchrotron x-rays.

  16. Finite Element Simulation and X-Ray Microdiffraction Study of Strain Partitioning in a Layered Nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Barabash, R. I. [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA; Agarwal, V. [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA; Koric, S. [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA; National Center for Supercomputing Applications, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA; Jasiuk, I. [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA; Tischler, J. Z. [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA

    2016-01-01

    The depth-dependent strain partitioning across the interfaces in the growth direction of the NiAl/Cr(Mo) nanocomposite between the Cr and NiAl lamellae was directly measured experimentally and simulated using a finite element method (FEM). Depth-resolved X-ray microdiffraction demonstrated that in the as-grown state both Cr and NiAl lamellae grow along the' open='<' separators='|'>111direction with the formation of as-grown distinct residual ~0.16% compressive strains for Cr lamellae and ~0.05% tensile strains for NiAl lamellae. Three-dimensional simulations were carried out using an implicit FEM. First simulation was designed to study residual strains in the composite due to cooling resulting in formation of crystals. Strains in the growth direction were computed and compared to those obtained from the microdiffraction experiments. Second simulation was conducted to understand the combined strains resulting from cooling and mechanical indentation of the composite. Numerical results in the growth direction of crystal were compared to experimental results confirming the experimentally observed trends.

  17. Magnetic X-Ray Scattering with Synchrotron Radiation

    DEFF Research Database (Denmark)

    Moncton, D. E.; Gibbs, D.; Bohr, Jakob

    1986-01-01

    With the availability of high-brilliance synchrotron radiation from multiple wigglers, magnetic X-ray scattering has become a powerful new probe of magnetic structure and phase transitions. Similar to the well-established magnetic neutron scattering technique, magnetic X-ray scattering methods have...

  18. Study of UO2 mechanical behaviour implanted with helium ions using X-ray micro-diffraction and mechanical modeling

    International Nuclear Information System (INIS)

    Ibrahim, Marcelle

    2015-01-01

    In order to study the mechanical behavior of nuclear fuel during direct long term storage, UO 2 polycrystals were implanted with Helium ions at a thin surface layer (1 μm approximately), which leads to stress and strain fields in the layer. Strains were measured, at the grains scale, by X-ray micro-diffraction, using synchrotron radiation (ESRF). Image analysis methods were developed for an automatic analysis of the large number of diffraction patterns. Applying statistical tools to Laue patterns allows an automatic detection of low quality images, and enhances the measurement precision. At low layer thickness, the mechanical interaction between grains can be neglected. At higher thickness, experimental results showed a higher mechanical interaction near grain boundaries that can be modeled using finite elements method. Geostatistical tools were used to quantify these interactions. The swelling and the elastic constants in the implanted layer can be estimated through the measured strains on a large number of grains with different orientations. This work allows the determination of the swelling of nuclear fuel in irradiation conditions, as well as the modification of its elastic properties. (author) [fr

  19. Synchrotron X-Ray Radiation and Deformation Studies

    DEFF Research Database (Denmark)

    Fæster Nielsen, Søren

    In the present thesis two different synchrotron X-ray diffraction techniques capable of producing non-destructive information from the bulk of samples, have been investigated. Traditionally depth resolu-tion in diffraction experiments is obtained by inserting pinholes in both the incoming...... machining. The conical slit has six 25µm thick conically shaped openings matching six of the Debye-Scherrer cones from a fcc powder. By combining the conical slit with a micro-focused incoming beam of hard X-rays an embedded gauge volume is defined. Using a 2D detector, fast and complete information can...... boundary morphology. Another X-ray diffraction technique was applied on the three-dimensional X-ray diffraction (3DXRD) microscope at the ESRF synchrotron. The microscope uses a new technique based on ray tracing of diffracted high energy X-rays, providing a fast and non-destructive scheme for mapping...

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

    Energy Technology Data Exchange (ETDEWEB)

    Jones, Keith W.

    1999-09-01

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

  1. A synchrotron radiation facility for x-ray astronomy

    DEFF Research Database (Denmark)

    Hall, C.J.; Lewis, R.A.; Christensen, Finn Erland

    1997-01-01

    A proposal for an x-ray optics test facility based at a synchrotron radiation source is presented. The facility would incorporate a clean preparation area, and a large evacuable test area. The advantages of using a synchrotron as the source of the test radiation are discussed. These include the a...

  2. Synchrotron X-ray induced solution precipitation of nanoparticles

    CERN Document Server

    Lee, H J; Hwu, Y; Tsai, W L

    2003-01-01

    By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

  3. Micromirror-based manipulation of synchrotron x-ray beams

    Science.gov (United States)

    Walko, D. A.; Chen, Pice; Jung, I. W.; Lopez, D.; Schwartz, C. P.; Shenoy, G. K.; Wang, Jin

    2017-08-01

    Synchrotron beamlines typically use macroscopic, quasi-static optics to manipulate x-ray beams. We present the use of dynamic microelectromechanical systems-based optics (MEMS) to temporally modulate synchrotron x-ray beams. We demonstrate this concept using single-crystal torsional MEMS micromirrors oscillating at frequencies of 75 kHz. Such a MEMS micromirror, with lateral dimensions of a few hundred micrometers, can interact with x rays by operating in grazing-incidence reflection geometry; x rays are deflected only when an x-ray pulse is incident on the rotating micromirror under appropriate conditions, i.e., at an angle less than the critical angle for reflectivity. The time window for such deflections depends on the frequency and amplitude of the MEMS rotation. We demonstrate that reflection geometry can produce a time window of a few microseconds. We further demonstrate that MEMS optics can isolate x rays from a selected synchrotron bunch or group of bunches. With ray-trace simulations we explain the currently achievable time windows and suggest a path toward improvements.

  4. Light source for synchrotron radiation x-ray topography study at Beijing Synchrotron Radiation Laboratory (BSRL)

    International Nuclear Information System (INIS)

    Zhao Jiyong; Jiang Jianhua; Tian Yulian

    1992-01-01

    Characteristics of the synchrotron radiation source for X-ray topography study at Beijing Synchrotron Radiation Laboratory (BSRL) is described, local geometrical resolution of topographies is discussed, and the diffracting intensities of white beam topography is given

  5. [Clinical applications of synchrotron radiation X-ray].

    Science.gov (United States)

    Uyama, C

    1994-09-01

    Synchrotron Radiation X-ray (SR X-ray) is an extremely strong X-ray source with a photon number more than 10(4) compared with that of the current X-ray tube. X-rays obtained by monochromatizing SR X-ray have been applied to new techniques for medical diagnosis. Several studies are now being conducted at the beam site for medical use at the Accumulation Ring of the High Energy Physics Research Institute, Tsukuba. Applications being studied include (1) energy subtraction coronary angiography. (2) microdetection of metas in samples excised from subjects. (3) monochromatic X-ray computed tomography and so on. Energy subtraction coronary angiography might have a safety advantage over the current selective coronary angiography. Microdetection of mandatory metals and poisonous heavy metals in in vivo samples contributes to the development of pathologic knowledge and clinical treatment of cancer and heavy metal toxications. Monochromatic X-ray CT is expected to detect diseases in the early stage due to increased accuracy in CT values.

  6. High-intensity laser synchrotron x-ray source

    International Nuclear Information System (INIS)

    Pogorelsky, I.V.

    1995-10-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high-brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the Laser Synchrotron Light Source (LSLS) concept is still waiting for a convincing demonstration. Available at the BNL's Accelerator Test Facility (ATF), a high-brightness electron beam and the high-power C0 2 laser may be used as prototype LSLS brick stones. In a feasible demonstration experiment, 10-GW, 100-ps C0 2 laser beam will be brought to a head-on collision with a 10-ps, 0.5-nC, 70 MeV electron bunch. Flashes of well-collimated, up to 9.36-keV (∼ Angstrom) x-rays of 10-ps pulse duration, with a flux of ∼10 19 photons/sec will be produced via linear Compton backscattering. The x-ray spectrum is tunable proportionally to a variable e-beam energy. A natural short-term extension of the proposed experiment would be further enhancement of the x-ray flux to a 10 21 -10 22 photons/sec level, after the ongoing ATF CO 2 laser upgrade to 1 TW peak power and electron bunch shortening to 3 ps. The ATF LSLS x-ray beamline, exceeding by orders of magnitude the peak fluxes attained at the National Synchrotron Light Source (NSLS) x-ray storage ring, may become attractive for certain users, e.g., for biological x-ray microscopy. In addition, a terawatt CO 2 laser will enable harmonic multiplication of the x-ray spectrum via nonlinear Compton scattering

  7. Quantitative X-ray microtomography with synchrotron radiation

    International Nuclear Information System (INIS)

    Donath, T.

    2007-01-01

    Synchrotron-radiation-based computed microtomography (SR μ CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR μ CT measurements have been further improved by enhancements that were made to the SR μ CT apparatus and to the reconstruction chain. For high-resolution SR μ CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR μ CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

  8. X-ray diffraction microtomography using synchrotron radiation

    CERN Document Server

    Barroso, R C; Jesus, E F O; Oliveira, L F

    2001-01-01

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

  9. Hard X-ray Sources for the Mexican Synchrotron Project

    Science.gov (United States)

    Reyes-Herrera, Juan

    2016-10-01

    One of the principal tasks for the design of the Mexican synchrotron was to define the storage ring energy. The main criteria for choosing the energy come from studying the electromagnetic spectrum that can be obtained from the synchrotron, because the energy range of the spectrum that can be obtained will determine the applications available to the users of the future light source. Since there is a public demand of hard X-rays for the experiments in the synchrotron community users from Mexico, in this work we studied the emission spectra from some hard X-ray sources which could be the best options for the parameters of the present Mexican synchrotron design. The calculations of the flux and the brightness for one Bending Magnet and four Insertion Devices are presented; specifically, for a Superconducting Bending Magnet (SBM), a Superconducting Wiggler (SCW), an In Vacuum Short Period Undulator (IV-SPU), a Superconducting Undulator (SCU) and for a Cryogenic Permanent Magnet Undulator (CPMU). Two commonly available synchrotron radiation programs were used for the computation (XOP and SRW). From the results, it can be concluded that the particle beam energy from the current design is enough to have one or more sources of hard X-rays. Furthermore, a wide range of hard X-ray region can be covered by the analyzed sources, and the choice of each type should be based on the specific characteristics of the X-ray beam to perform the experiments at the involved beamline. This work was done within the project Fomix Conacyt-Morelos ”Plan Estrategico para la construccion y operación de un Sincrotron en Morelos” (224392).

  10. An X-ray microprobe facility using synchrotron radiation

    International Nuclear Information System (INIS)

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

    1990-01-01

    An X-ray microprobe for trace elemental analysis at micrometer spatial resolutions, using synchrotron radiation (SR), is under development. The facility consists of two beamlines, one including a 1:1 focusing mirror and the other an 8:1 ellipsoidal mirror. At present, open-quotes white lightclose quotes is used for excitation of the characteristic X-ray fluorescence lines. Sensitivities in thin biological samples are in the range of 2-20 fg in 100 μm 2 areas in 5 min irradiation times. Scanning techniques, as well as microtomography and chemical speciation, are discussed. Application to a specific biomedical study is included

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-21

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

  12. Diamond detectors for synchrotron radiation X-ray applications

    International Nuclear Information System (INIS)

    De Sio, A.; Pace, E.; Cinque, G.; Marcelli, A.; Achard, J.; Tallaire, A.

    2007-01-01

    Due to its unique physical properties, diamond is a very appealing material for the development of electronic devices and sensors. Its wide band gap (5.5 eV) endows diamond based devices with low thermal noise, low dark current levels and, in the case of radiation detectors, high visible-to-X-ray signal discrimination (visible blindness) as well as high sensitivity to energies greater than the band gap. Furthermore, due to its radiation hardness diamond is very interesting for applications in extreme environments, or as monitor of high fluency radiation beams. In this work the use of diamond based detectors for X-ray sensing is discussed. On purpose, some photo-conductors based on different diamond types have been tested at the DAFNE-L synchrotron radiation laboratory at Frascati. X-ray sensitivity spectra, linearity and stability of the response of these diamond devices have been measured in order to evidence the promising performance of such devices

  13. Soft X-ray microscopy and lithography with synchrotron radiation

    International Nuclear Information System (INIS)

    Gudat, W.

    1977-12-01

    Considerable progress in the technique microscopy with soft X-ray radiation has been achieved in particular through the application of synchrotron radiation. Various methods which are currently being studied theoretically or already being used practically will be described briefly. Attention is focussed on the method of contact microscopy. Various biological specimens have been investigated by this method with a resolution as good as 100 A. X-ray lithography which in the technical procedure is very similar to contact microscopy gives promise for the fabrication of high quality submicron structures in electronic device production. Important factors limiting the resolution and determining the performance of contact microscopy and X-ray lithography will be discussed. (orig.) [de

  14. Quantitative X-ray microtomography with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Donath, T. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Materialforschung

    2007-07-01

    Synchrotron-radiation-based computed microtomography (SR{sub {mu}}CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR{sub {mu}}CT measurements have been further improved by enhancements that were made to the SR{sub {mu}}CT apparatus and to the reconstruction chain. For high-resolution SR{sub {mu}}CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR{sub {mu}}CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

  15. Applications of synchrotron X-rays in microelectronics industry research

    International Nuclear Information System (INIS)

    Jordan-Sweet, Jean L.; Detavernier, Christophe; Lavoie, Christian; Mooney, Patricia M.; Toney, Michael F.

    2005-01-01

    The high flux and density of X-rays produced at synchrotrons provide the microelectronics industry with a powerful probe of the structure and behavior of a wide array of solid materials that are being developed for use in devices of the future. They also are of great use in determining why currently-used materials and processes sometimes fail. This paper describes the X20 X-ray beamline facility operated by IBM at the National Synchrotron Light Source, and presents a series of three industry challenges and results that illustrate the variety of techniques used and problems addressed. The value of this research ranges from solving short-term, technically specific problems to increasing our academic understanding of materials in general. Techniques discussed include high-resolution diffraction, time-resolved diffraction, texture measurements, and grazing-incidence diffraction

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

    Energy Technology Data Exchange (ETDEWEB)

    Gasperini, F. M. [Medical Science Program, Fluminense Federal Univ., Niteroi (Brazil); Pereira, G. R. [Dept. of Metallurgical and Materials Engineering, Federal Univ. of Rio de Janeiro (Brazil); Granjeiro, J. M. [Molecular and Cell Biology Dept., Fluminense Federal Univ., Niteroi, Rio de Janeiro (Brazil); Calasans-Maia, M. D. [Oral Surgery Dept., Fluminense Federal Univ., Niteroi, Rio de Janeiro (Brazil); Rossi, A. M. [Biomaterials Laboratory, Brazilian Center of Physics Research, Rio de Janeiro (Brazil); Perez, C. A. [Brazilian Synchrotron Laboratory, Campinas, Sao Paulo (Brazil); Lopes, R. T.; Lima, I. [Nuclear Engineering Laboratory, Federal Univ. of Rio de Janeiro (Brazil)

    2011-07-01

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

  17. Chemical crystallography with pulsed neutrons and synchrotron x-rays

    International Nuclear Information System (INIS)

    Carrondo, M.A.; Jeffrey, G.A.

    1988-01-01

    Solid-state chemists and physicists, crystallographers and molecular biologists who are using or who plan to use the special properties of pulsed neutron spallation and synchrotron X-ray sources will find this book invaluable. Those scientists who have not yet gained experience in working with such sources will find the basic physics of the radiations, their production and their scattering properties explained, together with descriptions of the different types of diffraction experiments which use them

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

    International Nuclear Information System (INIS)

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

    1990-10-01

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

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

    CERN Document Server

    Giacomini, J C

    1996-01-01

    The purpose of this project was to utilize dual energy, monochromatic X-rays produced from synchrotrons radiation in order to obtain noninvasive medical imaging. The application of synchrotrons radiation to medical imaging is based on the principle of iodine dichromography, first described by Bertil Jacobson of the Karolinska Institute in 1953. Medical imaging using synchrotrons radiation and K-edge dichromography was pioneered at Stanford University under the leadership of Dr. Ed Rubenstein, and the late Nobel Laureate in Physics, Dr. Robert Hofstadter. With progressive refinements in hardware, clinical-quality images were obtained of human coronary arteries utilizing peripheral injections of iodinated contrast agent. These images even now are far superior to those being presented by investigators using MRI as an imaging tool for coronary arteries. However, new supplies and instruments in the cardiac catheterization laboratory have served to transform coronary angiography into an outpatient procedure, with r...

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

    International Nuclear Information System (INIS)

    Suzuki, Masayo; Yamamoto, Masaki; Kumasaka, Takashi; Sato, Kazumichi; Toyokawa, Hidenori; Aries, Ian F.; Jerram, Paul A.; Ueki, Tatzuo

    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

  1. 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.

  2. Study of moire fringes using synchrotron X-rays

    International Nuclear Information System (INIS)

    Yoshimura, Jun-ichi

    1992-01-01

    It has recently been shown that X-ray moire fringes are not exactly the projection of the intensity distribution of the wave field on the exit surface of the crystal, but do oscillate along the beam path behind the crystal. Such nonprojectiveness of moire fringes is inexplicable by the conventional understanding of moire fringes, and therefore is of interest from a fundamental viewpoint as well as practical one. In this paper the phenomena of the nonprojectiveness are described on the basis of the latest experimental data obtained by synchrotron radiation. (author)

  3. Oxides neutron and synchrotron X-ray diffraction studies

    CERN Document Server

    Sosnowska, I M

    1999-01-01

    We review some results from several areas of oxide science in which neutron scattering and X-ray synchrotron scattering exercise a complementary role to high-resolution transmission electron microscopy. The very high-resolution time-of-flight neutron diffraction technique and its role in studies of the magnetic structure of oxides is especially reviewed. The selected topics of structural studies for the chosen oxides are: crystal and magnetic structure of the so-called cellular random systems, magnetic structure and phase transitions in ferrites and the behaviour of water in non-stoichiometric protonic conductors and in the opal silica-water system. (40 refs).

  4. Synchrotron X-ray diffraction using triple-axis spectrometry

    International Nuclear Information System (INIS)

    Als-Nielsen, J.

    1980-12-01

    High resolution X-ray diffraction studies of (i) monolayers of the noble gases Kr and Ar physiosorbed on graphite (ii) smectic A fluctuations in the nematic and the smectic A phases of liquid crystals are described. The apparatus used is a triple axis spectrometer situated at the storage ring DORIS at Hasylab, DESY, Hamburg. A monochromatic, well collimated beam is extracted from the synchrotron radiation spectrum by Bragg reflection from perfect Si or Ge crystals. The direction of the beam scattered from the sample is determined by Bragg reflection from a perfect Si or Ge crystal. High intensities even with resolution extending beyond the wavelength of visible light can be obtained. (Auth.)

  5. Precise stress measurements with white synchrotron x rays

    International Nuclear Information System (INIS)

    Weidner, Donald J.; Vaughan, Michael T.; Wang Liping; Long, Hongbo; Li Li; Dixon, Nathaniel A.; Durham, William B.

    2010-01-01

    In situ measurement of stress in polycrystalline samples forms the basis for studies of the mechanical properties of materials with very broad earth science and materials science applications. Synchrotron x rays have been used to define the local elastic strain in these samples, which in turn define stress. Experimental work to date has been carried out on a prototype detection system that provided a strain measurement precision >10 -4 , which corresponds to a stress resolution >50 MPa for silicate minerals. Here we report operation of a new, permanent, energy dispersive detection system for white radiation, which has been developed at the National Synchrotron Light Source. The new system provides differential strain measurements with a precision of 3x10 -5 for volumes that are 50x50x500 μm 3 . This gives a stress precision of about 10 MPa for silicate minerals.

  6. Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science

    Czech Academy of Sciences Publication Activity Database

    Švarcová, Silvie; Kočí, Eva; Bezdička, Petr; Hradil, David; Hradilová, J.

    2010-01-01

    Roč. 398, č. 2 (2010), s. 1061-1076 ISSN 1618-2642 R&D Projects: GA AV ČR KJB200320901 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray micro-diffraction * quantitative phase analysis * forensic Subject RIV: CA - Inorganic Chemistry Impact factor: 3.841, year: 2010

  7. Domain Size of Phase-Separated NaxCoO2 as Investigated by X-Ray Microdiffraction

    Directory of Open Access Journals (Sweden)

    Hideharu Niwa

    2017-03-01

    Full Text Available O3-NaCoO 2 is a promising cathode material for sodium ion secondary batteries (SIBs. Na x CoO 2 shows phase separation (PS into the O3 and O ′ 3 phases in the Na concentration range of 0.89 ⩽ x ⩽ 0.99. In order to estimate the domain size (r in the two-phase region, we performed X-ray microdiffraction (XRMD of thin films of Na x CoO 2 at x = 0.97 and ∼1. We found that r (≈400 nm of the O ′ 3 domain is comparable to the particle size d (=331 ± 87 nm in the as-grown O3-NaCoO 2 film. This observation suggests that individual particles of Na x CoO 2 are single phase to minimize the strain at the O3–O ′ 3 phase boundary.

  8. X-ray micro-diffraction analysis of reconstructed bone at Zr prosthetic surface with sub-micrometre spatial resolution

    International Nuclear Information System (INIS)

    Cedola, A; Stanic, V; Burghammer, M; Lagomarsino, S; Rustichelli, F; Giardino, R; Aldini, N Nicoli; Fini, M; Komlev, V; Fonzo, S Di

    2003-01-01

    The purpose of the present investigation is to demonstrate the power of the x-ray micro-diffraction technique in biological studies. In particular the reported experiment concerns the study of the interface between a Zr prosthetic device implanted in a rat femur and the newly-formed bone, with a spatial resolution of 0.5 μm. The obtained results give interesting information on the Zr deformation and on the crystallographic phase, the grain size and the orientation of the new bone. Moreover the study reveals a marked difference in the structure of the reconstructed bone with respect to the native bone, which cannot be appreciated with other techniques. (note)

  9. 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

  10. Engineered bone from bone marrow stromal cells: a structural study by an advanced x-ray microdiffraction technique

    International Nuclear Information System (INIS)

    Cedola, A; Mastrogiacomo, M; Burghammer, M; Komlev, V; Giannoni, P; Favia, A; Cancedda, R; Rustichelli, F; Lagomarsino, S

    2006-01-01

    The mechanism of mineralized matrix deposition was studied in a tissue engineering approach in which bone tissue is formed when porous ceramic constructs are loaded with bone marrow stromal cells and implanted in vivo. We investigated the local interaction between the mineral crystals of the engineered bone and the biomaterial by means of microdiffraction, using a set-up based on an x-ray waveguide. We demonstrated that the newly formed bone is well organized inside the scaffold pore, following the growth model of natural bone. Combining wide angle (WAXS) and small angle (SAXS) x-ray scattering with high spatial resolution, we were able to determine the orientation of the crystallographic c-axis inside the bone crystals, and the orientation of the mineral crystals and collagen micro-fibrils with respect to the scaffold. In this work we analysed six samples and for each of them two pores were studied in detail. Similar results were obtained in all cases but we report here only the most significant sample. (note)

  11. A dedicated superbend x-ray microdiffraction beamline for materials, geo-, and environmental sciences at the advanced light source

    Energy Technology Data Exchange (ETDEWEB)

    Advanced Light Source; Kunz, Martin; Tamura, Nobumichi; Chen, Kai; MacDowell, Alastair A.; Celestre, Richard S.; Church, Matthew M.; Fakra, Sirine; Domning, Edward E.; Glossinger, James M.; Kirschman, Jonathan L.; Morrison, Gregory Y.; Plate, Dave W.; Smith, Brian V.; Warwick, Tony; Padmore, Howard A.; Ustundag, Ersan; Yashchuk, Valeriy V.

    2009-03-24

    A new facility for microdiffraction strain measurements and microfluorescence mapping has been built on beamline 12.3.2 at the advanced light source of the Lawrence Berkeley National Laboratory. This beamline benefits from the hard x-radiation generated by a 6 T superconducting bending magnet (superbend) This provides a hard x-ray spectrum from 5 to 22 keV and a flux within a 1 mu m spot of ~;;5x109 photons/ s (0.1percent bandwidth at 8 keV). The radiation is relayed from the superbend source to a focus in the experimental hutch by a toroidal mirror. The focus spot is tailored bytwo pairs of adjustable slits, which serve as secondary source point. Inside the lead hutch, a pair of Kirkpatrick-Baez (KB) mirrors placed in a vacuum tank refocuses the secondary slit source onto the sample position. A new KB-bending mechanism with active temperature stabilization allows for more reproducible and stable mirror bending and thus mirror focusing. Focus spots around 1 um are routinely achieved and allow a variety of experiments, which have in common the need of spatial resolution. The effective spatial resolution (~;;0.2 mu m) is limited by a convolution of beam size, scan-stage resolution, and stage stability. A four-bounce monochromator consisting of two channel-cut Si(111) crystals placed between the secondary source and KB-mirrors allows for easy changes between white-beam and monochromatic experiments while maintaining a fixed beam position. High resolution stage scans are performed while recording a fluorescence emission signal or an x-ray diffraction signal coming from either a monochromatic or a white focused beam. The former allows for elemental mapping, whereas the latter is used to produce two-dimensional maps of crystal-phases, -orientation, -texture, and -strain/stress. Typically achieved strain resolution is in the order of 5x10-5 strain units. Accurate sample positioning in the x-ray focus spot is achieved with a commercial laser-triangulation unit. A Si

  12. Synchrotron X-ray tomographic microscopy of fossil embryos.

    Science.gov (United States)

    Donoghue, Philip C J; Bengtson, Stefan; Dong, Xi-ping; Gostling, Neil J; Huldtgren, Therese; Cunningham, John A; Yin, Chongyu; Yue, Zhao; Peng, Fan; Stampanoni, Marco

    2006-08-10

    Fossilized embryos from the late Neoproterozoic and earliest Phanerozoic have caused much excitement because they preserve the earliest stages of embryology of animals that represent the initial diversification of metazoans. However, the potential of this material has not been fully realized because of reliance on traditional, non-destructive methods that allow analysis of exposed surfaces only, and destructive methods that preserve only a single two-dimensional view of the interior of the specimen. Here, we have applied synchrotron-radiation X-ray tomographic microscopy (SRXTM), obtaining complete three-dimensional recordings at submicrometre resolution. The embryos are preserved by early diagenetic impregnation and encrustation with calcium phosphate, and differences in X-ray attenuation provide information about the distribution of these two diagenetic phases. Three-dimensional visualization of blastomere arrangement and diagenetic cement in cleavage embryos resolves outstanding questions about their nature, including the identity of the columnar blastomeres. The anterior and posterior anatomy of embryos of the bilaterian worm-like Markuelia confirms its position as a scalidophoran, providing new insights into body-plan assembly among constituent phyla. The structure of the developing germ band in another bilaterian, Pseudooides, indicates a unique mode of germ-band development. SRXTM provides a method of non-invasive analysis that rivals the resolution achieved even by destructive methods, probing the very limits of fossilization and providing insight into embryology during the emergence of metazoan phyla.

  13. Microfocussing of synchrotron X-rays using X-ray refractive lens ...

    Indian Academy of Sciences (India)

    2014-07-02

    Jul 2, 2014 ... ring (black) is fixed from polyimide side and (g) finally the metal substrate is etched to prepare the X-ray mask. standardized for the present X-ray lithography beamline. X-ray exposures are carried out in 3–10 keV region selected using two X-ray mirrors kept at grazing incidence angles. The total power ...

  14. Experimental capabilities at beamline 12.3.2, X-ray Microdiffraction, of the Advanced Light Source

    Science.gov (United States)

    Tamura, N.; Stan, C. V.; Kunz, M.

    2016-12-01

    Analytical techniques implemented at the microdiffraction beamline 12.3.2 of the Advanced Light Source (ALS) may be of interest to the geoscience community. We have developed angular (ADXRD) and energy (Laue) dispersive diffraction techniques coupled with elemental identification using x-ray fluorescence (XRF) and a 1-2 μm x-ray beam spot diameter. This instrumental setup enables the collection of a wide variety of data, including qualitative compositional mapping and single crystal and polycrystalline diffraction, under a wide variety of pressure or temperature conditions, and with micron-scale resolution. Additionally, the tunable wavelength allows for collection of high-quality single crystal data without the need for sample rotation. We can generate 2D phase maps with 1 μm resolution, and map out strain conditions in situ. These types of measurements allow us to reconstruct rock deformation history and constrain the mechanical properties of rocks, as well as identify accessory mineral phases that may be hard to find with standard laboratory techniques. Here we present various experimental setups that may be of interest to the mineralogy/petrology community. In particular, we highlight: 2D Laue/XRF/ADXRD scans, monochromatic scanning for single crystal structure solution, heating/cooling stage with temperature ranges between -200 C - 900 C, strain gauge with differential heating/cooling, and the diamond anvil cell coupled with Laue or monochromatic x-ray diffraction. Many of these techniques are unavailable at other facilities, and may greatly extend the range of experimental capabilities within the community.

  15. 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 ...

  16. Microfocussing of synchrotron X-rays using X-ray refractive lens ...

    Indian Academy of Sciences (India)

    2014-07-02

    Jul 2, 2014 ... Abstract. 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 Dia- mond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at ...

  17. 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 ...

  18. Microdiffraction: X-rays as a probe to reveal flux divergences ininterconnects

    Energy Technology Data Exchange (ETDEWEB)

    Spolenak, R.; Tamura, N.; Patel, J.R.

    2006-01-01

    Most reliability issues in interconnect systems occur at a local scale and many of them include the local build-up of stresses. Typical failure mechanisms are electromigration and stress voiding in interconnect lines and fatigue in surface acoustic wave devices. Thus a local probe is required for the investigation of these phenomena. In this paper the application of the Laue microdiffraction technique to investigate flux divergences in interconnect systems will be described. The deviatoric strain tensor of single grains can be correlated with the local microstructure, orientation and defect density. Especially the latter led to recent results about the correlation of stress build-up and orientation in Cu lines and electromigration-induced grain rotation in Cu and Al lines.

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

    Energy Technology Data Exchange (ETDEWEB)

    Schulze, D. (Purdue Univ., Lafayette, IN (USA)); Anderson, S. (Michigan State Univ., East Lansing, MI (USA)); Mattigod, S. (Pacific Northwest Lab., Richland, WA (USA))

    1990-07-01

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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-15

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

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

    International Nuclear Information System (INIS)

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

    1990-07-01

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

  4. White Beam, X-Ray, Energy-Dispersive Diffractometry using Synchrotron Radiation

    DEFF Research Database (Denmark)

    Gerward, Leif; Buras, B.; Olsen, J. Staun

    1978-01-01

    The special features of left double quote white right double quote beam X-ray energy-dispersive diffractometry using synchrotron radiation are discussed on the basis of experiments performed at the Deutsches Electronen-Synchrotron, DESY.......The special features of left double quote white right double quote beam X-ray energy-dispersive diffractometry using synchrotron radiation are discussed on the basis of experiments performed at the Deutsches Electronen-Synchrotron, DESY....

  5. In-situ study of electromigration-induced grain rotation in Pb-free solder joint by synchrotron microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-10-31

    The rotation of Sn grains in Pb-free flip chip solder joints hasn't been reported in literature so far although it has been observed in Sn strips. In this letter, we report the detailed study of the grain orientation evolution induced by electromigration by synchrotron based white beam X-ray microdiffraction. It is found that the grains in solder joint rotate more slowly than in Sn strip even under higher current density. On the other hand, based on our estimation, the reorientation of the grains in solder joints also results in the reduction of electric resistivity, similar to the case of Sn strip. We will also discuss the reason why the electric resistance decreases much more in strips than in the Sn-based solders, and the different driving force for the grain growth in solder joint and in thin film interconnect lines.

  6. Utilization of synchrotron radiation in analytical chemistry. Soft X-ray emission and absorption spectroscopy

    International Nuclear Information System (INIS)

    Muramatsu, Yasuji

    2015-01-01

    Synchrotron soft X-ray spectroscopy includes three major types of spectroscopy such as X-ray absorption spectroscopy (XAS), X-ray emission spectroscopy (XES), and X-ray photoelectron spectroscopy (XPS). This paper takes up XAS and XES of soft X-rays, and briefly describes the principle. XAS is roughly classified into XANES (X-ray absorption near-edge structure) and EXAFS (extended X-ray absorption fine structure), and XANES is mainly used in the analysis based on XAS of soft X-rays. As the examples of the latest soft X-ray analyses, the following are introduced: (1) bandgap of boron implantation diamond and the local structure of boron, (2) catalytic sites in solid fuel cell carbon electrode, and (3) soft X-ray analysis under atmospheric pressure. (A.O.)

  7. Actinide science with soft x-ray synchrotron radiation

    International Nuclear Information System (INIS)

    Shuh, D.

    2002-01-01

    Several workshops, some dating back more than fifteen years, recognised both the potential scientific impact and opportunities that would be made available by the capability to investigate actinide materials in the vacuum ultraviolet (VUV)/soft X-ray region of the synchrotron radiation (SR) spectrum. This spectral region revolutionized the approach to surface materials chemistry and physics nearly two decades ego. The actinide science community was unable to capitalize on these SR methodologies for the study of actinide materials until recently because of radiological safety concerns. ,The Advanced Light Source (ALS) at LBNL is a third-generation light source providing state-of-the-art performance in the VUV/soft X-ray region. Along with corresponding improvements in detector and vacuum technology, the ALS has rendered experiments with small amounts of actinide materials possible. In particular, it has been the emergence and development of micro-spectroscopic techniques that have enabled investigations of actinide materials at the ALS. The primary methods for the experimental investigation of actinide materials in the VUV/soft X-ray region are the complementary photoelectron spectroscopies, near-edge X-ray absorption fine structure (NEXAFS) and X-ray emission spectroscopy (XES) techniques. Resonant photo-emission is capable of resolving the 5f electron contributions to actinide bonding and can be used to characterise the electronic structure of actinide materials. This technique is clearly a most important methodology afforded by the tunable SR source. Core level and valence band photoelectron spectroscopies are valuable for the characterisation of the electronic properties of actinide materials, as well as for general analytical purposes. High-resolution core-level photo-emission and resonant photo-emission measurements from the a (monoclinic) and δ (FCC) allotropic phases of plutonium metal have been collected on beam line 7.0 at the ALS and the spectra show

  8. Application of synchrotron through-the-substrate microdiffraction to crystals in polished thin sections

    Directory of Open Access Journals (Sweden)

    Jordi Rius

    2015-07-01

    Full Text Available The synchrotron through-the-substrate X-ray microdiffraction technique (tts-μXRD is extended to the structural study of microvolumes of crystals embedded in polished thin sections of compact materials [Rius, Labrador, Crespi, Frontera, Vallcorba & Melgarejo (2011. J.Synchrotron Rad. 18, 891–898]. The resulting tts-μXRD procedure includes some basic steps: (i collection of a limited number of consecutive two-dimensional patterns (frames for each randomly oriented crystal microvolume; (ii refinement of the metric from the one-dimensional diffraction pattern which results from circularly averaging the sum of collected frames; (iii determination of the reciprocal lattice orientation of each randomly oriented crystal microvolume which allows assigning the hkl indices to the spots and, consequently, merging the intensities of the different frames into a single-crystal data set (frame merging; and (iv merging of the individual crystal data sets (multicrystal merging to produce an extended data set suitable for structure refinement/solution. Its viability for crystal structure solution by Patterson function direct methods (δ recycling and for accurate single-crystal least-squares refinements is demonstrated with some representative examples from petrology in which different glass substrate thicknesses have been employed. The section of the crystal microvolume must be at least of the same order of magnitude as the focus of the beam (15 × 15 µm in the provided examples. Thanks to its versatility and experimental simplicity, this methodology should be useful for disciplines as disparate as petrology, materials science and cultural heritage.

  9. Trace element characterization using a synchrotron radiation X-ray microprobe

    OpenAIRE

    早川, 慎二郎

    1996-01-01

    A scanning X-ray microprobe using synchrotron radiation was developed employing an X-ray focusing system with total reflection mirrors. Utilizing a Wolter mirror system, a hard X-ray microbeam was first realized. With an energy tunable X-ray microprobe, sensitivity in X-ray fluorescence (XRF) analysis can be optimized for the element of interest at less than 1 ppm in relative concentration. Moreover, small area X-ray absorption fine structure (XAFS) measurements with XRF detection can provide...

  10. Geoscience Applications of Synchrotron X-ray Computed Microtomography

    Science.gov (United States)

    Rivers, M. L.

    2009-05-01

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

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

    International Nuclear Information System (INIS)

    Giacomini, John C.

    1996-01-01

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

  12. Soft X-ray diffractometer for synchrotron radiation

    CERN Document Server

    Gau, T S; Liu, K Y; Chung, C H; Chen, C K; Lai, S C; Shu, C H; Huang, Y S; Chao, C H; Lee, Y R; Chen, C T; Chang, S L

    2001-01-01

    An ultra-high vacuum soft X-ray diffractometer has been constructed and commissioned at the Synchrotron Radiation Research Center (SRRC) to investigate materials structures in mesoscale. The diffractometer, housed in a UHV tank, consists of a 6-circle goniometer, together with the systems for beam-collimation, signal detection, vacuum, and control panels. The kappa-phi (cursive,open) Greek-psi goniostat is adopted for the sample orientation. Crystal samples can be rotated along a given reciprocal lattice vector by using psi scan. Two orthogonal axes, gamma (or 2 theta) and delta, are used to move the detector. The detector is a semiconductor pin diode, which can be used in UHV ambient. This 6-circle goniometer allows for sample scanning of a wide range in the momentum space. The motors used for goniometer rotation and slit selection are UHV compatible. The UHV tank is placed on an XYZ table capable of positioning the center of the goniometer onto the incident beam. Test experiments have been carried on the 1-...

  13. Local structure of metallic chips examined by X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Saksl, K., E-mail: ksaksl@imr.saske.sk [Institut of Materials Research, Slovak Academy of Sciences, Watsonova 47, 040 01 Košice (Slovakia); Rokicki, P. [The Faculty of Mechanical Engineering and Aeronautics, Rzeszow University of Technology, Al. Powstancow Warszawy 12, 35-959 Rzeszow (Poland); Siemers, C. [Institut fuer Werkstoffe, Technische Universitaet Braunschweig, Langer Kamp 8, 38106 Braunschweig (Germany); Ostroushko, D. [Faculty of Metallurgy and Materials Engineering, VŠB – Technical University of Ostrava, 17.listopadu 15, 708 33 Ostrava (Czech Republic); Bednarčík, J.; Rütt, U. [HASYLAB at DESY, Notkestr. 85, D-22607 Hamburg (Germany)

    2013-12-25

    Highlights: •We present a detailed microstructure and phase analysis of chips produced by cutting. •3D analysis proved mixed nature of shear bands propagation to the material. •We examine phase composition of the chips by focused X-ray beam. •Crystallites in segment and shear band change their orientation up to 10°. -- Abstract: Nickel-base alloys are used in high-temperature applications whenever steels or titanium alloys cannot be applied anymore. This class of alloys is furthermore used in low-temperature applications in the oil or gas industry in case the corrosion resistance of stainless steels in related liquid media is not sufficient and titanium alloys would be too expensive. Nickel-base alloys, however, due to their high strength and toughness can be machined only at low cutting speeds as otherwise poor surface quality and enhanced tool wear is observed. From all aspects influencing the machinability, the chip formation mechanism is the key factor and only a thorough understanding of this mechanism can lead to an optimisation of the cutting process. In the current study, a detailed microstructure and phase analysis of Alloy 625 chips produced in an orthogonal cutting process at conventional cutting speeds is presented. Utilising hard monochromatic X-rays focused down to micrometre size, microstructural differences between distinct structural units of the chips, namely, the segments and shear bands, are investigated. Scanning cross sections of the chips with this small beam allowed us to determine misorientation between the segments and shear bands crystal lattices which as we found are not changing abruptly but continuously, with an absolute difference up to 10°.

  14. Synchrotron radiation X-ray powder diffraction techniques applied in hydrogen storage materials - A review

    OpenAIRE

    Honghui Cheng; Chen Lu; Jingjing Liu; Yongke Yan; Xingbo Han; Huiming Jin; Yu Wang; Yi Liu; Changle Wu

    2017-01-01

    Synchrotron radiation is an advanced collimated light source with high intensity. It has particular advantages in structural characterization of materials on the atomic or molecular scale. Synchrotron radiation X-ray powder diffraction (SR-XRPD) has been successfully exploited to various areas of hydrogen storage materials. In the paper, we will give a brief introduction on hydrogen storage materials, X-ray powder diffraction (XRPD), and synchrotron radiation light source. The applications of...

  15. Mesoscale structural characterization within bulk materials by high-energy X-ray microdiffraction

    DEFF Research Database (Denmark)

    Lienert, U.; Poulsen, H.F.; Kvick, Å.

    2001-01-01

    that provide the required intensity and spatial resolution perpendicular to the incident beam. A focus size of 1.2 mum was achieved. Modified crossed-beam techniques are being developed that define the longitudinal resolution, i.e., the component of the gauge volume parallel to the incident beam. We present......A novel diffraction technique for the local three-dimensional characterization within polycrystalline bulk materials is presented. The technique uses high-energy synchrotron radiation (40 keV .... Four examples of applications are presented....

  16. Microbial biofilm study by synchrotron X-ray microscopy

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

  18. Scanning soft x-ray microscopy with a fresnel zoneplate at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Kenney, J.M.; Kirz, J.; Rarback, H.; Feder, R.; Sayre, D.; Howells, M.

    1983-01-01

    We have built a scanning transmission soft x-ray microscope located at the National Synchrotron Light Source (NSLS). Images of biological specimens have been formed with submicron resolution. A Fresnel zoneplate serves as the focusing element

  19. Recent trends of X-ray detectors in synchrotron radiation science

    CERN Document Server

    Suzuki, M

    2003-01-01

    This article attempts to describe the recent trends of X-ray detectors in synchrotron radiation science in the light of not only the advance but also the stagnation of which are seriously dependent upon the current semiconductor technology. (author)

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

    International Nuclear Information System (INIS)

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

    1995-06-01

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

  1. Report of the workshop on transferring X-ray Lithography Synchrotron (XLS) technology to industry

    Energy Technology Data Exchange (ETDEWEB)

    Marcuse, W.

    1987-01-01

    This paper reports on plans to develop an x-ray synchrotron for use in lithography. The primary concern of the present paper is technology transfer from national laboratories to private industry. (JDH)

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

    NARCIS (Netherlands)

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

    2016-01-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge

  3. Antiferroelectric surface layers in a liquid crystal as observed by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Gramsbergen, E. F.; de Jeu, W. H.; Als-Nielsen, Jens Aage

    1986-01-01

    The X-ray reflectivity form the surface of a liquid crystal with terminally polar (cyano substituted) molecules has been studied using a high-resolution triple-axis X-ray spectrometer in combination with a synchrotron source. It is demonstrated that at the surface of the smectic Al phase a few...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-12-15

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

  5. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

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

    1983-01-01

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

  6. Synchrotron radiation sources: their properties and applications for VUV and X-ray spectroscopy

    International Nuclear Information System (INIS)

    Koch, E.E.

    1976-09-01

    Synchrotron radiation from accelerators and storage rings offers far reaching possibilities for many fields of basic and applied physics. The properties of synchrotron radiation, existing and planned synchrotron radiation facilities, as well as instrumental aspects are discussed. In order to illustrate the usefulness of the synchrotron radiation sources a few highlights from atomic, molelucar, and solid state spectroscopy are presented and examples from x-ray experiments and from the field of applied physics are given. (orig.) [de

  7. Data and videos for ultrafast synchrotron X-ray imaging studies of metal solidification under ultrasound

    Directory of Open Access Journals (Sweden)

    Bing Wang

    2018-04-01

    Full Text Available The data presented in this article are related to the paper entitled ‘Ultrafast synchrotron X-ray imaging studies of microstructure fragmentation in solidification under ultrasound’ [Wang et al., Acta Mater. 144 (2018 505-515]. This data article provides further supporting information and analytical methods, including the data from both experimental and numerical simulation, as well as the Matlab code for processing the X-ray images. Six videos constructed from the processed synchrotron X-ray images are also provided.

  8. Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes

    International Nuclear Information System (INIS)

    Streli, C.; Wobrauschek, P.; Bauer, V.; Kregsamer, P.; Goergl, R.; Pianetta, P.; Ryon, R.; Pahlke, S.; Fabry, L.

    1997-01-01

    Total reflection X-ray fluorescence analysis (TXRF) of light elements, such as C, O and Al (atomic numbers 5-13) generally has poor sensitivity and detection limits due to poor excitation and low fluorescent yields. Special excitation sources are necessary to compensate for these physical limitations. Synchrotron radiation is the ideal source for TXRF due to its high intensity and wide spectral range extending into the low energy region required for light elements. For more routine use, special X-ray tubes can be constructed. Experiments have been performed at the Standford Synchrotron Radiation Laboratory (SSRL) using beamline III-4, which is specially designed for the sue of low energy photons. Light elements on Si wafers have been analyzed, leading to detection limits below 100 fg for Na, Mg and Al, which corresponds to about 10 9 atoms. A new vacuum chamber is introduced meeting the requirements of wafer handling without the risk of contamination and offering the possibility of scanning a certain area of the wafer. Boron was detected on a wafer with 10 14 atoms cm -2 implanted in the surface layer. A special windowless X-ray tube with Mo, Al and Si as anode materials was also tested. With the optimization of anode geometry, beam path and excitation conditions, a detection limit of 5 pg (corresponds to 10 11 atoms) for Al was achieved. (Author)

  9. Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes

    Energy Technology Data Exchange (ETDEWEB)

    Streli, C.; Wobrauschek, P.; Bauer, V.; Kregsamer, P.; Goergl, R. [Atominstitut der Oesterreichischen Universitaeten, Wien (Austria); Pianetta, P. [Stanford Synchrotron Radiation Lab. (Canada); Ryon, R. [Lawrence Livermore National Lab. CA (United States); Pahlke, S.; Fabry, L. [Wacker Siltronic AG, Burghausen (Germany)

    1997-06-20

    Total reflection X-ray fluorescence analysis (TXRF) of light elements, such as C, O and Al (atomic numbers 5-13) generally has poor sensitivity and detection limits due to poor excitation and low fluorescent yields. Special excitation sources are necessary to compensate for these physical limitations. Synchrotron radiation is the ideal source for TXRF due to its high intensity and wide spectral range extending into the low energy region required for light elements. For more routine use, special X-ray tubes can be constructed. Experiments have been performed at the Standford Synchrotron Radiation Laboratory (SSRL) using beamline III-4, which is specially designed for the sue of low energy photons. Light elements on Si wafers have been analyzed, leading to detection limits below 100 fg for Na, Mg and Al, which corresponds to about 10{sup 9}atoms. A new vacuum chamber is introduced meeting the requirements of wafer handling without the risk of contamination and offering the possibility of scanning a certain area of the wafer. Boron was detected on a wafer with 10{sup 14} atoms cm{sup -2} implanted in the surface layer. A special windowless X-ray tube with Mo, Al and Si as anode materials was also tested. With the optimization of anode geometry, beam path and excitation conditions, a detection limit of 5 pg (corresponds to 10{sup 11} atoms) for Al was achieved. (Author).

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

    Energy Technology Data Exchange (ETDEWEB)

    Khounsary, A.

    1999-10-29

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

  11. Synchrotron X-ray studies of liquid-vapor interfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage

    1986-01-01

    The density profile ρ(z) across a liquid-vapor interface may be determined by the reflectivity R(θ) of X-rays at grazing angle incidence θ. The relation between R(θ) and ρ(z) is discussed, and experimental examples illustrating thermal roughness of simple liquids and smectic layering of liquid...

  12. Report on the fifth workshop on synchrotron x ray lithography

    Science.gov (United States)

    Williams, G. P.; Godel, J. B.; Brown, G. S.; Liebmann, W.

    Semiconductors comprise a greater part of the United States economy than the aircraft, steel, and automobile industries combined. In future the semiconductor manufacturing industry will be forced to switch away from present optical manufacturing methods in the early to mid 1990s. X ray lithography has emerged as the leading contender for continuing production below the 0.4 micron level. Brookhaven National Laboratory began a series of workshops on x ray lithography in 1986 to examine key issues and in particular to enable United States industry to take advantage of the technical base established in this field. Since accelerators provide the brightest sources for x ray lithography, most of the research and development to date has taken place at large accelerator-based research centers such as Brookhaven, the University of Wisconsin, and Stanford. The goals of this Fifth Brookhaven Workshop were to review progress and goals since the last workshop and to establish a blueprint for the future. The meeting focused on the exposure tool, that is, a term defined as the source plus beamline and stepper. In order to assess the appropriateness of schedules for the development of this tool, other aspects of the required technology such as masks, resists and inspection and repair were also reviewed. To accomplish this, two working groups were set up, one to review the overall aspects of x ray lithography and set a time frame, the other to focus on sources.

  13. Synchrotron radiation X-ray microfluorescence techniques and ...

    Indian Academy of Sciences (India)

    raphy system was implemented to analyse human prostate and breast samples and an X-ray mi- crofluorescence system was .... at the lumbar vertebral body of Wistar rat which are trabecular regions with dimensions smaller than those found in human femora, as can be seen in figure 4. Similar behaviour. (a). (b). Figure 5.

  14. Simulations of X-ray synchrotron beams using the EGS4 code system in medical applications

    International Nuclear Information System (INIS)

    Orion, I.; Henn, A.; Sagi, I.; Dilmanian, F.A.; Pena, L.; Rosenfeld, A.B.

    2001-01-01

    X-ray synchrotron beams are commonly used in biological and medical research. The availability of intense, polarized low-energy photons from the synchrotron beams provides a high dose transfer to biological materials. The EGS4 code system, which includes the photoelectron angular distribution, electron motion inside a magnetic field, and the LSCAT package, found to be the appropriate Monte Carlo code for synchrotron-produced X-ray simulations. The LSCAT package was developed in 1995 for the EGS4 code to contain the routines to simulate the linear polarization, the bound Compton, and the incoherent scattering functions. Three medical applications were demonstrated using the EGS4 Monte Carlo code as a proficient simulation code system for the synchrotron low-energy X-ray source. (orig.)

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

    International Nuclear Information System (INIS)

    Tranquada, J.M.

    2008-01-01

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

  16. X-ray Synchrotron Radiation in a Plasma Wiggler

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Shuoquin; /UCLA /SLAC, SSRL

    2005-09-27

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

  17. 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

    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......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...... diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure...

  18. Noninvasive 3D Structural Analysis of Arthropod by Synchrotron X-Ray Phase Contrast Tomography

    Directory of Open Access Journals (Sweden)

    Shengkun Yao

    2015-01-01

    Full Text Available X-ray imaging techniques significantly advanced our understanding of materials and biology, among which phase contrast X-ray microscopy has obvious advantages in imaging biological specimens which have low contrast by conventional absorption contrast microscopy. In this paper, three-dimensional microstructure of arthropod with high contrast has been demonstrated by synchrotron X-ray in-line phase contrast tomography. The external morphology and internal structures of an earthworm were analyzed based upon tomographic reconstructions with and without phase retrieval. We also identified and characterized various fine structural details such as the musculature system, the digestive system, the nervous system, and the circulatory system. This work exhibited the high efficiency, high precision, and wide potential applications of synchrotron X-ray phase contrast tomography in nondestructive investigation of low-density materials and biology.

  19. Noninvasive 3D Structural Analysis of Arthropod by Synchrotron X-Ray Phase Contrast Tomography

    International Nuclear Information System (INIS)

    Yao, S.; Zong, Y.; Fan, J.; Sun, Z.; Jiang, H.

    2015-01-01

    X-ray imaging techniques significantly advanced our understanding of materials and biology, among which phase contrast X-ray microscopy has obvious advantages in imaging biological specimens which have low contrast by conventional absorption contrast microscopy. In this paper, three-dimensional microstructure of arthropod with high contrast has been demonstrated by synchrotron X-ray in-line phase contrast tomography. The external morphology and internal structures of an earthworm were analyzed based upon tomographic reconstructions with and without phase retrieval. We also identified and characterized various fine structural details such as the musculature system, the digestive system, the nervous system, and the circulatory system. This work exhibited the high efficiency, high precision, and wide potential applications of synchrotron X-ray phase contrast tomography in nondestructive investigation of low-density materials and biology.

  20. 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 diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure...

  1. Model experiment of in vivo synchrotron X-ray diffraction of human kidney stones

    Energy Technology Data Exchange (ETDEWEB)

    Ancharov, A.I. [Institute of Solid State Chemistry and Mechanochemistry SB RAS, Novosibirsk (Russian Federation)]. E-mail: ancharov@mail.ru; Potapov, S.S. [Institute of Mineralogy UB RAS, Miass (Russian Federation); Moiseenko, T.N. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Feofilov, I.V. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Nizovskii, A.I. [Boreskov Institute of Catalysis SB RAS, Novosibirsk (Russian Federation)

    2007-05-21

    The diffraction of synchrotron radiation (SR) was used to explore the phase composition of kidney stones placed into a specific object phantom, which imitated the human body. As an imitation of the patient breath, the kidney stone was moved vertically and rotated to an angle of 15{sup o} during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern.

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

    Energy Technology Data Exchange (ETDEWEB)

    DOWD,B.A.

    1999-07-23

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Barton, M.Q.; Craft, B.; Williams, G.P. (eds.)

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  5. Synchrotron X-ray PIV Technique for Measurement of Blood Flow Velocity

    International Nuclear Information System (INIS)

    Kim, Guk Bae; Lee, Sang Joon; Je, Jung Ho

    2007-01-01

    Synchrotron X-ray micro-imaging method has been used to observe internal structures of various organisms, industrial devices, and so on. However, it is not suitable to see internal flows inside a structure because tracers typically employed in conventional optical flow visualization methods cannot be detectable with the X-ray micro-imaging method. On the other hand, a PIV (particle image velocimetry) method which has recently been accepted as a reliable quantitative flow visualization technique can extract lots of flow information by applying digital image processing techniques However, it is not applicable to opaque fluids such as blood. In this study, we combined the PIV method and the synchrotron X-ray micro-imaging technique to compose a new X-ray PIV technique. Using the X-ray PIV technique, we investigated the optical characteristics of blood for a coherent synchrotron X-ray beam and quantitatively visualized real blood flows inside an opaque tube without any contrast media. The velocity field information acquired would be helpful for investigating hemorheologic characteristics of the blood flow

  6. Effect of toroidal mirror on spatial coherence of synchrotron hard X-ray beams

    International Nuclear Information System (INIS)

    Wang Hua; Yan Shuai; Yan Fen; Mao Chengwen; Liang Dongxun; He Yan; Jiang Sheng; Li Aiguo; Yu Xiaohan

    2012-01-01

    The Gaussian Schell-model source theory is used to describe the hard X-ray micro focusing beamline with an undulator of the Shanghai Synchrotron Radiation Facility. Based on the model and general Huygens-Fresnel principle, propagation of cross-spectral density function in free space is studied. Equivalent source hypothesis is proposed and the effect of toroidal mirror on spatial coherence of the hard X-ray beams is studied. The theoretical results are consistent with the experimental results. Only divergence angles of the incident and outgoing X-rays are considered in the equivalent source hypothesis, hence an easy extension of the hypothesis to other beamline optical elements. (authors)

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

    International Nuclear Information System (INIS)

    Rosemeier, R.G.; Green, R.E. Jr.

    1982-01-01

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

  8. Thermal, structural, and fabrication aspects of diamond windows for high power synchrotron x-ray beamlines

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Phillips, W.

    1992-01-01

    Recent advances in chemical vapor deposition (CVD) technology have made it possible to produce thin free-standing diamond foils that can be used as the window material in high heat load, synchrotron beamlines. Numerical simulations suggest that these windows can offer an attractive and at times the only altemative to beryllium windows for use in third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, as are the microstructure characteristics bearing on diamond's performance in this role. Analytic and numerical results are also presented to provide a basis for the design and testing of such windows

  9. A CCD-based area detector for X-ray crystallography using synchrotron and laboratory sources

    International Nuclear Information System (INIS)

    Phillips, W.C.; Li Youli; Stanton, M.; Xie Yuanhui; O'Mara, D.; Kalata, K.

    1993-01-01

    The design and characteristics of a CCD-based area detector suitable for X-ray crystallographic studies using both synchrotron and laboratory sources are described. The active area is 75 mm in diameter, the FWHM of the point response function is 0.20 mm, and for Bragg peaks the dynamic range is 900 and the DQE ∼0.3. The 1320x1035-pixel Kodak CCD is read out into an 8 Mbyte memory system in 0.14 s and digitized to 12 bits. X-ray crystallographic data collected at the NSLS synchrotron from cubic insulin crystals are presented. (orig.)

  10. Effects of synchrotron x-rays on PVD deposited and ion implanted α-Si

    International Nuclear Information System (INIS)

    Yu, K.M.; Wang, L.; Walukiewicz, W.; Muto, S.; McCormick, S.; Abelson, J.R.

    1997-01-01

    The authors have studied the effects of intense X-ray irradiation on the structure of amorphous Si films. The films were obtained by either physical vapor deposition or by implantation of high energy ions into crystalline Si. They were exposed to different total doses of synchrotron X-rays. From the EXAFS and EXELFS measurements they find that an exposure to X-rays increases the Si coordination number. Also in the PVD films a prolonged X-ray exposure enlarges, by about 2%, the Si-Si bond length. Raman spectroscopy shows that Si amorphized with high energy ions contains small residual amounts of crystalline material. Irradiation of such films with X-rays annihilates those crystallites resulting in homogeneously amorphous layer with a close to four-fold coordination of Si atoms. This rearrangement of the local structure has a pronounced effect on the crystallization process of the amorphous films. Thermal annealing of X-ray irradiated ion amorphized films leads to nearly defect free solid phase epitaxy at 500 C. Also they observe a delay in the onset of the crystallization process in X-ray irradiated PVD films. They associate this with a reduced concentration of nucleation centers in the x-ray treated materials

  11. Beryllium window flange for synchrotron radiation X-ray beamline fabricated by hot isostatic press method

    International Nuclear Information System (INIS)

    Asaoka, Seiji; Maezawa, Hideki; Nishida, Kiyotoshi; Sakamoto, Naoki.

    1995-01-01

    The synchrotron radiation experimental facilities in National Laboratory for High Energy Physics are the experimental facilities for joint utilization, that possess the positron storage ring of 2.5 GeV exclusively used for synchrotron radiation. Synchrotron radiation is led through a mainstay beam channel to the laboratory, and in the beam line of X-ray, it is used for experiment through the taking-out window made of beryllium. At this time, the function of the taking-out window is to shut off between the ultrahigh vacuum in the mainstay beam channel and the atmosphere, and to cut the low energy component of synchrotron radiation spectra. The experiment using X-ray is carried out mostly in the atmosphere. The design of the efficient cooling water channel which is compatible with the flange construction is important under the high thermal load of synchrotron radiation. The beryllium window flange for synchrotron radiation X-ray was made by HIP method, and the ultrahigh vacuum test, the high pressure water flow test and the actual machine test were carried out by heat cycle. The properties required for the window material, the requirement of the construction, the new development of HIP method, and the experiments for evaluating the manufactured beryllium window are described. (K.I.)

  12. 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.

  13. Synchrotron radiation and free-electron lasers principles of coherent X-ray generation

    CERN Document Server

    Kim, Kwang-Je; Lindberg, Ryan

    2017-01-01

    Learn about the latest advances in high-brightness X-ray physics and technology with this authoritative text. Drawing upon the most recent theoretical developments, pre-eminent leaders in the field guide readers through the fundamental principles and techniques of high-brightness X-ray generation from both synchrotron and free-electron laser sources. A wide range of topics is covered, including high-brightness synchrotron radiation from undulators, self-amplified spontaneous emission, seeded high-gain amplifiers with harmonic generation, ultra-short pulses, tapering for higher power, free-electron laser oscillators, and X-ray oscillator and amplifier configuration. Novel mathematical approaches and numerous figures accompanied by intuitive explanations enable easy understanding of key concepts, whilst practical considerations of performance-improving techniques and discussion of recent experimental results provide the tools and knowledge needed to address current research problems in the field. This is a comp...

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  15. A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility.

    Science.gov (United States)

    Tiwari, M K; Gupta, P; Sinha, A K; Kane, S R; Singh, A K; Garg, S R; Garg, C K; Lodha, G S; Deb, S K

    2013-03-01

    A microfocus X-ray fluorescence spectroscopy beamline (BL-16) at the Indian synchrotron radiation facility Indus-2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X-ray fluorescence mapping, X-ray microspectroscopy and total-external-reflection fluorescence characterization. The beamline is installed on a bending-magnet source with a working X-ray energy range of 4-20 keV, enabling it to excite K-edges of all elements from S to Nb and L-edges from Ag to U. The optics of the beamline comprises of a double-crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick-Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.

  16. Progress in X-ray synchrotron diffraction studies of muscle contraction. Ch. 19

    International Nuclear Information System (INIS)

    Wakabayashi, Katsuzo

    1991-01-01

    This chapter provides a review of applications of synchrotron radiation (SR) to X-ray diffraction studies on the dynamic aspects of muscle contraction and is, at the same time, a progress report on the technical developments specifically related to muscle research. The introduction of SR as an intense X-ray source and the development of high ability detectors have led to enormous improvement in the quality of data from time-resolved X-ray diffraction studies of muscle contraction. The X-ray diffraction pattern taken during contraction shows that the force generation of a muscle proceeds upon interaction of the incommensurate structures of the thin and thick filaments. In this framework a distinct intensity change of the weaker reflections from the thin filaments was detected. However, there was still no strong evidence of direct physical attachment of myosin heads to actin during contraction. (author). 170 refs.; 52 figs.; 3 tabs

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

    Science.gov (United States)

    Withers, P J

    2015-03-06

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored.

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

    Energy Technology Data Exchange (ETDEWEB)

    Kakuno, E. M.; Giacomolli, B. A.; Scorzato, C. R. [Universidade Federal do Pampa - UNIPAMPA-Bage, 96413-170 (Brazil); Laboratorio Nacional de Luz Sincrotron - LNLS, 13086-100 (Brazil)

    2012-05-17

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

  19. Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

    Indian Academy of Sciences (India)

    Abstract. An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from var- ious elemental metals and standard ...

  20. High-pressure phases of uranium monophosphide studied by synchrotron x-ray diffraction

    DEFF Research Database (Denmark)

    Olsen, J. Staun; Gerward, Leif; Benedict, U.

    1988-01-01

    X-ray diffraction studies have been performed on UP powder for pressures up to 51 GPa using synchrotron radiation and a diamond-anvil cell. At ambient pressure UP has the rocksalt structure. The bulk modulus has been determined to B0=102(4) GPa and its pressure derivative to B0’=4.0(8). The cubic...

  1. Synchrotron-based X-ray microscopic studies for bioeffects of nanomaterials.

    Science.gov (United States)

    Zhu, Ying; Cai, Xiaoqing; Li, Jiang; Zhong, Zengtao; Huang, Qing; Fan, Chunhai

    2014-04-01

    There have been increasing interests in studying biological effects of nanomaterials, which are nevertheless faced up with many challenges due to the nanoscale dimensions and unique chemical properties of nanomaterials. Synchrotron-based X-ray microscopy, an advanced imaging technology with high spatial resolution and excellent elemental specificity, provides a new platform for studying interactions between nanomaterials and living systems. In this article, we review the recent progress of X-ray microscopic studies on bioeffects of nanomaterials in several living systems including cells, model organisms, animals and plants. We aim to provide an overview of the state of the art, and the advantages of using synchrotron-based X-ray microscopy for characterizing in vitro and in vivo behaviors and biodistribution of nanomaterials. We also expect that the use of a combination of new synchrotron techniques should offer unprecedented opportunities for better understanding complex interactions at the nano-biological interface and accounting for unique bioeffects of nanomaterials. Synchrotron-based X-ray microscopy is a non-destructive imaging technique that enables high resolution spatial mapping of metals with elemental level detection methods. This review summarizes the current use and perspectives of this novel technique in studying the biology and tissue interactions of nanomaterials. Copyright © 2014 Elsevier Inc. All rights reserved.

  2. A Spectrometer for X-Ray Energy-Dispersive Diffraction using Synchrotron Radiation

    DEFF Research Database (Denmark)

    Staun Olsen, Janus; Buras, B; Gerward, Leif

    1981-01-01

    Describes a white-beam X-ray energy-dispersive diffractometer built for Hasylab in Hamburg, FRG, using the synchrotron radiation from the electron storage ring DORIS. The following features of the instrument are discussed: horizontal or vertical scattering plane, collimators, sample environment, ...

  3. Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

    Indian Academy of Sciences (India)

    An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic ...

  4. CCD [charge-coupled device] sensors in synchrotron x-ray detectors

    International Nuclear Information System (INIS)

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

    1987-01-01

    The intense photon flux from advanced synchrotron light sources, such as the 7-GeV synchrotron being designed at Argonne, require integrating-type detectors. Charge-coupled devices (CCDs) are well suited as synchrotron x-ray detectors. When irradiated indirectly via a phosphor followed by reducing optics, diffraction patterns of 100 cm 2 can be imaged on a 2 cm 2 CCD. With a conversion efficiency of ∼1 CCD electron/x-ray photon, a peak saturation capacity of >10 6 x rays can be obtained. A programmable CCD controller operating at a clock frequency of 20 MHz has been developed. The readout rate is 5 x 10 6 pixels/s and the shift rate in the parallel registers is 10 6 lines/s. The test detector was evaluated in two experiments. In protein crystallography diffraction patterns have been obtained from a lysozyme crystal using a conventional rotating anode x-ray generator. Based on these results we expect to obtain at a synchrotron diffraction images at the rate of ∼1 frame/s or a complete 3-dimensional data set from a single crystal in ∼2 min. 16 refs., 16 figs., 2 tabs

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

    International Nuclear Information System (INIS)

    Southworth, S.; Gemmell, D.

    1996-08-01

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

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

    International Nuclear Information System (INIS)

    Liu Chian; Ice, G.E.; Liu, W.; Assoufid, L.; Qian, J.; Shi, B.; Khachatryan, R.; Wieczorek, M.; Zschack, P.; Tischler, J.Z.

    2012-01-01

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

  7. Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

    International Nuclear Information System (INIS)

    Bae, Sungchul; Meral, Cagla; Oh, Jae-eun; Moon, Juhyuk; Kunz, Martin; Monteiro, Paulo J.M.

    2014-01-01

    The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS

  8. Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

    Energy Technology Data Exchange (ETDEWEB)

    Bae, Sungchul [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States); Meral, Cagla [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States); Department of Civil Engineering, Middle East Technical University, 06800 Ankara (Turkey); Oh, Jae-eun [School of Urban and Environmental Engineering, Ulsan National Institute of Science and Technology, Ulsan 689-798 (Korea, Republic of); Moon, Juhyuk [Civil Engineering Program, Department of Mechanical Engineering, State University of New York at Stony Brook, NY 11794 (United States); Kunz, Martin [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Monteiro, Paulo J.M., E-mail: monteiro@ce.berkeley.edu [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States)

    2014-05-01

    The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.

  9. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    International Nuclear Information System (INIS)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G.; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E.

    2016-01-01

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

  10. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    Energy Technology Data Exchange (ETDEWEB)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G. [Imperial College London, London (United Kingdom); Drakopoulos, Michael [Diamond Light Source, I12 Joint Engineering, Environmental, Processing (JEEP) Beamline, Didcot, Oxfordshire (United Kingdom); Rack, Alexander [European Synchrotron Radiation Facility, Grenoble (France); Eakins, Daniel E., E-mail: d.eakins@imperial.ac.uk [Imperial College London, London (United Kingdom)

    2016-03-24

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

  11. Synchrotron radiation X-ray powder diffraction techniques applied in hydrogen storage materials - A review

    Directory of Open Access Journals (Sweden)

    Honghui Cheng

    2017-02-01

    Full Text Available Synchrotron radiation is an advanced collimated light source with high intensity. It has particular advantages in structural characterization of materials on the atomic or molecular scale. Synchrotron radiation X-ray powder diffraction (SR-XRPD has been successfully exploited to various areas of hydrogen storage materials. In the paper, we will give a brief introduction on hydrogen storage materials, X-ray powder diffraction (XRPD, and synchrotron radiation light source. The applications of ex situ and in situ time-resolved SR-XRPD in hydrogen storage materials, are reviewed in detail. Future trends and proposals in the applications of the advanced XRPD techniques in hydrogen storage materials are also discussed.

  12. A powerful flare from Sgr A* confirms the synchrotron nature of the X-ray emission

    Science.gov (United States)

    Ponti, G.; George, E.; Scaringi, S.; Zhang, S.; Jin, C.; Dexter, J.; Terrier, R.; Clavel, M.; Degenaar, N.; Eisenhauer, F.; Genzel, R.; Gillessen, S.; Goldwurm, A.; Habibi, M.; Haggard, D.; Hailey, C.; Harrison, F.; Merloni, A.; Mori, K.; Nandra, K.; Ott, T.; Pfuhl, O.; Plewa, P. M.; Waisberg, I.

    2017-06-01

    We present the first fully simultaneous fits to the near-infrared (NIR) and X-ray spectral slope (and its evolution) during a very bright flare from Sgr A*, the supermassive black hole at the Milky Way's centre. Our study arises from ambitious multiwavelength monitoring campaigns with XMM-Newton, NuSTAR and SINFONI. The average multiwavelength spectrum is well reproduced by a broken power law with ΓNIR = 1.7 ± 0.1 and ΓX = 2.27 ± 0.12. The difference in spectral slopes (ΔΓ = 0.57 ± 0.09) strongly supports synchrotron emission with a cooling break. The flare starts first in the NIR with a flat and bright NIR spectrum, while X-ray radiation is detected only after about 103 s, when a very steep X-ray spectrum (ΔΓ = 1.8 ± 0.4) is observed. These measurements are consistent with synchrotron emission with a cooling break and they suggest that the high-energy cut-off in the electron distribution (γmax) induces an initial cut-off in the optical-UV band that evolves slowly into the X-ray band. The temporal and spectral evolution observed in all bright X-ray flares are also in line with a slow evolution of γmax. We also observe hints for a variation of the cooling break that might be induced by an evolution of the magnetic field (from B ˜ 30 ± 8 G to B ˜ 4.8 ± 1.7 G at the X-ray peak). Such drop of the magnetic field at the flare peak would be expected if the acceleration mechanism is tapping energy from the magnetic field, such as in magnetic reconnection. We conclude that synchrotron emission with a cooling break is a viable process for Sgr A*'s flaring emission.

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

    International Nuclear Information System (INIS)

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

    1992-01-01

    X-ray windows are often used on the front end of synchrotron beamlines to isolate the ultra high vacuum of the storage ring from the downstream environment. The windows are usually made of low atomic number materials, such as beryllium, for maximum x-ray transmission, and they must survive and remain vacuum tight during repeated thermal cycles. The intense x-ray beams generated by the wigglers and undulators at high energy storage rings can deposit substantial amounts of localized heat in the (actively cooled) windows leading to high temperatures, and vacuum or structural failure. Thermal filters upstream of the windows can be used to reduce the radiation absorbed in the windows. This solution has limitations, however, since a small amount of filtering may still leave an unacceptable amount of heat to be absorbed in the windows, while substantial filtering will absorb a large amount of the useful photons. Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond films that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptional thermal, structural, and physical properties of diamond. Numerical simulation indicates that diamond windows offer an attractive alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical results are presented to provide a basis for design and testing of such windows

  14. X-ray phase contrast imaging: From synchrotrons to conventional sources

    International Nuclear Information System (INIS)

    Olivo, A.; Castelli, E.

    2014-01-01

    Phase-based approaches can revolutionize X-ray imaging and remove its main limitation: poor image contrast arising from low attenuation differences. They exploit the unit decrement of the real part of the refractive index, typically 1000 times larger than the imaginary part driving attenuation. This increases the contrast of all details, and enables the detection of features classically considered 'X-ray invisible'. Following pioneering experiments dating back to the mid-sixties, X-ray phase contrast imaging 'exploded' in the mid-nineties, when third generation synchrotron sources became more widely available. Applications were proposed in fields as diverse as material science, palaeontology, biology, food science, cultural heritage preservation, and many others. Among these applications, medicine has been constantly considered the most important; among medical applications, mammography is arguably the one that attracted most attention. Applications to mammography were pioneered by the SYRMEP (SYnchrotron Radiation for MEdical Physics) group in Trieste, which was already active in the area through a combination of innovative ways to do imaging at synchrotrons and development of novel X-ray detectors. This pioneering phase led to the only clinical experience of phase contrast mammography on human patients, and spawned a number of ideas as to how these advances could be translated into clinical practice.

  15. Synchrotron X-ray adaptative monochromator: study and realization of a prototype

    International Nuclear Information System (INIS)

    Dezoret, D.

    1995-01-01

    This work presents a study of a prototype of a synchrotron X-ray monochromator. The spectral qualities of this optic are sensitive to the heat loads which are particularly important on third synchrotron generation like ESRF. Indeed, powers generated by synchrotron beams can reach few kilowatts and power densities about a few tens watts per square millimeters. The mechanical deformations of the optical elements of the beamlines issue issue of the heat load can damage their spectral efficiencies. In order to compensate the deformations, wa have been studying the transposition of the adaptive astronomical optics technology to the x-ray field. First, we have considered the modifications of the spectral characteristics of a crystal induced by x-rays. We have established the specifications required to a technological realisation. Then, thermomechanical and technological studies have been required to transpose the astronomical technology to an x-ray technology. After these studies, we have begun the realisation of a prototype. This monochromator is composed by a crystal of silicon (111) bonded on a piezo-electric structure. The mechanical control is a loop system composed by a infrared light, a Shack-Hartmann CDD and wave front analyser. This system has to compensate the deformations of the crystal in the 5 kcV to 60 kcV energy range with a power density of 1 watt per square millimeters. (authors)

  16. X-ray detectors for diffraction studies and their use with synchrotron radiation

    International Nuclear Information System (INIS)

    Milch, J.

    1976-02-01

    All techniques for X-ray diffraction studies on biological materials exhibit certain limitations. The characteristics of several X-ray detection systems, namely film, multiwire proportional counter and image intensified TV, are discussed and compared for application to specific biological studies. For the high count-rate situation existing at a synchrotron, it is shown that film is a good choice, but that the image intensified TV exhibits significant advantages. The details of such a system now being used at Princeton with a low intensity source are given and current results presented

  17. Antiferroelectric surface layers in a liquid crystal as observed by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Gramsbergen, E. F.; de Jeu, W. H.; Als-Nielsen, Jens Aage

    1986-01-01

    The X-ray reflectivity form the surface of a liquid crystal with terminally polar (cyano substituted) molecules has been studied using a high-resolution triple-axis X-ray spectrometer in combination with a synchrotron source. It is demonstrated that at the surface of the smectic Al phase a few...... antiferroelectric double layers develop that can be distinguished from the bulk single layer structure. A model is developed that separates the electron density in a contribution from the molecular form factor, and from the structure factor of the mono- and the bilayers, respectively. It shows that (i) the first...

  18. A Furnace for Diffraction Studies using Synchrotron X-Ray Radiation

    DEFF Research Database (Denmark)

    Buras, B.; Lebech, Bente; Kofoed, W.

    1984-01-01

    A furnace for diffraction studies using synchrotron X-ray radiation is described. The furnace can be operated between ambient temperature and 1 800 °C with a temperature stability better than 5 °C for temperatures above 300 °C. Kapton windows allow almost 360° access for the X-ray beam in the hor...... in the horizontal scattering plane and the furnace may be used in both conventional monochromatic beam angle-dispersive and white-beam energy-dispersive diffraction experiments. Details of the furnace windows, heating element, thermometry and sample mount are given....

  19. Synchrotron X-ray and neutron diffraction studies in solid-state chemistry

    International Nuclear Information System (INIS)

    Cheetham, A.K.; Wilkinson, A.P.

    1992-01-01

    Since the scatterers are different - X-rays are scattered by the electrons of an atom, neutrons by the nuclei - the questions addressed by the two diffraction experiments have been complementary. For example, neighboring elements of the periodic table could be distinguished formerly only by neutron diffraction. Now, however, this is also partly possible with high-energy synchrotron radiation. This review describes recent applications of X-ray and neutron diffraction methods in solid-state chemistry and how the maximal information can be extracted by a combination of techniques. (orig.)

  20. X-ray fluorescence in Member States: Austria. Synchrotron radiation induced TXRF-XANES

    International Nuclear Information System (INIS)

    Meirer, Florian; Wobrauschek, Peter; Streli, Christina; Pepponi, Giancarlo

    2009-01-01

    X ray Absorption Near Edge Structure (XANES) analysis was used in combination with Total reflection X ray Fluorescence (TXRF) at different Synchrotron Radiation (SR) facilities to perform elemental analysis and speciation at trace levels. TXRF-XANES was used to perform analysis of contaminations on Silicon wafer surfaces and determine the oxidation state of Fe. Urban aerosols were sampled size fractioned and the oxidation state of Fe was determined for each impactor stage again using TXRF-XANES. The feasibility of XANES analysis at trace element levels using different SR-XRF setups was demonstrated. (author)

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

    Science.gov (United States)

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

    2015-01-01

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

  2. Optimizing a synchrotron based x-ray lithography system for IC manufacturing

    Science.gov (United States)

    Kovacs, Stephen; Speiser, Kenneth; Thaw, Winston; Heese, Richard N.

    1990-05-01

    The electron storage ring is a realistic solution as a radiation source for production grade, industrial X-ray lithography system. Today several large scale plans are in motion to design and implement synchrotron storage rings of different types for this purpose in the USA and abroad. Most of the scientific and technological problems related to the physics, design and manufacturing engineering, and commissioning of these systems for microlithography have been resolved or are under extensive study. However, investigation on issues connected to application of Synchrotron Orbit Radiation (SOR ) in chip production environment has been somewhat neglected. In this paper we have filled this gap pointing out direct effects of some basic synchrotron design parameters and associated subsystems (injector, X-ray beam line) on the operation and cost of lithography in production. The following factors were considered: synchrotron configuration, injection energy, beam intensity variability, number of beam lines and wafer exposure concept. A cost model has been worked out and applied to three different X-ray Lithography Source (XLS) systems. The results of these applications are compared and conclusions drawn.

  3. Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries.

    Science.gov (United States)

    Lin, Feng; Liu, Yijin; Yu, Xiqian; Cheng, Lei; Singer, Andrej; Shpyrko, Oleg G; Xin, Huolin L; Tamura, Nobumichi; Tian, Chixia; Weng, Tsu-Chien; Yang, Xiao-Qing; Meng, Ying Shirley; Nordlund, Dennis; Yang, Wanli; Doeff, Marca M

    2017-11-08

    Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancement of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allow for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy, and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools and are also discussed toward the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole

  4. Microfocussing of synchrotron X-rays using X-ray refractive lens developed at Indus-2 deep X-ray lithography beamline

    International Nuclear Information System (INIS)

    Dhamgaye, V.P.; Tiwari, M.K.; Lodha, G.S.; Sawhney, K.J.S.

    2014-01-01

    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 sources are compared. (author)

  5. Synchrotron X-ray micro-beam studies of ancient Egyptian make-up

    International Nuclear Information System (INIS)

    Martinetto, P.; Anne, M.; Dooryhee, E.; Drakopoulos, M.; Dubus, M.; Salomon, J.; Simionovici, A.; Walter, Ph.

    2001-01-01

    Vases full of make-up are most often present in the burial furniture of Egyptian tombs dated from the pharaonic period. The powdered cosmetics made of isolated grains are analysed to identify their trace element signature. From this signature we identify the provenance of the mineral ingredients in the make-up and we observe different impurities in products, which have been demonstrated as synthetic substances by previous works. Focused X-ray micro-beam (2x5 μm 2 ) is successively tuned at 11 keV, below the L III absorption edge of Pb, and 31.8 keV for global characterisation of the metal impurities. The fluorescence signal integrated over each single grain is detected against the X-ray micro-diffraction pattern collected in transmission with a bi-dimensional detector. Furthermore, for galena grains rich in Zn, the XANES signal at the K-absorption edge of Zn shows its immediate nearest-neighbour environment

  6. Phase-contrast computed microtomography with 50 keV synchrotron x-rays

    International Nuclear Information System (INIS)

    Raven, C.; Snigirev, A.; Snigireva, I.; Spanne, P.; Suvorov, A.

    1996-01-01

    The possibilities to determine the internal structure of low density materials by a simple microtomography setup with high energy synchrotron x-rays are demonstrated experimentally. The coherent properties of a 50 keV x-ray beam at the ESRF wiggler beamline are used to observe phase-contrast images of a boron fiber, which has negligible absorption in this energy range. Images of the boron fiber are recorded with a high-resolution x-ray film at various distances up to 2 m. For microtomography studies, 61 images are taken over an angular range of 180 degrees. In the reconstructed cross sections, the hollow, 15-mm-diameter core of the fiber is clearly visible. copyright 1996 American Institute of Physics

  7. Diamond monochromator for high heat flux synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1992-12-01

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond mollochromator system. In this Paper, we consider various aspects, advantage and disadvantages, and promises and pitfalls of such a system and evaluate the comparative an monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of diamond-based monochromator is within present technical means

  8. Characterisation of microfocused beam for synchrotron powder diffraction using a new X-ray camera

    International Nuclear Information System (INIS)

    Thomas, C; Potter, J; Tang, C C; Lennie, A R

    2012-01-01

    The powder diffraction beamline I11, Diamond Light Source, is being continually upgraded as requirements of the user community evolve. Intensities of X-rays from the I11 in-vacuum electron undulator in the 3 GeV synchrotron fall off at higher energies. By focusing higher energy X-rays, we can overcome flux limitations, and open up new diffraction experiments. Here, we describe characterisation of microfocusing using compound refractive lenses (CRL). For a relatively modest outlay, we have developed an experimental setup and a novel X-ray camera with good sensitivity and a resolution specification suitable for characterising these focusing optics. We show that vertical oscillations in the focused beam compromise resolution of the source imaged by the CRL. Nevertheless, we have measured CRL focusing properties, and demonstrate the use of energy scanning to determine lens alignment. Real benefits of the intensity gain are illustrated.

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  11. System of laser pump and synchrotron radiation probe microdiffraction to investigate optical recording process

    International Nuclear Information System (INIS)

    Yasuda, Nobuhiro; Fukuyama, Yoshimitsu; Osawa, Hitoshi; Kimura, Shigeru; Ito, Kiminori; Tanaka, Yoshihito; Matsunaga, Toshiyuki; Kojima, Rie; Hisada, Kazuya; Tsuchino, Akio; Birukawa, Masahiro; Yamada, Noboru; Sekiguchi, Koji; Fujiie, Kazuhiko; Kawakubo, Osamu; Takata, Masaki

    2013-01-01

    We have developed a system of laser-pump and synchrotron radiation probe microdiffraction to investigate the phase-change process on a nanosecond time scale of Ge 2 Sb 2 Te 5 film embedded in multi-layer structures, which corresponds to real optical recording media. The measurements were achieved by combining (i) the pump-laser system with a pulse width of 300 ps, (ii) a highly brilliant focused microbeam with wide peak-energy width (ΔE/E ∼ 2%) made by focusing helical undulator radiation without monochromatization, and (iii) a precise sample rotation stage to make repetitive measurements. We successfully detected a very weak time-resolved diffraction signal by using this system from 100-nm-thick Ge 2 Sb 2 Te 5 phase-change layers. This enabled us to find the dependence of the crystal-amorphous phase change process of the Ge 2 Sb 2 Te 5 layers on laser power.

  12. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br; Zucchi, Orgheda L.D.A. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas de Ribeirao Preto]. E-mail: olzucchi@fcfrp.usp.br

    2005-07-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 {mu}L of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1{mu}g.L{sup -1} for Mn and Fe to 15{mu}g.L{sup -1} for P. (author)

  13. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    International Nuclear Information System (INIS)

    Moreira, Silvana; Vives, Ana Elisa S. de; Nascimento Filho, Virgilio F.; Zucchi, Orgheda L.D.A.

    2005-01-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 μL of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1μg.L -1 for Mn and Fe to 15μg.L -1 for P. (author)

  14. Analysis of beers from Brazil with synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Moreira, S.; Vives, A.E.S.; Brienza, S.M.B.; Zucchi, O.L.A.D.; Jesus, E.F.O. de; Nascimento Filho, V.F.

    2006-01-01

    In this study the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian legislation and the nutritional values established by National Agricultural Library (NAL, USA). The measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 μl of beers containing an internal standard used to correct geometry effects was analyzed without pretreatment. The measuring time was 100 seconds and the detection limits obtained varied from 1 μg x l -1 for Mn and Fe to 15 μg x l -1 for P. (author)

  15. National Synchrotron Light Source users manual: Guide to the VUV and x-ray beam lines

    International Nuclear Information System (INIS)

    Gmuer, N.F.; White-DePace, S.M.

    1987-08-01

    The success of the National Synchrotron Light Source in the years to come will be based, in large part, on the size of the users community and the diversity of the scientific disciplines represented by these users. In order to promote this philosophy, this National Synchrotron Light Source (NSLS) Users Manual: Guide to the VUV and X-Ray Beam Lines, has been published. This manual serves a number of purposes. In an effort to attract new research, it will present to the scientific community-at-large the current and projected architecture and capabilities of the various VUV and x-ray beam lines and storage rings. We anticipate that this publication will be updated periodically in order to keep pace with the constant changes at the NSLS

  16. Nondestructive analysis of silver in gold foil using synchrotron radiation X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Nakanishi, Toshio; Shimoda, Osamu; Nishiwaki, Yoshinori; Miyamoto, Naoki

    2005-01-01

    Small particles of gold foil detached from an indoor decoration might be important evidence to associate a suspect with a crime scene. We have investigated the application of elemental analysis using synchrotron radiation X-ray fluorescence spectrometry to discriminate small particles of gold foil. Eight kinds of gold foil samples collected in Japan were used in the experiments. As a result of synchrotron radiation X-ray fluorescence spectrometry, only two elements, gold and silver, were detected from all gold foil samples. The intensity ratios of AgK α /AuL α showed good correlation with the content ratios of Ag/Au. The variation of intensity ratio within a same sample was sufficiently small compared with those of different samples. Therefore the comparison of this intensity ratio can be an effective method to discriminate small particles originating from different types of gold foil. (author)

  17. Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

    Science.gov (United States)

    Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

    2000-01-01

    A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

  18. Synchrotron X-ray CT of rose peduncles. Evaluation of tissue damage by radiation

    Energy Technology Data Exchange (ETDEWEB)

    Herppich, Werner B. [Leibniz-Institut fuer Agrartechnik Potsdam-Bornim e.V., Potsdam (Germany). Abt. Technik im Gartenbau; Matsushima, Uzuki [Iwate Univ., Morioka (Japan). Faculty of Agriculture; Graf, Wolfgang [Association for Technology and Structures in Agriculture (KTBL), Darmstadt (Germany); Zabler, Simon [Fraunhofer-Institut fuer Integrierte Schaltungen (IIS), Wuerzburg (Germany). Project group NanoCT Systems (NCTS); Dawson, Martin [Salford Univ., Greater Manchester (United Kingdom); Choinka, Gerard; Manke, Ingo [Helmholtz Center Berlin for Materials and Energy (HZB), Berlin (Germany)

    2015-02-01

    ''Bent-neck'' syndrome, an important postharvest problem of cut roses, is probably caused by water supply limitations and/or the structural weakness of vascular bundles of the peduncle tissue. For this reason, advanced knowledge about the microstructures of rose peduncles and their cultivar specific variations may lead to a better understanding of the underlying mechanisms. Synchrotron X-ray computed tomography (SXCT), especially phase-based CT, is a highly suitable technique to nondestructively investigate plants' micro anatomy. SXCT with monochromatic X-ray beams of 30, 40 and 50 keV photon energy was used to evaluate the three-dimensional inner structures of the peduncles of 3 rose cultivars that differ greatly in their bent-neck susceptibility. Results indicated that this technique achieves sufficiently high spatial resolution to investigate complex tissues. However, further investigations with chlorophyll fluorescence analysis (CFA) and optical microscope imagery reveal different kinds of heavy damage of the irradiated regions induced by synchrotron X-rays; in a cultivar-specific manner, partial destruction of cell walls occurred a few hours after X-ray irradiation. Furthermore, a delayed inhibition of photosynthesis accompanied by the degradation of chlorophyll was obvious from CFA within hours and days after the end of CT measurements. Although SXCT is certainly well suited for three-dimensional anatomical analysis of rose peduncles, the applied technique is not nondestructive.

  19. Electron density measurement with dual-energy x-ray CT using synchrotron radiation

    International Nuclear Information System (INIS)

    Torikoshi, Masami; Tsunoo, Takanori; Sasaki, Makoto; Endo, Masahiro; Noda, Yutaka; Ohno, Yumiko; Kohno, Toshiyuki; Hyodo, Kazuyuki; Uesugi, Kentaro; Yagi, Naoto

    2003-01-01

    Monochromatic x-ray computed tomography (CT) at two different energies provides information about electron density of human tissue without ambiguity due to the beam hardening effect. This information makes the treatment planning for proton and heavy-ion radiotherapy more precise. We have started a feasibility study on dual energy x-ray CT by using synchrotron radiation. A translation-rotation scanning CT system was developed for quantitative measurement in order to clarify what precision in the measurement was achieved. Liquid samples of solutions of K 2 HPO 4 and solid samples of tissue equivalent materials were used to simulate human tissue. The experiments were carried out using monochromatic x-rays with energies of 40, 70 and 80 keV produced by monochromatizing synchrotron radiation. The solid samples were also measured in a complementary method using high-energy carbon beams to evaluate the electron densities. The measured electron densities were compared with the theoretical values or the values measured in the complementary method. It was found that these values were in agreement in 0.9% on average. Effective atomic numbers were obtained as well from dual-energy x-ray CT. The tomographic image based on each of the electron densities and the effective atomic number presents a different feature of the material, and its contrast drastically differs from that in a conventional CT image

  20. High resolution hard x-ray microscope on a second generation synchrotron source

    International Nuclear Information System (INIS)

    Tian Yangchao; Li Wenjie; Chen Jie; Liu Longhua; Liu Gang; Tian Jinping; Xiong Ying; Tkachuk, Andrei; Gelb, Jeff; Hsu, George; Yun Wenbing

    2008-01-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  1. Synchrotron X-ray Investigations of Mineral-Microbe-Metal Interactions

    International Nuclear Information System (INIS)

    Kemner, Kenneth M.; O'Loughlin, Edward J.; Kelly, Shelly D.; Boyanov, Maxim I.

    2005-01-01

    Interactions between microbes and minerals can play an important role in metal transformations (i.e. changes to an element's valence state, coordination chemistry, or both), which can ultimately affect that element's mobility. Mineralogy affects microbial metabolism and ecology in a system; microbes, in turn, can affect the system's mineralogy. Increasingly, synchrotron-based X-ray experiments are in routine use for determining an element's valence state and coordination chemistry, as well as for examining the role of microbes in metal transformations.

  2. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines

    International Nuclear Information System (INIS)

    Alcock, Simon G.; Nistea, Ioana; Sutter, John P.; Sawhney, Kawal; Fermé, Jean-Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    A next-generation bimorph mirror with piezos bonded to the side faces of a monolithic substrate was created. When replacing a first-generation bimorph mirror suffering from the junction effect, the new type of mirror significantly improved the size and shape of the reflected synchrotron X-ray beam. No evidence of the junction effect was observed even after eight months of continuous beamline usage. Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the ‘junction effect’: a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts

  3. Synchrotron radiation phase-contrast X-ray CT imaging of acupuncture points

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Dongming; Yan, Xiaohui; Zhang, Xinyi [Fudan University, Synchrotron Radiation Research Center, State Key Laboratory of Surface Physics and Department of Physics, Shanghai (China); Liu, Chenglin [Physics Department of Yancheng Teachers' College, Yancheng (China); Dang, Ruishan [The Second Military Medical University, Shanghai (China); Xiao, Tiqiao [Chinese Academy of Sciences, Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Shanghai (China); Zhu, Peiping [Chinese Academy of Sciences, Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, Beijing (China)

    2011-08-15

    Three-dimensional (3D) topographic structures of acupuncture points were investigated by using synchrotron radiation in-line X-ray phase contrast computerized tomography. Two acupuncture points, named Zhongji (RN3) and Zusanli (ST36), were studied. We found an accumulation of microvessels at each acupuncture point region. Images of the tissues surrounding the acupuncture points do not show such kinds of structure. This is the first time that 3D images have revealed the specific structures of acupuncture points. (orig.)

  4. Synchrotron radiation phase-contrast X-ray CT imaging of acupuncture points

    International Nuclear Information System (INIS)

    Zhang, Dongming; Yan, Xiaohui; Zhang, Xinyi; Liu, Chenglin; Dang, Ruishan; Xiao, Tiqiao; Zhu, Peiping

    2011-01-01

    Three-dimensional (3D) topographic structures of acupuncture points were investigated by using synchrotron radiation in-line X-ray phase contrast computerized tomography. Two acupuncture points, named Zhongji (RN3) and Zusanli (ST36), were studied. We found an accumulation of microvessels at each acupuncture point region. Images of the tissues surrounding the acupuncture points do not show such kinds of structure. This is the first time that 3D images have revealed the specific structures of acupuncture points. (orig.)

  5. Parallel beam microradiography of dental hard tissue using synchrotron radiation and X-ray image magnification

    International Nuclear Information System (INIS)

    Takagi, S.; Chow, L.C.; Brown, W.E.; Dobbyn, R.C.; Kuriyama, M.

    1984-01-01

    A novel technique utilizing a highly parallel beam of monochromatic synchrotron radiation combined with X-ray image magnification has been used to obtain microradiographs of caries lesions in relatively thick tooth sections. Preliminary results reveal structural features not previously reported. This technique holds the promise of allowing one to follow the structural changes accompanying the formation, destruction and chemical repair of mineralized tissue in real time. (orig.)

  6. A method for measuring the time structure of synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Moses, W.W.; Derenzo, S.E.

    1989-08-01

    We describe a method employing a plastic scintillator coupled to a fast photomultiplier tube to generate a timing pulse from the x-ray bursts emitted from a synchrotron radiation source. This technique is useful for performing synchrotron experiments where detailed knowledge of the timing distribution is necessary, such as time resolved spectroscopy or fluorescence lifetime experiments. By digitizing the time difference between the timing signal generated on one beam crossing with the timing signal generated on the next beam crossing, the time structure of a synchrotron beam can be analyzed. Using this technique, we have investigated the single bunch time structure at the National Synchrotron Light Source (NSLS) during pilot runs in January, 1989, and found that the majority of the beam (96%) is contained in one rf bucket, while the remainder of the beam (4%) is contained in satellite rf buckets preceeding and following the main rf bucket by 19 ns. 1 ref., 4 figs

  7. High-energy synchrotron radiation x-ray microscopy: Present status and future prospects

    International Nuclear Information System (INIS)

    Jones, K.W.; Gordon, B.M.; Spanne, P.; Rivers, M.L.; Sutton, S.R.

    1991-01-01

    High-energy radiation synchrotron x-ray microscopy is used to characterize materials of importance to the chemical and materials sciences and chemical engineering. The x-ray microscope (XRM) forms images of elemental distributions fluorescent x rays or images of mass distributions by measurement of the linear attenuation coefficient of the material. Distributions of sections through materials are obtained non-destructively using the technique of computed microtomography. The energy range of the x rays used for the XRM ranges from a few keV at the minimum value to more than 100 keV, which is sufficient to excite the K-edge of all naturally occurring elements. The work in progress at the Brookhaven NSLS X26 and X17 XRM is described in order to show the current status of the XRM. While there are many possible approaches to the XRM instrumentation, this instrument gives state-of-the-art performance in most respects and serves as a reasonable example of the present status of the instrumentation in terms of the spatial resolution and minimum detection limits obtainable. The examples of applications cited give an idea of the types of research fields that are currently under investigation. They can be used to illustrate how the field of x-ray microscopy will benefit from the use of bending magnets and insertion devices at the Advanced Photon Source. 8 refs., 5 figs

  8. Versatile, reprogrammable area pixel array detector for time-resolved synchrotron x-ray applications

    Energy Technology Data Exchange (ETDEWEB)

    Gruner, Sol [Cornell Univ., Ithaca, NY (United States)

    2010-05-01

    The final technical report for DOE grant DE-SC0004079 is presented. The goal of the grant was to perform research, development and application of novel imaging x-ray detectors so as to effectively utilize the high intensity and brightness of the national synchrotron radiation facilities to enable previously unfeasible time-resolved x-ray research. The report summarizes the development of the resultant imaging x-ray detectors. Two types of detector platforms were developed: The first is a detector platform (called a Mixed-Mode Pixel Array Detector, or MM-PAD) that can image continuously at over a thousand images per second while maintaining high efficiency for wide dynamic range signals ranging from 1 to hundreds of millions of x-rays per pixel per image. Research on an even higher dynamic range variant is also described. The second detector platform (called the Keck Pixel Array Detector) is capable of acquiring a burst of x-ray images at a rate of millions of images per second.

  9. Apparatus development for high-pressure X-ray diffraction using synchrotron radiation

    International Nuclear Information System (INIS)

    Martinez, L.G.; Orlando, M.T.D.; Rossi, J.L.; Passamai Junior, J.L.; Melo, F.C.L.; Ferreira, F.F.

    2006-01-01

    Some phenomena in the field of condensed matter physics can be studied when the matter is submitted to extreme conditions of pressure, magnetic fields or temperatures. Once submitted to these conditions it is generally necessary to measure the properties of the matter in situ. The existence of a synchrotron light laboratory in Brazil opens up the chance of studying materials in extreme conditions by techniques like X-ray diffraction and absorption. However, when compared to high-energy synchrotrons accelerators, the Brazilian source offers a narrower energy range and lower flux. These facts impose limitation to perform diffraction experiments by energy dispersion and, consequently, the use of pressure cells with denser anvils like diamond. However, for a lower-pressure range, preliminary studies showed the viability of measurements in an angular dispersion configuration. This allows the use of silicon carbide anvils B 4C . In this work it is described the development of a hydrostatic pressure cell suitable for X-rays diffraction measurements in the Brazilian Synchrotron Light Laboratory using materials and technologies developed by the institutions and researchers involved in this project (IPEN, UFES, CTA and LNLS). This development can provide the scientific community with the possibility of performing X-ray diffraction measurements under hydrostatic pressure, initially up to 2 GPa, with possibilities of increasing the maximum pressure to higher values, with or without application of magnetic fields and high or low temperatures. (author)

  10. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines.

    Science.gov (United States)

    Alcock, Simon G; Nistea, Ioana; Sutter, John P; Sawhney, Kawal; Fermé, Jean Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼ 0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts.

  11. A hard X-ray scanning microprobe for fluorescence imaging and microdiffraction at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Cai, L.; Lai, B.; Yun, W.; Ilinski, P.; Legnini, D.; Maser, J.; Rodrigues, W.

    1999-01-01

    A hard x-ray scanning microprobe based on zone plate optics and undulator radiation, in the energy region from 6 to 20 keV, has reached a focal spot size (FWHM) of 0.15 microm (v) x 0.6 microm (h), and a photon flux of 4 x 10 9 photons/sec/0.01%BW. Using a slit 44 meters upstream to create a virtual source, a circular beam spot of 0.15 microm in diameter can be obtained with a photon flux of one order of magnitude less. During fluorescence mapping of trace elements in a single human ovarian cell, the microprobe exhibited an imaging sensitivity for Pt (L a line) of 80 attograms/microm 2 for a count rate of 10 counts per second. The x-ray microprobe has been used to map crystallographic strain and multiquantum well thickness in micro-optoelectronic devices produced with the selective area growth technique

  12. Use of a synchrotron radiation x-ray microprobe for elemental analysis at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Gordon, B.M.

    1980-01-01

    The National Synchrotron Light Source (NSLS) is a facility consisting of a 700 MeV and a 2.5 GeV electron storage ring and dedicated to providing synchrotron radiation in the energy range from the vacuum ultraviolet to high energy x rays. Some of the properties of synchrotron radiation that contribute to its usefulness for x-ray fluorescence are: a continuous, tunable energy spectrum, strong collimation in the horizontal plane, high polarization in the storage ring plane, and relatively low energy deposition. The highest priority is for the development of an x-ray microprobe beam line capable of trace analysis in the parts per million range with spatial resolution as low as one micrometer. An eventual capability for bulk sample analysis is also planned with sensitivities in the more favorable cases beings low as 50 parts per billion in dry biological tissue. The microprobe technique has application to a variety of fields including the geological, medical, materials and environmental sciences. Examples of investigations include multielemental trace analysis across grain boundaries for the study of diffusion and cooling processes in geological and materials sciences samples; in leukocytes and other types of individual cells for studying the relationship between trace element concentrations and disease or nutrition; and in individual particles in air pollution samples

  13. High-speed X-ray imaging pixel array detector for synchrotron bunch isolation

    International Nuclear Information System (INIS)

    Philipp, Hugh T.; Tate, Mark W.; Purohit, Prafull; Shanks, Katherine S.; Weiss, Joel T.; Gruner, Sol M.

    2016-01-01

    A high-speed pixel array detector for time-resolved X-ray imaging at synchrotrons has been developed. The ability to isolate single synchrotron bunches makes it ideal for time-resolved dynamical studies. A wide-dynamic-range imaging X-ray detector designed for recording successive frames at rates up to 10 MHz is described. X-ray imaging with frame rates of up to 6.5 MHz have been experimentally verified. The pixel design allows for up to 8–12 frames to be stored internally at high speed before readout, which occurs at a 1 kHz frame rate. An additional mode of operation allows the integration capacitors to be re-addressed repeatedly before readout which can enhance the signal-to-noise ratio of cyclical processes. This detector, along with modern storage ring sources which provide short (10–100 ps) and intense X-ray pulses at megahertz rates, opens new avenues for the study of rapid structural changes in materials. The detector consists of hybridized modules, each of which is comprised of a 500 µm-thick silicon X-ray sensor solder bump-bonded, pixel by pixel, to an application-specific integrated circuit. The format of each module is 128 × 128 pixels with a pixel pitch of 150 µm. In the prototype detector described here, the three-side buttable modules are tiled in a 3 × 2 array with a full format of 256 × 384 pixels. The characteristics, operation, testing and application of the detector are detailed

  14. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources.

    Science.gov (United States)

    Rutherford, Michael E; Chapman, David J; White, Thomas G; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E

    2016-05-01

    The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits).

  15. A hard x-ray scanning microprobe for fluorescence imaging and microdiffraction at the Advanced Photon Source

    Energy Technology Data Exchange (ETDEWEB)

    Cai, L.; Lai, B.; Yun, W.; Ilinski, P.; Legnini, D.; Maser, J.; Rodrigues, W.

    1999-11-02

    A hard x-ray scanning microprobe based on zone plate optics and undulator radiation, in the energy region from 6 to 20 keV, has reached a focal spot size (FWHM) of 0.15 {micro}m (v) x 0.6 {micro}m (h), and a photon flux of 4 x 10{sup 9} photons/sec/0.01%BW. Using a slit 44 meters upstream to create a virtual source, a circular beam spot of 0.15 {micro}m in diameter can be obtained with a photon flux of one order of magnitude less. During fluorescence mapping of trace elements in a single human ovarian cell, the microprobe exhibited an imaging sensitivity for Pt (L{sub a} line) of 80 attograms/{micro}m{sup 2} for a count rate of 10 counts per second. The x-ray microprobe has been used to map crystallographic strain and multiquantum well thickness in micro-optoelectronic devices produced with the selective area growth technique.

  16. Effects of synchrotron radiation spectrum energy on polymethyl methacrylate photosensitivity to deep x-ray lithography

    CERN Document Server

    Mekaru, H; Hattori, T

    2003-01-01

    Since X-ray lithography requires a high photon flux to achieve deep resist exposure, a synchrotron radiation beam, which is not monochromatized, is generally used as a light source. If the synchrotron radiation beam is monochromatized, photon flux will decrease rapidly. Because of this reason, the wavelength dependence of the resist sensitivity has not been investigated for deep X-ray lithography. Measuring the spectrum of a white beam with a Si solid-state detector (SSD) is difficult because a white beam has a high intensity and an SSD has a high sensitivity. We were able to measure the spectrum and the photocurrent of a white beam from a beam line used for deep X-ray lithography by keeping the ring current below 0.05 mA. We evaluated the characteristics of the output beam based on the measured spectrum and photocurrent, and used them to investigate the relationship between the total exposure energy and the dose-processing depth with polymethyl methacrylate (PMMA). We found that it is possible to guess the p...

  17. Conical geometry for sagittal focusing as applied to X rays from synchrotrons

    International Nuclear Information System (INIS)

    Ice, G.E.; Sparks, C.J.

    1993-06-01

    The authors describe a method for simultaneously focusing and monochromatization of X rays from a fan of radiation having up to 15 mrad divergence in one dimension. This geometry is well suited to synchrotron radiation sources at magnifications of one-fifth to two and is efficient for X-ray energies between 3 and 40 keV (0.48 and 6.4 fJ). The method uses crystals bent to part of a cone for sagittal focusing and allows for the collection of a larger divergence with less mixing of the horizontal into the vertical divergence than is possible with X-ray mirrors. They describe the geometry required to achieve the highest efficiency when a conical crystal follows a flat crystal in a nondispersive two-crystal monochromator. At a magnification of one-third, the geometry is identical to a cylindrical focusing design described previously. A simple theoretical calculation is shown to agree well with ray-tracing results. Minimum aberrations are observed at magnifications near one. Applications of the conical focusing geometry to existing and future synchrotron radiation facilities are discussed

  18. Heat transfer issues in high-heat-load synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Mills, D.M.

    1994-09-01

    In this paper, a short description of the synchrotron radiation x-ray sources and the associated power loads is given, followed by a brief description of typical synchrotron components and their heat load. It is emphasized that the design goals for most of these components is to limit (a) temperature, (b) stresses, or (c) strains in the system. Each design calls for a different geometry, material selection, and cooling scheme. Cooling schemes that have been utilized so far are primarily single phase and include simple macrochannel cooling, microchannel cooling, contact cooling, pin-post cooling, porous-flow cooling, jet cooling, etc. Water, liquid metals, and various cryogenic coolants have been used. Because the trend in x-ray beam development is towards brighter (i.e., more powerful) beams and assuming that no radical changes in the design of x-ray generating machines occurs in the next few years, it is fair to state that the utilization of various effective cooling schemes and, in particular, two-phase flow (e.g., subcooled boiling) warrants further investigation. This, however, requires a thorough examination of stability and reliability of two-phase flows for high-heat-flux components operating in ultrahigh vacuum with stringent reliability requirements

  19. Diffraction measurements of residual macrostress and microstress using x-rays, synchrotron and neutrons

    International Nuclear Information System (INIS)

    Tanaka, Keisuke; Akiniwa, Yoshiaki

    2004-01-01

    The present paper reviews some recent developments of the measurements of the macrostress and microstress by diffraction using X-rays, synchrotron and neutrons especially in Japan. These three methods are based on the same principle of the diffraction of crystals, and have different advantages. The conventional X-rays detect the stress very near the surface, while the neutron diffraction takes the stress in the interior of the materials. High-energy X-rays from synchrotron sources have the penetration depth in between and are suitable for the measurement of subsurface stresses. After describing the developments of the fundamentals of the methods, the paper covers the recent applications of the diffraction methods to the residual stress analysis in textured thin films, the nondestructive determination of the subsurface distribution of residual stress in shot-peened materials, local stress measurements near the crack tip, the stress measurements of single crystals, macrostress and microstress measurements in composites, and the determination of the internal distribution of the residual stress in welded joints. (author)

  20. Synthesis of nanoparticles through x-ray radiolysis using synchrotron radiation

    Science.gov (United States)

    Yamaguchi, A.; Okada, I.; Fukuoka, T.; Ishihara, M.; Sakurai, I.; Utsumi, Y.

    2016-09-01

    The synthesis and deposition of nanoparticles consisting of Cu and Au in a CuSO4 solution with some kinds of alcohol and electroplating solution containing gold (I) trisodium disulphite under synchrotron X-ray radiation was investigated. The functional group of alcohol plays an important in nucleation, growth and aggregation process of copper and cupric oxide particles. We found that the laboratory X-ray source also enables us to synthesize the NPs from the metallic solution. As increasing X-ray exposure time, the full length at half width of particle size distribution is broader and higher-order nanostructure containing NPs clusters is formed. The surface-enhanced Raman scattering (SERS) of 4, 4'-bipyridine (4bpy) in aqueous solution was measured using higher-order nanostructure immobilized on silicon substrates under systematically-varied X-ray exposure. This demonstration provide a clue to develop a three-dimensional printing and sensor for environmental analyses and molecular detection through simple SERS measurements.

  1. X-ray absorption spectroscopy investigations on radioactive matter using MARS beamline at SOLEIL synchrotron

    Energy Technology Data Exchange (ETDEWEB)

    Llorens, Isabelle; Solari, Pier Lorenzo; Sitaud, Bruno [Synchrotron SOLEIL - l' Orme des Merisiers Saint Aubin, Gif-sur-Yvette (France); and others

    2014-07-01

    The MARS beamline at the SOLEIL synchrotron is dedicated to the characterization of radioactive material samples. One great advantage of the beamline is the possibility to characterize about 380 radionuclides by different X-ray techniques in the same place. This facility is unique in Europe. A wide energy range from around 3.5 keV to 36 keV K-edges from K to Cs, and L3 edges from Cd to Am and beyond can be used. The MARS beamline is optimized for X-ray absorption spectroscopy techniques (XANES/EXAFS), powder diffraction (XRD) but X-ray fluorescence (XRF) analysis, High Energy Resolution Fluorescence Detected-XAS (HERFD-XAS), X-ray Emission (XES) and μ-XAS/XRD are also possible. A description of the beamline as well as its performances are given in a first part. Then some scientific examples of XAS studies from users are presented which cover a wide variety of topics in radiochemistry and nuclear materials.

  2. Time resolved X-ray micro-diffraction measurements of the dynamic local layer response to electric field in antiferroelectric liquid crystals

    CERN Document Server

    Takahashi, Y; Takanishi, Y; Ogasawara, T; Takezoe, H

    2001-01-01

    The time-resolved synchrotron X-ray microbeam diffraction experiment has been carried out to reveal the local layer response to the electric field in the antiferroelectric liquid crystal. The X-ray microbeam of a few mu m spatial resolution was obtained with Kirkpatrick-Baez optics. The time-resolved small angle diffraction experiment was performed with a time resolution ranging from 10 mu s to a few ms. The reversible local layer change between the horizontal chevron and the quasi-bookshelf structure was confirmed by the triangular wave form. The transient layer response for the step form electric field was observed. The layer response closely related with an electric field induced antiferroelectric to ferroelectric phase transition.

  3. Small area analysis using micro-diffraction techniques

    International Nuclear Information System (INIS)

    Goehner, Raymond P.; Tissot, Ralph G. Jr.; Michael, Joseph R.

    2000-01-01

    An overall trend toward smaller electronic packages and devices makes it increasingly important and difficult to obtain meaningful diffraction information from small areas. X-ray micro-diffraction, electron back-scattered diffraction (EBSD) and Kossel are micro-diffraction techniques used for crystallographic analysis including texture, phase identification and strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements of areas between 10 microm to 100 microm. For areas this small glass capillary optics are used for producing a usable collimated x-ray beam. These optics are designed to reflect x-rays below the critical angle therefore allowing for larger solid acceptance angle at the x-ray source resulting in brighter smaller x-ray beams. The determination of residual strain using micro-diffraction techniques is very important to the semiconductor industry. Residual stresses have caused voiding of the interconnect metal which then destroys electrical continuity. Being able to determine the residual stress helps industry to predict failures from the aging effects of interconnects due to this stress voiding. Stress measurements would be impossible using a conventional x-ray diffractometer; however, utilizing a 30 microm glass capillary these small areas are readily assessable for analysis. Kossel produces a wide angle diffraction pattern from fluorescent x-rays generated in the sample by an e-beam in a SEM. This technique can yield very precise lattice parameters for determining strain. Fig. 2 shows a Kossel pattern from a Ni specimen. Phase analysis on small areas is also possible using an energy dispersive spectrometer (EBSD) and x-ray micro-diffraction techniques. EBSD has the advantage of allowing the user to observe the area of interest using the excellent imaging capabilities of the SEM. An EDS detector has been

  4. Development of confocal X-ray fluorescence (XRF) microscopy at the Cornell high energy synchrotron source

    International Nuclear Information System (INIS)

    Woll, A.R.; Huang, R.; Mass, J.; Bisulca, C.; Bilderback, D.H.; Gruner, S.; Gao, N.

    2006-01-01

    A confocal X-ray fluorescence microscope was built at the Cornell High Energy Synchrotron Source (CHESS) to obtain compositional depth profiles of historic paintings. The microscope consists of a single-bounce, borosilicate monocapillary optic to focus the incident beam onto the painting and a commercial borosilicate polycapillary lens to collect the fluorescent X-rays. The resolution of the microscope was measured by scanning a variety of thin metal films through this confocal volume while monitoring the fluorescence signal. The capabilities of the technique were then probed using test paint microstructures with up to four distinct layers, each having a thickness in the range of 10-80 microns. Results from confocal XRF were compared with those from stand-alone XRF and visible light microscopy of the paint cross-sections. A large area, high-resolution scanner is currently being built to perform 3D scans on moderately sized paintings. (orig.)

  5. Source assemblage types for cratonic diamonds from X-ray synchrotron diffraction

    Science.gov (United States)

    Nestola, F.; Alvaro, M.; Casati, M. N.; Wilhelm, H.; Kleppe, A. K.; Jephcoat, A. P.; Domeneghetti, M. C.; Harris, J. W.

    2016-11-01

    Three single crystals of clinopyroxene trapped within three different gem-quality diamonds from the Udachnaya kimberlite (Siberia, Russia) were analysed in situ by single-crystal synchrotron X-ray diffraction in order to obtain information on their chemical composition and infer source assemblage type. A non-destructive approach was used with high-energy (≈ 60 keV; λ ≈ 0.206 Å) at I15, the extreme-conditions beamline at Diamond Light Source. A dedicated protocol was used to center the mineral inclusions located deep inside the diamonds in the X-ray beam. Our results reveal that two of the inclusions can be associated with peridotitic paragenesis whereas the third is eclogitic. This study also demonstrates that this non-destructive experimental approach is extremely efficient in evaluating the origin of minerals trapped in their diamond hosts.

  6. Synchrotron hard X-ray imaging of shock-compressed metal powders

    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 poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  7. Metals determination in wood treated by synchrotron radiation X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Silva, Richard Maximiliano da Cunha [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil)]. E-mail: maxcunha@cena.usp.br; Medeiros, Jean Gabriel da Silva; Tomazello Filho, Mario [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]. E-mail: jeangm@esalq.usp.br; mtomazel@esalq.usp.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Barroso, Regina Cely [Universidade do Estado, Rio de Janeiro, RJ (Brazil)]. E-mail: cely@uerj.br

    2005-07-01

    The paper describes the use of X-Ray fluorescence analysis for distribution and quantification of metals in the hardwood (Eucalyptus sp) and softwood (Pinus sp) treated with CCA (copper-chromium-arsenic). The sapwood/heartwood for hardwood sample and the growth-rings for softwood sample were analyzed. The samples were scanned in 320 mm steps in the vertical direction. For excitation of the elements a white beam synchrotron radiation of {approx} 320 x 180 mm was employed and for the X-ray detection a Si(Li) semiconductor detector. The elements K, Ca, Cr, Mn, Cu, Zn and As were determined. Fundamental parameters were used to quantify the elements concentrations. (author)

  8. Metals determination in wood treated by synchrotron radiation X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Vives, Ana Elisa Sirito de; Medeiros, Jean Gabriel da Silva; Tomazello Filho, Mario

    2005-01-01

    The paper describes the use of X-Ray fluorescence analysis for distribution and quantification of metals in the hardwood (Eucalyptus sp) and softwood (Pinus sp) treated with CCA (copper-chromium-arsenic). The sapwood/heartwood for hardwood sample and the growth-rings for softwood sample were analyzed. The samples were scanned in 320 mm steps in the vertical direction. For excitation of the elements a white beam synchrotron radiation of ∼ 320 x 180 mm was employed and for the X-ray detection a Si(Li) semiconductor detector. The elements K, Ca, Cr, Mn, Cu, Zn and As were determined. Fundamental parameters were used to quantify the elements concentrations. (author)

  9. High-resolution X-ray scattering topography using synchrotron radiation microbeam

    International Nuclear Information System (INIS)

    Chikaura, Yoshinori; Suzuki, Yoshifumi; Kii, Hideki

    1994-01-01

    Although spatial resolution is the most essential factor determining the function of X-ray topography, it has not been improved in 30 years in spite of increasing requirements for highly-resolvable topography in materials science. X-ray scattering topography using a microbeam is a method capable of overcoming this resolution problem. Because the maximum resolution of an apparatus using a sealed-off tube is limited to 20μm, we designed and constructed scattering topography equipment using a synchrotron radiation microbeam. In the experiment, the slit system forms the microbeam 7 μm in diameter. We observed a cellulose distribution in bamboo as a testing material. When the scanning step was 2 μm, we attained spatial resolution less than 5 μm. (author)

  10. Optics for protein microcrystallography using synchrotron and laboratory X-ray sources

    International Nuclear Information System (INIS)

    Varghese, J.N.; Van Donkelaar, A.; Balaic, D.X.; Barnea, Z.

    2000-01-01

    Full text: For protein crystallography, a highly-intense focused beam overcomes a serious constraint in current biological research: the inability of many protein molecules to form crystals larger than a few tens of microns in size. High structure-resolution X-ray diffraction analysis of microcrystals is currently only being studied at synchrotron X-ray sources. We shall examine how this is being carried out, and also report the development of a novel tapered glass monocapillary toroidal-mirror optic, which achieves a high-intensity, low-divergence focused beam from a rotating-anode Xray generator. We have used this optic, which demonstrates an ∼28x intensity gain at the beam focus to solve the structure of a plant exoglucanse/inhibtor complex microcrystal to 2.8 Angstroms, with volume equivalent to a 30-micron-edge cube

  11. X-rays from synchrotron: A new challenge for neutron scattering

    International Nuclear Information System (INIS)

    Shirane, G.

    1983-01-01

    A brief review is given of current developments in X-ray scattering techniques at synchrotron radiation facilities. Highly collimated, intense sources of white radiation open up new areas of research in condensed matter physics and challenge the traditional domains of neutron scattering. These include energy dispersive scattering, the use of anomalous dispersion, magnetic diffraction and direct energy analysis by backscattering. The relative merits of X-ray and neutron scattering techniques will be discussed. The unique advantage of neutron scattering is the capability of performing polarization analysis. We will discuss in some detail the current developments at Brookhaven inelastic scattering of polarized neutrons. In addition, we will also discuss special technical problems associated with the search for phasons utilizing a high-resolution triple axis spectrometer. (orig.)

  12. Nanostructure of protective rust layer on weathering steel examined using synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Yamashita, Masato; Uchida, Hitoshi; Konishi, Hiroyuki; Mizuki, Jun'ichiro

    2004-01-01

    The X-ray absorption fine structure (XAFS) spectrum of pure goethite around the Fe K absorption edge and that of the protective rust layer formed on weathering steel exposed for 17 years in an atmospheric environment around the Cr K edge, have been examined using synchrotron radiation X-rays. It was found that the rust layer on the weathering steel mainly consisted of Cr-goethite. By examining the fine structure at the Cr K edge and the Fe K edge, we concluded that Cr 3+ in the rust layer is coordinated with O 2- and is positioned in the double chains of vacant sites in the network of FeO 3 (OH) 3 octahedra in the goethite crystal. This Cr 3+ site indicates that the protective effect of the rust layer is due to the dense aggregation of fine crystals of Cr-goethite with cation selectivity. (author)

  13. Low energy X-ray grating interferometry at the Brazilian Synchrotron

    Science.gov (United States)

    Koch, F. J.; O'Dowd, F. P.; Cardoso, M. B.; Da Silva, R. R.; Cavicchioli, M.; Ribeiro, S. J. L.; Schröter, T. J.; Faisal, A.; Meyer, P.; Kunka, D.; Mohr, J.

    2017-06-01

    Grating based X-ray differential phase contrast imaging has found a large variety of applications in the last decade. Different types of samples call for different imaging energies, and efforts have been made to establish the technique all over the spectrum used for conventional X-ray imaging. Here we present a two-grating interferometer working at 8.3 keV, implemented at the bending magnet source of the IMX beamline of the Brazilian Synchrotron Light Laboratory. The low design energy is made possible by gratings fabricated on polymer substrates, and makes the interferometer mainly suited to the investigation of light and thin samples. We investigate polymer microspheres filled with Fe2O3 nanoparticles, and find that these particles give rise to a significant visibility reduction due to small angle scattering.

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

    Science.gov (United States)

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

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

  15. CCD-based detector for protein crystallography with synchrotron X-rays

    International Nuclear Information System (INIS)

    Strauss, M.G.; Westbrook, E.M.; Naday, I.; Coleman, T.A.; Westbrook, M.L.; Travis, D.J.; Sweet, R.M.; Pflugrath, J.W.; Stanton, M.

    1990-01-01

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 10 9 X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensity, and focus the image onto a CCD having 512x512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of 4x4 pixel resolution element, comparable in size to a diffraction peak, was 10 4 . The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 μm on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1deg frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1deg frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a=275 A) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources. (orig.)

  16. CCD-based detector for protein crystallography with synchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Strauss, M.G.; Westbrook, E.M.; Naday, I.; Coleman, T.A.; Westbrook, M.L.; Travis, D.J. (Argonne National Lab., IL (USA)); Sweet, R.M. (Brookhaven National Lab., Upton, NY (USA)); Pflugrath, J.W. (Cold Spring Harbor Lab., NY (USA)); Stanton, M. (Brandeis Univ., Waltham, MA (USA))

    1990-11-15

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 10{sup 9} X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensity, and focus the image onto a CCD having 512x512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of 4x4 pixel resolution element, comparable in size to a diffraction peak, was 10{sup 4}. The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 {mu}m on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1deg frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1deg frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a=275 A) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources. (orig.).

  17. CCD-based detector for protein crystallography with synchrotron X-rays

    Science.gov (United States)

    Strauss, M. G.; Westbrook, E. M.; Naday, I.; Coleman, T. A.; Westbrook, M. L.; Travis, D. J.; Sweet, R. M.; Pflugrath, J. W.; Stanton, M.

    1990-11-01

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 109 X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensify, and focus the image onto a CCD having 512×512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of a 4×4 pixel resolution element, comparable in size to a diffraction peak, was 104. The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 μm on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1° frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1° frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a = 275 Å) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources.

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

    International Nuclear Information System (INIS)

    Gentle, I.

    2002-01-01

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

  19. DOE/DMS workshop on future synchrotron VUV and x-ray beam Lines

    International Nuclear Information System (INIS)

    Green, P.H.

    1992-03-01

    This document contains an overview of the participating DOE Laboratory beam line interests and the projected science to be addressed on these beam lines, both at new and existing synchrotron facilities. The scientific programs associated with present and planned synchrotron research by DOE Laboratories are discussed in chapters titled ''VUV and Soft X-Ray Research'' and ''Hard X-Ray Research.'' This research encompasses a broad range of the nation's scientific and technical research needs from fundamental to applied, in areas including environmental, biological, and physical sciences; new materials; and energy-related technologies. The projected cost of this proposed construction has been provided in tabular form using a uniform format so that anticipated DOE and outside funding agency contributions for construction and for research and development can be determined. The cost figures are, of course, subject to uncertainties of detailed design requirements and the availability of facility-designed generic components and outside vendors. The report also contains a compendium (as submitted by the beam line proposers) of the design capabilities, the anticipated costs, and the scientific programs of projected beam line construction at the four synchrotron facilities. A summary of the projected cost of these beam lines to be requested of DOE is compiled

  20. X-ray beam splitting design for concurrent imaging at hard X-ray FELs and synchrotron facilities

    Czech Academy of Sciences Publication Activity Database

    Oberta, Peter; Mokso, R.

    2013-01-01

    Roč. 729, NOV (2013), s. 85-89 ISSN 0168-9002 R&D Projects: GA MPO FR-TI1/412 Institutional research plan: CEZ:AV0Z10100522 Keywords : diffractive-refractive optics * hard X-ray FEL * X-ray imaging Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.316, year: 2013 http://www.sciencedirect.com/science/article/pii/S0168900213009613

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

    Science.gov (United States)

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

    2016-04-01

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

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

    Science.gov (United States)

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

    2007-10-15

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

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

    Science.gov (United States)

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

    2010-09-01

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

  4. Microscopy and elemental analysis in tissue samples using computed microtomography with synchrotron x-rays

    International Nuclear Information System (INIS)

    Spanne, P.; Rivers, M.L.

    1988-01-01

    The initial development shows that CMT using synchrotron x-rays can be developed to μm spatial resolution and perhaps even better. This creates a new microscopy technique which is of special interest in morphological studies of tissues, since no chemical preparation or slicing of the sample is necessary. The combination of CMT with spatial resolution in the μm range and elemental mapping with sensitivity in the ppM range results in a new tool for elemental mapping at the cellular level. 7 refs., 1 fig

  5. Raphide crystal structure in agave tequilana determined by x-ray originating from synchrotron radiation

    International Nuclear Information System (INIS)

    Tadokoro, Makoto; Ozawa, Yoshiki; Mitsumi, Minoru; Toriumi, Kohshiro; Ogura, Tetsuya

    2005-01-01

    The first single crystal structure of small natural raphides in an agave plant is completely determined using an intense X-ray originating from a synchrotron radiation. The SEM image shows that the tip of the crystal is approximately hundreds of nanometer in width sharply grow to stick to the tissue of herbivorous vermin. Furthermore, the crystal develops cracks that propagate at an inclination of approximately 45deg towards the direction of crystal growth such that the crystal easily splits into small pieces in the tissue. (author)

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

    Science.gov (United States)

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

    2016-03-01

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

  7. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    Energy Technology Data Exchange (ETDEWEB)

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

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

    Science.gov (United States)

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

    2014-04-01

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  9. Non-destructive synchrotron X-ray diffraction mapping of a Roman painting

    International Nuclear Information System (INIS)

    Dooryhee, E.; Anne, M.; Hodeau, J.-L.; Martinetto, P.; Rondot, S.; Bardies, I.; Salomon, J.; Walter, P.; Vaughan, G.B.M.

    2005-01-01

    The history and the properties of materials are deduced not only from their elemental and molecular signatures, but also from their exact phase compositions, and from the structures and the defects of their constituents. Here we implement a non-destructive synchrotron X-ray based method, which combines both the quantitative structural content of diffraction and the imaging mode. As a demonstration case, the pigments of a Roman wall painting are examined. The joined elemental and mineral maps mimic the major features of the painting. Different structural phases made of common atomic elements are differentiated. Textures and graininess are measured and related to the artist's know-how. (orig.)

  10. X-ray photoelectron spectroscopy study of synchrotron radiation irradiation of a polytetrafluoroethylene surface

    CERN Document Server

    Haruyama, Y; Matsui, S; Ideta, T; Ishigaki, H

    2003-01-01

    The effect of synchrotron radiation (SR) irradiation of a polytetrafluoroethylene (PTFE) surface was investigated using X-ray photoelectron spectroscopy (XPS). After the SR irradiation, the relative intensity of the F ls peak to the C ls peak decreased markedly. The chemical composition ratio to the F atoms to C atoms was estimated to be 0.29. From the curve fitting analysis of C ls and F ls XPS spectra, the chemical components and their intensity ratio were determined. The reason for the chemical composition change by the SR irradiation was discussed. (author)

  11. Electron multiplier as a detector for soft x rays from synchrotron and laser plasma sources

    Science.gov (United States)

    Buckley, Christopher J.; Dermody, Geraint; Khaleque, Naz I.; Michette, Alan G.; Pfauntsch, Slawka J.; Turcu, I. C. Edmond; Allott, Ric M.

    1998-11-01

    An electron-tubes-LTD 129EM electron multiplier tube has been modified to act as a detector of soft x-rays. the first dynode was coated with 100 nm of CsI and the assembly was mounted in a small vacuum chamber with 100 nm thick silicon nitride entrance window. Initial tests show the detector is linear up to an input flux of approximately 1MHz on a synchrotron source and has proved effective in providing pulse height discrimination when used on a pulsed laser plasma source.

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

    Energy Technology Data Exchange (ETDEWEB)

    Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in; Singh, A. K., E-mail: mktiwari@rrcat.gov.in; Das, Gangadhar, E-mail: mktiwari@rrcat.gov.in; Chowdhury, Anupam, E-mail: mktiwari@rrcat.gov.in; Lodha, G. S., E-mail: mktiwari@rrcat.gov.in [Indus Synchrotrons Utilisation Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India)

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  13. Total and available metal contents in sediments by synchrotron radiation total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Sobrinho, Gilmar A. [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fecf.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), SP (Brazil); Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia

    2002-07-01

    In this work the total and available contents of Al, Si, Cl, K, Mn, Fe, Co, Ni, Cu, Zn, Sr, Zr, Ba, Ce and Pb in sediments from river Atibaia were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence technique. The detection limits for K series varies from 200 ng.mL{sup -1} for Al to 2 ng.mL{sup -1} for Zn while for L series the value varies from 20 ng.mL{sup -1} for Ba to 10 ng.mL{sup -1} for Pb. The samples were submitted to two different processes, in order to obtain the total and biological available metal contents. The information about metal content is a important parameter for a correct evaluation about the hydrologic cycle in Piracicaba basin. All the measure were carried out at the National Synchrotron Light Laboratory, Campinas, SP, Brazil, using a white beam for excitation. (author)

  14. Extending the possibilities in phase space analysis of synchrotron radiation x-ray optics.

    Science.gov (United States)

    Ferrero, Claudio; Smilgies, Detlef-Matthias; Riekel, Christian; Gatta, Gilles; Daly, Peter

    2008-08-01

    A simple analytical approach to phase space analysis of the performance of x-ray optical setups (beamlines) combining several elements in position-angle-wavelength space is presented. The mathematical description of a large class of optical elements commonly used on synchrotron beamlines has been reviewed and extended with respect to the existing literature and is reported in a revised form. Novel features are introduced, in particular, the possibility to account for imperfections on mirror surfaces and to incorporate nanofocusing devices like refractive lenses in advanced beamline setups using the same analytical framework. Phase space analysis results of the simulation of an undulator beamline with focusing optics at the European Synchrotron Radiation Facility compare favorably with results obtained by geometric ray-tracing methods and, more importantly, with experimental measurements. This approach has been implemented into a simple and easy-to-use program toolkit for optical calculations based on the Mathematica software package.

  15. Investigation of mineral distribution in bone by synchrotron X-ray fluorescence microscopy after tibolone therapy

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Rio de Janeiro State Univ., Nova Friburgo, RJ (Brazil). Dept. of Mechanical Engineering and Energy; Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Carvalho, A.C.B.; Henriques, H.N.; Guzman-Silva, M.A. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Lab. of Experimental Pathology; Sales, E.; Lopes, R.T. [Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Granjeiro, J.M. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Dept. of Cellular and Molecular Biology

    2011-07-01

    Tibolone is a synthetic steroid with estrogenic, androgenic, and progestagenic properties used for the prevention of postmenopausal osteoporosis and treatment of climacteric symptoms. Tibolone shows almost no action on breast and endometrium, which are target-organs for estrogens and progesterone activity. The aim of this work was to investigate the spatial distribution of calcium and zinc minerals in the femoral head of ovariectomized rat in order to evaluate the effects of the long-term administration of tibolone. For that purpose X-ray microfluorescence was used with synchrotron radiation imaging technique which was performed at Brazilian Light Synchrotron Laboratory, Campinas, SP. Minerals were not homogeneously distributed in trabecular bone areas; a higher concentration of calcium in the trabecular regions at femoral heads was found in ovariectomized and tibolone-treated rats compared to ovariectomized and control groups. (orig.)

  16. Multielemental analysis in Brazilian cigarettes using total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T.; Moreira, Silvana

    2005-01-01

    In order to identify major and trace elements in conventional and light Brazilian cigarettes, Total Reflection X-Ray Fluorescence with Synchrotron Radiation (SR-TXRF) was used. The fluorescence measurements were carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo. This technique enables detection limit is in the ngg -1 range, which is very useful in elemental tobacco smoke analysis, since it presents most of its elements at a trace level. The major elements identified in tobacco samples were: S, Cl, K, Ca, Mn, Fe and Cd, and the trace elements were: Ti, Cr, Ni, Cu, Zn, Br, Rb, Sr and Ba. However in tobacco smoke samples, there were only two major elements: K and Ca, the others were present a trace level. The rate transfer of tobacco to tobacco smoke was about 2.5 % for all elements studied. (author)

  17. Online monitoring the detector calibration process at a synchrotron X-ray source

    Science.gov (United States)

    Li, Huapng; Zhao, Yidong; Zheng, Lei; Tang, Kun; Liu, Shuhu; Zhao, Xiaoliang; Zhao, Yashuai; Li, Fan

    2017-12-01

    This paper describes an online noble gas monitor used for the detector calibration process with a cryogenic radiometer. The process is implemented under a high-flux synchrotron radiation X-ray source in the energy range from 2100 to 6000 eV at the Beijing Synchrotron Radiation Facility (BSRF). This online monitoring system aims to lower the uncertainty of the calibration results caused by electron beam decay in the storage ring during the detector calibration process. Because the calibration process is performed under the high vacuum condition, an ionization chamber with adjustable Kr gas pressure is chosen as the monitoring device. To decrease the electronic noise, a method for obtaining the signal by collecting the counts within a specified time has been applied. Under the properly controlled conditions, the uncertainty of the calibration results introduced by the online monitoring system is estimated to be better than 0.15%, which can meet the demands of various high-precision calibration processes.

  18. Synchrotron radiation based micro X-ray fluorescence analysis of the calibration samples used in surface sensitive total reflection and grazing emission X-ray fluorescence techniques

    Science.gov (United States)

    Kubala-Kukuś, A.; Banaś, D.; Pajek, M.; Szlachetko, J.; Jagodziński, P.; Susini, J.; Salomé, M.

    2013-12-01

    Total reflection X-ray fluorescence (TXRF) and grazing emission X-ray fluorescence (GEXRF) are surface sensitive techniques and can be used for detailed surface studies of different materials, including ultra-low concentration contamination or the lateral and depth distributions of elements. The calibration procedure typically used involves placing a micro-droplet (˜μl) of the standard solution onto a silicon wafer (or quartz backing). After evaporation of the solvent, the residual amount of elements is used as a reference standard. Knowledge of the distribution of residue material on the substrate surface is crucial for precise quantification. In the present work the investigation of the lateral distribution of elements in the multielemental calibrating samples, containing the 23 most commonly studied elements, by using the synchrotron radiation based micro X-ray fluorescence is presented. The goal of this project was the study of a uniformity of the elemental distributions and determination of the residual elements morphology depending on the temperature of the drying process. The X-ray images were compared with optical and SEM images. Paper presents in details the experimental setup, sample preparation procedures, measurements and results. In the analysis of the X-ray images of the sample dried in high temperature the censoring approach was applied improving the quality of statistical analysis. The information on the elements distribution in the calibrating samples can be useful for developing more accurate calibration procedures applied in quantitative analysis of surface sensitive TXRF and GEXRF techniques.

  19. STEADY X-RAY SYNCHROTRON EMISSION IN THE NORTHEASTERN LIMB OF SN 1006

    International Nuclear Information System (INIS)

    Katsuda, Satoru; Petre, Robert; Mori, Koji; Reynolds, Stephen P.; Long, Knox S.; Winkler, P. Frank; Tsunemi, Hiroshi

    2010-01-01

    We investigate time variations and detailed spatial structures of X-ray synchrotron emission in the northeastern limb of SN 1006, using two Chandra observations taken in 2000 and 2008. We extract spectra from a number of small (∼10'') regions. After taking account of proper motion and isolating the synchrotron from the thermal emission, we study time variations in the synchrotron emission in the small regions. We find that there are no regions showing strong flux variations. Our analysis shows an apparent flux decline in the overall synchrotron flux of ∼4% at high energies, but we suspect that this is mostly a calibration effect, and that flux is actually constant to ∼1%. This is much less than the variation found in other remnants where it was used to infer magnetic-field strengths up to 1 mG. We attribute the lack of variability to the smoothness of the synchrotron morphology, in contrast to the small-scale knots found to be variable in other remnants. The smoothness is to be expected for a Type Ia remnant encountering uniform material. Finally, we find a spatial correlation between the flux and the cutoff frequency in synchrotron emission. The simplest interpretation is that the cutoff frequency depends on the magnetic-field strength. This would require that the maximum energy of accelerated electrons is not limited by synchrotron losses, but by some other effect. Alternatively, the rate of particle injection and acceleration may vary due to some effect not yet accounted for, such as a dependence on shock obliquity.

  20. Advancements and Application of Microsecond Synchrotron X-ray Footprinting at the Advanced Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Sayan; Celestre, Rich; Feng, Jun; Ralston, Corie

    2016-01-02

    The method of synchrotron X-ray protein footprinting (XF-MS) is used to determine protein conformational changes, folding, protein-protein and protein-ligand interactions, providing information which is often difficult to obtain using X-ray crystallography and other common structural biology methods [1 G. Xu and M.R. Chance, Chemical Reviews 107, 3514–3543 (2007). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] –3 V.N. Bavro, Biochem Soc Trans 43, 983–994 (2015). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] ]. The technique uses comparative in situ labeling of solvent-accessible side chains by highly reactive hydroxyl radicals (•OH) in buffered aqueous solution under different assay conditions. In regions where a protein is folded or binds a partner, these •OH susceptible sites are inaccessible to solvent, and therefore protected from labeling. The •OH are generated by the ionization of water using high-flux-density X-rays. High-flux density is a key factor for XF-MS labeling because obtaining an adequate steady-state concentration of hydroxyl radical within a short irradiation time is necessary to minimize radiation-induced secondary damage and also to overcome various scavenging reactions that reduce the yield of labeled side chains.

  1. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources

    Energy Technology Data Exchange (ETDEWEB)

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mirian L.A.F.; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (CT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray CT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumba (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based CT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies.

  2. Synchrotron Vacuum Ultraviolet Light and Soft X-Ray Radiation Effects on Aluminized Teflon FEP Investigated

    Science.gov (United States)

    Dever, Joyce A.; Townsend, Jacqueline A.; Gaier, James R.; Jalics, Alice I.

    1999-01-01

    Since the Hubble Space Telescope (HST) was deployed in low Earth orbit in April 1990, two servicing missions have been conducted to upgrade its scientific capabilities. Minor cracking of second-surface metalized Teflon FEP (DuPont; fluorinated ethylene propylene) surfaces from multilayer insulation (MLI) was first observed upon close examination of samples with high solar exposure retrieved during the first servicing mission, which was conducted 3.6 years after deployment. During the second HST servicing mission, 6.8 years after deployment, astronaut observations and photographic documentation revealed significant cracks in the Teflon FEP layer of the MLI on both the solar- and anti-solar-facing surfaces of the telescope. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included identifying the low-Earth-orbit environmental constituent(s) responsible for the cracking and embrittling of Teflon FEP which was observed during the second servicing mission. The NASA Lewis Research Center provided significant support to this effort. Because soft x-ray radiation from solar flares had been considered as a possible cause for the degradation of the mechanical properties of Teflon FEP (ref. 1), the effects of soft xray radiation and vacuum ultraviolet light on Teflon FEP were investigated. In this Lewisled effort, samples of Teflon FEP with a 100-nm layer of vapor-deposited aluminum (VDA) on the backside were exposed to synchrotron radiation of various vacuum ultraviolet and soft x-ray wavelengths between 18 nm (69 eV) and 0.65 nm (1900 eV). Synchrotron radiation exposures were conducted using the National Synchrotron Light Source at Brookhaven National Laboratory. Samples of FEP/VDA were exposed with the FEP surface facing the synchrotron beam. Doses and fluences were compared with those estimated for the 20-yr Hubble Space Telescope mission.

  3. Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

    Science.gov (United States)

    Post, J. E.; Bish, D. L.; Heaney, P. J.

    2006-05-01

    Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase

  4. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    International Nuclear Information System (INIS)

    Wang, Y.; Qun, Y.; Ablett, J.

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  5. Analysis of synchrotron X-ray diffraction patterns from fluorotic enamel samples

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Ana P.G.; Braz, Delson, E-mail: anapaulagalmeida@gmail.co [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Lab. de Instrumentacao Nuclear; Colaco, Marcos V.; Barroso, Regina C., E-mail: cely@uerj.b [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica; Porto, Isabel M., E-mail: belporto@ig.com.b [Universidade Estadual de Campinas (UNICAMP), Piracicaba, SP (Brazil). Faculdade de Odontologia; Gerlach, Raquel F., E-mail: rfgerlach@forp.usp.b [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Odontologia; Droppa Junior, Roosevelt, E-mail: rdroppa@lnls.b [Associacao Brasileira de Tecnologia de Luz Sincrotron (ABTLuS), Campinas, SP (Brazil)

    2009-07-01

    With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basics physical-chemistry reactions of demineralisation and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The hexagonal symmetry seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using technique Synchrotron X-ray diffraction in order to determine the crystal structure and crystallinity of on fluoroapatite (FAp) crystal present in fluoritic enamel. All the scattering profile measurements was carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. (author)

  6. Evaluation of osteoporotic bone structure through synchrotron radiation X-ray microfluorescence images

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)], E-mail: inaya@lin.ufrj.br; Anjos, M.J. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil); Physics Institute, UERJ (Brazil); Farias, M.L.F. [University Hospital, UFRJ (Brazil); Pantaleao, T.U.; Correa da Costa, V.M. [Biophysics Institute, UFRJ (Brazil); Lopes, R.T. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)

    2008-12-15

    The abnormal accumulation or deficiency of trace elements may theoretically impair the formation of bone and contribute to osteoporosis. In this context, the knowledge of major and trace elements is very important in order to clarify many issues regarding diseases of the bone, such as osteoporosis, that remain unresolved. Several kinds of imaging techniques can be useful to access morphology and the minerals present in osteoporotic bones. In this work, synchrotron radiation X-ray microfluorescence was used as an X-ray imaging technique to investigate bone structures. Therefore, this research aims to improve the knowledge about some aspects of bone quality. The measurements were carried out at the Brazilian Synchrotron Laboratory Light Laboratory, in Brazil. A white beam with an energy range of 4-23 keV, a 45 deg./45 deg. geometry and a capillary optics were used. It was demonstrated that bone quality can and must be evaluated not only by considering the architecture of bones but also by taking into account the concentration and the distribution of minerals. Our results showed that the elemental distributions in bone zones on a micron scale were very helpful to understand functions in those structures.

  7. ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

    International Nuclear Information System (INIS)

    Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

    1987-01-01

    A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

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

    Science.gov (United States)

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

    2013-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-12-01

    and stirring rate (shear rate). The X-rays used are from a high intensity synchrotron radiation source, enabling polymorphic phase transformations for a variety of fat mixtures to observed. Copyright (1999) Australian X-ray Analytical Association Inc.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

    and stirring rate (shear rate). The X-rays used are from a high intensity synchrotron radiation source, enabling polymorphic phase transformations for a variety of fat mixtures to observed. Copyright (1999) Australian X-ray Analytical Association Inc

  11. Energy dispersive detector for white beam synchrotron x-ray fluorescence imaging

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Matthew D., E-mail: Matt.Wilson@stfc.ac.uk; Seller, Paul; Veale, Matthew C. [Science and Technology Facilities Council, Rutherford Appleton Laboratory, Harwell Campus,UK (United Kingdom); Connolley, Thomas [Diamond Light Source, I12 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal [Diamond Light Source, B16 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Grant, Patrick S.; Liotti, Enzo; Lui, Andrew [Department of Materials, University of Oxford Parks Road, Oxford (United Kingdom)

    2016-07-27

    A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm{sup 2} with one of the 80×80 pixels imaging an area equivalent to 13µm{sup 2}. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60 s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10µm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1 s timescale.

  12. The study of stress application and corrosion cracking on Ni-16 Cr-9 Fe (Alloy 600) C-ring samples by polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chao, Jing; Fuller, Marina L Suominen; McIntyre, N Stewart; Carcea, Anatolie G; Newman, Roger C; Kunz, Martin; Tamura, Nobumichi [Toronto; (UWO); (LBNL)

    2012-03-27

    Microscopic strains associated with stress corrosion cracks have been investigated in stressed C-rings of Ni-16 Cr-9 Fe (Alloy 600) boiler tubing. Polychromatic X-ray microdiffraction was used to measure deviatoric strain tensors and the distribution of dislocations near cracks that had been propagated in electrochemically accelerated corrosion tests. An associated investigation of the C-ring-induced strains prior to corrosion showed significant tensile strain in the stress axis direction by the torsional closure of the alloy tube section in the C-ring test. Significant grain lattice rotation and pronounced plastic strain at some grain boundaries were noted. Stress-corrosion-cracking-generated intergranular cracks were produced in two Alloy 600 specimens after 6 h and 18 h tests. The diffraction patterns and resultant strain tensors were mapped around the cracked area to a 1 μm spatial resolution. The strain tensor transverse to the crack growth direction showed tensile strain at the intergranular region just ahead of the crack tip for both specimens. Both cracks were found to follow grain boundary pathways that had the lowest angle of misorientation. Dislocation distributions within each grain were qualitatively obtained from the shapes of the diffraction spots and the effect of 'hard' and 'soft' grains on the crack pathway was explored for both 6 h and 18 h specimens. The Schmid factor of one of the grains adjacent to the crack at the 6 h and 18 h initiation sites was found to be the lowest, compared to Schmid factors calculated for surface grains away from the initiation site, and also along the crack path into the bulk.

  13. Optical systems for synchrotron radiation: lecture 4. Soft x-ray imaging systems

    International Nuclear Information System (INIS)

    Howells, M.R.

    1986-04-01

    The history and present techniques of soft x-ray imaging are reviewed briefly. The physics of x-ray imaging is described, including the temporal and spatial coherence of x-ray sources. Particular technologies described are: contact x-ray microscopy, zone plate imaging, scanned image zone plate microscopy, scanned image reflection microscopy, and soft x-ray holography and diffraction

  14. Synchrotron high angular resolution microdiffraction analysis of selective area grown optoelectronic waveguide arrays

    International Nuclear Information System (INIS)

    Kazimirov, A; Sirenko, A A; Bilderback, D H; Cai, Z-H; Lai, B; Huang, R; Ougazzaden, A

    2006-01-01

    A synchrotron microbeam high-angular resolution diffraction setup based on a phase zone plate and a perfect Si(004) analyzer crystal was introduced to generate an x-ray microbeam with a lateral size of 0.24 μm and an angular resolution of 2 arcsec. The microbeam high angular resolution x-ray diffraction was applied to study InGaAlAs-based multiple quantum well (MQW) ridge-waveguide arrays produced by metal-organic vapour-phase epitaxy in a selective area growth regime with a central waveguide width varying from 1.6 to 60 μm. The analysis of the period T and the strain S in MQW ridge structures determined from the high-resolution diffraction data is presented. It was found that the MQW period is uniform across the ridge within the error bar of ΔT = ± 0.25 nm. Within the waveguide array, the MQW period and strain can be adequately described by a gas-phase diffusion model

  15. A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

    Science.gov (United States)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

    Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

  16. A compact dispersive refocusing Rowland circle X-ray emission spectrometer for laboratory, synchrotron, and XFEL applications

    Science.gov (United States)

    Holden, William M.; Hoidn, Oliver R.; Ditter, Alexander S.; Seidler, Gerald T.; Kas, Joshua; Stein, Jennifer L.; Cossairt, Brandi M.; Kozimor, Stosh A.; Guo, Jinghua; Ye, Yifan; Marcus, Matthew A.; Fakra, Sirine

    2017-07-01

    X-ray emission spectroscopy is emerging as an important complement to x-ray absorption fine structure spectroscopy, providing a characterization of the occupied electronic density of states local to the species of interest. Here, we present details of the design and performance of a compact x-ray emission spectrometer that uses a dispersive refocusing Rowland (DRR) circle geometry to achieve excellent performance for the 2-2.5 keV range, i.e., especially for the K-edge emission from sulfur and phosphorous. The DRR approach allows high energy resolution even for unfocused x-ray sources. This property enables high count rates in laboratory studies, approaching those of insertion-device beamlines at third-generation synchrotrons, despite use of only a low-powered, conventional x-ray tube. The spectrometer, whose overall scale is set by use of a 10-cm diameter Rowland circle and a new small-pixel complementary metal-oxide-semiconductor x-ray camera, is easily portable to synchrotron or x-ray free electron laser beamlines. Photometrics from measurements at the Advanced Light Source show excellent overall instrumental efficiency. In addition, the compact size of this instrument lends itself to future multiplexing to gain large factors in net collection efficiency or its implementation in controlled gas gloveboxes either in the lab or in an endstation.

  17. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Menzel, Magnus [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Scharf, Oliver [IfG Institute for Scientific Instruments GmbH, Berlin (Germany); Radtke, Martin; Reinholz, Uwe; Buzanich, Günther [BAM Federal Institute of Materials Research and Testing, Berlin (Germany); Lopez, Velma M.; McIntosh, Kathryn [Los Alamos National Laboratory, Los Alamos, NM (United States); Streli, Christina [Atominstitut, TU Wien, Vienna (Austria); Havrilla, George Joseph [Los Alamos National Laboratory, Los Alamos, NM (United States)

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. - Highlights: • Use of a color X-ray camera and drop on demand printing to diagnose X-ray shading • Specimens were obtained uniform and well-defined in shape and concentration by printing. • Direct visualization and determination of shading in such specimens using the camera.

  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. Maturation stress generation in poplar tension wood studied by synchrotron radiation microdiffraction.

    Science.gov (United States)

    Clair, Bruno; Alméras, Tancrède; Pilate, Gilles; Jullien, Delphine; Sugiyama, Junji; Riekel, Christian

    2011-01-01

    Tension wood is widespread in the organs of woody plants. During its formation, it generates a large tensile mechanical stress called maturation stress. Maturation stress performs essential biomechanical functions such as optimizing the mechanical resistance of the stem, performing adaptive movements, and ensuring the long-term stability of growing plants. Although various hypotheses have recently been proposed, the mechanism generating maturation stress is not yet fully understood. In order to discriminate between these hypotheses, we investigated structural changes in cellulose microfibrils along sequences of xylem cell differentiation in tension and normal wood of poplar (Populus deltoides × Populus trichocarpa 'I45-51'). Synchrotron radiation microdiffraction was used to measure the evolution of the angle and lattice spacing of crystalline cellulose associated with the deposition of successive cell wall layers. Profiles of normal and tension wood were very similar in early development stages corresponding to the formation of the S1 layer and the outer part of the S2 layer. Subsequent layers were found with a lower microfibril angle (MFA), corresponding to the inner part of the S2 layer of normal wood (MFA approximately 10°) and the G layer of tension wood (MFA approximately 0°). In tension wood only, this steep decrease in MFA occurred together with an increase in cellulose lattice spacing. The relative increase in lattice spacing was found close to the usual value of maturation strains. Analysis showed that this increase in lattice spacing is at least partly due to mechanical stress induced in cellulose microfibrils soon after their deposition, suggesting that the G layer directly generates and supports the tensile maturation stress in poplar tension wood.

  20. Chemical shifts of K-X-ray absorption edges on copper in different compounds by X-ray absorption spectroscopy (XAS) with Synchrotron radiation

    Science.gov (United States)

    Joseph, D.; Basu, S.; Jha, S. N.; Bhattacharyya, D.

    2012-03-01

    Cu K X-ray absorption edges were measured in compounds such as CuO, Cu(CH3CO2)2, Cu(CO3)2, and CuSO4 where Cu is present in oxidation state of 2+, using the energy dispersive EXAFS beamline at INDUS-2 Synchrotron radiation source at RRCAT, Indore. Energy shifts of ˜4-7 eV were observed for Cu K X-ray absorption edge in the above compounds compared to its value in elemental copper. The difference in the Cu K edge energy shifts in the different compounds having same oxidation state of Cu shows the effect of different chemical environments surrounding the cation in the above compounds. The above chemical effect has been quantitatively described by determining the effective charges on Cu cations in the above compounds.

  1. Investigations of the phase transition in V3O5 using energy dispersive X-ray diffraction and synchrotron radiation white beam X-ray topography

    International Nuclear Information System (INIS)

    Asbrink, S.; Gerward, L.; Staun Olsen, J.

    1985-01-01

    The reversible first order phase transition in V 3 O 5 at T t =155 0 C has been studied using a specially constructed oven, where the temperature can be kept constant within a few hundredths of a degree for several hours. Energy dispersive diffraction measurements have beem made in a temperature region around the phase transition with the fixed crystal method and the θ/2θ scanning method. White beam X-ray topographs have been obtained from the same crystal in the same temperature region using synchrotron radiation. The integrated intensities of the strong h 0 0 reflections show anomalies that are correlated with the corresponding X-ray topographs. Thus, an unexpected increase of crystal perfection is observed a few hundredths of a degree below T t . The energy dependence of the intensity maximum at T t for strong reflections has been determined and semi-quantitatively explained on the basis of extinction theory. (orig.)

  2. A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline.

    Science.gov (United States)

    Fittschen, U; Guilherme, A; Böttger, S; Rosenberg, D; Menzel, M; Jansen, W; Busker, M; Gotlib, Z P; Radtke, M; Riesemeier, H; Wobrauschek, P; Streli, C

    2016-05-01

    An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml(-1)) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.

  3. Protein folding and protein metallocluster studies using synchrotron small angler X-ray scattering

    International Nuclear Information System (INIS)

    Eliezer, D.

    1994-06-01

    Proteins, biological macromolecules composed of amino-acid building blocks, possess unique three dimensional shapes or conformations which are intimately related to their biological function. All of the information necessary to determine this conformation is stored in a protein's amino acid sequence. The problem of understanding the process by which nature maps protein amino-acid sequences to three-dimensional conformations is known as the protein folding problem, and is one of the central unsolved problems in biophysics today. The possible applications of a solution are broad, ranging from the elucidation of thousands of protein structures to the rational modification and design of protein-based drugs. The scattering of X-rays by matter has long been useful as a tool for the characterization of physical properties of materials, including biological samples. The high photon flux available at synchrotron X-ray sources allows for the measurement of scattering cross-sections of dilute and/or disordered samples. Such measurements do not yield the detailed geometrical information available from crystalline samples, but do allow for lower resolution studies of dynamical processes not observable in the crystalline state. The main focus of the work described here has been the study of the protein folding process using time-resolved small-angle x-ray scattering measurements. The original intention was to observe the decrease in overall size which must accompany the folding of a protein from an extended conformation to its compact native state. Although this process proved too fast for the current time-resolution of the technique, upper bounds were set on the probable compaction times of several small proteins. In addition, an interesting and unexpected process was detected, in which the folding protein passes through an intermediate state which shows a tendency to associate. This state is proposed to be a kinetic molten globule folding intermediate

  4. Protein folding and protein metallocluster studies using synchrotron small angler X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Eliezer, D.

    1994-06-01

    Proteins, biological macromolecules composed of amino-acid building blocks, possess unique three dimensional shapes or conformations which are intimately related to their biological function. All of the information necessary to determine this conformation is stored in a protein`s amino acid sequence. The problem of understanding the process by which nature maps protein amino-acid sequences to three-dimensional conformations is known as the protein folding problem, and is one of the central unsolved problems in biophysics today. The possible applications of a solution are broad, ranging from the elucidation of thousands of protein structures to the rational modification and design of protein-based drugs. The scattering of X-rays by matter has long been useful as a tool for the characterization of physical properties of materials, including biological samples. The high photon flux available at synchrotron X-ray sources allows for the measurement of scattering cross-sections of dilute and/or disordered samples. Such measurements do not yield the detailed geometrical information available from crystalline samples, but do allow for lower resolution studies of dynamical processes not observable in the crystalline state. The main focus of the work described here has been the study of the protein folding process using time-resolved small-angle x-ray scattering measurements. The original intention was to observe the decrease in overall size which must accompany the folding of a protein from an extended conformation to its compact native state. Although this process proved too fast for the current time-resolution of the technique, upper bounds were set on the probable compaction times of several small proteins. In addition, an interesting and unexpected process was detected, in which the folding protein passes through an intermediate state which shows a tendency to associate. This state is proposed to be a kinetic molten globule folding intermediate.

  5. Characterization of metal additive manufacturing surfaces using synchrotron X-ray CT and micromechanical modeling

    Science.gov (United States)

    Kantzos, C. A.; Cunningham, R. W.; Tari, V.; Rollett, A. D.

    2017-12-01

    Characterizing complex surface topologies is necessary to understand stress concentrations created by rough surfaces, particularly those made via laser power-bed additive manufacturing (AM). Synchrotron-based X-ray microtomography (μ XCT ) of AM surfaces was shown to provide high resolution detail of surface features and near-surface porosity. Using the CT reconstructions to instantiate a micromechanical model indicated that surface notches and near-surface porosity both act as stress concentrators, while adhered powder carried little to no load. Differences in powder size distribution had no direct effect on the relevant surface features, nor on stress concentrations. Conventional measurements of surface roughness, which are highly influenced by adhered powder, are therefore unlikely to contain the information relevant to damage accumulation and crack initiation.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  7. Multi-elemental analysis of produced water by synchrotron radiation total reflection X-ray fluorescence.

    Science.gov (United States)

    Pimentel, P M; Anjos, M J; Melo, D M A; Melo, M A F; Gonçalves, L M; Silva, C N; Lopes, R T

    2008-02-15

    The synchrotron radiation total reflection X-ray fluorescence (SRTXRF) technique was used for the analysis of heavy metals in produced water samples from oil field in Rio Grande do Norte, in order to determine potential sources of pollution. Since the inorganic components in produced water generally resembling sea water, pre-concentration procedures have been applied to increase the concentration of the analyte of interest and to minimize the salt matrix effects. This technique allows us to determine the contents of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Hg and Pb in 20 produced water samples. The great majority of the sampling points presented low elemental concentration value. However, in some sample, the Fe, Ni, Cu, Zn and Hg concentration were higher than the established limits by the Brazilian legislation.

  8. Generating picosecond x-ray pulses in synchrotron light sources using dipole kickers

    Directory of Open Access Journals (Sweden)

    W. Guo

    2007-02-01

    Full Text Available The duration of the x-ray pulse generated at a synchrotron light source is typically tens of picoseconds. Shorter pulses are highly desired by the users. In electron storage rings, the vertical beam size is usually orders of magnitude less than the bunch length due to radiation damping; therefore, a shorter pulse can be obtained by slitting the vertically tilted bunch. Zholents proposed tilting the bunch using rf deflection. We found that tilted bunches can also be generated by a dipole magnet kick. A vertical tilt is developed after the kick in the presence of nonzero chromaticity. The tilt was successfully observed and a 4.2-ps pulse was obtained from a 27-ps electron bunch at the Advanced Photon Source. Based on this principle, we propose a short-pulse generation scheme that produces picosecond x-ray pulses at a repetition rate of 1–2 kHz, which can be used for pump-probe experiments.

  9. NATO Advanced Study Institute on Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays

    CERN Document Server

    Jeffrey, George

    1988-01-01

    X-ray and neutron crystallography have played an increasingly impor­ tant role in the chemical and biochemical sciences over the past fifty years. The principal obstacles in this methodology, the phase problem and com­ puting, have been overcome. The former by the methods developed in the 1960's and just recognised by the 1985 Chemistry Nobel Prize award to Karle and Hauptman, the latter by the dramatic advances that have taken place in computer technology in the past twenty years. Within the last decade, two new radiation sources have been added to the crystallographer's tools. One is synchrotron X-rays and the other is spallation neutrons. Both have much more powerful fluxes than the pre­ vious sources and they are pulsed rather than continuos. New techniques are necessary to fully exploit the intense continuos radiation spectrum and its pulsed property. Both radiations are only available from particular National Laboratories on a guest-user basis for scientists outside these Na­ tional Laboratories. Hi...

  10. Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings

    International Nuclear Information System (INIS)

    Reiche, I.; Radtke, M.; Berger, A.; Goerner, W.; Merchel, S.; Riesemeier, H.; Bevers, H.

    2006-01-01

    New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606-1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of μg/cm 2 . Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is - together with external micro-proton-induced X-ray emission - the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French-German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection. (orig.)

  11. Effect of Cobalt Fillers on Polyurethane Segmentations Investigated by Synchrotron Small Angle X-Ray Scattering

    Directory of Open Access Journals (Sweden)

    Krit Koyvanich

    2013-01-01

    Full Text Available The segmentation between rigid and rubbery chains in polyurethanes (PUs influences polymeric properties and implementations. Several models have successfully been proposed to visualize the configuration between the hard segment (HS and soft segment (SS. For particulate PU composites, the arrangement of HS and SS is more complicated because the fillers tend to disrupt the chain formation and segmentation. In this work, the effect of ferromagnetic cobalt (Co powders (average diameter 2 μm on PU synthesized from a reaction between polyether polyol (soft segment and diphenylmethane-4,4′-diisocyanate (hard segment was studied with varying loadings (0, 20, 40, and 60 wt.%. The 300 μm thick PU/Co samples were tape-casted and then received heat treatment at 80°C for 180 min. From synchrotron small angle X-ray scattering (SAXS, the plot of the X-ray scattering intensity (I against the scattering vector (q exhibited a typical single peak of PU whose intensity was reduced by the increase in the Co loading. Characteristic SAXS peaks in the case of 0-20 wt.% Co agreed well with the scattering by globular hard segment domains according to Zernike-Prins and Percus-Yevick models. The higher Co loadings led to larger deviations from all theoretical models.

  12. Synchrotron X-Ray Studies of Model SOFC Cathodes, Part I: Thin Film Cathodes.

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Kee-Chul; Ingram, Brian; Ilavsky, Jan; Lee, Shiwoo; Fuoss, Paul; You, Hoydoo

    2017-11-15

    We present synchrotron x-ray investigations of thin film La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) model cathodes for solid oxide fuel cells, grown on electrolyte substrates by pulse laser deposition, in situ during half-cell operations. We observed dynamic segregations of cations, such as Sr and Co, on the surfaces of the film cathodes. The effects of temperature, applied potentials, and capping layers on the segregations were investigated using a surfacesensitive technique of total external reflection x-ray fluorescence. We also studied patterned thin film LSCF cathodes using high-resolution micro-beam diffraction measurements. We find chemical expansion decreases for narrow stripes. This suggests the expansion is dominated by the bulk pathway reactions. The chemical expansion vs. the distance from the electrode contact was measured at three temperatures and an oxygen vacancy activation energy was estimated to be ~1.4 eV.

  13. High resolution X-ray detector for synchrotron-based microtomography

    CERN Document Server

    Stampanoni, M; Wyss, P; Abela, R; Patterson, B; Hunt, S; Vermeulen, D; Rueegsegger, P

    2002-01-01

    Synchrotron-based microtomographic devices are powerful, non-destructive, high-resolution research tools. Highly brilliant and coherent X-rays extend the traditional absorption imaging techniques and enable edge-enhanced and phase-sensitive measurements. At the Materials Science Beamline MS of the Swiss Light Source (SLS), the X-ray microtomographic device is now operative. A high performance detector based on a scintillating screen optically coupled to a CCD camera has been developed and tested. Different configurations are available, covering a field of view ranging from 715x715 mu m sup 2 to 7.15x7.15 mm sup 2 with magnifications from 4x to 40x. With the highest magnification 480 lp/mm had been achieved at 10% modulation transfer function which corresponds to a spatial resolution of 1.04 mu m. A low-noise fast-readout CCD camera transfers 2048x2048 pixels within 100-250 ms at a dynamic range of 12-14 bit to the file server. A user-friendly graphical interface gives access to the main parameters needed for ...

  14. $YB_{66} a new soft X-ray monochromator for synchrotron radiation

    CERN Document Server

    Wong, J; Rowen, M; Schäfers, F; Müller, B R; Rek, Z U

    1999-01-01

    For pt.I see Nucl. Instrum. Methods Phys. Res., vol.A291, p.243-8, 1990. YB/sub 66/, a complex boron-rich man-made crystal, has been singled out as a potential monochromator material to disperse synchrotron soft X-rays in the 1-2 keV region. Results of a series of systematic property characterizations pertinent for this application are presented in this paper. These include Laue diffraction patterns and high-precision lattice-constant determination, etch rate, stoichiometry, thermal expansion, soft X-ray reflectivity and rocking-curve measurements, thermal load effects on monochromator performance, nature of intrinsic positive glitches and their reduction. The 004 reflection of YB/sub 66/ has a reflectance of ~3 in this spectral region. The width of the rocking curve varies from 0.25 eV at 1.1 keV to 1.0 eV at 2 keV, which is a factor of two better than that of beryl(1010) in the same energy range, and enables measurements of high-resolution XANES spectra at the Mg, Al and Si K- edges. The thermal bump on the...

  15. Characterization and quantification of cerebral edema induced by synchrotron x-ray microbeam radiation therapy

    International Nuclear Information System (INIS)

    Serduc, Raphael; Looij, Yohan van de; Francony, Gilles; Verdonck, Olivier; Sanden, Boudewijn van der; Farion, Regine; Segebarth, Christoph; Remy, Chantal; Lahrech, Hana; Laissue, Jean; Braeuer-Krisch, Elke; Siegbahn, Erik Albert; Bravin, Alberto; Prezado, Yolanda

    2008-01-01

    Cerebral edema is one of the main acute complications arising after irradiation of brain tumors. Microbeam radiation therapy (MRT), an innovative experimental radiotherapy technique using spatially fractionated synchrotron x-rays, has been shown to spare radiosensitive tissues such as mammal brains. The aim of this study was to determine if cerebral edema occurs after MRT using diffusion-weighted MRI and microgravimetry. Prone Swiss nude mice's heads were positioned horizontally in the synchrotron x-ray beam and the upper part of the left hemisphere was irradiated in the antero-posterior direction by an array of 18 planar microbeams (25 mm wide, on-center spacing 211 mm, height 4 mm, entrance dose 312 Gy or 1000 Gy). An apparent diffusion coefficient (ADC) was measured at 7 T 1, 7, 14, 21 and 28 days after irradiation. Eventually, the cerebral water content (CWC) was determined by microgravimetry. The ADC and CWC in the irradiated (312 Gy or 1000 Gy) and in the contralateral non-irradiated hemispheres were not significantly different at all measurement times, with two exceptions: (1) a 9% ADC decrease (p < 0.05) was observed in the irradiated cortex 1 day after exposure to 312 Gy, (2) a 0.7% increase (p < 0.05) in the CWC was measured in the irradiated hemispheres 1 day after exposure to 1000 Gy. The results demonstrate the presence of a minor and transient cellular edema (ADC decrease) at 1 day after a 312 Gy exposure, without a significant CWC increase. One day after a 1000 Gy exposure, the CWC increased, while the ADC remained unchanged and may reflect the simultaneous presence of cellular and vasogenic edema. Both types of edema disappear within a week after microbeam exposure which may confirm the normal tissue sparing effect of MRT. For more information on this article, see medicalphysicsweb.org

  16. Characterization and quantification of cerebral edema induced by synchrotron x-ray microbeam radiation therapy

    Science.gov (United States)

    Serduc, Raphaël; van de Looij, Yohan; Francony, Gilles; Verdonck, Olivier; van der Sanden, Boudewijn; Laissue, Jean; Farion, Régine; Bräuer-Krisch, Elke; Siegbahn, Erik Albert; Bravin, Alberto; Prezado, Yolanda; Segebarth, Christoph; Rémy, Chantal; Lahrech, Hana

    2008-03-01

    Cerebral edema is one of the main acute complications arising after irradiation of brain tumors. Microbeam radiation therapy (MRT), an innovative experimental radiotherapy technique using spatially fractionated synchrotron x-rays, has been shown to spare radiosensitive tissues such as mammal brains. The aim of this study was to determine if cerebral edema occurs after MRT using diffusion-weighted MRI and microgravimetry. Prone Swiss nude mice's heads were positioned horizontally in the synchrotron x-ray beam and the upper part of the left hemisphere was irradiated in the antero-posterior direction by an array of 18 planar microbeams (25 mm wide, on-center spacing 211 mm, height 4 mm, entrance dose 312 Gy or 1000 Gy). An apparent diffusion coefficient (ADC) was measured at 7 T 1, 7, 14, 21 and 28 days after irradiation. Eventually, the cerebral water content (CWC) was determined by microgravimetry. The ADC and CWC in the irradiated (312 Gy or 1000 Gy) and in the contralateral non-irradiated hemispheres were not significantly different at all measurement times, with two exceptions: (1) a 9% ADC decrease (p edema (ADC decrease) at 1 day after a 312 Gy exposure, without a significant CWC increase. One day after a 1000 Gy exposure, the CWC increased, while the ADC remained unchanged and may reflect the simultaneous presence of cellular and vasogenic edema. Both types of edema disappear within a week after microbeam exposure which may confirm the normal tissue sparing effect of MRT. For more information on this article, see medicalphysicsweb.org

  17. Characterization and quantification of cerebral edema induced by synchrotron x-ray microbeam radiation therapy

    Energy Technology Data Exchange (ETDEWEB)

    Serduc, Raphael; Looij, Yohan van de; Francony, Gilles; Verdonck, Olivier; Sanden, Boudewijn van der; Farion, Regine; Segebarth, Christoph; Remy, Chantal; Lahrech, Hana [INSERM, U836, F-38043 Grenoble (France); Laissue, Jean [Institute of Pathology, University of Bern (Switzerland); Braeuer-Krisch, Elke; Siegbahn, Erik Albert; Bravin, Alberto; Prezado, Yolanda [European Synchrotron Radiation Facility, F-38043 Grenoble (France)], E-mail: serduc@esrf.fr

    2008-03-07

    Cerebral edema is one of the main acute complications arising after irradiation of brain tumors. Microbeam radiation therapy (MRT), an innovative experimental radiotherapy technique using spatially fractionated synchrotron x-rays, has been shown to spare radiosensitive tissues such as mammal brains. The aim of this study was to determine if cerebral edema occurs after MRT using diffusion-weighted MRI and microgravimetry. Prone Swiss nude mice's heads were positioned horizontally in the synchrotron x-ray beam and the upper part of the left hemisphere was irradiated in the antero-posterior direction by an array of 18 planar microbeams (25 mm wide, on-center spacing 211 mm, height 4 mm, entrance dose 312 Gy or 1000 Gy). An apparent diffusion coefficient (ADC) was measured at 7 T 1, 7, 14, 21 and 28 days after irradiation. Eventually, the cerebral water content (CWC) was determined by microgravimetry. The ADC and CWC in the irradiated (312 Gy or 1000 Gy) and in the contralateral non-irradiated hemispheres were not significantly different at all measurement times, with two exceptions: (1) a 9% ADC decrease (p < 0.05) was observed in the irradiated cortex 1 day after exposure to 312 Gy, (2) a 0.7% increase (p < 0.05) in the CWC was measured in the irradiated hemispheres 1 day after exposure to 1000 Gy. The results demonstrate the presence of a minor and transient cellular edema (ADC decrease) at 1 day after a 312 Gy exposure, without a significant CWC increase. One day after a 1000 Gy exposure, the CWC increased, while the ADC remained unchanged and may reflect the simultaneous presence of cellular and vasogenic edema. Both types of edema disappear within a week after microbeam exposure which may confirm the normal tissue sparing effect of MRT. For more information on this article, see medicalphysicsweb.org.

  18. Synchrotron-based X-ray absorption spectroscopy for art conservation: looking back and looking forward.

    Science.gov (United States)

    Cotte, Marine; Susini, Jean; Dik, Joris; Janssens, Koen

    2010-06-15

    A variety of analytical techniques augmented by the use of synchrotron radiation (SR), such as X-ray fluorescence (SR-XRF) and X-ray diffraction (SR-XRD), are now readily available, and they differ little, conceptually, from their common laboratory counterparts. Because of numerous advantages afforded by SR-based techniques over benchtop versions, however, SR methods have become popular with archaeologists, art historians, curators, and other researchers in the field of cultural heritage (CH). Although the CH community now commonly uses both SR-XRF and SR-XRD, the use of synchrotron-based X-ray absorption spectroscopy (SR-XAS) techniques remains marginal, mostly because CH specialists rarely interact with SR physicists. In this Account, we examine the basic principles and capabilities of XAS techniques in art preservation. XAS techniques offer a combination of features particularly well-suited for the chemical analysis of works of art. The methods are noninvasive, have low detection limits, afford high lateral resolution, and provide exceptional chemical sensitivity. These characteristics are highly desirable for the chemical characterization of precious, heterogeneous, and complex materials. In particular, the chemical mapping capability, with high spatial resolution that provides information about local composition and chemical states, even for trace elements, is a unique asset. The chemistry involved in both the object's history (that is, during fabrication) and future (that is, during preservation and restoration treatments) can be addressed by XAS. On the one hand, many studies seek to explain optical effects occurring in historical glasses or ceramics by probing the molecular environment of relevant chromophores. Hence, XAS can provide insight into craft skills that were mastered years, decades, or centuries ago but were lost over the course of time. On the other hand, XAS can also be used to characterize unwanted reactions, which are then considered

  19. X-ray Microprobe for Fluorescence and Diffraction Analysis

    International Nuclear Information System (INIS)

    Ice, G.E.

    2005-01-01

    X-ray diffraction (see unit 1.1) and x-ray excited fluorescence analysis are powerful techniques for the nondestructive measurement of crystal structure and chemical composition. X-ray fluorescence analysis is inherently nondestructive with orders of magnitude lower power deposited for the same detectable limit as with fluorescence excited by charged particle probes (Sparks, 1980). X-ray diffraction analysis is sensitive to crystal structure with orders-of-magnitude greater sensitivity to crystallographic strain than electron probes (Rebonato, et al. 1989). When a small-area x-ray microbeam is used as the probe, chemical composition (Z>14), crystal structure, crystalline texture, and crystalline strain distributions can be determined. These distributions can be studied both at the surface of the sample and deep within the sample (Fig. 1). Current state-of-the-art can achieve an ∼1 mm-D x-ray microprobe and an ∼0.1 mm-D x-ray microprobe has been demonstrated (Bilderback, et al., 1994). Despite their great chemical and crystallographic sensitivities, x-ray microprobe techniques have until recently been restricted by inefficient x-ray focusing optics and weak x-ray sources; x-ray microbeam analysis was largely superseded by electron techniques in the 50's. However, interest in x-ray microprobe techniques has now been revived (Howells, et al., 1983; Ice and Sparks, 1984; Chevallier, et al., 1997; Riekel 1992; Thompson, el al., 1992; and Making and Using... 1997) by the development of efficient x-ray focusing optics and ultra-high intensity synchrotron x-ray sources (Buras and Tazzari, 1984; Shenoy, et al., 1988). These advances have increased the achievable microbeam flux by more than 11 orders of magnitude (Fig. 2) (Ice, 1997); the flux in a tunable 1 mm-D beam on a 'so called' 3rd-generation synchrotron source such as the APS can exceed the flux in a fixed-energy mm2 beam on a conventional source. These advances make x-ray microfluorescence and x-ray

  20. Chemical Mapping of Paleontological and Archeological Artifacts with Synchrotron X-Rays

    Science.gov (United States)

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

    2012-07-01

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

  1. Using Synchrotron X-ray Fluorescence Microprobes in the Study of Metal Homeostasis in Plants

    International Nuclear Information System (INIS)

    Punshon, T.; Guerinot, M.; Lanzirotti, A.

    2009-01-01

    Background and Aims: This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope: The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions: SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis.

  2. Synchrotron radiation total reflection x-ray fluorescence analysis; of polymer coated silicon wafers

    International Nuclear Information System (INIS)

    Brehm, L.; Kregsamer, P.; Pianetta, P.

    2000-01-01

    It is well known that total reflection x-ray fluorescence (TXRF) provides an efficient method for analyzing trace metal contamination on silicon wafer surfaces. New polymeric materials used as interlayer dielectrics in microprocessors are applied to the surface of silicon wafers by a spin-coating process. Analysis of these polymer coated wafers present a new challenge for TXRF analysis. Polymer solutions are typically analyzed for bulk metal contamination prior to application on the wafer using inductively coupled plasma mass spectrometry (ICP-MS). Questions have arisen about how to relate results of surface contamination analysis (TXRF) of a polymer coated wafer to bulk trace analysis (ICP-MS) of the polymer solutions. Experiments were done to explore this issue using synchrotron radiation (SR) TXRF. Polymer solutions were spiked with several different concentrations of metals. These solutions were applied to silicon wafers using the normal spin-coating process. The polymer coated wafers were then measured using the SR-TXRF instrument set-up at the Stanford Synchrotron Radiation Laboratory (SSRL). Several methods of quantitation were evaluated. The best results were obtained by developing calibration curves (intensity versus ppb) using the spiked polymer coated wafers as standards. Conversion of SR-TXRF surface analysis results (atoms/cm 2 ) to a volume related concentration was also investigated. (author)

  3. Ring artifact reduction in synchrotron x-ray tomography through helical acquisition

    Science.gov (United States)

    Pelt, Daniël M.; Parkinson, Dilworth Y.

    2018-03-01

    In synchrotron x-ray tomography, systematic defects in certain detector elements can result in arc-shaped artifacts in the final reconstructed image of the scanned sample. These ring artifacts are commonly found in many applications of synchrotron tomography, and can make it difficult or impossible to use the reconstructed image in further analyses. The severity of ring artifacts is often reduced in practice by applying pre-processing on the acquired data, or post-processing on the reconstructed image. However, such additional processing steps can introduce additional artifacts as well, and rely on specific choices of hyperparameter values. In this paper, a different approach to reducing the severity of ring artifacts is introduced: a helical acquisition mode. By moving the sample parallel to the rotation axis during the experiment, the sample is detected at different detector positions in each projection, reducing the effect of systematic errors in detector elements. Alternatively, helical acquisition can be viewed as a way to transform ring artifacts to helix-like artifacts in the reconstructed volume, reducing their severity. We show that data acquired with the proposed mode can be transformed to data acquired with a virtual circular trajectory, enabling further processing of the data with existing software packages for circular data. Results for both simulated data and experimental data show that the proposed method is able to significantly reduce ring artifacts in practice, even compared with popular existing methods, without introducing additional artifacts.

  4. Sulfur fixation in wood mapped by synchrotron X-ray studies: implications for environmental archives.

    Science.gov (United States)

    Fairchild, Ian I; Loader, Neil J; Wynn, Peter M; Frisia, Silvia; Thomas, Peter A; Lageard, Jonathan G A; De Momi, Anna; Hartland, Adam; Borsato, Andrea; La Porta, Nicola; Susini, Jean

    2009-03-01

    There is a shortage of archives of sulfur that can be used to investigate industrial orvolcanic pollution in terrestrial catchments, but the role of S as a nutrient, coupled with sparse published evidence, suggests that trees are promising targets. We focused on two conifer species (Picea abies (L.) Karst and Abies alba Miller) from an Alpine site in NE Italy. Bulk analyses of Abies demonstrate that S concentrations were higher in the second half of the 20th century but with some high outliers possibly reflecting particulate impurities. X-ray synchrotron analyses confirmed the observed time trend, which is similar to that of a nearby stalagmite, and reflects an atmospheric pollution record mediated by storage in the soil and ecosystem. S and P were found to be localized in the inner cell wall (ca. 2 microm wide), local thickenings of which probably account for some outlying high values of S in synchrotron studies. S occurs as a mixture of oxidation states (0 to +0.5, +2, +5, and +6) which are consistent in space and time. The results indicate that wood older than a few years contains archive-quality S but that robust conclusions require multiple replicate analyses.

  5. Hard X-ray photoelectron spectroscopy on the GALAXIES beamline at the SOLEIL synchrotron

    Energy Technology Data Exchange (ETDEWEB)

    Céolin, D.; Ablett, J.M.; Prieur, D.; Moreno, T. [Synchrotron SOLEIL, l’Orme des Merisiers, Saint-Aubin, FR-91192 Gif-sur-Yvette Cedex (France); Rueff, J.-P. [Synchrotron SOLEIL, l’Orme des Merisiers, Saint-Aubin, FR-91192 Gif-sur-Yvette Cedex (France); Laboratoire de Chimie Physique-Matière et Rayonnement, Université Pierre et Marie Curie and CNRS UMR7614, FR-75231 Paris Cedex 05 (France); Marchenko, T.; Journel, L.; Guillemin, R.; Pilette, B.; Marin, T. [Laboratoire de Chimie Physique-Matière et Rayonnement, Université Pierre et Marie Curie and CNRS UMR7614, FR-75231 Paris Cedex 05 (France); Simon, M., E-mail: marc.simon@upmc.fr [Synchrotron SOLEIL, l’Orme des Merisiers, Saint-Aubin, FR-91192 Gif-sur-Yvette Cedex (France); Laboratoire de Chimie Physique-Matière et Rayonnement, Université Pierre et Marie Curie and CNRS UMR7614, FR-75231 Paris Cedex 05 (France)

    2013-10-15

    Highlights: ► We developed a new HAXPES endstation at the French synchrotron facility SOLEIL. ► The setup is operational for both solid state and gas phase experiments. ► Beamline performances allow working in the Auger Raman conditions. ► Beamline flux compensates for ionization cross section decrease at high photon energy. ► Spectrometer compensates for ionization cross section decrease at high photon energy. -- Abstract: We report on the newly operational HAXPES endstation located on the GALAXIES beamline of the SOLEIL French synchrotron facility. The photon energy provided by the beamline covers the 2.4–12 keV range, and electrons of kinetic energy up to 12 keV can be analyzed. The HAXPES station is comprised of a UHV analysis chamber designed for investigating both solid samples and gases for the first time at high kinetic energy, and a fully equipped preparation chamber. We present the first results of X-ray photoemission and photoabsorption collected with this setup.

  6. Synchrotron Radiation Total Reflection X-ray Fluorescence Spectroscopy for Microcontamination Analysis on Silicon Wafer Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Takaura, Norikatsu

    1997-10-01

    As dimensions in state-of-the-art CMOS devices shrink to less than 0.1 pm, even low levels of impurities on wafer surfaces can cause device degradation. Conventionally, metal contamination on wafer surfaces is measured using Total Reflection X-Ray Fluorescence Spectroscopy (TXRF). However, commercially available TXRF systems do not have the necessary sensitivity for measuring the lower levels of contamination required to develop new CMOS technologies. In an attempt to improve the sensitivity of TXRF, this research investigates Synchrotron Radiation TXRF (SR TXRF). The advantages of SR TXRF over conventional TXRF are higher incident photon flux, energy tunability, and linear polarization. We made use of these advantages to develop an optimized SR TXRF system at the Stanford Synchrotron Radiation Laboratory (SSRL). The results of measurements show that the Minimum Detection Limits (MDLs) of SR TXRF for 3-d transition metals are typically at a level-of 3x10{sup 8} atoms/cm{sup 2}, which is better than conventional TXRF by about a factor of 20. However, to use our SR TXRF system for practical applications, it was necessary to modify a commercially available Si (Li) detector which generates parasitic fluorescence signals. With the modified detector, we could achieve true MDLs of 3x10{sup 8} atoms/cm{sup 2} for 3-d transition metals. In addition, the analysis of Al on Si wafers is described. Al analysis is difficult because strong Si signals overlap the Al signals. In this work, the Si signals are greatly reduced by tuning the incident beam energy below the Si K edge. The results of our measurements show that the sensitivity for Al is limited by x-ray Raman scattering. Furthermore, we show the results of theoretical modeling of SR TXRF backgrounds consisting of the bremsstrahlung generated by photoelectrons, Compton scattering, and Raman scattering. To model these backgrounds, we extended conventional theoretical models by taking into account several aspects particular

  7. Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

    Science.gov (United States)

    Neutze, Richard; Moffat, Keith

    2012-01-01

    X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

  8. High resolution hard X-ray photoemission using synchrotron radiation as an essential tool for characterization of thin solid films

    International Nuclear Information System (INIS)

    Kim, J.J.; Ikenaga, E.; Kobata, M.; Takeuchi, A.; Awaji, M.; Makino, H.; Chen, P.P.; Yamamoto, A.; Matsuoka, T.; Miwa, D.; Nishino, Y.; Yamamoto, T.; Yao, T.; Kobayashi, K.

    2006-01-01

    Recently, we have shown that hard X-ray photoemission spectroscopy using undulator X-rays at SPring-8 is quite feasible with both high resolution and high throughput. Here we report an application of hard X-ray photoemission spectroscopy to the characterization of electronic and chemical states of thin solid films, for which conventional PES is not applicable. As a typical example, we focus on the problem of the scatter in the reported band-gap values for InN. We show that oxygen incorporation into the InN film strongly modifies the valence and plays a crucial role in the band gap problem. The present results demonstrate the powerful applicability of high resolution photoemission spectroscopy with hard X-rays from a synchrotron source

  9. Studies of protein structure in solution and protein folding using synchrotron small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lingling [Stanford Univ., CA (United States)

    1996-04-01

    Synchrotron small angle x-ray scattering (SAXS) has been applied to the structural study of several biological systems, including the nitrogenase complex, the heat shock cognate protein (hsc70), and lysozyme folding. The structural information revealed from the SAXS experiments is complementary to information obtained by other physical and biochemical methods, and adds to our knowledge and understanding of these systems.

  10. Efficient Analytical Approaches to the Optics of Compound Refractive Lenses for Use with Synchrotron X-rays

    DEFF Research Database (Denmark)

    Poulsen, Stefan Othmar; Poulsen, Henning Friis

    2014-01-01

    The properties of compound refractive lenses (CRLs) of biconcave parabolic lenses for focusing and imaging synchrotron X-rays have been investigated theoretically by ray transfer matrix analysis and Gaussian beam propagation. We present approximate analytical expressions, that allow fast estimati...

  11. Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Soo In; George, Graham N.; Lawrence, John R.; Kaminskyj, Susan G. W.; Dynes, James J.; Lai, Barry; Pickering, Ingrid J.

    2016-10-04

    Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to the same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se0). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se0 using the Se LIII edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50–700 nm, suggesting Se0 nanoparticles. The intimate association of Se0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.

  12. Theoretical analysis of the background intensity distribution in X-ray Birefringence Imaging using synchrotron bending-magnet radiation

    Science.gov (United States)

    Sutter, John P.; Dolbnya, Igor P.; Collins, Stephen P.; Harris, Kenneth D. M.; Edwards-Gau, Gregory R.; Palmer, Benjamin A.

    2015-04-01

    In the recently developed technique of X-ray Birefringence Imaging, molecular orientational order in anisotropic materials is studied by exploiting the birefringence of linearly polarized X-rays with energy close to an absorption edge of an element in the material. In the experimental setup, a vertically deflecting high-resolution double-crystal monochromator is used upstream from the sample to select the appropriate photon energy, and a horizontally deflecting X-ray polarization analyzer, consisting of a perfect single crystal with a Bragg reflection at Bragg angle of approximately 45°, is placed downstream from the sample to measure the resulting rotation of the X-ray polarization. However, if the experiment is performed on a synchrotron bending-magnet beamline, then the elliptical polarization of the X-rays out of the electron orbit plane affects the shape of the output beam. Also, because the monochromator introduces a correlation between vertical position and photon energy to the X-ray beam, the polarization analyzer does not select the entire beam, but instead selects a diagonal stripe, the slope of which depends on the Bragg angles of the monochromator and the polarization analyzer. In the present work, the final background intensity distribution is calculated analytically because the phase space sampling methods normally used in ray traces are too inefficient for this setup. X-ray Birefringence Imaging data measured at the Diamond Light Source beamline B16 agree well with the theory developed here.

  13. Theoretical analysis of the background intensity distribution in X-ray Birefringence Imaging using synchrotron bending-magnet radiation

    Energy Technology Data Exchange (ETDEWEB)

    Sutter, John P., E-mail: john.sutter@diamond.ac.uk; Dolbnya, Igor P.; Collins, Stephen P. [Diamond Light Source Ltd., Chilton, Didcot, Oxfordshire OX11 0DE (United Kingdom); Harris, Kenneth D. M.; Edwards-Gau, Gregory R. [School of Chemistry, Cardiff University, Park Place, Cardiff CF10 3AT, Wales (United Kingdom); Palmer, Benjamin A. [Department of Structural Biology, Weizmann Institute of Science, 234 Herzl St., Rehovot 7610001 (Israel)

    2015-04-28

    In the recently developed technique of X-ray Birefringence Imaging, molecular orientational order in anisotropic materials is studied by exploiting the birefringence of linearly polarized X-rays with energy close to an absorption edge of an element in the material. In the experimental setup, a vertically deflecting high-resolution double-crystal monochromator is used upstream from the sample to select the appropriate photon energy, and a horizontally deflecting X-ray polarization analyzer, consisting of a perfect single crystal with a Bragg reflection at Bragg angle of approximately 45°, is placed downstream from the sample to measure the resulting rotation of the X-ray polarization. However, if the experiment is performed on a synchrotron bending-magnet beamline, then the elliptical polarization of the X-rays out of the electron orbit plane affects the shape of the output beam. Also, because the monochromator introduces a correlation between vertical position and photon energy to the X-ray beam, the polarization analyzer does not select the entire beam, but instead selects a diagonal stripe, the slope of which depends on the Bragg angles of the monochromator and the polarization analyzer. In the present work, the final background intensity distribution is calculated analytically because the phase space sampling methods normally used in ray traces are too inefficient for this setup. X-ray Birefringence Imaging data measured at the Diamond Light Source beamline B16 agree well with the theory developed here.

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

    Science.gov (United States)

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

    1993-01-01

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

  15. In situ hydration of sulphoaluminate cement mixtures monitored by synchrotron x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Turrillas, X. [Institut de Ciencia de Materials de Barcelona (ICMAB-CSIC), Barcelona (Spain); Martinez, L.G.; Carvalho, A.M.; Carezzato, G.L. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Rossetto, C.M. [Faculdade de Tecnologia de Sao Paulo (FATEC), SP (Brazil)

    2016-07-01

    Full text: The hydration of calcium sulpho-aluminate cement mixtures was studied in situ by synchrotron X-ray diffraction at the XRD1 beamline of the Laboratorio Nacional de Luz Sincrotron (LNLS) in Campinas, SP. The powder specimens were introduced in borosilicate glass capillary tubes of 0.7 mm of internal diameter and imbued with deionized water. As the hydration reaction is very fast the capillaries were placed on the goniometer and the data collection was started after two minutes of mixing with water. The X-ray energy chosen to get an adequate flux for these short time acquisitions was 12 keV or more precisely 1.033258 Å, determined with polycrystalline corundum standard. Diffraction patterns were collected sequentially every 35 seconds for several hours at temperatures ranging from 40 degC to 55 degC with an accuracy better than 0.1 degC attained with the help of a hot air blower. The diffracted signal was collected with an array of twenty-four Mythen detectors at 760 mm from the capillary tube. The diffraction patterns had appropriate statistics to determine the kinetics of the reaction either by quantitative Rietveld analysis or by fitting isolated diffraction peaks to Gaussian curves as a function of time. The most important phases involved in the hydration are Klein´s salt, also known as Ye’elimite, Ca4(AlO2)6SO4, and gypsum, CaSO4.2H2O to yield Ettringite, Ca6Al2(SO4)3(OH)12 - 26H2O, phase responsible for the mechanical properties. (author)

  16. Probing platinum degradation in polymer electrolyte membrane fuel cells by synchrotron X-ray microscopy.

    Science.gov (United States)

    Berejnov, Viatcheslav; Martin, Zulima; West, Marcia; Kundu, Sumit; Bessarabov, Dmitri; Stumper, Jürgen; Susac, Darija; Hitchcock, Adam P

    2012-04-14

    Synchrotron-based scanning transmission X-ray spectromicroscopy (STXM) was used to characterize the local chemical environment at and around the platinum particles in the membrane (PTIM) which form in operationally tested (end-of-life, EOL) catalyst coated membranes (CCMs) of polymer electrolyte membrane fuel cells (PEM-FC). The band of metallic Pt particles in operationally tested CCM membranes was imaged using transmission electron microscopy (TEM). The cathode catalyst layer in the beginning-of-life (BOL) CCMs was fabricated using commercially available catalysts created from Pt precursors with and without nitrogen containing ligands. The surface composition of these catalyst powders was measured by X-ray Photoelectron Spectroscopy (XPS). The local chemical environment of the PTIM in EOL CCMs was found to be directly related to the Pt precursor used in CCM fabrication. STXM chemical mapping at the N 1s edge revealed a characteristic spectrum at and around the dendritic Pt particles in CCMs fabricated with nitrogen containing Pt-precursors. This N 1s spectrum was identical to that of the cathode and different from the membrane. For CCM samples fabricated without nitrogen containing Pt-precursors the N 1s spectrum at the Pt particles was indistinguishable from that of the adjacent membrane. We interpret these observations to indicate that nitrogenous ligands in the nitrogen containing precursors, or decomposition product(s) from that source, are transported together with the dissolved Pt from the cathode into the membrane as a result of the catalyst degradation process. This places constraints on possible mechanisms for the PTIM band formation process.

  17. Fabrication of an 8:1 ellipsoidal mirror for a synchrotron x-ray microprobe

    International Nuclear Information System (INIS)

    Jones, K.W.; Takacs, P.Z.; Hastings, J.B.; Casstevens, J.M.; Pionke, C.D.

    1987-01-01

    The fabrication of an 8:1 demagnifying ellipsoidal mirror to be used for an x-ray microprobe at the National Synchrotron Light Source X-26 beam port is described. The design aim was to produce a mirror that could be used over the photon energy range from about 3 to 17 keV. The 300-mm long mirror was required to operate at a grazing angle of 5 mr. The semimajor axis was 4500 mm and the semiminor axis 14.142 mm. Surface roughness of 1 nm or less and slope errors of 1 arc second parallel to the long axis and 200 arc seconds parallel to the short direction were specified. Production of the first electroless nickel-coated aluminum mirror using a diamond-turning technique has been completed. The mirror meets the 1 arc sec surface figure specification except for areas near the ends of the mirror. The reasons for these deviations arise from subtle details of the diamond-turning process which have not been fully incorporated in to the computer program that controls the diamond-turning machines. Further work in computer correction of repeatable errors of the diamond-turning machine can eliminate the waviness at the ends of the mirror. The diamond-turned mirror surface was not fully polished under this effort and therefore does not meet the roughness specification; however, surface smoothness of a fully polished cylindrical mirror manufactured using the same techniques does not meet the specification. It can be concluded that it is now technically feasible to meet the required specifications for the mirror and that the x-ray microprobe based on its use can be achieved

  18. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Science.gov (United States)

    Fittschen, Ursula Elisabeth Adriane; Menzel, Magnus; Scharf, Oliver; Radtke, Martin; Reinholz, Uwe; Buzanich, Günther; Lopez, Velma M.; McIntosh, Kathryn; Streli, Christina; Havrilla, George Joseph

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation.

  19. K-Edge Subtraction Angiography with Synchrotron X-Rays; TOPICAL

    International Nuclear Information System (INIS)

    Giacomini, John C.

    1996-01-01

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

  20. Synchrotron X-ray Applications Toward an Understanding of Elastic Anisotropy

    Science.gov (United States)

    Kanitpanyacharoen, Waruntorn

    The contribution of this dissertation is to expand the current knowledge of factors and mechanisms that influence the development of preferred orientation of minerlas and pores in different materials, ranging from rocks in Earth's crust to minerals in the deep Earth. Preferred orientation--a main contributing component to elastic anisotropy--is however very challenging to quantify. The overall focus of this thesis thus aims to (1) apply the capabilities of synchrotron X-ray techniques to determine preferred orientations of hexagonal metals and shales under different conditions and (2) enhance our understanding of their relationships to the elastic properties. Lattice preferred orientation (LPO) or 'texture' of hexagonal close-packed iron (hcp- Fe) crystals during deformation has been suggested as the cause of the elastic anisotropy observed in Earth's inner core. However, relatively little is known about LPO of other hcp metals. An investigation of a wide range of hcp metals (Cd, Zn, Os, and Hf) as analogs to hcp-Fe was thus undertaken to better understand deformation mechanisms at high pressure and temperature in Chapter 2. Results show that all hcp metals preferentially align their c-axes near the compression axis during deformation but with considerable differences. The gradual texture evolution in Cd and Zn is mainly controlled by basal slip systems while a rapid texture development in Os and Hf at ambient temperature is due to a dominant role of tensile twinning, with some degree of basal slip. At elevated temperature, tensile twinning is suppressed and texturing is governed by combined basal and prismatic slip. Under all conditions, basal slip appears to be the main deformation mechanism in hcp metals at high pressure and temperature. These findings are similar to those of hcp-Fe and useful to better understand the deformation mechanisms of hcp metals and their implications for elastic anisotropy. In Chapter 3, a high-energy synchrotron X-ray diffraction

  1. Construction of a forensic soil database of the Hokkaido region in Japan by synchrotron radiation X-ray analysis

    International Nuclear Information System (INIS)

    Shirota, Yusuke; Hirao, Masataka; Abe, Yoshinari; Nakai, Izumi; Osaka, Keiichi; Itou, Masayoshi

    2017-01-01

    The purpose of the present study is to construct a nation-wide forensic soil database, which allows for the identification of soil evidence based on heavy element and heavy mineral signatures determined by two synchrotron radiation (SR) X-ray techniques, i.e., a high-energy synchrotron radiation X-ray fluorescence analysis and a synchrotron-radiation X-ray powder diffraction analysis, respectively. The heavy element and heavy mineral compositions of the stream sediments collected at 3024 points located all over Japan were measured by the two SR X-ray techniques. The present paper focuses on a regional characterization of the sediments collected from the Hokkaido areas. The concentrations of heavy elements and heavy minerals in the Hokkaido areas were visualized as maps that enable us to compare the heavy element and heavy mineral compositions with the geological context of the samples. Based on a hierarchical cluster analysis using the semi-quantitative compositions of the heavy minerals, we could successfully classify the sediments into six groups corresponding to their background geologies. A Bonferroni multiple comparison demonstrated that these six groups also have significant differences in the heavy element composition. From these examinations, we could demonstrate that detailed regional identification of unknown samples is possible by analyzing both heavy element and heavy mineral compositions of each sample. (author)

  2. X-ray diffraction measurement of liquid As2Se3 by using third-generation synchrotron radiation source

    OpenAIRE

    Kajihara, Yukio; Inui, Masanori; Matsuda, Kazuhiro; Tamura, Kozaburo; Hosokawa, Shinya

    2007-01-01

    X-ray diffraction (XD) measurements of liquid As2Se3 were carried out in the temperature range up to 1600◦C where the temperature is well beyond the semiconductor to metal (SC-M) transition temperature around 1000◦C . The measurements were done by using third-generation synchrotron radiation source at SPring-8 and the obtained structure factors have much improvements over the previous XD measurements by using in house X-ray sources with regard to the momentum transfer range and the data stati...

  3. In situ analysis of cracks in structural materials using synchrotron X-ray tomography and diffraction

    International Nuclear Information System (INIS)

    Steuwer, A.; Edwards, L.; Pratihar, S.; Ganguly, S.; Peel, M.; Fitzpatrick, M.E.; Marrow, T.J.; Withers, P.J.; Sinclair, I.; Singh, K.D.; Gao, N.; Buslaps, T.; Buffiere, J.-Y.

    2006-01-01

    The structural integrity and performance of many components and structures are dominated by cracks and hence the study of cracked bodies study is of major economical and social importance. Despite nearly 30 years of study, there is still no detailed consensus regarding either the fundamental parameters that drive cracks or the precise mechanisms of their growth in most materials. Thus, virtually all crack life prediction models currently in engineering use are largely phenomenological rather than physically based. Historically, a major hindrance to our understanding of crack initiation and propagation has been the inability to measure either the crack tip stresses or the crack morphology deep within materials. The development of very high-resolution strain and tomography mapping on third generation synchrotron sources such as the ESRF has opened up the possibility of developing complementary techniques to monitor the entire plastic/process zone growth mechanisms and the accompanying crack tip field and crack wake field around growing cracks. If realized, such techniques would produce unique information that would be invaluable both in validating present finite element simulations of fatigue crack growth and in developing the future high accuracy simulations necessary for the development of physically realistic fatigue life-prediction models. Recent technique developments at the ESRF, Grenoble, opens up the possibility of imaging cracks and crack tip stress/strain fields, and the ability to study the extend of crack closure and overload effects, even under in situ loading. In this paper, first results from synchrotron X-ray diffraction and tomography experiments performed on ID11 and ID19 (respectively) at the ESRF, Grenoble, are presented and discussed in comparison with predictions from finite element modeling

  4. Classification of lead white pigments using synchrotron radiation micro X-ray diffraction

    Science.gov (United States)

    Welcomme, E.; Walter, P.; Bleuet, P.; Hodeau, J.-L.; Dooryhee, E.; Martinetto, P.; Menu, M.

    2007-12-01

    Lead white pigment was used and synthesised for cosmetic and artistic purposes since the antiquity. Ancient texts describe the various recipes, and preparation processes as well as locations of production. In this study, we describe the results achieved on several paint samples taken from Matthias Grünewald’s works. Grünewald, who was active between 1503 and 1524, was a major painter at the beginning of the German Renaissance. Thanks to X-ray diffraction analysis using synchrotron radiation, it is possible to associate the composition of the paint samples with the masters ancient recipes. Different approaches were used, in reflection and transmission modes, directly on minute samples or on paint cross-sections embedded in resin. Characterisation of lead white pigments reveals variations in terms of composition, graininess and proportion of mineral phases. The present work enlightens the presence of lead white as differentiable main composition groups, which could be specific of a period, a know-how or a geographical origin. In this way, we aim at understanding the choices and the trading of pigments used to realise paintings during northern European Renaissance.

  5. Classification of lead white pigments using synchrotron radiation micro X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Welcomme, E.; Walter, P.; Menu, M. [Centre de Recherche et de Restauration des Musees de France - CNRS UMR 171, Paris (France); Bleuet, P. [European Synchrotron Radiation Facility, BP 220, Grenoble Cedex (France); Hodeau, J.L.; Dooryhee, E.; Martinetto, P. [Institut Neel CNRS-UPR 503-1, 25, Av. des Martyrs, BP 166, Grenoble Cedex 9 (France)

    2007-12-15

    Lead white pigment was used and synthesised for cosmetic and artistic purposes since the antiquity. Ancient texts describe the various recipes, and preparation processes as well as locations of production. In this study, we describe the results achieved on several paint samples taken from Matthias Gruenewald's works. Gruenewald, who was active between 1503 and 1524, was a major painter at the beginning of the German Renaissance. Thanks to X-ray diffraction analysis using synchrotron radiation, it is possible to associate the composition of the paint samples with the masters ancient recipes. Different approaches were used, in reflection and transmission modes, directly on minute samples or on paint cross-sections embedded in resin. Characterisation of lead white pigments reveals variations in terms of composition, graininess and proportion of mineral phases. The present work enlightens the presence of lead white as differentiable main composition groups, which could be specific of a period, a know-how or a geographical origin. In this way, we aim at understanding the choices and the trading of pigments used to realise paintings during northern European Renaissance. (orig.)

  6. Characterization of enamel caries lesions in rat molars using synchrotron X-ray microtomography

    Energy Technology Data Exchange (ETDEWEB)

    Free, R.D.; DeRocher, K.; Stock, S.R.; Keane, D.; Scott-Anne, K.; Bowen, W.H.; Joester, D. (Rochester); (NWU)

    2017-08-18

    Dental caries is a ubiquitous infectious disease with a nearly 100% lifetime prevalence. Rodent caries models are widely used to investigate the etiology, progression and potential prevention or treatment of the disease. To explore the suitability of these models for deeper investigations of intact surface zones during enamel caries, the structures of early-stage carious lesions in rats were characterized and compared with previous reports on white spot enamel lesions in humans. Synchrotron X-ray microcomputed tomography non-destructively mapped demineralization in carious rat molar specimens across a range of caries severity, identifying 52 lesions across the 30 teeth imaged. Of these lesions, 13 were shown to have intact surface zones. Depth profiles of fractional mineral density were qualitatively similar to lesions in human teeth. However, the thickness of the surface zone in the rat model ranges from 10 to 58 µm, and is therefore significantly thinner than in human enamel. These results indicate that a fraction of lesions in rat caries possess an intact surface zone and are qualitatively similar to human lesions at the micrometer scale. This suggests that rat caries models may be a suitable analog through which to investigate the structure of surface zone enamel and its role during dental caries.

  7. Synchrotron X-ray Absorption and In Vitro Bioactivity of Magnetic Macro/Mesoporous Bioactive Glasses

    Directory of Open Access Journals (Sweden)

    Thanida Charoensuk

    2015-12-01

    Full Text Available Iron oxides in macro/mesoporous bioactive glasses were characterized by synchrotron X-ray absorption near edge structure (XANES spectroscopy. This magnetic phase was introduced by adding Fe(NO33 9H2O during the sol-gel synthesis. The obtained bioactive glass scaffolds exhibited superparamagnetism, in which the magnetization was increased with the increase in the Fe molar ratio from 10 to 20%. The linear combination fits of the XANES spectra indicated that the increase in the Fe molar ratio to 20% enhanced the γ-Fe2O3 formation at the expense of the α- Fe2O3 phase. This variation also promoted the formation of fine-grained bone-like apatites on the surface of the scaffolds in the in vitro test. The apatite growth between three and seven days was confirmed by the changing elemental compositions. However, the highest magnetic proportion led to the distortion of the skeleton walls and the collapse of the porous networks.

  8. Synchrotron X-ray computed microtomography study on gas hydrate decomposition in a sedimentary matrix

    Science.gov (United States)

    Yang, Lei; Falenty, Andrzej; Chaouachi, Marwen; Haberthür, David; Kuhs, Werner F.

    2016-09-01

    In-situ synchrotron X-ray computed microtomography with sub-micrometer voxel size was used to study the decomposition of gas hydrates in a sedimentary matrix. Xenon-hydrate was used instead of methane hydrate to enhance the absorption contrast. The microstructural features of the decomposition process were elucidated indicating that the decomposition starts at the hydrate-gas interface; it does not proceed at the contacts with quartz grains. Melt water accumulates at retreating hydrate surface. The decomposition is not homogeneous and the decomposition rates depend on the distance of the hydrate surface to the gas phase indicating a diffusion-limitation of the gas transport through the water phase. Gas is found to be metastably enriched in the water phase with a concentration decreasing away from the hydrate-water interface. The initial decomposition process facilitates redistribution of fluid phases in the pore space and local reformation of gas hydrates. The observations allow also rationalizing earlier conjectures from experiments with low spatial resolutions and suggest that the hydrate-sediment assemblies remain intact until the hydrate spacers between sediment grains finally collapse; possible effects on mechanical stability and permeability are discussed. The resulting time resolved characteristics of gas hydrate decomposition and the influence of melt water on the reaction rate are of importance for a suggested gas recovery from marine sediments by depressurization.

  9. Crystal structure and charge density analysis of Li2NH by synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Noritake, T.; Nozaki, H.; Aoki, M.; Towata, S.; Kitahara, G.; Nakamori, Y.; Orimo, S.

    2005-01-01

    Complex hydrides, such as lithium amide (LiNH 2 ) and lithium imide (Li 2 NH), have recently been noticed as one of the most promising materials for reversible hydrogen storage. In this paper, we reveal the bonding nature of hydrogen in Li 2 NH crystal by synchrotron powder X-ray diffraction measurement at room temperature. The crystal structure was refined by Rietveld method and the charge density distribution was analyzed by maximum entropy method (MEM). The Li 2 NH crystal is anti-fluorite type structure (space group Fm3-bar m) consisting of Li and NH. Hydrogen atom occupies randomly the 48h (Wyckoff notation) sites around N atom. The refined lattice constant is a=5.0742(2)A. The charge density distribution around NH anion in Li 2 NH is almost spherical. The number of electrons within the sphere around the Li and NH is estimated from the obtained charge density distribution. As the result, the ionic charge is expressed as [Li 0.99+ ] 2 [NH] 1.21- . Therefore, it is confirmed experimentally that Li 2 NH is ionically bonded

  10. X-ray tomographic and laminographic microscopy (XTM, XLM) using synchrotron radiation

    International Nuclear Information System (INIS)

    Wyss, P.; Obrist, A.; Hofmann, J.; Luethi, T.; Sennhauser, U.; Thurner, P.; Stampanoni, M.; Abela, R.; Patterson, B.; Mueller, R.

    2003-01-01

    Inner structures of composite materials, components or tissues have to be characterised with micrometer and even submicrometer resolution. It is often highly desirable that specimens stay unchanged after a first characterization to allow meaningful subsequent tests. This justifies major efforts for an ongoing improvement of nondestructive radiographical and tomographical methods for morphological characterization. Radiography and tomography as well as laminography can fulfill these requirements. X-ray sources and detectors have been improved. This applies for synchrotron-beamline systems as well as for tube based systems. A novel detector concept has been implemented in the XTM station at the SLS of the PSI in Villigen, Switzerland. This microtomography station at the SLS has started its operation in spring 2002. A selection of results related to industrial and scientific applications is presented in this contribution. Special emphasis will be given to first results of tomography with limited numbers of projections which is comparable to laminography. This method allows to characterise e.g. ribbons of tissue under load

  11. Deformation in Metallic Glasses Studied by Synchrotron X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Takeshi Egami

    2016-01-01

    Full Text Available High mechanical strength is one of the superior properties of metallic glasses which render them promising as a structural material. However, understanding the process of mechanical deformation in strongly disordered matter, such as metallic glass, is exceedingly difficult because even an effort to describe the structure qualitatively is hampered by the absence of crystalline periodicity. In spite of such challenges, we demonstrate that high-energy synchrotron X-ray diffraction measurement under stress, using a two-dimensional detector coupled with the anisotropic pair-density function (PDF analysis, has greatly facilitated the effort of unraveling complex atomic rearrangements involved in the elastic, anelastic, and plastic deformation of metallic glasses. Even though PDF only provides information on the correlation between two atoms and not on many-body correlations, which are often necessary in elucidating various properties, by using stress as means of exciting the system we can garner rich information on the nature of the atomic structure and local atomic rearrangements during deformation in glasses.

  12. Classification of lead white pigments using synchrotron radiation micro X-ray diffraction

    International Nuclear Information System (INIS)

    Welcomme, E.; Walter, P.; Menu, M.; Bleuet, P.; Hodeau, J.L.; Dooryhee, E.; Martinetto, P.

    2007-01-01

    Lead white pigment was used and synthesised for cosmetic and artistic purposes since the antiquity. Ancient texts describe the various recipes, and preparation processes as well as locations of production. In this study, we describe the results achieved on several paint samples taken from Matthias Gruenewald's works. Gruenewald, who was active between 1503 and 1524, was a major painter at the beginning of the German Renaissance. Thanks to X-ray diffraction analysis using synchrotron radiation, it is possible to associate the composition of the paint samples with the masters ancient recipes. Different approaches were used, in reflection and transmission modes, directly on minute samples or on paint cross-sections embedded in resin. Characterisation of lead white pigments reveals variations in terms of composition, graininess and proportion of mineral phases. The present work enlightens the presence of lead white as differentiable main composition groups, which could be specific of a period, a know-how or a geographical origin. In this way, we aim at understanding the choices and the trading of pigments used to realise paintings during northern European Renaissance. (orig.)

  13. Detection of genetically altered copper levels in Drosophila tissues by synchrotron x-ray fluorescence microscopy.

    Directory of Open Access Journals (Sweden)

    Jessica C Lye

    Full Text Available Tissue-specific manipulation of known copper transport genes in Drosophila tissues results in phenotypes that are presumably due to an alteration in copper levels in the targeted cells. However direct confirmation of this has to date been technically challenging. Measures of cellular copper content such as expression levels of copper-responsive genes or cuproenzyme activity levels, while useful, are indirect. First-generation copper-sensitive fluorophores show promise but currently lack the sensitivity required to detect subtle changes in copper levels. Moreover such techniques do not provide information regarding other relevant biometals such as zinc or iron. Traditional techniques for measuring elemental composition such as inductively coupled plasma mass spectroscopy are not sensitive enough for use with the small tissue amounts available in Drosophila research. Here we present synchrotron x-ray fluorescence microscopy analysis of two different Drosophila tissues, the larval wing imaginal disc, and sectioned adult fly heads and show that this technique can be used to detect changes in tissue copper levels caused by targeted manipulation of known copper homeostasis genes.

  14. Solving mercury (Hg) speciation in soil samples by synchrotron X-ray microspectroscopic techniques

    International Nuclear Information System (INIS)

    Terzano, Roberto; Santoro, Anna; Spagnuolo, Matteo; Vekemans, Bart; Medici, Luca; Janssens, Koen; Goettlicher, Joerg; Denecke, Melissa A.; Mangold, Stefan; Ruggiero, Pacifico

    2010-01-01

    Direct mercury (Hg) speciation was assessed for soil samples with a Hg concentration ranging from 7 up to 240 mg kg -1 . Hg chemical forms were identified and quantified by sequential extractions and bulk- and micro-analytical techniques exploiting synchrotron generated X-rays. In particular, microspectroscopic techniques such as μ-XRF, μ-XRD and μ-XANES were necessary to solve bulk Hg speciation, in both soil fractions 3 S 2 Cl 2 ), and an amorphous phase containing Hg bound to chlorine and sulfur. The amount of metacinnabar and amorphous phases increased in the fraction <2 μm. No interaction among Hg-species and soil components was observed. All the observed Hg-species originated from the slow weathering of an inert Hg-containing waste material (K106, U.S. EPA) dumped in the area several years ago, which is changing into a relatively more dangerous source of pollution. - Direct mercury (Hg) speciation in chlor-alkali plant contaminated soils enabled the identification of potentially dangerous Hg-S/Cl amorphous species.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  16. Rainwater analysis by synchrotron radiation-total reflection X-ray fluorescence

    Science.gov (United States)

    López, María L.; Ceppi, Sergio A.; Asar, María L.; Bürgesser, Rodrigo E.; Ávila, Eldo E.

    2015-11-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation was used to quantify the elemental concentration of rainwater in Córdoba, Argentina. Standard solutions with gallium as internal standard were prepared for the calibration curves. Rainwater samples of 5 μl were added to an acrylic reflector, allowed to dry, and analyzed for 200 s measuring time. The elemental concentrations of As, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sr, V, and Zn were determined. The electrical conductivity, pH, and elemental concentrations were compared to data previously reported for the soluble fraction of rainwater at different sites. A factor analysis was performed in order to determine the sources that contributed to the elemental concentration in rainwater. Anthropogenic sources were identified as traffic pollution, vehicular emissions, and metallurgical factories. The quality of rainwater was analyzed by comparing the concentrations of all the elements in rainwater samples with the WHO guideline values for drinking water. The results show the need to control the atmospheric emissions in order to preserve the quality of rainwater. SR-TXRF analysis of chemical composition of rainwater in Córdoba represents the very first contribution in the region to the knowledge of the concentration of trace metals in the soluble fraction of rainwater. These data are scarce, especially in the Southern Hemisphere.

  17. Phantom and animal imaging studies using PLS synchrotron X-rays

    CERN Document Server

    Hee Joung Kim; Kyu Ho Lee; Hai Jo Jung; Eun Kyung Kim; Jung Ho Je; In Woo Kim; Yeukuang, Hwu; Wen Li Tsai; Je Kyung Seong; Seung Won Lee; Hyung Sik Yoo

    2001-01-01

    Ultra-high resolution radiographs can be obtained using synchrotron X-rays. A collaboration team consisting of K-JIST, POSTECH and YUMC has recently commissioned a new beamline (5C1) at Pohang Light Source (PLS) in Korea for medical applications using phase contrast radiology. Relatively simple image acquisition systems were set up on 5C1 beamline, and imaging studies were performed for resolution test patterns, mammographic phantom, and animals. Resolution test patterns and mammographic phantom images showed much better image resolution and quality with the 5C1 imaging system than the mammography system. Both fish and mouse images with 5C1 imaging system also showed much better image resolution with great details of organs and anatomy compared to those obtained with a conventional mammography system. A simple and inexpensive ultra-high resolution imaging system on 5C1 beamline was successfully implemented. The authors were able to acquire ultra-high resolution images for, resolution test patterns, mammograph...

  18. A synchrotron X-ray diffraction study of non-proportional strain-path effects

    International Nuclear Information System (INIS)

    Collins, D.M.; Erinosho, T.; Dunne, F.P.E.; Todd, R.I.; Connolley, T.; Mostafavi, M.; Kupfer, H.; Wilkinson, A.J.

    2017-01-01

    Common alloys used in sheet form can display a significant ductility benefit when they are subjected to certain multiaxial strain paths. This effect has been studied here for a polycrystalline ferritic steel using a combination of Nakajima bulge testing, X-ray diffraction during biaxial testing of cruciform samples and crystal plasticity finite element (CPFE) modelling. Greatest gains in strain to failure were found when subjecting sheets to uniaxial loading followed by balanced biaxial deformation, resulting in a total deformation close to plane-strain. A combined strain of approximately double that of proportional loading was achieved. The evolution of macrostrain, microstrain and texture during non-proportional loading were evaluated by in-situ high energy synchrotron diffraction. The results have demonstrated that the inhomogeneous strain accumulation from non-proportional deformation is strongly dependent on texture and the applied strain-ratio of the first deformation pass. Experimental diffraction evidence is supported by results produced by a novel method of CPFE-derived diffraction simulation. Using constitutive laws selected on the basis of good agreement with measured lattice strain development, the CPFE model demonstrated the capability to replicate ductility gains measured experimentally.

  19. Synchrotron X-ray Scattering from Self-organized Soft Nanostructures in Clays

    Science.gov (United States)

    Fossum, J. O.

    2009-04-01

    In the general context of self-organization of nanoparticles (in our case clay particles), and transitions in such structures, we study interconnected universal complex physical phenomena such as: (i) spontaneous gravitationally induced phase separation and nematic self-organization in systems of anisotropic clay nanoparticles in aqueous suspension, including studies of isotropic to nematic transitions [1,2] (ii) transitions from biaxial to uniaxial nematics by application of external magnetic field to self-organized systems of the same anisotropic (diamagnetic) clay nanoparticle systems [3,4] (iii) guided self-organization into chainlike structures of the same anisotropic clay nanoparticles in oil suspension when subjected to external electrical fields (electrorheological structures of polarized nanoparticles), and the stability of, and transitions of, such structures, when subjected to external mechanical stress [5,6] The experimental techniques used by us include synchrotron X-ray scattering, neutron scattering, rheometry. microscopy and magnetic resonance. We have demonstrated that clays may be used as good model systems for studies of universal physical phenomena and transitions in self-organized nanostructured soft and complex matter. Self-organization and related transitions in clay systems in particular, may have practical relevance for nano-patterning, properties of nanocomposites, and macroscopically anisotropic gels, among many other applications [7]. The synchrotron experiments have been performed at LNLS-Brazil, PLS- Korea, BNL-USA and ESRF-France. Acknowledgments: Collaborators, postdocs and students at NTNU-Norway, UiO-Norway, IFE-Norway, BNL-USA, LNLS-Brazil, UFPE-Brazil, UnB-Brazil, Univ. Amsterdam-Netherlands, Univ.Paris 7-France and other places. This research has been supported by the Research Council of Norway (RCN), through the NANOMAT, SUP and FRINAT Programs. References 1. J.O. Fossum, E. Gudding, D.d.M. Fonseca, Y. Meheust, E. DiMasi, T

  20. X-ray study of a test quadrant of the SODART telescopes using the expanded beam x-ray optics facility at the Daresbury synchrotron

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Frederiksen, P.

    1994-01-01

    The imaging properties of a test model of the SODART telescopes have been studied using an expanded beam X-ray facility at the Daresbury synchrotron. The encircled power and the point spread function at three energies 6.627 keV, 8.837 keV and 11.046 keV have been measured using 1D and 2D position......V the HPD is 2.5 - 3.0 arcmin for all detectors whereas it is somewhat larger at 11.046 keV for HEPC and LEPC but essentially unchanged for SIXA. Finally, the data are used to point to improvements that can be introduced during the manufacture of the flight telescopes....

  1. X-ray study of a SODART flight telescope using the expanded beam x-ray optics beamline at the Daresbury synchrotron

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Frederiksen, P. K.

    1995-01-01

    The on- and off-axis imaging properties of the first of two SODART flight telescopes have been studied using the expanded beam x-ray facility at the Daresbury synchrotron. From on- axis measurements the encircled power distribution and the point spread function at three energies 6.627 keV, 8.837 ke...... element solid state array detector (SIXA). We found that the HPD decreases with increasing energy due to poorer figure error of the outermost mirrors. The HPD falls in the range from 2.3 to 3 arcmin for all detectors. Residual misalignment of the individual quadrants of the telescope was found...... to contribute to the HPD by approximately 10%. If 33% of the geometric telescope area near the edges of the quadrants are covered a reduction of 10% of the HPD can be obtained. On- and off-axis images generated from the one dimensional intensity distribution are presented. Finally the data have been used...

  2. Research in x-ray optics with the ultimate aim of constructing a synchrotron radiation pumped soft x-ray lithium laser

    International Nuclear Information System (INIS)

    Csonka, P.L.

    1988-01-01

    One of the primary components of the proposed synchrotron radiation (SR) pumped Li X-Ray Laser which the present research (DOE Proposal No. DE-FG06-85ER-13309) undertook to develop, was a vacuum-based high density plasma of predominantly monatomic Lithium as the lasing medium. A monomer density in excess of 10 19 particles/cm 3 at temperatures > 1600 degree C, in volume of roughly 1cm x 0.001cm x 0.001cm was estimated as being necessary for attaining useful gain. Originally two different methods of achieving this were considered, namely: laser-driven ablation of solid Li, and steady-state thermal emission of Li gas from an orifice in a suitable chamber. Due to uncertainties associated with the first option, the resources of the present development program were focused primarily on the latter technique. 9 figs

  3. Spatial imaging and speciation of Cu in rice (Oryza sativa L.) roots using synchrotron-based X-ray microfluorescence and X-ray absorption spectroscopy.

    Science.gov (United States)

    Lu, Lingli; Xie, Ruohan; Liu, Ting; Wang, Haixing; Hou, Dandi; Du, Yonghua; He, Zhenli; Yang, Xiaoe; Sun, Hui; Tian, Shengke

    2017-05-01

    Knowledge of elemental localization and speciation in rice (Oryza sativa L.) roots is crucial for elucidating the mechanisms of Cu accumulation so as to facilitate the development of strategies to inhibit Cu accumulation in rice grain grown in contaminated soils. Using synchrotron-based X-ray microfluorescence and X-ray absorption spectroscopy, we investigated the distribution patterns and speciation of Cu in rice roots treated with 50 μM Cu for 7 days. A clear preferential localization of Cu in the meristematic zone was observed in root tips as compared with the elongation zone. Investigation of Cu in the root cross sections revealed that the intensity of Cu in the vascular bundles was more than 10-fold higher than that in the other scanned sites (epidermis and cortex) in rice roots. The dominant chemical form of Cu (79.1%) in rice roots was similar to that in the Cu-cell wall compounds. These results suggest that although Cu can be easily transported into the vascular tissues in rice roots, most of the metal absorbed by plants is retained in the roots owing to its high binding to the cell wall compounds, thus preventing metal translocation to the aerial parts of the plants. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

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

    2018-01-01

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

  5. Synchrotron radiation sources and condensers for projection x-ray lithography

    International Nuclear Information System (INIS)

    Murphy, J.B.; MacDowell, A.A.; White, D.L.; Wood, O.R. II

    1992-01-01

    The design requirements for a compact electron storage ring that could be used as a soft x-ray source for projection lithography are discussed. The design concepts of the x-ray optics that are required to collect and condition the radiation in divergence, uniformity and direction to properly illuminate the mask and the particular x-ray projection camera used are discussed. Preliminary designs for an entire soft x-ray projection lithography system using an electron storage ring as a soft X-ray source are presented. It is shown that by combining the existing technology of storage rings with large collection angle condensers, a powerful and reliable source of 130 Angstrom photons for production line projection x-ray lithography is possible

  6. Synchrotron radiation induced x-ray micro analysis: A realistic alternative for electron- and ion beam microscopy?

    International Nuclear Information System (INIS)

    Janssens, K.; Adams, F.

    1992-01-01

    Synchrotron Radiation induced X-ray micro Fluorescence analysis (μ-SRXRF) is compared with more conventional microanalytical techniques such as Secondary Ion Microscopy (SIMS) and Electron Probe X-ray Microanalysis (EPXMA) for two typical microanalytical applications. SRXRF and EPXMA are employed for the analysis of individual particles, showing the complementary character of both techniques. By means of element mapping of trace constituents in a heterogeneous feldspar, the strong and weak points of SRXRF in comparison to EPXMA and SIMS are illustrated. The most striking difference between SRXRF and the other two microanalytical methods is the ability of SRXRF to probe deep into the investigated Material, whereas SIMS and EPXMA only investigate the upper surface of the material. The possibilities of SRXRF at third generation synchrotron rings is also briefly discussed

  7. HIGH-PERFORMANCE COMPUTING FOR THE STUDY OF EARTH AND ENVIRONMENTAL SCIENCE MATERIALS USING SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY.

    Energy Technology Data Exchange (ETDEWEB)

    FENG,H.; JONES,K.W.; MCGUIGAN,M.; SMITH,G.J.; SPILETIC,J.

    2001-10-12

    Synchrotron x-ray computed microtomography (CMT) is a non-destructive method for examination of rock, soil, and other types of samples studied in the earth and environmental sciences. The high x-ray intensities of the synchrotron source make possible the acquisition of tomographic volumes at a high rate that requires the application of high-performance computing techniques for data reconstruction to produce the three-dimensional volumes, for their visualization, and for data analysis. These problems are exacerbated by the need to share information between collaborators at widely separated locations over both local and tide-area networks. A summary of the CMT technique and examples of applications are given here together with a discussion of the applications of high-performance computing methods to improve the experimental techniques and analysis of the data.

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

    Science.gov (United States)

    Uysal, Ahmet

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

  9. Synchrotron X-ray adaptative monochromator: study and realization of a prototype; Monochromateur adaptatif pour rayonnement X synchrotron: etude et realisation d`un prototype

    Energy Technology Data Exchange (ETDEWEB)

    Dezoret, D.

    1995-12-12

    This work presents a study of a prototype of a synchrotron X-ray monochromator. The spectral qualities of this optic are sensitive to the heat loads which are particularly important on third synchrotron generation like ESRF. Indeed, powers generated by synchrotron beams can reach few kilowatts and power densities about a few tens watts per square millimeters. The mechanical deformations of the optical elements of the beamlines issue issue of the heat load can damage their spectral efficiencies. In order to compensate the deformations, wa have been studying the transposition of the adaptive astronomical optics technology to the x-ray field. First, we have considered the modifications of the spectral characteristics of a crystal induced by x-rays. We have established the specifications required to a technological realisation. Then, thermomechanical and technological studies have been required to transpose the astronomical technology to an x-ray technology. After these studies, we have begun the realisation of a prototype. This monochromator is composed by a crystal of silicon (111) bonded on a piezo-electric structure. The mechanical control is a loop system composed by a infrared light, a Shack-Hartmann CDD and wave front analyser. This system has to compensate the deformations of the crystal in the 5 kcV to 60 kcV energy range with a power density of 1 watt per square millimeters. (authors).

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

    Science.gov (United States)

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

    2009-08-01

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

  11. Design status of the 2.5 GeV National Synchrotron Light Source x-ray ring

    International Nuclear Information System (INIS)

    Krinsky, S.; Blumberg, L.; Bittner, J.; Galayda, J.; Heese, R.; Schuchman, J.C.; van Steenbergen, A.

    1979-01-01

    The present state of the design of the 2.5 GeV electron storage ring for the National Synchrotron Light Source is described. This ring will serve as a dedicated source of synchrotron radiation in the wavelength range 0.1 A to 30 A. While maintaining the basic high brigtness features of the eariler developed lattice structure, recent work resulted in a more economical magnet system, is simplified chromaticity corrections, and improved distribution of the X-ray beam lines. In addition, the adequacy of the dynamic aperture for stable betatron oscillations has been verified for a variety of betatron tunes

  12. Demonstration experiment of a laser synchrotron source for tunable, monochromatic x-rays at 500 eV

    Energy Technology Data Exchange (ETDEWEB)

    Ting, A.; Fischer, R.; Fisher, A. [Naval Research Lab., Washington, DC (United States)] [and others

    1995-12-31

    A Laser Synchrotron Source (LSS) was proposed to generate short-pulsed, tunable x-rays by Thomson scattering of laser photons from a relativistic electron beam. A proof-of-principle experiment was performed to generate x-ray photons of 20 eV. A demonstration experiment is being planned and constructed to generate x-ray photons in the range of {approximately}500 eV. Laser photons of {lambda}=1.06 {mu}m are Thomson backscattered by a 4.5 MeV electron beam which is produced by an S-band RF electron gun. The laser photons are derived from either (i) a 15 Joules, 3 nsec Nd:glass laser, (ii) the uncompressed nsec: pulse of the NRL table-top terawatt (T{sup 3}) laser, or (iii) the compressed sub-picosec pulse of the T{sup 3} laser. The RF electron gun is being constructed with initial operation using a thermionic cathode. It will be upgraded to a photocathode to produce high quality electron beams with high current and low emittance. The x-ray pulse structure consists of {approximately}10 psec within an envelope of a macropulse whose length depends on the laser used. The estimated x-ray photon flux is {approximately}10{sup 18} photons/sec, and the number of photons per macropulse is {approximately}10{sup 8}. Design parameters and progress of the experiment will be presented.

  13. CCD[charge-coupled device]-based synchrotron x-ray detector for protein crystallography: Performance projected from an experiment

    International Nuclear Information System (INIS)

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

    1986-01-01

    The intense x radiation from a synchrotron source could, with a suitable detector, provide a complete set of diffraction images from a protein crystal before the crystal is damaged by radiation (2 to 3 min). An area detector consisting of a 40 mm dia. x-ray fluorescing phosphor, coupled with an image intensifier and lens to a CCD image sensor, was developed to determine the effectiveness of such a detector in protein crystallography. The detector was used in an experiment with a rotating anode x-ray generator. Diffraction patterns from a lysozyme crystal obtained with this detector are compared to those obtained with film. The two images appear to be virtually identical. The flux of 10 4 x-ray photons/s was observed on the detector at the rotating anode generator. At the 6-GeV synchrotron being designed at Argonne, the flux on an 80 x 80 mm 2 detector is expected to be >10 9 photons/s. The projected design of such a synchrotron detector shows that a diffraction-peak count >10 6 could be obtained in ∼0.5 s. With an additional ∼0.5 s readout time of a 512 x 512 pixel CCD, the data acquisition time per frame would be ∼1 s so that ninety 1 0 diffraction images could be obtained, with approximately 1% precision, in less than 3 min

  14. Ion distributions at charged aqueous surfaces: Synchrotron X-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Bu, Wei [Iowa State Univ., Ames, IA (United States)

    2009-01-01

    Surface sensitive synchrotron X-ray scattering studies were performed to obtain the distribution of monovalent ions next to a highly charged interface at room temperature. To control surface charge density, lipids, dihexadecyl hydrogen-phosphate (DHDP) and dimysteroyl phosphatidic acid (DMPA), were spread as monolayer materials at the air/water interface, containing CsI at various concentrations. Five decades in bulk concentrations (CsI) are investigated, demonstrating that the interfacial distribution is strongly dependent on bulk concentration. We show that this is due to the strong binding constant of hydronium H3O+ to the phosphate group, leading to proton-transfer back to the phosphate group and to a reduced surface charge. Using anomalous reflectivity off and at the L3 Cs+ resonance, we provide spatial counterion (Cs+) distributions next to the negatively charged interfaces. The experimental ion distributions are in excellent agreement with a renormalized surface charge Poisson-Boltzmann theory for monovalent ions without fitting parameters or additional assumptions. Energy Scans at four fixed momentum transfers under specular reflectivity conditions near the Cs+ L3 resonance were conducted on 10-3 M CsI with DHDP monolayer materials on the surface. The energy scans exhibit a periodic dependence on photon momentum transfer. The ion distributions obtained from the analysis are in excellent agreement with those obtained from anomalous reflectivity measurements, providing further confirmation to the validity of the renormalized surface charge Poisson-Boltzmann theory for monovalent ions. Moreover, the dispersion corrections f0 and f00 for Cs+ around L3 resonance, revealing the local environment of a Cs+ ion in the solution at the interface, were extracted simultaneously with output of ion distributions.

  15. Visualizing Metal Content and Intracellular Distribution in Primary Hippocampal Neurons with Synchrotron X-Ray Fluorescence.

    Directory of Open Access Journals (Sweden)

    Robert A Colvin

    Full Text Available Increasing evidence suggests that metal dyshomeostasis plays an important role in human neurodegenerative diseases. Although distinctive metal distributions are described for mature hippocampus and cortex, much less is known about metal levels and intracellular distribution in individual hippocampal neuronal somata. To solve this problem, we conducted quantitative metal analyses utilizing synchrotron radiation X-Ray fluorescence on frozen hydrated primary cultured neurons derived from rat embryonic cortex (CTX and two regions of the hippocampus: dentate gyrus (DG and CA1. Comparing average metal contents showed that the most abundant metals were calcium, iron, and zinc, whereas metals such as copper and manganese were less than 10% of zinc. Average metal contents were generally similar when compared across neurons cultured from CTX, DG, and CA1, except for manganese that was larger in CA1. However, each metal showed a characteristic spatial distribution in individual neuronal somata. Zinc was uniformly distributed throughout the cytosol, with no evidence for the existence of previously identified zinc-enriched organelles, zincosomes. Calcium showed a peri-nuclear distribution consistent with accumulation in endoplasmic reticulum and/or mitochondria. Iron showed 2-3 distinct highly concentrated puncta only in peri-nuclear locations. Notwithstanding the small sample size, these analyses demonstrate that primary cultured neurons show characteristic metal signatures. The iron puncta probably represent iron-accumulating organelles, siderosomes. Thus, the metal distributions observed in mature brain structures are likely the result of both intrinsic neuronal factors that control cellular metal content and extrinsic factors related to the synaptic organization, function, and contacts formed and maintained in each region.

  16. Accommodation stresses in hydride precipitates by synchrotron x-ray diffraction

    International Nuclear Information System (INIS)

    Santisteban, J R; Vicente, M A; Vizcaino, P; Banchik, A D; Almer, J

    2012-01-01

    Hydride-forming materials (Zr, Ti, Nb, etc) are affected by a sub-critical crack growth mechanism that involves the diffusion of H to the stressed region ahead of a crack, followed by nucleation and fracture of hydrides at the crack tip [1]. The phenomenon is intermittent, with the crack propagating through the hydride and stopping when it reaches the matrix. By repeating these processes, the crack propagates through a component at a rate that is highly dependent on the temperature history of the component. Most research effort to understand this phenomenon has occurred within the nuclear industry, as it affects the safe operation of pressure tubes (Zr2.5%Nb) and the long-term storage of nuclear fuel (Zircaloy cladding). Stress-induced hydride formation is a consequence of the volume dilatation that accompanies hydride formation (of the order of 15%), which is elastoplastically accommodated by the matrix and precipitate. Compressive stresses are expected within hydride precipitates due to the constraint imposed by the matrix. Such 'accommodation' stresses are essential ingredients in all theoretical models developed to assess the crack growth rate dependence on operational variables such as temperature, applied stress intensity factor, or overall H concentration [2]. Yet little experimental information is available about the magnitude and directionality of such accommodation stresses. Synchrotron X-ray diffraction is the only technique capable of quantifying such stresses. Here we briefly describe the fundaments of the technique, when used through an area detector placed in transmission geometry. The results of the experiments have allowed us to produce a comprehensive picture about the magnitude and origin of accommodation stresses in δ zirconium hydride platelets (author)

  17. Lead tolerance and cellular distribution in Elsholtzia splendens using synchrotron radiation micro-X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jie [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); Tian, Shengke [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); University of Florida, Institute of Food and Agricultural Science, Indian River Research and Education Center, Fort Pierce, FL 34945 (United States); Lu, Lingli; Shohag, M.J.I.; Liao, Haibing [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); Yang, Xiaoe, E-mail: xyang@zju.edu.cn [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Elsholtzia splendens had a good ability of lead tolerance and accumulation. Black-Right-Pointing-Pointer Pb was mostly restricted to the vascular bundles and epidermis tissues. Black-Right-Pointing-Pointer Pb and Ca shared most similar distribution patterns in E. splendens. - Abstract: Hydroponic experiments were conducted to investigate the tolerance and spatial distribution of lead (Pb) in Elsholtzia splendens-a copper (Cu) accumulator plant using synchrotron-based micro-X-ray fluorescence. According to chlorophyll concentration and chlorophyll fluorescence parameters, E. splendens displayed certain tolerance at 100 {mu}M Pb treatment. Lead concentration in roots, stems and leaves of E. splendens reached 45,183.6, 1657.6, and 380.9 mg kg{sup -1}, respectively. Pb was mostly accumulated in the roots, and there were also high concentrations of Pb been transported into stems and leaves. Micro-XRF analysis of the stem and leaf cross section revealed that Pb was mostly restricted in the vascular bundles and epidermis tissues of both stem and leaf of E. splendens. The correlation between distribution of K, Ca, Zn and Pb were analyzed. There were significant positive correlations (P < 0.01) among Pb and Ca, K, Zn distribution both in stem and leaf of E. splendens. However, among the three elements, Ca shared the most similar distribution pattern and the highest correlation coefficients with Pb in both stem and leaf cross section of E. splendens. This suggests that Ca may play an important role in Pb accumulation in stem and leaf of E. splendens.

  18. Development of synchrotron x-ray micro-spectroscopic techniques and application to problems in low temperature geochemistry. Progress report

    Energy Technology Data Exchange (ETDEWEB)

    1993-10-01

    The focus of the technical development effort has been the development of apparatus and techniques for the utilization of X-ray Fluorescence (XRF), Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Absorption Near Edge Structure (XANES) spectroscopies in a microprobe mode. The present XRM uses white synchrotron radiation (3 to 30 keV) from a bending magnet for trace element analyses using the x-ray fluorescence technique Two significant improvements to this device have been recently implemented. Focusing Mirror: An 8:1 ellipsoidal mirror was installed in the X26A beamline to focus the incident synchrotron radiation and thereby increase the flux on the sample by about a factor of 30. Incident Beam Monochromator: The monochromator has been successfully installed and commissioned in the X26A beamline upstream of the mirror to permit analyses with focused monochromatic radiation. The monochromator consists of a channel-cut silicon (111) crystal driven by a Klinger stepping motor translator. We have demonstrated the operating range of this instrument is 4 and 20 keV with 0.01 eV steps and produces a beam with a {approximately}10{sup {minus}4} energy bandwidth. The primary purpose of the monochromator is for x-ray absorption spectroscopy (XAS) measurements but it is also used for selective excitation in trace element microanalysis. To date, we have conducted XANES studies on Ti, Cr, Fe, Ce and U, spanning the entire accessible energy range and including both K and L edge spectra. Practical detection limits for microXANES are 10--100 ppM for 100 {mu}m spots.

  19. A novel technique combining high-resolution synchrotron x-ray microtomography and x-ray diffraction for characterization of micro particulates

    International Nuclear Information System (INIS)

    Merrifield, David R; Ramachandran, Vasuki; Roberts, Kevin J; Armour, Wesley; Axford, Danny; Basham, Mark; Connolley, Thomas; Evans, Gwyndaf; McAuley, Katherine E; Owen, Robin L; Sandy, James

    2011-01-01

    The processing of solids, such as crystals, is strongly influenced by the surface properties of the material. In recent years the pharmaceutical industry has shown great interest in identifying, or chemically speciating, the molecular components of crystal faces. Formerly, characterization of the molecular identity of crystal faces was restricted to the study of large single crystals. This would have been primarily for structure determination as part of the drug registration process. Diamond Light Source in Oxfordshire is a new synchrotron facility in the UK, having 18 operational beamlines with 4 more in the construction phase. Beamlines at this medium energy light source enable the study of micron-sized objects in great detail. It is well known that x-ray microtomography (XMT) can be used to investigate the external morphology of a crystal whereas x-ray diffraction (XRD) is used to study the molecular orientation, structure and packing within the crystal. The objective of this research is to assess the feasibility of, and thereby develop a new methodology for, characterizing the molecular identity of a particular face of a crystalline particle at a scale of scrutiny of 20–50 µm by combining these two powerful techniques. This work demonstrates the application of XMT and XRD to investigate respectively the shape and crystalline phase/orientation of relevant test crystals. This research has applications in the pharmaceutical industry in that when the exact molecular nature of a particular face is known, the important physico-pharmaceutical properties stemming from that can be better understood. Some initial data are presented and discussed

  20. 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...

  1. A redox equilibrator for the preparation of cytochrome oxidase of mixed valence states and intermediate compounds for x-ray synchrotron studies

    International Nuclear Information System (INIS)

    Chance, B.; Moore, J.; Powers, L.; Ching, Y.

    1982-01-01

    A redox titrator for the preparation of small volumes of highly concentrated biological samples of X-ray synchrotron studies provides for the redox equilibration at temperatures of 40 to -30 0 C. Anaerobic transfer directly to the X-ray sample chamber and mixing of an additional reagent just prior to freeze-trapping of the redox-equilibrated sample are provided

  2. X-ray television area detectors for macromolecular structural studies with synchrotron radiation sources

    International Nuclear Information System (INIS)

    Arndt, U.W.; Gilmore, D.J.

    1978-01-01

    Two-dimensional X-ray diffraction patterns may be recorded quantitatively by means of X-ray-to-electron converters which are scanned in a television-type raster scan. Detectors of this type are capable of operating over the whole range of counting rates from very low to higher than those with which other types of converters can deal. The component parts of an X-ray television detector are examined and the limits to the precision of the measurements are analysed. (Auth.)

  3. Synchrotron-radiation-induced formation of salt particles on an X-ray lithography mask

    International Nuclear Information System (INIS)

    Utsumi, Y.; Takahashi, J.; Hosokawa, T.

    1998-01-01

    The suppression and removal of contaminants on X-ray masks are required for the application of X-ray lithography to practical semiconductor production, because contamination is easily transferred to the replicated resist patterns and degrades the LSI patterns in order to study contamination of a Ta/SiN X-ray mask, its growth process was investigated using an atmospheric reaction chamber and in situ observation apparatus for gases at atmospheric pressure. It was found that the contamination particles were ammonium sulfate and oxalate. The sources of the salt particle were also identified

  4. 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

  5. Measurements of internal stresses in bond coating using high energy x-rays from synchrotron radiation source

    CERN Document Server

    Suzuki, K; Akiniwa, Y; Nishio, K; Kawamura, M; Okado, H

    2002-01-01

    Thermal barrier coating (TBC) techniques enable high temperature combustion of turbines made of Ni-base alloy. TBC is made of zirconia top coating on NiCoCrAlY bond coating. The internal stresses in the bond coating play essential role in the delamination or fracture of TBC in service. With the X-rays from laboratory equipments, it is impossible to measure nondestructively the internal stress in the bond coating under the top coating. synchrotron radiations with a high energy and high brightness have a large penetration depth as compared with laboratory X-rays. Using the high energy X-rays from the synchrotron radiation, it is possible to measure the internal stress in the bond coating through the top coating. In this study, the furnace, which can heat a specimen to 1473 K, was developed for the stress measurement of the thermal barrier coatings. The internal stresses in the bond coating were measured at the room temperature, 773 K, 1073 K and 1373 K by using the 311 diffraction from Ni sub 3 Al with about 73...

  6. Characterization of porosity in a 19th century painting ground by synchrotron radiation X-ray tomography

    Energy Technology Data Exchange (ETDEWEB)

    Gervais, Claire [Swiss Institute for Art Research (SIK-ISEA), Zuerich (Switzerland); Bern University of the Arts, Bern (Switzerland); Boon, Jaap J. [Swiss Institute for Art Research (SIK-ISEA), Zuerich (Switzerland); JAAP Enterprise for MOLART Advice, Amsterdam (Netherlands); Marone, Federica [Paul Scherrer Institute, Swiss Light Source (SLS), Villigen (Switzerland); Ferreira, Ester S.B. [Swiss Institute for Art Research (SIK-ISEA), Zuerich (Switzerland)

    2013-04-15

    The study of the early oeuvre of the Swiss painter Cuno Amiet (1868-1961) has revealed that, up to 1907, many of his grounds were hand applied and are mainly composed of chalk, bound in protein. These grounds are not only lean and absorbent, but also, as Synchrotron radiation X-ray microtomography has shown, porous. Our approach to the characterization of pore structure and quantity, their connectivity, and homogeneity is based on image segmentation and application of a clustering algorithm to high-resolution X-ray tomographic data. The issues associated with the segmentation of the different components of a ground sample based on X-ray imaging data are discussed. The approach applied to a sample taken from ''Portrait of Max Leu'' (1899) by Amiet revealed the presence of three sublayers within the ground with distinct porosity features, which had not been observed optically in cross-section. The upper and lower layers are highly porous with important connectivity and thus prone to water uptake/storage. The middle layer however shows low and nonconnected porosity at the resolution level of the X-ray tomography images, so that few direct water absorption paths through the entire sample exist. The potential of the method to characterize porosity and to understand moisture-related issues in paint layer degradation are discussed. (orig.)

  7. Application of synchrotron x-ray microbeam spectroscopy to the determination of metal distribution and speciation in biological tissues

    Energy Technology Data Exchange (ETDEWEB)

    Punshon, T.; Jackson, B.P.; Lanzirotti, A.; Hopkins, W.A.; Bertsch, P.M.; Burger, J. [Rutgers State University, Piscataway, NJ (United States). Division of Life Science

    2005-07-01

    Resolving the distribution and speciation of metal(loid)s within biological environmental samples is essential for understanding bioavailability, trophic transfer, and environmental risk. We used synchrotron x-ray microspectroscopy to analyze a range of samples that had been exposed to metal(loid) contamination. Microprobe x-ray fluorescence elemental mapping ({mu} SXRF) of decomposing rhizosphere microcosms consisting of Ni- and U-contaminated soil planted with wheat (Triticum aestivum) showed the change in Ni and U distribution over a 27-day period, with a progressive movement of U into decaying tissue. mu SXRF maps showed the micrometer-scale distribution of Ca, Mn, Fe, Ni, and U in roots of willow (Salix nigra L.) growing on a former radiological settling pond, with U located outside of the epidermis and Ni inside the cortex. X-ray computed tomography (CMT) of woody tissue of this same affected willow showed that small points of high Ni fluorescence observed previously are actually a Ni-rich substance contained within an individual xylem vessel. {mu} SXRF and x-ray absorption near-edge spectroscopy (XANES) linked the elevated Se concentrations in sediments of a coal fly ash settling pond with oral deformities of bullfrog tadpoles (Rana catesbeiana). Se distribution was localized within the deformed mouthparts, and with an oxidation state of Se (-II) consistent with organo-Se compounds, it suggests oral deformities are caused by incorporation of Se into proteins.

  8. Characterization of porosity in a 19th century painting ground by synchrotron radiation X-ray tomography

    International Nuclear Information System (INIS)

    Gervais, Claire; Boon, Jaap J.; Marone, Federica; Ferreira, Ester S.B.

    2013-01-01

    The study of the early oeuvre of the Swiss painter Cuno Amiet (1868-1961) has revealed that, up to 1907, many of his grounds were hand applied and are mainly composed of chalk, bound in protein. These grounds are not only lean and absorbent, but also, as Synchrotron radiation X-ray microtomography has shown, porous. Our approach to the characterization of pore structure and quantity, their connectivity, and homogeneity is based on image segmentation and application of a clustering algorithm to high-resolution X-ray tomographic data. The issues associated with the segmentation of the different components of a ground sample based on X-ray imaging data are discussed. The approach applied to a sample taken from ''Portrait of Max Leu'' (1899) by Amiet revealed the presence of three sublayers within the ground with distinct porosity features, which had not been observed optically in cross-section. The upper and lower layers are highly porous with important connectivity and thus prone to water uptake/storage. The middle layer however shows low and nonconnected porosity at the resolution level of the X-ray tomography images, so that few direct water absorption paths through the entire sample exist. The potential of the method to characterize porosity and to understand moisture-related issues in paint layer degradation are discussed. (orig.)

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

    Science.gov (United States)

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

    2015-11-01

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

  10. Phased-Resolved Strain Measuremetns in Hydrated Ordinary Portland Cement Using Synchrotron x-Rays (Prop. 2003-033)

    International Nuclear Information System (INIS)

    Biernacki, Joseph J.; Watkins, Thomas R.; Parnham, C.J.; Hubbard, Camden R.; Bai, J.

    2006-01-01

    X-ray diffraction methods developed for the determination of residual stress states in crystalline materials have been applied to study residual strains and strains because of mechanical loading of ordinary portland cement paste. Synchrotron X-rays were used to make in situ measurements of interplanar spacings in the calcium hydroxide (CH) phase of hydrated neat portland cement under uniaxial compression. The results indicate that strains on the order of 1/100 000 can be resolved providing an essentially new technique by which to measure the phase-resolved meso-scale mechanical behavior of cement under different loading conditions. Evaluation of these strain data in view of published elastic parameters for CH suggests that the CH carries a large fraction of the applied stress and that plastic interactions with the matrix are notable.

  11. Fabrication Of Supersmooth Spherical Quartz Blank For Soft X-Ray Synchrotron Radiation Grating Monochromator In China

    Science.gov (United States)

    Changxin, Zhou; Deming, Shu; Wuming, Liu

    1989-07-01

    A spherical grating monochromator (SGM) has been designed and installed in beamline 48913 at Beijing Electron Positron Collider (BEPC) for synchrotron radiation soft x-ray photoemission experiments. There are four laminar gratings in this monochromator to covering the region of 10 -1100ev. On three of them, which covering the soft x-ray range, a supersmooth blank surface with large radial (57M) and high figuring accuracy (>λ/50) is required to suit the monochromator high resolving power desgn (>2000) and reduce the beam power loss. In this paper, the methods of fabrication and metrology has been described, the test results of this plank using WYKO and ZYGO show that the surface roughness of this blank is about 2Å RMS with 0.014 figure tolerance.

  12. Discovery and Structure Determination of an Unusual Sulfide Telluride through an Effective Combination of TEM and Synchrotron Microdiffraction.

    Science.gov (United States)

    Fahrnbauer, Felix; Rosenthal, Tobias; Schmutzler, Tilo; Wagner, Gerald; Vaughan, Gavin B M; Wright, Jonathan P; Oeckler, Oliver

    2015-08-17

    The structure elucidation of the novel sulfide telluride Pb8Sb8S15Te5 demonstrates a new versatile procedure that exploits the synergism of electron microscopy and synchrotron diffraction methods for accurate structure analyses of side-phases in heterogeneous microcrystalline samples. Suitable crystallites of unknown compounds can be identified by transmission electron microscopy and relocated and centered in a microfocused synchrotron beam by means of X-ray fluorescence scans. The refined structure model is then confirmed by simulating HRTEM images of the same crystallite. Pb8Sb8S15Te5 consists of chains of heterocubane-like units. Cation coordination polyhedra form unusually entwined chains of edge- and face-sharing bicapped trigonal prisms. The structure data are precise enough for bond-valence calculations, which confirm the disordered atom distribution. On this basis, optimization of physical properties becomes feasible. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Gadolinium Deposition in Nephrogenic Systemic Fibrosis: An Examination of Tissue using Synchrotron X-ray Fluorescence Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    High, W.; Ranville, J; Brown, M; Punshon, T; Lanzirotti, A; Jackson, B

    2010-01-01

    Nephrogenic systemic fibrosis is a fibrosing disorder associated with gadolinium (Gd)-based contrast agents dosed during renal insufficiency. In two patients, Gd deposition in tissue affected by nephrogenic systemic fibrosis was quantified using inductively coupled plasma mass spectrometry. The presence of Gd was confirmed and mapped using synchrotron x-ray fluorescence spectroscopy. Affected skin and soft tissue from the lower extremity demonstrated 89 and 209 ppm ({micro}g/g, dry weight, formalin fixed) in cases 1 and 2, respectively. In case 2, the same skin and soft tissue was retested after paraffin embedding, with the fat content removed by xylene washes, and this resulted in a measured value of 189 ppm ({micro}g/g, dry weight, paraffin embedded). Synchrotron x-ray fluorescence spectroscopy confirmed Gd in the affected tissue of both cases, and provided high-sensitivity and high-resolution spatial mapping of Gd deposition. A gradient of Gd deposition in tissue correlated with fibrosis and cellularity. Gd deposited in periadnexal locations within the skin, including hair and eccrine ducts, where it colocalized to areas of high calcium and zinc content. Because of the difficulty in obtaining synchrotron x-ray fluorescence spectroscopy scans, tissue from only two patients were mapped. A single control with kidney disease and gadolinium-based contrast agent exposure did not contain Gd. Gd content on a gravimetric basis was impacted by processing that removed fat and altered the dry weight of the specimens. Gradients of Gd deposition in tissue corresponded to fibrosis and cellularity. Adnexal deposition of Gd correlated with areas of high calcium and zinc content.

  14. 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.

  15. 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

    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......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...

  16. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography.

    Science.gov (United States)

    Umetani, K; Fukushima, K

    2013-03-01

    An X-ray intravital microscopy technique was developed to enable in vivo visualization of the coronary, cerebral, and pulmonary arteries in rats without exposure of organs and with spatial resolution in the micrometer range and temporal resolution in the millisecond range. We have refined the system continually in terms of the spatial resolution and exposure time. X-rays transmitted through an object are detected by an X-ray direct-conversion type detector, which incorporates an X-ray SATICON pickup tube. The spatial resolution has been improved to 6 μm, yielding sharp images of small arteries. The exposure time has been shortened to around 2 ms using a new rotating-disk X-ray shutter, enabling imaging of beating rat hearts. Quantitative evaluations of the X-ray intravital microscopy technique were extracted from measurements of the smallest-detectable vessel size and detection of the vessel function. The smallest-diameter vessel viewed for measurements is determined primarily by the concentration of iodinated contrast material. The iodine concentration depends on the injection technique. We used ex vivo rat hearts under Langendorff perfusion for accurate evaluation. After the contrast agent is injected into the origin of the aorta in an isolated perfused rat heart, the contrast agent is delivered directly into the coronary arteries with minimum dilution. The vascular internal diameter response of coronary arterial circulation is analyzed to evaluate the vessel function. Small blood vessels of more than about 50 μm diameters were visualized clearly at heart rates of around 300 beats/min. Vasodilation compared to the control was observed quantitatively using drug manipulation. Furthermore, the apparent increase in the number of small vessels with diameters of less than about 50 μm was observed after the vasoactive agents increased the diameters of invisible small blood vessels to visible sizes. This technique is expected to offer the potential for direct

  17. Conventional and Synchrotron X-Ray Topography of Defects in the Core Region of SrLaGaO4

    International Nuclear Information System (INIS)

    Malinowska, A.; Lefeld-Sosnowska, M.; Wieteska, K.; Wierzchowski, W.; Pajaczkowska, A.; Graeff, W.

    2008-01-01

    SrLaGaO 4 single crystals are perspective substrate materials for high temperature superconductors thin films, elements of thermal radiation receivers and other electronic devices. The defect structure of the Czochralski grown SrLaGaO 4 crystal was investigated by means of X-ray topography exploring both conventional and synchrotron sources. The crystal lattice defects in the core region of the crystal were investigated. The regular network of defects arranged in rows only in direction was observed. Owing to high resolution of synchrotron radiation white beam back reflection topographs one can distinguish individual spots forming the lines of the rows. It can be supposed that these elongated rod-like volume defects are located in f100g lattice planes forming a kind of walls. They are built approximately of the same phase as crystal but crystallize at a different moment than a rest of the crystal due to the constitutional supercooling. (authors)

  18. Individual particle analysis of coarse air suspended particulate material by synchrotron radiation X-ray micro fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Melo Junior, Ariston [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Perez, Carlos Alberto [Laboratorio Nacional de Luz Sincrotron (LNLS), Campinas, SP (Brazil)]. E-mail: perez@lnls.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    The purpose of this work is evaluate the size of individual particles present in the air suspended particulate material collected in Campinas, Sao Paulo State, and analyze quantitatively the particles using the synchrotron radiation X-ray micro fluorescence ({mu}-SRXRF) associated with the fundamental parameter method to correct attenuation/absorption effects by the matrix. The particles analyzed have size between 50-10 {mu}m and to perform the spatial distribution a white beam of synchrotron radiation condensed by a conical capillary (13 {mu}m diameter) was used. For the quantitative analysis punctual measures in thin films standards in Mylar subtract were performed. The elements detected were Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. (author)

  19. Individual particle analysis of coarse air suspended particulate material by synchrotron radiation X-ray micro fluorescence

    International Nuclear Information System (INIS)

    Moreira, Silvana; Melo Junior, Ariston; Vives, Ana Elisa S. de; Nascimento Filho, Virgilio F.

    2005-01-01

    The purpose of this work is evaluate the size of individual particles present in the air suspended particulate material collected in Campinas, Sao Paulo State, and analyze quantitatively the particles using the synchrotron radiation X-ray micro fluorescence (μ-SRXRF) associated with the fundamental parameter method to correct attenuation/absorption effects by the matrix. The particles analyzed have size between 50-10 μm and to perform the spatial distribution a white beam of synchrotron radiation condensed by a conical capillary (13 μm diameter) was used. For the quantitative analysis punctual measures in thin films standards in Mylar subtract were performed. The elements detected were Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. (author)

  20. Multielemental analysis in organic products and seed of linum by X-ray total reflection fluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Lab. de Instrumentacao Nuclear]. E-mail: renata@lin.ufrj.br; Carmo, Maria da Graca T. do [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Nutricao; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fec.com.br

    2005-07-01

    The main goal of this study is to determining the trace and major elements levels in organic seeds samples, like soy, rice, bean and in Brazilian and Canadian linum seed by X-ray Total Reflection Fluorescence with Synchrotron Radiation (SR-TXRF). The measurements were carried out in the XRF beamline at the Light Synchrotron National Laboratory (Campinas, Brazil). The organic soy presented major concentrations of P, Ca, Ti, Fe, Ni, Cu, Zn, Br, Rb and Sr than organic bean and rice. Brazilian linum samples presented higher concentrations of S, P, Ca, Ni, Cu, Sr, Zr and Mo than Canadian one, even than organic samples. However potassium, iron and zinc were more pronounced in the Canadian seed of linum (author)

  1. Synchrotron x-ray fluorescence analyses of stratospheric cosmic dust: New results for chondritic and nickel-depleted particles

    International Nuclear Information System (INIS)

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

    1989-06-01

    Trace element abundance determinations were performed using synchrotron x-ray fluorescence on nine particles collected from the stratosphere and classified as ''cosmic''. Improvements to the Synchrotron Light Source allowed the detection of all elements between Cr and Mo, with the exceptions of Co and As, in our largest particle. The minor and trace element abundance patterns of three Ni-depleted particles were remarkably similar to those of extraterrestrial igneous rocks. Fe/Ni and Fe/Mn ratios suggest that one of these may be of lunar origin. All nine particles exhibited an enrichment in Br, ranging form 1.3 to 38 times the Cl concentration. Br concentrations were uncorrelated with particle size, as would be expected for a surface correlated component acquires from the stratosphere. 27 refs., 4 figs., 2 tabs

  2. A powerful flare from Sgr A* confirms the synchrotron nature of the X-ray emission

    NARCIS (Netherlands)

    Ponti, G.; George, E.; Scaringi, S.; Zhang, S.; Jin, C.; Dexter, J.; Terrier, R.; Clavel, M.; Degenaar, N.; Eisenhauer, F.; Genzel, R.; Gillessen, S.; Goldwurm, A.; Habibi, M.; Haggard, D.; Hailey, C.; Harrison, F.; Merloni, A.; Mori, K.; Nandra, K.; Ott, T.; Pfuhl, O.; Plewa, P.M.; Waisberg, I.

    2017-01-01

    We present the first fully simultaneous fits to the near-infrared (NIR) and X-ray spectral slope (and its evolution) during a very bright flare from Sgr A*, the supermassive black hole at the Milky Way's centre. Our study arises from ambitious multiwavelength monitoring campaigns with XMM-Newton,

  3. Report of the fifth workshop on synchrotron x-ray lithography

    International Nuclear Information System (INIS)

    Williams, G.P.; Godel, J.B.; Brown, G.S.

    1989-01-01

    Semiconductors comprise a greater part of the United States economy than the aircraft, steel and automobile industries combined. In future the semiconductor manufacturing industry will be forced to switch away from present optical manufacturing methods in the early to mid 1990's. X-ray lithography has emerged as the leading contender for continuing production below the 0.4 micron level. Brookhaven National Laboratory began a series of workshops on x-ray lithography in 1986 to examine key issues and in particular to enable United States industry to take advantage of the technical base established in this field. Since accelerators provide the brightest sources for x-ray lithography, most of the research and development to date has taken place at large accelerator-based research centers such as Brookhaven, the University of Wisconsin and Stanford. The goals of this Fifth Brookhaven Workshop were to review progress and goals since the last workshop and to establish a blueprint for the future. The meeting focused on the ''Exposure Tool,'' that is, a term defined as the source plus beamline and stepper. In order to assess the appropriateness of schedules for the development of this tool, other aspects of the required technology such as masks, resists and inspection and repair were also reviewed. To accomplish this, two working groups were set up, one to review the overall aspects of x-ray lithography and set a time frame, the other to focus on sources

  4. Report of the fifth workshop on synchrotron x-ray lithography

    Energy Technology Data Exchange (ETDEWEB)

    Williams, G.P.; Godel, J.B. (Brookhaven National Lab., Upton, NY (USA)); Brown, G.S. (Stanford Univ., CA (USA). Stanford Synchrotron Radiation Lab.); Liebmann, W. (Suss (Karl) America, Essex Junction, VT (USA))

    1989-01-01

    Semiconductors comprise a greater part of the United States economy than the aircraft, steel and automobile industries combined. In future the semiconductor manufacturing industry will be forced to switch away from present optical manufacturing methods in the early to mid 1990's. X-ray lithography has emerged as the leading contender for continuing production below the 0.4 micron level. Brookhaven National Laboratory began a series of workshops on x-ray lithography in 1986 to examine key issues and in particular to enable United States industry to take advantage of the technical base established in this field. Since accelerators provide the brightest sources for x-ray lithography, most of the research and development to date has taken place at large accelerator-based research centers such as Brookhaven, the University of Wisconsin and Stanford. The goals of this Fifth Brookhaven Workshop were to review progress and goals since the last workshop and to establish a blueprint for the future. The meeting focused on the Exposure Tool,'' that is, a term defined as the source plus beamline and stepper. In order to assess the appropriateness of schedules for the development of this tool, other aspects of the required technology such as masks, resists and inspection and repair were also reviewed. To accomplish this, two working groups were set up, one to review the overall aspects of x-ray lithography and set a time frame, the other to focus on sources.

  5. BioCARS: a synchrotron resource for time-resolved X-ray science.

    Science.gov (United States)

    Graber, T; Anderson, S; Brewer, H; Chen, Y S; Cho, H S; Dashdorj, N; Henning, R W; Kosheleva, I; Macha, G; Meron, M; Pahl, R; Ren, Z; Ruan, S; Schotte, F; Srajer, V; Viccaro, P J; Westferro, F; Anfinrud, P; Moffat, K

    2011-07-01

    BioCARS, a NIH-supported national user facility for macromolecular time-resolved X-ray crystallography at the Advanced Photon Source (APS), has recently completed commissioning of an upgraded undulator-based beamline optimized for single-shot laser-pump X-ray-probe measurements with time resolution as short as 100 ps. The source consists of two in-line undulators with periods of 23 and 27 mm that together provide high-flux pink-beam capability at 12 keV as well as first-harmonic coverage from 6.8 to 19 keV. A high-heat-load chopper reduces the average power load on downstream components, thereby preserving the surface figure of a Kirkpatrick-Baez mirror system capable of focusing the X-ray beam to a spot size of 90 µm horizontal by 20 µm vertical. A high-speed chopper isolates single X-ray pulses at 1 kHz in both hybrid and 24-bunch modes of the APS storage ring. In hybrid mode each isolated X-ray pulse delivers up to ~4 × 10(10) photons to the sample, thereby achieving a time-averaged flux approaching that of fourth-generation X-FEL sources. A new high-power picosecond laser system delivers pulses tunable over the wavelength range 450-2000 nm. These pulses are synchronized to the storage-ring RF clock with long-term stability better than 10 ps RMS. Monochromatic experimental capability with Biosafety Level 3 certification has been retained.

  6. 3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

    Science.gov (United States)

    Toda, Hiroyuki

    2014-11-01

    technique to the deformation behavior of a polycrystalline aluminium alloy will be demonstrated in the presentation [6].The synchrotron-based microtomography has been mainly utilized to light materials due to their good X-ray transmission. In the present talk, the application of the synchrotron-based microtomography to steels will be also introduced. Degradation of contrast and spatial resolution due to forward scattering could be avoided by selecting appropriate experimental conditions in order to obtain superior spatial resolution close to the physical limit even in ferrous materials [7]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  7. Microbeam X-ray fluorescence mapping of Cu and Fe in human prostatic carcinoma cell lines using synchrotron radiation

    International Nuclear Information System (INIS)

    Rocha, K.M.J.; Leitao, R.G.; Oliveira-Barros, E.G.; Oliveira, M.A.; Canellas, C.G.L.; Anjos, M.J.; Nasciutti, L.E.; Lopes, R.T.; Universidade Federal do Rio de Janeiro; Universidade do Estado do Rio de Janeiro

    2017-01-01

    Cancer is a worldwide public health problem and prostate cancer continues to be one of the most common fatal cancers in men. Copper plays an important role in the aetiology and growth of tumours however, whether intratumoral copper is actually elevated in prostate cancer patients has not been established. Iron, an important trace element, plays a vital function in oxygen metabolism, oxygen uptake, and electron transport in mitochondria, energy metabolism, muscle function, and hematopoiesis. The X-ray microfluorescence technique (μXRF) is a rapid and non-destructive method of elemental analysis that provides useful elemental information about samples without causing damage or requiring extra sample preparations. This study investigated the behavior of cells in spheroids of human prostate cells, tumour cell line (DU145) and normal cell line (RWPE-1), after supplementation with zinc chloride by 24 hours using synchrotron X-ray microfluorescence (μSRXRF). The measurements were performed with a standard geometry of 45 deg of incidence, excited by a white beam using a pixel of 25 μm and a time of 300 ms/pixel at the XRF beamline at the Synchrotron Light National Laboratory (Campinas, Brazil). The results by SRμXRF showed non-uniform Cu and Fe distributions in all the spheroids analyzed. (author)

  8. In situ X-ray diffraction of surface oxide on type 430 stainless steel in breakaway condition using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Saeki, Isao, E-mail: isaos@mmm.muroran-it.ac.jp [Department of Materials Science and Engineering, Muroran Institute of Technology, 27-1 Mizumoto, Muroran, Hokkaido 050-8585 (Japan); Sugiyama, Yusuke [Graduate School of Engineering, Muroran Institute of Technology, 27-1 Mizumoto, Muroran, Hokkaido 050-8585 (Japan); Hayashi, Shigenari; Yamauchi, Akira [Graduate School of Engineering, Hokkaido University, Kita 13 Nishi 8, Kita-ku, Sapporo, Hokkaido 006-8628 (Japan); Doi, Takashi; Nishiyama, Yoshitaka [Corporate R and D Laboratories, Sumitomo Metals Industries Ltd., 1-8 Fuso-cho, Amagasaki, Hyogo 660-0891 (Japan); Kyo, Shoji [Power Engineering R and D Centre, Kansai Electric Power Co., Inc., 3-11-20 Wakaoji, Amagasaki, Hyogo 661-0794 (Japan); Suzuki, Shigeru [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Sato, Masugu [Japan Synchrotron Radiation Research Institute, 1-1-1 Koto, Sayo-cho, Hyogo 679-5198 (Japan); Fujimoto, Shinji [Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan)

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer Breakaway studied with Synchrotron radiation X-ray. Black-Right-Pointing-Pointer Local equilibria between phases established during high-temperature oxidation. Black-Right-Pointing-Pointer Chemical failure model well describes the breakaway. - Abstract: Changes in the crystal structure of type 430 stainless steel and the oxides on its surface were studied in situ at 1373 K using a high-intensity synchrotron X-ray source provided by SPring-8 in Japan. The surface of the steel was initially covered with Cr{sub 2}O{sub 3}, which was then converted to FeCr{sub 2}O{sub 4}, and finally Fe{sub 3}O{sub 4} and Fe{sub 2}O{sub 3} formed on it. These results indicated that the reason for the breakaway oxidation in type 430 stainless steel is Cr depletion beneath Cr{sub 2}O{sub 3} layer and the subsequent ionisation of Fe, not the simple mechanical failure of Cr{sub 2}O{sub 3}.

  9. A compressed sensing based reconstruction algorithm for synchrotron source propagation-based X-ray phase contrast computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Melli, Seyed Ali, E-mail: sem649@mail.usask.ca [Department of Electrical and Computer Engineering, University of Saskatchewan, Saskatoon, SK (Canada); Wahid, Khan A. [Department of Electrical and Computer Engineering, University of Saskatchewan, Saskatoon, SK (Canada); Babyn, Paul [Department of Medical Imaging, University of Saskatchewan, Saskatoon, SK (Canada); Montgomery, James [College of Medicine, University of Saskatchewan, Saskatoon, SK (Canada); Snead, Elisabeth [Western College of Veterinary Medicine, University of Saskatchewan, Saskatoon, SK (Canada); El-Gayed, Ali [College of Medicine, University of Saskatchewan, Saskatoon, SK (Canada); Pettitt, Murray; Wolkowski, Bailey [College of Agriculture and Bioresources, University of Saskatchewan, Saskatoon, SK (Canada); Wesolowski, Michal [Department of Medical Imaging, University of Saskatchewan, Saskatoon, SK (Canada)

    2016-01-11

    Synchrotron source propagation-based X-ray phase contrast computed tomography is increasingly used in pre-clinical imaging. However, it typically requires a large number of projections, and subsequently a large radiation dose, to produce high quality images. To improve the applicability of this imaging technique, reconstruction algorithms that can reduce the radiation dose and acquisition time without degrading image quality are needed. The proposed research focused on using a novel combination of Douglas–Rachford splitting and randomized Kaczmarz algorithms to solve large-scale total variation based optimization in a compressed sensing framework to reconstruct 2D images from a reduced number of projections. Visual assessment and quantitative performance evaluations of a synthetic abdomen phantom and real reconstructed image of an ex-vivo slice of canine prostate tissue demonstrate that the proposed algorithm is competitive in reconstruction process compared with other well-known algorithms. An additional potential benefit of reducing the number of projections would be reduction of time for motion artifact to occur if the sample moves during image acquisition. Use of this reconstruction algorithm to reduce the required number of projections in synchrotron source propagation-based X-ray phase contrast computed tomography is an effective form of dose reduction that may pave the way for imaging of in-vivo samples.

  10. Increased cell survival and cytogenetic integrity by spatial dose redistribution at a compact synchrotron X-ray source

    Science.gov (United States)

    Ilicic, Katarina; Dierolf, Martin; Günther, Benedikt; Walsh, Dietrich W. M.; Schmid, Ernst; Eggl, Elena; Achterhold, Klaus; Gleich, Bernhard; Combs, Stephanie E.; Molls, Michael; Schmid, Thomas E.; Pfeiffer, Franz; Wilkens, Jan J.

    2017-01-01

    X-ray microbeam radiotherapy can potentially widen the therapeutic window due to a geometrical redistribution of the dose. However, high requirements on photon flux, beam collimation, and system stability restrict its application mainly to large-scale, cost-intensive synchrotron facilities. With a unique laser-based Compact Light Source using inverse Compton scattering, we investigated the translation of this promising radiotherapy technique to a machine of future clinical relevance. We performed in vitro colony-forming assays and chromosome aberration tests in normal tissue cells after microbeam irradiation compared to homogeneous irradiation at the same mean dose using 25 keV X-rays. The microplanar pattern was achieved with a tungsten slit array of 50 μm slit size and a spacing of 350 μm. Applying microbeams significantly increased cell survival for a mean dose above 2 Gy, which indicates fewer normal tissue complications. The observation of significantly less chromosome aberrations suggests a lower risk of second cancer development. Our findings provide valuable insight into the mechanisms of microbeam radiotherapy and prove its applicability at a compact synchrotron, which contributes to its future clinical translation. PMID:29049300

  11. Cracking evolution behaviors of lightweight materials based on in situ synchrotron X-ray tomography: A review

    Science.gov (United States)

    Luo, Y.; Wu, S. C.; Hu, Y. N.; Fu, Y. N.

    2018-03-01

    Damage accumulation and failure behaviors are crucial concerns during the design and service of a critical component, leading researchers and engineers to thoroughly identifying the crack evolution. Third-generation synchrotron radiation X-ray computed microtomography can be used to detect the inner damage evolution of a large-density material or component. This paper provides a brief review of studying the crack initiation and propagation inside lightweight materials with advanced synchrotron three-dimensional (3D) X-ray imaging, such as aluminum materials. Various damage modes under both static and dynamic loading are elucidated for pure aluminum, aluminum alloy matrix, aluminum alloy metal matrix composite, and aluminum alloy welded joint. For aluminum alloy matrix, metallurgical defects (porosity, void, inclusion, precipitate, etc.) or artificial defects (notch, scratch, pit, etc.) strongly affect the crack initiation and propagation. For aluminum alloy metal matrix composites, the fracture occurs either from the particle debonding or voids at the particle/matrix interface, and the void evolution is closely related with fatigued cycles. For the hybrid laser welded aluminum alloy, fatigue cracks usually initiate from gas pores located at the surface or sub-surface and gradually propagate to a quarter ellipse or a typical semi-ellipse profile.

  12. Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

    Science.gov (United States)

    Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

    2016-07-01

    Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

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

    Science.gov (United States)

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

    2012-11-01

    An in situ stress analysis by means of synchrotron x-ray diffraction was carried out during laser surface hardening of steel. A single exposure set-up that based on a special arrangement of two fast silicon strip line detectors was established, allowing for fast stress analysis according to the sin2ψ x-ray analysis method. For the in situ experiments a process chamber was designed and manufactured, which is described in detail. First measurements were carried out at the HZG undulator imaging beamline (IBL, beamline P05) at the synchrotron storage ring PETRA III, DESY, Hamburg (Germany). The laser processing was carried out using a 6 kW high power diode laser system. Two different laser optics were compared, a Gaussian optic with a focus spot of ø 3 mm and a homogenizing optic with a rectangular spot dimension of 8 × 8 mm2. The laser processing was carried out using spot hardening at a heating-/cooling rate of 1000 K/s and was controlled via pyrometric temperature measurement using a control temperature of 1150 °C. The set-up being established during the measuring campaign allowed for this first realization data collection rates of 10Hz. The data evaluation procedure applied enables the separation of thermal from elastic strains and gains unprecedented insight into the laser hardening process.

  14. Increased cell survival and cytogenetic integrity by spatial dose redistribution at a compact synchrotron X-ray source.

    Directory of Open Access Journals (Sweden)

    Karin Burger

    Full Text Available X-ray microbeam radiotherapy can potentially widen the therapeutic window due to a geometrical redistribution of the dose. However, high requirements on photon flux, beam collimation, and system stability restrict its application mainly to large-scale, cost-intensive synchrotron facilities. With a unique laser-based Compact Light Source using inverse Compton scattering, we investigated the translation of this promising radiotherapy technique to a machine of future clinical relevance. We performed in vitro colony-forming assays and chromosome aberration tests in normal tissue cells after microbeam irradiation compared to homogeneous irradiation at the same mean dose using 25 keV X-rays. The microplanar pattern was achieved with a tungsten slit array of 50 μm slit size and a spacing of 350 μm. Applying microbeams significantly increased cell survival for a mean dose above 2 Gy, which indicates fewer normal tissue complications. The observation of significantly less chromosome aberrations suggests a lower risk of second cancer development. Our findings provide valuable insight into the mechanisms of microbeam radiotherapy and prove its applicability at a compact synchrotron, which contributes to its future clinical translation.

  15. Correlative cryo-fluorescence and cryo-soft X-ray tomography of adherent cells at European synchrotrons.

    Science.gov (United States)

    Carzaniga, Raffaella; Domart, Marie-Charlotte; Duke, Elizabeth; Collinson, Lucy M

    2014-01-01

    Cryo-soft X-ray tomography (cryo-SXT) is a synchrotron-hosted imaging technique used to analyze the ultrastructure of intact, cryo-prepared cells. Correlation of cryo-fluorescence microscopy and cryo-SXT can be used to localize fluorescent proteins to organelles preserved close to native state. Cryo-correlative light and X-ray microscopy (cryo-CLXM) is particularly useful for the study of organelles that are susceptible to chemical fixation artifacts during sample preparation for electron microscopy. In our recent work, we used cryo-CLXM to characterize GFP-LC3-positive early autophagosomes in nutrient-starved HEK293A cells (Duke et al., 2013). Cup-shaped omegasomes were found to form at "hot-spots" on the endoplasmic reticulum. Furthermore, cryo-SXT image stacks revealed the presence of large complex networks of tubulated mitochondria in the starved cells, which would be challenging to model at this scale and resolution using light or electron microscopy. In this chapter, we detail the cryo-CLXM workflow that we developed and optimized for studying adherent mammalian cells. We show examples of data collected at the three European synchrotrons that currently host cryo-SXT microscopes, and describe how raw cryo-SXT datasets are processed into tomoX stacks, modeled, and correlated with cryo-fluorescence data to identify structures of interest. © 2014 Elsevier Inc. All rights reserved.

  16. Microbeam X-ray fluorescence mapping of Cu and Fe in human prostatic carcinoma cell lines using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Rocha, K.M.J.; Leitao, R.G.; Oliveira-Barros, E.G.; Oliveira, M.A.; Canellas, C.G.L.; Anjos, M.J.; Nasciutti, L.E.; Lopes, R.T., E-mail: kjose@nuclear.ufrj.br, E-mail: marcelin@lin.ufrj.br, E-mail: ricardo@lin.ufrj.br, E-mail: roberta@lin.ufrj.br, E-mail: eligouveab@gmail.com, E-mail: maria_aparecida_ufrj@yahoo.com.br, E-mail: luiz.nasciutti@histo.ufrj.br, E-mail: roberta.leitao@uerj.br, E-mail: marcelin@uerj.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Laboratorio de Instrumentacao Nuclear; Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Ciencias Biomedicas; Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Instituto de Fisica

    2017-11-01

    Cancer is a worldwide public health problem and prostate cancer continues to be one of the most common fatal cancers in men. Copper plays an important role in the aetiology and growth of tumours however, whether intratumoral copper is actually elevated in prostate cancer patients has not been established. Iron, an important trace element, plays a vital function in oxygen metabolism, oxygen uptake, and electron transport in mitochondria, energy metabolism, muscle function, and hematopoiesis. The X-ray microfluorescence technique (μXRF) is a rapid and non-destructive method of elemental analysis that provides useful elemental information about samples without causing damage or requiring extra sample preparations. This study investigated the behavior of cells in spheroids of human prostate cells, tumour cell line (DU145) and normal cell line (RWPE-1), after supplementation with zinc chloride by 24 hours using synchrotron X-ray microfluorescence (μSRXRF). The measurements were performed with a standard geometry of 45 deg of incidence, excited by a white beam using a pixel of 25 μm and a time of 300 ms/pixel at the XRF beamline at the Synchrotron Light National Laboratory (Campinas, Brazil). The results by SRμXRF showed non-uniform Cu and Fe distributions in all the spheroids analyzed. (author)

  17. Characterization of actinide bonding in Th(S2PMe2)4 by synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Iversen, B.B.; Larsen, F.K.; Pinkerton, A.A.; Martin, A.; Darovsky, A.; Reynolds, P.A.

    1998-01-01

    Extensive synchrotron (28 K) and conventional sealed-tube (9 K) X-ray diffraction data have been collected on Th(S 2 PMe 2 ) 4 . Modeling of the electron density of the complex shows the bonding is quite ionic with little diffuse f or d type bonding density. Furthermore a large polarization of the Th core is observed revealing some 5d-like involvement in the bonding. High-quality ab initio density functional calculations are not able to reproduce these features and instead predict rather covalent bonding with considerable 6d-5f mixing. The study suggests that this theoretical method exaggerates the covalent nature of actinide bonds. It is shown that the most direct measure of covalence -- charge transfer and electron distributions -- can be usefully estimated by X-ray diffraction even in this most unfavorable of cases, where many actinide core electrons are present. The use of very low temperature data is crucial in the study of heavy metal complexes in order to minimize systematic errors such as thermal diffuse scattering and anharmonicity. The fact that accurate synchrotron radiation diffraction data can be measured within days makes studies of compounds beyond the first transition series more frequently within reach

  18. 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)

  19. Metal-binding proteins scanning and determination by combining gel electrophoresis, synchrotron radiation X-ray fluorescence and atomic spectrometry.

    Science.gov (United States)

    Verbi, F M; Arruda, S C C; Rodriguez, A P M; Pérez, C A; Arruda, M A Z

    2005-02-28

    In the present work, protein bands from in vitro embriogenic callus (Citrus sinensis L. Osbeck) were investigated using micro-synchrotron radiation X-ray fluorescence (muSR-XRF) after sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) separation. Metal-binding protein quantification was done after microwave oven decomposition of gel by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF), flame atomic absorption spectrometry (FAAS) and flame atomic emission spectrometry (FAES). According to the analysis of the protein bands, it is possible to observe that both 81 and ca. 14 kDa proteins present different Fe signal intensity at different positions. The analysis of 53 kDa protein, showed even more interesting results. Besides Fe, the muSR-XRF experiments indicate the presence of Ca, Cu, K and Zn. Chemical elements such as Cu, K, Fe and Zn were determined by SR-TXRF, Mg by FAAS and Na by FAES. Ca was determined by SR-TXRF and FAAS only for accuracy check. In the mineralised protein bands of 81 and around 14 kDa band, only Fe was determined (105 and 21.8 microg g(-1)). For those protein bands (86-ca. 14 kDa) were determined, Ca, K, Cu and Zn in a wide concentration range (42.4-283, 2.47-96.8, 0.91-15.9 and 3.39-29.7 microg g(-1), respectively).

  20. A new fixed-target approach for serial crystallography at synchrotron light sources and X-ray free electron lasers

    Energy Technology Data Exchange (ETDEWEB)

    Roedig, Philip

    2017-07-15

    In the framework of this thesis, a new method for high-speed fixed-target serial crystallography experiments and its applicability to biomacromolecular crystallography at both synchrotron light sources and X-ray free electron lasers (XFELs) is presented. The method is based on a sample holder, which can carry up to 20,000 microcrystals and which is made of single-crystalline silicon. Using synchrotron radiation, the structure of Operophtera brumata cytoplasmic polyhedrosis virus type 18 polyhedrin, lysozyme and cubic insulin was determined by collecting X-ray diffraction data from multiple microcrystals. Data collection was shown to be possible at both cryogenic and ambient conditions. For room-temperature measurements, both global and specific indications of radiation damage were investigated and characterized. Due to the sieve-like structure of the chip, the microcrystals tend to arrange themselves according to the micropore pattern, which allows for efficient sampling of the sample material. In combination with a high-speed scanning stage, the sample holder was furthermore shown to be highly suitable for serial femtosecond crystallography experiments. By fast raster scanning of the chip through the pulsed X-ray beam of an XFEL, structure determination of a virus, using the example of bovine enterovirus type 2, has been demonstrated at an XFEL for the first time. Hit rates of up to 100% were obtained by the presented method, which refers to a reduction in sample consumption by at least three orders of magnitude with respect to common liquid-jet injection methods used for sample delivery. In this way, the typical time needed for data collection in serial femtosecond crystallography is significantly decreased. The presented technique for sample loading of the chip is easy to learn and results in efficient removal of the surrounding mother liquor, thereby reducing the generated background signal. Since the chip is made of single-crystalline silicon, in principle no

  1. A new fixed-target approach for serial crystallography at synchrotron light sources and X-ray free electron lasers

    International Nuclear Information System (INIS)

    Roedig, Philip

    2017-07-01

    In the framework of this thesis, a new method for high-speed fixed-target serial crystallography experiments and its applicability to biomacromolecular crystallography at both synchrotron light sources and X-ray free electron lasers (XFELs) is presented. The method is based on a sample holder, which can carry up to 20,000 microcrystals and which is made of single-crystalline silicon. Using synchrotron radiation, the structure of Operophtera brumata cytoplasmic polyhedrosis virus type 18 polyhedrin, lysozyme and cubic insulin was determined by collecting X-ray diffraction data from multiple microcrystals. Data collection was shown to be possible at both cryogenic and ambient conditions. For room-temperature measurements, both global and specific indications of radiation damage were investigated and characterized. Due to the sieve-like structure of the chip, the microcrystals tend to arrange themselves according to the micropore pattern, which allows for efficient sampling of the sample material. In combination with a high-speed scanning stage, the sample holder was furthermore shown to be highly suitable for serial femtosecond crystallography experiments. By fast raster scanning of the chip through the pulsed X-ray beam of an XFEL, structure determination of a virus, using the example of bovine enterovirus type 2, has been demonstrated at an XFEL for the first time. Hit rates of up to 100% were obtained by the presented method, which refers to a reduction in sample consumption by at least three orders of magnitude with respect to common liquid-jet injection methods used for sample delivery. In this way, the typical time needed for data collection in serial femtosecond crystallography is significantly decreased. The presented technique for sample loading of the chip is easy to learn and results in efficient removal of the surrounding mother liquor, thereby reducing the generated background signal. Since the chip is made of single-crystalline silicon, in principle no

  2. L X-ray intensity ratio measurements using selective L sub-shell photo-ionisation on synchrotron

    Science.gov (United States)

    Bansal, Himani; Tiwari, M. K.; Mittal, Raj

    2017-10-01

    Lα/Lℓ, Lβ /Lℓ and Lγ/Lℓ intensity ratios have been measured for elements in the range 66≤Z≤83 at tuned photon energies on synchrotron beam line-16 at Indus-2, India. For each element, three incident energies Ei were E3; EL3 EL1 where ELi are Li absorption edge energies of the element. Emitted L X-ray spectrum of an element constitutes a number of X-ray lines generally grouped into four main groups due to limited resolution of available detectors as Lℓ(L3-M1), Lα(L3-M4,5), Lβ(L1-M2,3,4,5,N4; L2-M3,4; L3-N1,4,5,O1,4,5) and Lγ(L2-N1,4,O1,4; L1-N2,3,5,O3,2). Lα and Lℓ both comprise only the lines feeding L3 level and Lβ group comprises X-ray lines feeding all the three sub-shells where as Lγ involves contribution from L1 and L2 feedings. Only E3 excitation gives the ratios free from intra sub-shell Coster-Kronig (CK) transitions while excitations E2 and E1 give CK affected Lβ/Lℓ and Lγ/Lℓ X-ray intensity ratios and Lα/Lℓ still remains free from CKs. The pattern of intensity ratios at three excitation energies of elements was well interpreted in terms of on/off of CK transitions (Bambynek et al., 1972; Campbell, 2003) and outer shell electron filling configuration (Scofield, 1973).

  3. Estimates of Imaging Times for Conventional and Synchrotron X-Ray Sources

    CERN Document Server

    Kinney, J

    2003-01-01

    The following notes are to be taken as estimates of the time requirements for imaging NIF targets in three-dimensions with absorption contrast. The estimates ignore target geometry and detector inefficiency, and focus only on the statistical question of detecting compositional (structural) differences between adjacent volume elements in the presence of noise. The basic equations, from the classic reference by Grodzins, consider imaging times in terms of the required number of photons necessary to provide an image with given resolution and noise. The time estimates, therefore, have been based on the calculated x-ray fluxes from the proposed Advanced Light Source (ALS) imaging beamline, and from the calculated flux for a tungsten anode x-ray generator operated in a point focus mode.

  4. Nanoscale examination of microdamage in sheep cortical bone using synchrotron radiation transmission x-ray microscopy.

    Directory of Open Access Journals (Sweden)

    Garry R Brock

    Full Text Available Microdamage occurs in bone through repeated and excessive loading. Accumulation of microdamage weakens bone, leading to a loss of strength, stiffness and energy dissipation in the tissue. Imaging techniques used to examine microdamage have typically been limited to the microscale. In the current study microdamage was examined at the nanoscale using transmission x-ray microscopy with an x-ray negative stain, lead-uranyl acetate. Microdamage was generated in notched and unnotched beams of sheep cortical bone (2×2×20 mm, with monotonic and fatigue loading. Bulk sections were removed from beams and stained with lead-uranyl acetate to identify microdamage. Samples were sectioned to 50 microns and imaged using transmission x-ray microscopy producing projection images of microdamage with nanoscale resolution. Staining indicated microdamage occurred in both the tensile and compressive regions. A comparison between monotonic and fatigue loading indicated a statistically significant greater amount of stain present in fatigue loaded sections. Microdamage occurred in three forms: staining to existing bone structures, cross hatch damage and a single crack extending from the notch tip. Comparison to microcomputed tomography demonstrated differences in damage morphology and total damage between the microscale and nanoscale. This method has future applications for understanding the underlying mechanisms for microdamage formation as well as three-dimensional nanoscale examination of microdamage.

  5. Synchrotron radiation micro-X-ray fluorescence analysis: A tool to increase accuracy in microscopic analysis

    CERN Document Server

    Adams, F

    2003-01-01

    Microscopic X-ray fluorescence (XRF) analysis has potential for development as a certification method and as a calibration tool for other microanalytical techniques. The interaction of X-rays with matter is well understood and modelling studies show excellent agreement between experimental data and calculations using Monte Carlo simulation. The method can be used for a direct iterative calculation of concentrations using available high accuracy physical constants. Average accuracy is in the range of 3-5% for micron sized objects at concentration levels of less than 1 ppm with focused radiation from SR sources. The end-station ID18F of the ESRF is dedicated to accurate quantitative micro-XRF analysis including fast 2D scanning with collection of full X-ray spectra. Important aspects of the beamline are the precise monitoring of the intensity of the polarized, variable energy beam and the high reproducibility of the set-up measurement geometry, instrumental parameters and long-term stability.

  6. Synchrotron based measurements of the soft x-ray performance of thin film multilayer structures

    International Nuclear Information System (INIS)

    Kania, D.R.; Bartlett, R.J.; Trela, W.J.

    1985-01-01

    Using synchrotron radiation, measuring system has been developed to test the performance of layered synthetic microstructures (LSMs) from 50 to 500 eV. The measurement techniques are reviewed, and results are compared to theoretical predictions of LSM performance

  7. Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Huan; Zhang, Weiguo; Qian, Yu; Liu, Wenliang; Yu, Lizhong; Yoo, Shinjae; Wang, Jun; Wang, Jia-Jun; Eng, Christopher; Liu, Chang-Jun; Tappero, Ryan

    2016-06-15

    This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn inPhragmites australisroot system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils.Phragmites australissamples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.

  8. Quantitative analysis of flow processes in a sand using synchrotron-based X-ray microtomography

    DEFF Research Database (Denmark)

    Wildenschild, Dorthe; Hopmans, J.W.; Rivers, M.L.

    2005-01-01

    Pore-scale multiphase flow experiments were developed to nondestructively visualize water flow in a sample of porous material using X-ray microtomography. The samples were exposed to similar boundary conditions as in a previous investigation, which examined the effect of initial flow rate...... by qualitative comparison and quantitative analysis in the form of a nearest neighbor analysis, that the dynamic effects seen in previous experiments are likely due to the fast and preferential drainage of large pores in the sample. Once a continuous drained path has been established through the sample, further...... drainage of the remaining pores, which have been disconnected from the main flowing water continuum, is prevented....

  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. A biosafety evaluation of synchrotron radiation X-ray to skin and bone marrow: single dose irradiation study of rats and macaques.

    Science.gov (United States)

    Lu, Yifan; Tang, Guanghui; Lin, Hui; Lin, Xiaojie; Jiang, Lu; Yang, Guo-Yuan; Wang, Yongting

    2017-06-01

    Very limited experimental data is available regarding the safe dosages related to synchrotron radiation (SR) procedures. We used young rats and macaques to address bone marrow and skin tolerance to various doses of synchrotron radiation. Rats were subjected to 0, 0.5, 2.5, 5, 25 or 100 Gy local SR X-ray irradiation at left hind limb. Rat blood samples were analyzed at 2-90 days after irradiation. The SR X-ray irradiated skin and tibia were sectioned for morphological examination. For non-human primate study, three male macaques were subjected to 0.5 or 2.5 Gy SR X-ray on crus. Skin responses of macaques were observed. All rats that received SR X-ray irradiation doses greater than 2.5 Gy experienced hair loss and bone-growth inhibition, which were accompanied by decreased number of follicles, thickened epidermal layer, and decreased density of bone marrow cells (p X-ray but showed significant hair loss when the dose was raised above 2.5 Gy. The safety threshold doses of SR X-ray for rat skin, bone marrow and macaque skin are between 0.5 and 2.5 Gy. Our study provided essential information regarding the biosafety of SR X-ray irradiation.

  11. Timepix3 as X-ray detector for time resolved synchrotron experiments

    Energy Technology Data Exchange (ETDEWEB)

    Yousef, Hazem, E-mail: hazem.yousef@diamond.ac.uk; Crevatin, Giulio; Gimenez, Eva N.; Horswell, Ian; Omar, David; Tartoni, Nicola

    2017-02-11

    The Timepix3 ASIC can be used very effectively for time resolved experiments at synchrotron facilities. We have carried out characterizations with the synchrotron beam in order to determine the time resolution and other characteristics such as the energy resolution, charge sharing and signals overlapping. The best time resolution achieved is 19 ns FWHM for 12 keV photons and 350 V bias voltage. The time resolution shows dependency on the photon energy as well as on the chip and acquisition parameters. - Highlights: • An estimate time resolution of the Timepix3 is produced based on the arrival time. • At high resolution, the time structure of the DLS synchrotron beam is resolved. • The arrival time information improves combining the charge split events. • The results enable performing a wide range of time resolved experiments.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  13. Synchrotron X-Ray Scattering as a Tool for Characterising Catalysts on Multiple Length Scales

    International Nuclear Information System (INIS)

    Hudspeth, Jessica M.; Kvashnina, Kristina O.; Kimber, Simon A.J.; Mitchell, Edward P.

    2015-01-01

    Optimising the properties of catalysts for industrial processes requires a detailed knowledge of their structure and properties on multiple length scales. Synchrotron light sources are ideal tools for characterising catalysts for industrial R and D, providing data with high temporal and spatial resolution, under realistic operating conditions, in a non-destructive way. Here, we describe the different synchrotron techniques that can be employed to gain a wealth of complementary information, and highlight recent developments that have allowed remarkable insight to be gained into working catalytic systems. These techniques have the potential to guide future industrial catalyst design. (authors)

  14. Polycapillary Optics Based Confocal Micro X-ray Fluorescence and X-ray Absorption Spectroscopy Setup at The European Synchrotron Radiation Facility Collaborative Research Group Dutch-Belgian Beamline, BM26A.

    Science.gov (United States)

    Bauters, Stephen; Tack, Pieter; Rudloff-Grund, Jennifer Helen; Banerjee, Dipanjan; Longo, Alessandro; Vekemans, Bart; Bras, Wim; Brenker, Frank E; van Silfhout, Roelof; Vincze, Laszlo

    2018-02-06

    A novel plug-and-play setup based on polycapillary X-ray optics enables three-dimensional (3D) confocal X-ray fluorescence (XRF) and X-ray absorption spectroscopy down to 8 × 8 × 11 μm 3 (17 keV) at the European Synchrotron Radiation Facility Collaborative Research Group Dutch-Belgian Beamline, BM26A. A complete description and analytical characterization is presented, together with two recently performed experimental cases. In Deep Earth diamond São Luiz-Frankfurt am Main 16, an olivine-rich inclusion was mapped with full 3D XRF elemental imaging. The preliminary tests on Iron Gall ink contained in an historical document, a letter from the court of King Philip II of Spain, reveal both the delicate nature of Iron Gall ink and the lack of Fe-Ni chemical bonding.

  15. Method for obtaining silver nanoparticle concentrations within a porous medium via synchrotron X-ray computed microtomography.

    Science.gov (United States)

    Molnar, Ian L; Willson, Clinton S; O'Carroll, Denis M; Rivers, Mark L; Gerhard, Jason I

    2014-01-21

    Attempts at understanding nanoparticle fate and transport in the subsurface environment are currently hindered by an inability to quantify nanoparticle behavior at the pore scale (within and between pores) within realistic pore networks. This paper is the first to present a method for high resolution quantification of silver nanoparticle (nAg) concentrations within porous media under controlled experimental conditions. This method makes it possible to extract silver nanoparticle concentrations within individual pores in static and quasi-dynamic (i.e., transport) systems. Quantification is achieved by employing absorption-edge synchrotron X-ray computed microtomography (SXCMT) and an extension of the Beer-Lambert law. Three-dimensional maps of X-ray mass linear attenuation are converted to SXCMT-determined nAg concentration and are found to closely match the concentrations determined by ICP analysis. In addition, factors affecting the quality of the SXCMT-determined results are investigated: 1) The acquisition of an additional above-edge data set reduced the standard deviation of SXCMT-determined concentrations; 2) X-ray refraction at the grain/water interface artificially depresses the SXCMT-determined concentrations within 18.1 μm of a grain surface; 3) By treating the approximately 20 × 10(6) voxels within each data set statistically (i.e., averaging), a high level of confidence in the SXCMT-determined mean concentrations can be obtained. This novel method provides the means to examine a wide range of properties related to nanoparticle transport in controlled laboratory porous medium experiments.

  16. Synchrotron X-ray powder diffraction studies on the order-disorder phase transition in lithium ferrites

    International Nuclear Information System (INIS)

    Darul, J.; Nowicki, W.; Piszora, P.; Baehtz, C.; Wolska, E.

    2005-01-01

    Investigations on the manganese substituted lithium ferrites reveal the strong influence of manganese ions on the ordering of Li + cations in the spinel-type crystal lattice. We present the effect of Mn 3+ substitution in the LiFe 5-x Mn x O 8 (0 ≤ x ≤ 1) samples on the order-disorder phase transition and on the thermal expansion of their spinel lattices. Synchrotron X-ray measurements have been performed in the temperature range 10-300 K and 300-1173 K. The diffraction experiments were carried out at the DESY-HASYLAB high-resolution powder diffractometer (beamline B2). The transition from ordered (cubic primitive, P4 1 32) to disordered (face centred cubic, Fd3m) structure was observed with the increasing Mn 3+ content

  17. Synchrotron X-ray Scattering Analysis of the Interaction Between Corn Starch and an Exogenous Lipid During Hydrothermal Treatment

    Energy Technology Data Exchange (ETDEWEB)

    E Hernandez-Hernandez; C Avila-Orta; B Hsiao; j Castro-Rosas; J Gallegos-Infante; J Morales-Castro; L Ochoa-Martinez; C Gomez-Aldapa

    2011-12-31

    Lipids have an important effect on starch physicochemical properties. There exist few reports about the effect of exogenous lipids on native corn starch structural properties. In this work, a study of the morphological, structural and thermal properties of native corn starch with L-alpha-lysophosphatidylcholine (LPC, the main phospholipid in corn) was performed under an excess of water. Synchrotron radiation, in the form of real-time small and wide-angle X-ray scattering (SAXS/WAXS), was used in order to track structural changes in corn starch, in the presence of LPC during a heating process from 30 to 85 C. When adding LCP, water absorption decreased within starch granule amorphous regions during gelatinization. This is explained by crystallization of the amylose-LPC inclusion complex during gelatinization, which promotes starch granule thermal stability at up to 95 C. Finally, a conceptual model is proposed for explaining the formation mechanism of the starch-LPC complex.

  18. Pair distribution functions of amorphous organic thin films from synchrotron X-ray scattering in transmission mode

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Chenyang; Teerakapibal, Rattavut; Yu, Lian; Zhang, Geoff G. Z.

    2017-07-10

    Using high-brilliance high-energy synchrotron X-ray radiation, for the first time the total scattering of a thin organic glass film deposited on a strongly scattering inorganic substrate has been measured in transmission mode. The organic thin film was composed of the weakly scattering pharmaceutical substance indomethacin in the amorphous state. The film was 130 µm thick atop a borosilicate glass substrate of equal thickness. The atomic pair distribution function derived from the thin-film measurement is in excellent agreement with that from bulk measurements. This ability to measure the total scattering of amorphous organic thin films in transmission will enable accuratein situstructural studies for a wide range of materials.

  19. Structure of La2Cu2O5 by high-resolution synchrotron X-ray powder diffraction

    International Nuclear Information System (INIS)

    La Placa, S.J.; Bringley, J.F.; Scott, B.A.; Cox, D.E.

    1993-01-01

    Dicopper(II) dilanthanum pentaoxide, La 2 Cu 2 O 5 , M r =484.90, orthorhombic, Pbam. At T=300 K: a=5.5490(1), b=10.4774(2), c=3.8796(1) A, V=225.557(8) A 3 , Z=2, D x =7.139 g cm -3 , λ=1.2000 A. Final R I =6.20, R p =14.6 and R wp =20.61%, 124 independent reflections observed. The structure has been refined from high-resolution synchrotron X-ray powder diffraction data using the Rietveld method. It is of the oxygen-defect perovskite type and is composed entirely of corner-shared CuO 5 square pyramids, which share oxygen vacancies forming vacancy tunnels along the c axis. The La atoms reside at a perovskite-like A-site and are tenfold coordinated by oxygen. (orig.)

  20. Pair distribution functions of amorphous organic thin films from synchrotron X-ray scattering in transmission mode

    Directory of Open Access Journals (Sweden)

    Chenyang Shi

    2017-09-01

    Full Text Available Using high-brilliance high-energy synchrotron X-ray radiation, for the first time the total scattering of a thin organic glass film deposited on a strongly scattering inorganic substrate has been measured in transmission mode. The organic thin film was composed of the weakly scattering pharmaceutical substance indomethacin in the amorphous state. The film was 130 µm thick atop a borosilicate glass substrate of equal thickness. The atomic pair distribution function derived from the thin-film measurement is in excellent agreement with that from bulk measurements. This ability to measure the total scattering of amorphous organic thin films in transmission will enable accurate in situ structural studies for a wide range of materials.

  1. X-ray metrology of an array of active edge pixel sensors for use at synchrotron light sources

    Science.gov (United States)

    Plackett, R.; Arndt, K.; Bortoletto, D.; Horswell, I.; Lockwood, G.; Shipsey, I.; Tartoni, N.; Williams, S.

    2018-01-01

    We report on the production and testing of an array of active edge silicon sensors as a prototype of a large array. Four Medipix3RX.1 chips were bump bonded to four single chip sized Advacam active edge n-on-n sensors. These detectors were then mounted into a 2 by 2 array and tested on B16 at Diamond Light Source with an x-ray beam spot of 2um. The results from these tests, compared with optical metrology demonstrate that this type of sensor is sensitive to the physical edge of the silicon, with only a modest loss of efficiency in the final two rows of pixels. We present the efficiency maps recorded with the microfocus beam and a sample powder diffraction measurement. These results give confidence that this sensor technology can be used effectively in larger arrays of detectors at synchrotron light sources.

  2. Fish samples as bioindicator of environmental quality: synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    International Nuclear Information System (INIS)

    Vives, Ana Elisa Sirito de; Moreira, Silvana; Brienza, Sandra Maria Boscolo; Zucchi, Orgheda Luiza Araujo Domingues; Nascimento Filho, Virgilio Franco do Centro de Energia Nuclear na Agricultura , Piracicaba, SP; Brazil)

    2005-01-01

    In this study fish were used as bioindicators of environmental contamination. The species were collected in Piracicaba River, Sao Paulo state, Brazil and the toxic elements concentrations were determined in muscle tissue and viscus (liver, intestine and stomach) by Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF). Were determined the elements Ti, Cr, Mn, Fe, Ni, Cu, Zn and Ba. The results were compared with values established by Brazilian Legislation for general food. The elements concentrations evidenced potential risk to human health and environmental quality alteration of the studied area. The measurements were realized at the 'Laboratorio Nacional de Luz Sincrotron' (LNLS) located in Campinas, Sao Paulo State, Brazil. (author)

  3. Fish samples as bioindicator of environmental quality: synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Brienza, Sandra Maria Boscolo [Universidade Metodista de Piracicaba (UNIMEP), SP (Brazil). Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)]. E-mail: virgilio@cena.usp.br

    2005-07-01

    In this study fish were used as bioindicators of environmental contamination. The species were collected in Piracicaba River, Sao Paulo state, Brazil and the toxic elements concentrations were determined in muscle tissue and viscus (liver, intestine and stomach) by Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF). Were determined the elements Ti, Cr, Mn, Fe, Ni, Cu, Zn and Ba. The results were compared with values established by Brazilian Legislation for general food. The elements concentrations evidenced potential risk to human health and environmental quality alteration of the studied area. The measurements were realized at the 'Laboratorio Nacional de Luz Sincrotron' (LNLS) located in Campinas, Sao Paulo State, Brazil. (author)

  4. Ecological study of the migration of eel by synchrotron radiation induced X-ray fluorescence imaging of otoliths

    International Nuclear Information System (INIS)

    Nakai, I.; Iwata, R.; Tsukamoto, K.

    1999-01-01

    Synchrotron radiation-induced X-ray fluorescence imaging is suitable for determining the distribution of trace elements in fish otoliths. The Sr/Ca ratio in an otolith is an indicator of salinity changes and can be used to clarify the migration history of the eel, a catadromous fish. The otoliths of eel collected from the Tone and Elbe rivers exhibited a typical catadromous pattern, i.e. birth and breeding occurred in the ocean, but the remainder of their lives was spent in fresh water. In contrast, eels from the East China Sea and North Sea exhibited an unusual sea-locking phenomenon, as they appear to have remained in marine habitats throughout their lives. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  5. Study of the distribution of actinides in human tissues using synchrotron radiation micro X-ray fluorescence spectrometry.

    Science.gov (United States)

    Vergucht, Eva; De Samber, Björn; Izmer, Andrei; Vekemans, Bart; Appel, Karen; Tolmachev, Sergei; Vincze, Laszlo; Vanhaecke, Frank

    2015-02-01

    This study aims at evaluating the capabilities of synchrotron radiation micro X-ray fluorescence spectrometry (SR micro-XRF) for qualitative and semi-quantitative elemental mapping of the distribution of actinides in human tissues originating from individuals with documented occupational exposure. The investigated lymph node tissues were provided by the United States Transuranium and Uranium Registries (USTUR) and were analyzed following appropriate sample pre-treatment. Semi-quantitative results were obtained via calibration by external standards and demonstrated that the uranium concentration level in the detected actinide hot spots reaches more than 100 μg/g. For the plutonium hot spots, concentration levels up to 31 μg/g were found. As illustrated by this case study on these unique samples, SR micro-XRF has a high potential for this type of elemental bio-imaging owing to its high sensitivity, high spatial resolution, and non-destructive character.

  6. Identification of cellulose fibres belonging to Spanish cultural heritage using synchrotron high resolution X-ray diffraction

    International Nuclear Information System (INIS)

    Herrera, L.K.; Justo, A.; Duran, A.; Haro, M.C.J. de; Franquelo, M.L.; Perez Rodriguez, J.L.

    2010-01-01

    A complete characterisation of fibres used in Spanish artwork is necessary to provide a complete knowledge of these natural fibres and their stage of degradation. Textile samples employed as painting supports on canvas and one sample of unprocessed plant material were chosen for this study. All the samples were investigated by synchrotron radiation X-ray diffraction (SR-XRD). Flax and cotton have the Cellulose I structure. The values of the crystalline index (CI) were calculated for both types of fibres. The structure of Cellulose IV was associated with the unprocessed plant material. The information obtained by SR-XRD was confirmed by laboratory techniques including scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). (orig.)

  7. Distribution of lead in lead-accumulating pteridophyte Blechnum niponicum, measured by synchrotron radiation micro X-ray fluorescence

    International Nuclear Information System (INIS)

    Kodera, Hirofumi; Nishioka, Hiroshi; Muramatsu, Yasuji; Terada, Yasuko

    2008-01-01

    The distribution of lead (Pb) accumulated in the pteridophyte Blechnum niponicum, a Pb-hyperaccumulator, was measured using synchrotron-radiation micro X-ray fluorescence (SR-μ-XRF) at BL37XU of SPring-8. From two dimensional (2D) imagings of Pb at the root, petiole, leaf vein, pinna epidermis and sorus in the Blechnum niponicum, the mechanism for the transportation and accumulation of Pb can be suggested to be as follows: Lead is accumulated in conductive tissues. Most of the Pb solubilized in the rhizosphere is fixed in the conductive tissue, with the remainder being transported with the transpiration stream to the above-ground parts of the plant. Lead transported to the upper parts of the plant ultimately remains at the terminal points of the transpiration stream, including the stomatal apparatus and water pores; it was shown that these sections contain high concentrations of Pb. (author)

  8. X-ray diffraction analysis of rust layer on a weathering steel bridge with surface treatment using synchrotron radiation

    International Nuclear Information System (INIS)

    Yamashita, Masato; Hara, Shuichi; Kamimura, Takayuki; Miyuki, Hideaki; Sato, Masugu

    2007-01-01

    We have examined the structure of rust layer formed on a weathering steel bridge, to which the surface treatment, employing the effect of Cr 2 (SO 4 ) 3 sophisticatedly designed to form the protective goethite (α-FeOOH) rust layer which contains a certain amount of Cr, Cr-goethite, was applied in 1996, using X-ray diffraction at SPring-8 synchrotron radiation facility. It was shown that the formation of α-FeOOH was promoted and/or crystal growth of γ-FeOOH was suppressed by the surface treatment. The increase in the protective ability index (PAI) of the rust layer indicates that the protective goethite was predominantly formed under the effect of the surface treatment. In conclusion, it can be said that the surface treatment worked well to promote the formation of the protective goethite rust layer on the weathering steel bridge during the 10-year exposure. (author)

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

    Science.gov (United States)

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

    2017-05-01

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

  10. The interaction of asbestos and iron in lung tissue revealed by synchrotron-based scanning X-ray microscopy

    Science.gov (United States)

    Pascolo, Lorella; Gianoncelli, Alessandra; Schneider, Giulia; Salomé, Murielle; Schneider, Manuela; Calligaro, Carla; Kiskinova, Maya; Melato, Mauro; Rizzardi, Clara

    2013-01-01

    Asbestos is a potent carcinogen associated with malignant mesothelioma and lung cancer but its carcinogenic mechanisms are still poorly understood. Asbestos toxicity is ascribed to its particular physico-chemical characteristics, and one of them is the presence of and ability to adsorb iron, which may cause an alteration of iron homeostasis in the tissue. This observational study reports a combination of advanced synchrotron-based X-ray imaging and micro-spectroscopic methods that provide correlative morphological and chemical information for shedding light on iron mobilization features during asbestos permanence in lung tissue. The results show that the processes responsible for the unusual distribution of iron at different stages of interaction with the fibres also involve calcium, phosphorus and magnesium. It has been confirmed that the dominant iron form present in asbestos bodies is ferritin, while the concurrent presence of haematite suggests alteration of iron chemistry during asbestos body permanence. PMID:23350030

  11. High-Speed Synchrotron X-ray Imaging Studies of the Ultrasound Shockwave and Enhanced Flow during Metal Solidification Processes

    Science.gov (United States)

    Tan, Dongyue; Lee, Tung Lik; Khong, Jia Chuan; Connolley, Thomas; Fezzaa, Kamel; Mi, Jiawei

    2015-07-01

    The highly dynamic behavior of ultrasonic bubble implosion in liquid metal, the multiphase liquid metal flow containing bubbles and particles, and the interaction between ultrasonic waves and semisolid phases during solidification of metal were studied in situ using the complementary ultrafast and high-speed synchrotron X-ray imaging facilities housed, respectively, at the Advanced Photon Source, Argonne National Laboratory, US, and Diamond Light Source, UK. Real-time ultrafast X-ray imaging of 135,780 frames per second revealed that ultrasonic bubble implosion in a liquid Bi-8 wt pctZn alloy can occur in a single wave period (30 kHz), and the effective region affected by the shockwave at implosion was 3.5 times the original bubble diameter. Furthermore, ultrasound bubbles in liquid metal move faster than the primary particles, and the velocity of bubbles is 70 ~ 100 pct higher than that of the primary particles present in the same locations close to the sonotrode. Ultrasound waves can very effectively create a strong swirling flow in a semisolid melt in less than one second. The energetic flow can detach solid particles from the liquid-solid interface and redistribute them back into the bulk liquid very effectively.

  12. OASYS (OrAnge SYnchrotron Suite): an open-source graphical environment for x-ray virtual experiments

    Science.gov (United States)

    Rebuffi, Luca; Sanchez del Rio, Manuel

    2017-08-01

    The evolution of the hardware platforms, the modernization of the software tools, the access to the codes of a large number of young people and the popularization of the open source software for scientific applications drove us to design OASYS (ORange SYnchrotron Suite), a completely new graphical environment for modelling X-ray experiments. The implemented software architecture allows to obtain not only an intuitive and very-easy-to-use graphical interface, but also provides high flexibility and rapidity for interactive simulations, making configuration changes to quickly compare multiple beamline configurations. Its purpose is to integrate in a synergetic way the most powerful calculation engines available. OASYS integrates different simulation strategies via the implementation of adequate simulation tools for X-ray Optics (e.g. ray tracing and wave optics packages). It provides a language to make them to communicate by sending and receiving encapsulated data. Python has been chosen as main programming language, because of its universality and popularity in scientific computing. The software Orange, developed at the University of Ljubljana (SLO), is the high level workflow engine that provides the interaction with the user and communication mechanisms.

  13. Structural Analysis on Reduced Graphene Oxide Prepared from Old Coconut Shell by Synchrotron X-Ray Scattering

    Science.gov (United States)

    Yogi Nugraheni, Ananda; Jayanti, Dwi Noor; Kurniasari; Soontaranon, Siriwat; Giri Rachman Putra, Edy; Darminto

    2017-05-01

    This work is aimed to identify the distribution of size and structure of the reduced graphene oxide (rGO) particles before and after the mechanical exfoliation process from coconut shell. The burnt sample was heated at 400°C in ambient air, followed by sonication and centrifugation method for various concentration. The characterization were performed by using wide angle X-ray scattering (WAXS) and synchrotron small angle X-ray scattering (SAXS). Based on SAXS result, the structure of rGO showed that in low range of momentum transfer (Q), the particle size was too big to be measured using SAXS. In the high Q, the graph shown the apparent absence of change in curvature which indicates that the small particles are typically seen on high Q range, having aggregate with a new shape and big particles. The average fitting slope is -3.3, implying that the particles structure tends to be fractal (rough) surface, where the particles form aggregates to become bigger size and irregular structure. Further, the WAXS characterization shows that the exfoliation step has not affected the rGO phase formed.

  14. Synchrotron X-ray diffraction investigation of the anomalous behavior of ice during freezing of aqueous systems.

    Science.gov (United States)

    Varshney, Dushyant B; Elliott, James A; Gatlin, Larry A; Kumar, Satyendra; Suryanarayanan, Raj; Shalaev, Evgenyi Y

    2009-05-07

    Simple aqueous systems, i.e., phosphate-glycine buffers and pure water, were studied at subambient temperatures by X-ray difractometry using a high-intensity synchrotron radiation source at the Advanced Photon Source of Argonne National Laboratory. Complex X-ray diffraction (XRD) patterns, with two or more poorly resolved peaks in place of each of the four diagnostic peaks of hexagonal ice, 100, 002, 101, and 102, referred as "splitting", were observed in the majority of cases. The splitting of up to 0.05 A (d-spacing) was detected for 100, 002, and 101 peaks, whereas 102 peak was less affected. Deformation of the lattice of hexagonal ice, probably due to local stress created on the ice/ice or ice/container interface during water-to-ice transformation, is proposed as a possible mechanism for the observed splitting of XRD peaks. Using molecular modeling, it was estimated that the observed shifts in the peak positions are equivalent to applying a hydrostatic pressure of 2-3 kbars. The splitting can be used to quantify stresses during freezing, which could improve our understanding of the role of water-to-ice transformation on the destabilization of proteins and other biological systems.

  15. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    International Nuclear Information System (INIS)

    Reischig, Peter; Helfen, Lukas; Wallert, Arie; Baumbach, Tilo; Dik, Joris

    2013-01-01

    The characterisation of the microstructure and micromechanical behaviour of paint is key to a range of problems related to the conservation or technical art history of paintings. Synchrotron-based X-ray laminography is demonstrated in this paper to image the local sub-surface microstructure in paintings in a non-invasive and non-destructive way. Based on absorption and phase contrast, the method can provide high-resolution 3D maps of the paint stratigraphy, including the substrate, and visualise small features, such as pigment particles, voids, cracks, wood cells, canvas fibres etc. Reconstructions may be indicative of local density or chemical composition due to increased attenuation of X-rays by elements of higher atomic number. The paint layers and their interfaces can be distinguished via variations in morphology or composition. Results of feasibility tests on a painting mockup (oak panel, chalk ground, vermilion and lead white paint) are shown, where lateral and depth resolution of up to a few micrometres is demonstrated. The method is well adapted to study the temporal evolution of the stratigraphy in test specimens and offers an alternative to destructive sampling of original works of art. (orig.)

  16. Evidence for quiescent synchrotron emission in the black hole X-ray transient Swift J1357.2–0933

    Directory of Open Access Journals (Sweden)

    Shahbaz T.

    2013-12-01

    Full Text Available We present high time-resolution optical and infrared observations of the edge-on black hole X-ray transient Swift J1357.2-0933. Our data taken in 2012 shows the system to be at its pre-outburst magnitude and so the system is in quiescence. In contrast to other X-ray transients, the quiescent light curves of Swift J1357.2-0933 do not show the secondary star’s ellipsoidal modulation. The optical and infrared light curves is dominated by variability with an optical fractional rms of about 20 per cent, much larger than what is observed in other systems. The quiescent ultraviolet to mid-IR spectral energy distribution in quiescence is dominated by a nonthermal component with a power–law index of −1.4, (the broad-band rms SED has a similar index which arises from optically thin synchrotron emission from a jet; the lack of a peak in the spectral energy distribution rules out advection-dominated models (based on [19].

  17. Synchrotron Radiation and Energy Dispersive X-Ray Fluorescence Applications on Elemental Distribution in Human Hair and Bones

    International Nuclear Information System (INIS)

    Carvalho, M.L.; Marques, A.F.; Brito, J.

    2003-01-01

    This work is an application of synchrotron microprobe X- Ray fluorescence in order to study elemental distribution along human hair samples of contemporary citizens. Furthermore, X-Ray fluorescence spectrometry is also used to analyse human bones of different historical periods: Neolithic and contemporary subjects. The elemental content in the bones allowed us to conclude about environmental contamination, dietary habits and health status influence in the corresponding citizens. All samples were collected post-mortem. Quantitative analysis was performed for Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr and Pb. Mn and Fe concentration were much higher in bones from pre-historic periods. On the contrary, Pb bone concentrations of contemporary subjects are much higher than in pre-historical ones, reaching 100 μg g-1, in some cases. Very low concentrations for Co, Ni, Br and Rb were found in all the analysed samples. Cu concentrations, allows to distinguish Chalcolithic bones from the Neolithic ones. The distribution of trace elements along human hair was studied for Pb and the obtained pattern was consistent with the theoretical model, based on the diffusion of this element from the root and along the hair. Therefore, the higher concentrations in hair for Pb of contemporary individuals were also observed in the bones of citizens of the same sampling sites. All samples were analysed directly without any chemical treatment

  18. The ab-initio crystal structure determination of UPd 2Sn by synchrotron X-ray powder diffraction

    Science.gov (United States)

    Marezio, M.; Cox, D. E.; Rossel, C.; Maple, M. B.

    1988-09-01

    The structure of the heavy-fermion compound UPd 2Sn has been determined by synchrotron x-ray radiation powder diffraction techniques. It is orthorhombic, space group Pnma [lattice parameters a = 9.9787(1), b = 4.58843(5), c = 6.89166(8) Å at room temperature] and Z = 4. All atoms, one U, one Sn, and two Pd are in 4d special positions at (x {1}/{4} z). The refinements were carried out by the Rietveld method with a pseudo-Voigt peak shape function. The final conventional R factors were: R wp = 21.3% and R E = 14.3%. The U positions in the unit cell were unequivocally located, but because of the similarity in x-ray scattering factors it was not possible to determine whether the Pd atoms and the Sn atoms are ordered or disordered on the other three sites. The structural arrangement of UPd 2Sn is of either MnCu 2Al, or ordered NaTl, or disordered Fe 3Al type, all these structures being cubic and b.c.c. related. The orthorhombic distortion is large and is probably due to a size effect of the U atoms which would be in a mixed ( {3+}/{4+}) valence state.

  19. Absorbed dose determination in kilovoltage X-ray synchrotron radiation using alanine dosimeters.

    Science.gov (United States)

    Butler, D J; Lye, J E; Wright, T E; Crossley, D; Sharpe, P H G; Stevenson, A W; Livingstone, J; Crosbie, J C

    2016-12-01

    Alanine dosimeters from the National Physical Laboratory (NPL) in the UK were irradiated using kilovoltage synchrotron radiation at the imaging and medical beam line (IMBL) at the Australian Synchrotron. A 20 × 20 mm 2 area was irradiated by scanning the phantom containing the alanine through the 1 mm × 20 mm beam at a constant velocity. The polychromatic beam had an average energy of 95 keV and nominal absorbed dose to water rate of 250 Gy/s. The absorbed dose to water in the solid water phantom was first determined using a PTW Model 31014 PinPoint ionization chamber traceable to a graphite calorimeter. The alanine was read out at NPL using correction factors determined for 60 Co, traceable to NPL standards, and a published energy correction was applied to correct for the effect of the synchrotron beam quality. The ratio of the doses determined by alanine at NPL and those determined at the synchrotron was 0.975 (standard uncertainty 0.042) when alanine energy correction factors published by Waldeland et al. (Waldeland E, Hole E O, Sagstuen E and Malinen E, Med. Phys. 2010, 37, 3569) were used, and 0.996 (standard uncertainty 0.031) when factors by Anton et al. (Anton M, Büermann L., Phys Med Biol. 2015 60 6113-29) were used. The results provide additional verification of the IMBL dosimetry.

  20. Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

    Indian Academy of Sciences (India)

    The first two parameters are discussed in the optical design part of ... 2.1.1 Optical design. Low divergence of incident beam is one of the basic character- istics of synchrotron radiation. It is known to vary as 1/γ where γ = (m/m0) = 1/ .... diffraction data of the powdered LaB6 sample were recorded under ambient conditions.

  1. Fluorescence imaging of reactive oxygen species by confocal laser scanning microscopy for track analysis of synchrotron X-ray photoelectric nanoradiator dose: X-ray pump-optical probe.

    Science.gov (United States)

    Jeon, Jae Kun; Han, Sung Mi; Kim, Jong Ki

    2016-09-01

    Bursts of emissions of low-energy electrons, including interatomic Coulomb decay electrons and Auger electrons (0-1000 eV), as well as X-ray fluorescence produced by irradiation of large-Z element nanoparticles by either X-ray photons or high-energy ion beams, is referred to as the nanoradiator effect. In therapeutic applications, this effect can damage pathological tissues that selectively take up the nanoparticles. Herein, a new nanoradiator dosimetry method is presented that uses probes for reactive oxygen species (ROS) incorporated into three-dimensional gels, on which macrophages containing iron oxide nanoparticles (IONs) are attached. This method, together with site-specific irradiation of the intracellular nanoparticles from a microbeam of polychromatic synchrotron X-rays (5-14 keV), measures the range and distribution of OH radicals produced by X-ray emission or superoxide anions ({\\rm{O}}_2^-) produced by low-energy electrons. The measurements are based on confocal laser scanning of the fluorescence of the hydroxyl radical probe 2-[6-(4'-amino)phenoxy-3H-xanthen-3-on-9-yl] benzoic acid (APF) or the superoxide probe hydroethidine-dihydroethidium (DHE) that was oxidized by each ROS, enabling tracking of the radiation dose emitted by the nanoradiator. In the range 70 µm below the irradiated cell, ^\\bullet{\\rm{OH}} radicals derived mostly from either incident X-ray or X-ray fluorescence of ION nanoradiators are distributed along the line of depth direction in ROS gel. In contrast, {\\rm{O}}_2^- derived from secondary electron or low-energy electron emission by ION nanoradiators are scattered over the ROS gel. ROS fluorescence due to the ION nanoradiators was observed continuously to a depth of 1.5 mm for both oxidized APF and oxidized DHE with relatively large intensity compared with the fluorescence caused by the ROS produced solely by incident primary X-rays, which was limited to a depth of 600 µm, suggesting dose enhancement as well as more

  2. Probing Intracellular Element Concentration Changes during Neutrophil Extracellular Trap Formation Using Synchrotron Radiation Based X-Ray Fluorescence

    Science.gov (United States)

    Niemiec, Maria J.; Laforce, Brecht; Garrevoet, Jan; Vergucht, Eva; De Rycke, Riet; Cloetens, Peter; Urban, Constantin F.; Vincze, Laszlo

    2016-01-01

    High pressure frozen (HPF), cryo-substituted microtome sections of 2 μm thickness containing human neutrophils (white blood cells) were analyzed using synchrotron radiation based X-ray fluorescence (SR nano-XRF) at a spatial resolution of 50 nm. Besides neutrophils from a control culture, we also analyzed neutrophils stimulated for 1–2 h with phorbol myristate acetate (PMA), a substance inducing the formation of so-called Neutrophil Extracellular Traps (or NETs), a defense system again pathogens possibly involving proteins with metal chelating properties. In order to gain insight in metal transport during this process, precise local evaluation of elemental content was performed reaching limits of detection (LODs) of 1 ppb. Mean weight fractions within entire neutrophils, their nuclei and cytoplasms were determined for the three main elements P, S and Cl, but also for the 12 following trace elements: K, Ca, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Sr and Pb. Statistical analysis, including linear regression provided objective analysis and a measure for concentration changes. The nearly linear Ca and Cl concentration changes in neutrophils could be explained by already known phenomena such as the induction of Ca channels and the uptake of Cl under activation of NET forming neutrophils. Linear concentration changes were also found for P, S, K, Mn, Fe, Co and Se. The observed linear concentration increase for Mn could be related to scavenging of this metal from the pathogen by means of the neutrophil protein calprotectin, whereas the concentration increase of Se may be related to its antioxidant function protecting neutrophils from the reactive oxygen species they produce against pathogens. We emphasize synchrotron radiation based nanoscopic X-ray fluorescence as an enabling analytical technique to study changing (trace) element concentrations throughout cellular processes, provided accurate sample preparation and data-analysis. PMID:27812122

  3. Spinel materials for Li-ion batteries: new insights obtained by operando neutron and synchrotron X-ray diffraction.

    Science.gov (United States)

    Bianchini, Matteo; Fauth, François; Suard, Emmanuelle; Leriche, Jean Bernard; Masquelier, Christian; Croguennec, Laurence

    2015-12-01

    In the last few decades Li-ion batteries changed the way we store energy, becoming a key element of our everyday life. Their continuous improvement is tightly bound to the understanding of lithium (de)intercalation phenomena in electrode materials. Here we address the use of operando diffraction techniques to understand these mechanisms. We focus on powerful probes such as neutrons and synchrotron X-ray radiation, which have become increasingly familiar to the electrochemical community. After discussing the general benefits (and drawbacks) of these characterization techniques and the work of customization required to adapt standard electrochemical cells to an operando diffraction experiment, we highlight several very recent results. We concentrate on important electrode materials such as the spinels Li1 + xMn2 - xO4 (0 ≤ x ≤ 0.10) and LiNi0.4Mn1.6O4. Thorough investigations led by operando neutron powder diffraction demonstrated that neutrons are highly sensitive to structural parameters that cannot be captured by other means (for example, atomic Debye-Waller factors and lithium site occupancy). Synchrotron radiation X-ray powder diffraction reveals how LiMn2O4 is subject to irreversibility upon the first electrochemical cycle, resulting in severe Bragg peak broadening. Even more interestingly, we show for the first time an ordering scheme of the elusive composition Li0.5Mn2O4, through the coexistence of Mn(3+):Mn(4+) 1:3 cation ordering and lithium/vacancy ordering. More accurately written as Li0.5Mn(3+)0.5Mn(4+)1.5O4, this intermediate phase loses the Fd\\overline 3m symmetry, to be correctly described in the P213 space group.

  4. High-resolution mucociliary transport measurement in live excised large animal trachea using synchrotron X-ray imaging.

    Science.gov (United States)

    Donnelley, Martin; Morgan, Kaye S; Awadalla, Maged; Farrow, Nigel R; Hall, Chris; Parsons, David W

    2017-05-16

    The Australian Synchrotron Imaging and Medical Beamline (IMBL) was designed as the world's widest synchrotron X-ray beam, enabling both clinical imaging and therapeutic applications for humans as well as the imaging of large animal models. Our group is developing methods for imaging the airways of newly developed CF animal models that display human-like lung disease, such as the CF pig, and we expect that the IMBL can be utilised to image airways in animals of this size. This study utilised samples of excised tracheal tissue to assess the feasibility, logistics and protocols required for airway imaging in large animal models such as pigs and sheep at the IMBL. We designed an image processing algorithm to automatically track and quantify the tracheal mucociliary transport (MCT) behaviour of 103 μm diameter high refractive index (HRI) glass bead marker particles deposited onto the surface of freshly-excised normal sheep and pig tracheae, and assessed the effects of airway rehydrating aerosols. We successfully accessed and used scavenged tracheal tissue, identified the minimum bead size that is visible using our chosen imaging setup, verified that MCT could be visualised, and that our automated tracking algorithm could quantify particle motion. The imaging sequences show particles propelled by cilia, against gravity, up the airway surface, within a well-defined range of clearance speeds and with examples of 'clumping' behaviour that is consistent with the in vivo capture and mucus-driven transport of particles. This study demonstrated that the wide beam at the IMBL is suitable for imaging MCT in ex vivo tissue samples. We are now transitioning to in vivo imaging of MCT in live pigs, utilising higher X-ray energies and shorter exposures to minimise motion blur.

  5. 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}).

  6. K-B microfocusing system using monolithic flexure-hinge mirrors for synchrotron X-rays

    CERN Document Server

    Chen, S J; Tseng, P C; Kuan, C K; Wang, D J; Chen, C T

    2001-01-01

    A Kirkpatrick-Baez (K-B) mirror system is designed while considering gain, efficiency, and focal spot size to theoretically achieve a spot size of 6.7x2.9 mu m sup 2 and a gain of 6.2x10 sup 3 in the elliptical polarization undulator (EPU) soft X-ray beamline. This mirror system, which contains two high order polynomial corrected cylindrical mirrors (i.e., horizontal microfocusing mirror, HMFM, and vertical microfocusing mirror, VMFM) with a monolithic flexure-hinge design, can collect and microfocus the undulator source into a nearly perfect point image. To ensure that the mirrors are easily mounted and adjusted, a modular system on a rotatable CF flange is designed to independently motorize each mirror with four degrees of freedom.

  7. Phases of phosphatidyl ethanolamine monolayers studied by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Helm, C.A.; Tippmann-Krayer, P.; Möhwald, H.

    1991-01-01

    For the first time, phospholid monolayers at the air/water interface have been studied by x-ray diffraction and reflection all along the isotherm from the laterally isotropic fluid (the so-called LE phase) to the ordered phases. The model used to analyze the data, and the accuracy of the parameters...... deduced, were tested by comparing the results obtained with two lipids having the same head group but different chain lengths. Compression of the fluid phase leads predominantly to a change of thickness of the hydrophobic moiety, much less of its density, with the head group extension remaining constant....... The main transition involves a considerable increase (approximately 10%) of the electron density in the hydrophobic region, a dehydration of the head group and a positional ordering of the aliphatic tails, albeit with low coherence lengths (approximately 10 spacings). On further compression of the film...

  8. The application of synchrotron x-ray absorption spectroscopy to problems of industrial heterogeneous catalysis

    International Nuclear Information System (INIS)

    Meitzner, G.

    1994-01-01

    A fundamental understanding of catalytic chemistry is valuable for fine-tuning existing processes and for inventing new ones. However, active phases are hard to study, being typically dilute species in amorphous solids comprising many elements. X-ray Absorption Spectroscopy (XAS) can be applied to most catalysts under the appropriate in situ conditions. The ability is unique in observing all the trace elements in the catalysts forming active phases, poisons, and catalysts for unwanted side reactions. Every spectrum contains independent information on the average chemical state, and physical environment, of absorbing atoms. This information can yield new processes, and improvements in existing ones, after the rate of empirical advances in a technology has diminished. The authors discuss XAS studies of metallic and non-metallic components in industrial heterogeneous catalysts. The novel observations made possible by in situ measurement conditions are emphasized

  9. The small-angle X-ray scattering beamline of the Brazilian Synchrotron Light Laboratory

    International Nuclear Information System (INIS)

    Kellermann, G.; Vicentin, F.; Tamura, E.; Rocha, M.; Tolentino, H.; Craievich, A.; Barbosa, A.; Torriani, I.

    1997-01-01

    This paper describes the small-angle scattering beamline built at the Brazilian synchrotron light laboratory (LNLS). Vertical focusing of the synchrotron beam is achieved by an elastically bent gold-plated cylindrical mirror. An asymmetric cut curved triangle-shaped silicon single crystal (111 reflection) is used for monochromatization and horizontal focusing. The mirror, monochromator optics and 2θ arm were designed to cover the spectral range between 1.0 and 2.0 A. Three slit sets, a secondary photon shutter, two beam monitors, filters and absorbers, a multi-sample holder, a vacuum path, a beam-stopper and a set of detectors are the basic components of the workstation. The stepping motors are equipped with specially designed encoders. All mechanical and pneumatic movements and detectors can be remotely controlled using a direct panel or a PC. (orig.)

  10. Application of high-resolution film for lithography to synchrotron X-ray topography

    International Nuclear Information System (INIS)

    Mizuno, Kaoru; Ito, Kazuyoshi; Iwami, Masayuki; Hashimoto, Eiji; Kino, Takao.

    1994-01-01

    A high-resolution film for lithography is applied to a detector for synchrotron radiation topography, instead of a nuclear plate. The film shows much better resolution than that of the plate although exposure time an about 500 times longer is required. The size distribution of interstitial loops grown as vacancy sources in a nearly perfect aluminum crystal after a temperature rise is examined from the while beam topograph. (author)

  11. Calibrating the X-ray attenuation of liquid water and correcting sample movement artefacts during in operando synchrotron X-ray radiographic imaging of polymer electrolyte membrane fuel cells.

    Science.gov (United States)

    Ge, Nan; Chevalier, Stéphane; Hinebaugh, James; Yip, Ronnie; Lee, Jongmin; Antonacci, Patrick; Kotaka, Toshikazu; Tabuchi, Yuichiro; Bazylak, Aimy

    2016-03-01

    Synchrotron X-ray radiography, due to its high temporal and spatial resolutions, provides a valuable means for understanding the in operando water transport behaviour in polymer electrolyte membrane fuel cells. The purpose of this study is to address the specific artefact of imaging sample movement, which poses a significant challenge to synchrotron-based imaging for fuel cell diagnostics. Specifically, the impact of the micrometer-scale movement of the sample was determined, and a correction methodology was developed. At a photon energy level of 20 keV, a maximum movement of 7.5 µm resulted in a false water thickness of 0.93 cm (9% higher than the maximum amount of water that the experimental apparatus could physically contain). This artefact was corrected by image translations based on the relationship between the false water thickness value and the distance moved by the sample. The implementation of this correction method led to a significant reduction in false water thickness (to ∼0.04 cm). Furthermore, to account for inaccuracies in pixel intensities due to the scattering effect and higher harmonics, a calibration technique was introduced for the liquid water X-ray attenuation coefficient, which was found to be 0.657 ± 0.023 cm(-1) at 20 keV. The work presented in this paper provides valuable tools for artefact compensation and accuracy improvements for dynamic synchrotron X-ray imaging of fuel cells.

  12. X-ray synchrotron microdosimetry: Experimental benchmark of a general-purpose Monte Carlo code

    Energy Technology Data Exchange (ETDEWEB)

    Hugtenburg, R.P. [Medical Physics and Clinical Engineering, School of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Queen Elizabeth Medical Centre, University Hospital Birmingham, NHS Trust, Birmingham (United Kingdom)], E-mail: r.p.hugtenburg@swansea.ac.uk; Baker, A.E.R. [School of Physics and Astronomy, University of Birmingham, Birmingham (United Kingdom); Green, S. [Queen Elizabeth Medical Centre, University Hospital Birmingham, NHS Trust, Birmingham (United Kingdom)

    2009-03-15

    Microdosimetry is useful in mixed-field radiation treatment strategies but relies on an understanding of electron physics at sub-micron dimensions. Monochromatic synchrotron light will be valuable in the development of Monte Carlo models of radiation transport at this length scale. In addition, synchrotron light offers new treatment strategies benefiting from high degrees of brightness and coherence including binary therapies such as photoactivation therapy (PAT) utilising photoelectric enhancement occurring in the kilovoltage range. Microdosimetric spectra for monoenergetic beams have been obtained in the range 15-33 keV with a tissue-equivalent proportional counter (TEPC) and have been compared to Monte Carlo calculations based on atomic models initially. Transport of electrons in molecular systems can also be considered where fundamental interaction data are also obtainable in synchrotron beams via photon scattering experiments utilising the optical model. In the absence of data from liquid water systems, MOSFET and silica-based optical fibre TLD are emerging contenders for experimental verification of microdosimetric spectra in the solid-state and glassy-state phases, respectively.

  13. Measuring the effect of oxygen deficiency on magnetic coupling in Ba(Co1-xMnx)O3-δ by synchrotron X-ray spectroscopy

    International Nuclear Information System (INIS)

    Shinoda, Ryoichi; Iwase, Akihiro; Matsui, Toshiyuki

    2015-01-01

    We report on the effect of oxygen deficiency on the structural and magnetic properties of Ba(Co 1-x Mn x )O 3 (x = 0.10–0.20) ceramics, as characterized by synchrotron X-ray spectroscopy. Different amounts of oxygen deficiency were introduced by an annealing process under vacuum. The stoichiometry of the oxygen ions in the ceramic samples gradually decreased from an ABO 3 -perovskite type to an ABO 2 type with increasing annealing temperature. Saturation magnetization decreased with increasing annealing temperature irrespective of the amount of Mn substitution, and the magnetic properties for the x = 0.10–0.20 samples changed from ferromagnetic to paramagnetic. According to the X-ray photoelectron spectroscopy (XPS) using synchrotron X-ray radiation and X-ray absorption near-edge structure (XANES) spectroscopy measurements for the x = 0.10 samples, the valence states of the Co and Mn ions gradually changed from tetravalent to trivalent to divalent with increasing annealing temperatures. The transient states of the structural and magnetic properties owing to the induced oxygen deficiency could be observed by synchrotron X-ray spectroscopy. (author)

  14. Translation of atherosclerotic plaque phase-contrast CT imaging from synchrotron radiation to a conventional lab-based X-ray source.

    Directory of Open Access Journals (Sweden)

    Tobias Saam

    Full Text Available OBJECTIVES: Phase-contrast imaging is a novel X-ray based technique that provides enhanced soft tissue contrast. The aim of this study was to evaluate the feasibility of visualizing human carotid arteries by grating-based phase-contrast tomography (PC-CT at two different experimental set-ups: (i applying synchrotron radiation and (ii using a conventional X-ray tube. MATERIALS AND METHODS: Five ex-vivo carotid artery specimens were examined with PC-CT either at the European Synchrotron Radiation Facility using a monochromatic X-ray beam (2 specimens; 23 keV; pixel size 5.4 µm, or at a laboratory set-up on a conventional X-ray tube (3 specimens; 35-40 kVp; 70 mA; pixel size 100 µm. Tomographic images were reconstructed and compared to histopathology. Two independent readers determined vessel dimensions and one reader determined signal-to-noise ratios (SNR between PC-CT and absorption images. RESULTS: In total, 51 sections were included in the analysis. Images from both set-ups provided sufficient contrast to differentiate individual vessel layers. All PCI-based measurements strongly predicted but significantly overestimated lumen, intima and vessel wall area for both the synchrotron and the laboratory-based measurements as compared with histology (all p0.53 per mm(2, 95%-CI: 0.35 to 0.70. Although synchrotron-based images were characterized by higher SNRs than laboratory-based images; both PC-CT set-ups had superior SNRs compared to corresponding conventional absorption-based images (p0.98 and >0.84 for synchrotron and for laboratory-based measurements; respectively. CONCLUSION: Experimental PC-CT of carotid specimens is feasible with both synchrotron and conventional X-ray sources, producing high-resolution images suitable for vessel characterization and atherosclerosis research.

  15. Synchrotron Radial X-ray Diffraction Studies of Deformation of Polycrystalline MgO

    Science.gov (United States)

    Girard, J.; Tsujino, N.; Mohiuddin, A.; Karato, S. I.

    2016-12-01

    X-ray diffraction analyses have been used for decades to study mechanical properties of polycrystalline samples during in-situ high-pressure deformation. When polycrystalline materials are deformed, stresses develop in grains and lead to lattice distortion. Using X-ray diffraction we can estimate the lattice strain for each (hkl) diffraction plans and calculate the applied stress for each (hkl), using [Singh, 1993] relation. However, this method doesn't take into account plastic anisotropy. As a results of plastic anisotropy present in the material, stress estimated from this method can be largely differ depending on (hkl) diffraction planes [Karato, 2009]. Studying the stress estimate for each (hkl) plane, might help us distinguish dominant deformation mechanisms activated during deformation such as diffusion (we will observe small stress variation as a function of (hkl) diffraction planes) or dislocation creep (we will observe a stress variation as a function of (hkl) diffraction planes that could also give us clues on potential slip system activity). In this study we observed stress evolution in MgO polycrystalline samples deformed under mantle pressure and temperature for (200) and (220) diffraction planes. Using a range MgO grain sizes we were able to control the active deformation mechanism (for e.g. diffusion creep or dislocation creep). For coarse-grained specimens, we observed strong (hkl) dependence of radial strain indicating the operation of dislocation creep. The observed (hkl) dependence changes with pressure suggesting a change in the slip system: at pressures higher than 27 GPa, (200) shows larger stress estimate than (220). In contrast, at lower pressures, (220) shows larger stress estimate than (200). This might indicate a slip system transition in MgO occurring under lower mantle conditions. From {110} plane to {100} plane. This is in good agreement with theoretical predictions and numerical calculation [Amodeo et al., 2012] and has an important

  16. Non-invasive 3D-visualization with sub-micron resolution using synchrotron-X-ray-tomography.

    Science.gov (United States)

    Heethoff, Michael; Helfen, Lukas; Cloetens, Peter

    2008-05-27

    Little is known about the internal organization of many micro-arthropods with body sizes below 1 mm. The reasons for that are the small size and the hard cuticle which makes it difficult to use protocols of classical histology. In addition, histological sectioning destroys the sample and can therefore not be used for unique material. Hence, a non-destructive method is desirable which allows to view inside small samples without the need of sectioning. We used synchrotron X-ray tomography at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France) to non-invasively produce 3D tomographic datasets with a pixel-resolution of 0.7microm. Using volume rendering software, this allows us to reconstruct the internal organization in its natural state without the artefacts produced by histological sectioning. These date can be used for quantitative morphology, landmarks, or for the visualization of animated movies to understand the structure of hidden body parts and to follow complete organ systems or tissues through the samples.

  17. Non-invasive airway health measurement using synchrotron x-ray microscopy of high refractive index glass microbeads

    Energy Technology Data Exchange (ETDEWEB)

    Donnelley, Martin, E-mail: martin.donnelley@adelaide.edu.au; Farrow, Nigel; Parsons, David [Respiratory & Sleep Medicine, Women’s and Children’s Hospital, North Adelaide, South Australia (Australia); Robinson Research Institute, University of Adelaide, South Australia (Australia); School of Paediatrics and Reproductive Health, University of Adelaide, South Australia (Australia); Morgan, Kaye; Siu, Karen [School of Physics, Monash University, Victoria (Australia)

    2016-01-28

    Cystic fibrosis (CF) is caused by a gene defect that compromises the ability of the mucociliary transit (MCT) system to clear the airways of debris and pathogens. To directly characterise airway health and the effects of treatments we have developed a synchrotron X-ray microscopy method that non-invasively measures the local rate and patterns of MCT behaviour. Although the nasal airways of CF mice exhibit the CF pathophysiology, there is evidence that nasal MCT is not altered in CF mice1. The aim of this experiment was to determine if our non-invasive local airway health assessment method could identify differences in nasal MCT rate between normal and CF mice, information that is potentially lost in bulk MCT measurements. Experiments were performed on the BL20XU beamline at the SPring-8 Synchrotron in Japan. Mice were anaesthetized, a small quantity of micron-sized marker particles were delivered to the nose, and images of the nasal airways were acquired for 15 minutes. The nasal airways were treated with hypertonic saline or mannitol to increase surface hydration and MCT. Custom software was used to locate and track particles and calculate individual and bulk MCT rates. No statistically significant differences in MCT rate were found between normal and CF mouse nasal airways or between treatments. However, we hope that the improved sensitivity provided by this technique will accelerate the ability to identify useful CF lung disease-modifying interventions in small animal models, and enhance the development and efficacy of proposed new therapies.

  18. Mapping of Lattice Strain in 4H-SiC Crystals by Synchrotron Double-Crystal X-ray Topography

    Science.gov (United States)

    Guo, Jianqiu; Yang, Yu; Raghothamachar, Balaji; Dudley, Michael; Stoupin, Stanislav

    2018-02-01

    The presence of lattice strain in n-doped 4H-SiC substrate crystals grown by a physical vapor transport method can strongly influence the performance of related power devices that are fabricated on them. Information on the level and the variation of lattice strain in these wafer crystals is thus important. In this study, a non-destructive method is developed based on synchrotron double-crystal x-ray topography to map lattice strains in 4H-SiC wafers. Measurements are made on two 4H-SiC substrate crystals—one is an unprocessed commercial wafer while the other was subject to a post-growth high-temperature heat treatment. Maps of different strain components are generated from the equi-misorientation contour maps recorded using synchrotron monochromatic radiation. The technique is demonstrated to be a powerful tool in estimating strain fields in 4H-SiC crystals. Analysis of the strain maps also shows that the normal strain components vary much more significantly than do the shear/rotation components, indicating that lattice dilation/compression rather than lattice tilt is the major type of deformation caused by both the incorporation of nitrogen dopants and the nucleation of basal plane dislocations.

  19. Spatially resolved synchrotron-induced X-ray fluorescence analyses of metal point drawings and their mysterious inscriptions

    International Nuclear Information System (INIS)

    Reiche, Ina; Radtke, Martin; Berger, Achim; Goerner, Wolf; Ketelsen, Thomas; Merchel, Silke; Riederer, Josef; Riesemeier, Heinrich; Roth, Michael

    2004-01-01

    Synchrotron-induced X-ray fluorescence (Sy-XRF) analysis was used to study the chemical composition of precious Renaissance silverpoint drawings. Drawings by famous artists such as Albrecht Duerer (1471-1528) and Jan van Eyck (approximately 1395-1441) must be investigated non-destructively. Moreover, extremely sensitive synchrotron- or accelerator-based techniques are needed since only small quantities of silver are deposited on the paper. New criteria for attributing these works to a particular artist could be established based on the analysis of the chemical composition of the metal points used. We illustrate how analysis can give new art historical information by means of two case studies. Two particular drawings, one of Albrecht Duerer, showing a profile portrait of his closest friend, 'Willibald Pirckheimer' (1503), and a second one attributed to Jan van Eyck, showing a 'Portrait of an elderly man', often named 'Niccolo Albergati', are the object of intense art historical controversy. Both drawings show inscriptions next to the figures. Analyses by Sy-XRF could reveal the same kind of silverpoint for the Pirckheimer portrait and its mysterious Greek inscription, contrary to the drawing by Van Eyck where at least three different metal points were applied. Two different types of silver marks were found in this portrait. Silver containing gold marks were detected in the inscriptions and over-subscriptions. This is the first evidence of the use of gold points for metal point drawings in the Middle Ages

  20. A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

    Energy Technology Data Exchange (ETDEWEB)

    Kanitpanyacharoen, Waruntorn [University of California, Berkeley, CA 94720 (United States); Parkinson, Dilworth Y. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); De Carlo, Francesco [Argonne National Laboratory, IL 60439 (United States); Marone, Federica [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Stampanoni, Marco [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); University and ETH Zürich, CH-8092 Zürich (Switzerland); Mokso, Rajmund [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); MacDowell, Alastair [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Wenk, Hans-Rudolf, E-mail: wenk@berkeley.edu [University of California, Berkeley, CA 94720 (United States)

    2013-01-01

    The 3D microstructure of shales is important to assess elastic anisotropic characteristics. In this study, microporosity and mineral components in two shale samples were investigated with X-ray tomographic microscopy at three synchrotron facilities: ALS, APS and SLS, and excellent agreement was observed. Synchrotron radiation X-ray tomographic microscopy (SRXTM) was used to characterize the three-dimensional microstructure, geometry and distribution of different phases in two shale samples obtained from the North Sea (sample N1) and the Upper Barnett Formation in Texas (sample B1). Shale is a challenging material because of its multiphase composition, small grain size, low but significant amount of porosity, as well as strong shape- and lattice-preferred orientation. The goals of this round-robin project were to (i) characterize microstructures and porosity on the micrometer scale, (ii) compare results measured at three synchrotron facilities, and (iii) identify optimal experimental conditions of high-resolution SRXTM for fine-grained materials. SRXTM data of these shales were acquired under similar conditions at the Advanced Light Source (ALS) of Lawrence Berkeley National Laboratory, USA, the Advanced Photon Source (APS) of Argonne National Laboratory, USA, and the Swiss Light Source (SLS) of the Paul Scherrer Institut, Switzerland. The data reconstruction of all datasets was handled under the same procedures in order to compare the data quality and determine phase proportions and microstructures. With a 10× objective lens the spatial resolution is approximately 2 µm. The sharpness of phase boundaries in the reconstructed data collected from the APS and SLS was comparable and slightly more refined than in the data obtained from the ALS. Important internal features, such as pyrite (high-absorbing), and low-density features, including pores, fractures and organic matter or kerogen (low-absorbing), were adequately segmented on the same basis. The average volume

  1. Characterisation of corrosion processes of using electron micro-probe, scanning probe microscopy and synchrotron-generated x-ray fluorescence imaging

    International Nuclear Information System (INIS)

    Neufeld, A.K.; Cole, I.S.; Furman, S.A.; Isaacs, H.S.

    2002-01-01

    Full text: With recent advances in computerized technology, the study of chemical reactions can now be visualized as they occur in real time and has resulted in analytical techniques with orders of magnitude greater sensitivity and resolution. This ability offers the corrosion scientist a unique opportunity to study the processes relevant to degradation science which could only be theoretically considered. Neufeld el al (1,2) have attempted to explain in great detail the mechanism of corrosion initiation of zinc by using X-ray micro-probe, Scanning Kelvin probe, and more recently by using synchrotron-generated X-rays and X-ray fluorescence imaging. New results are presented from the synchrotron studies where the transport of ions in-situ has been investigated. The synthesis of information from the techniques will also be discussed in its relevance to atmospheric corrosion processes. Copyright (2002) Australian Society for Electron Microscopy Inc

  2. Beamline fast and automatic attenuation system for X-Ray detectors at Synchrotron Soleil

    Science.gov (United States)

    Renaud, G.; Garreau, Y.; Betinelli, P.; Tournieux, A.; Bisou, J.; Monteiro, P.; Elattaoui, X.

    2013-03-01

    Attenuators are commonly used on beamlines to control incident photon flux. Attenuators are mainly controlled by software. In some experimental cases using various diffraction techniques, this architecture is not fast enough to manage high flux variation. The fast attenuation system inserts and extracts filters quickly, allowing very fast beam attenuation at the maximum rate allowed by the filter mechanism and the beam detector response. To build the solution, we used an off-the-shelf CPCI General Purpose board (GPIO) from TEWS that is based on a SPARTAN-3 Xilinx FPGA: We have developed a daughter board and an embedded VHDL program. The logic is dedicated to maintaining incident detector photon flux within an acceptable range for optimized measurements and protecting the X ray detector against over-exposure. This system is part of a continuous scan process. Some low level process logic is also embedded in order to optimize data exchange. During continuous scanning, this process allows each experimental data item collected to be associated with its corresponding photon flux value. This system is in operation on the SIXS beamline and will be soon installed on the DIFFABS beamline. This paper describes the principle and the results obtained with this solution and the possible improvements and perspectives (interfacing more complex detectors such as XPad).

  3. Beamline fast and automatic attenuation system for X-Ray detectors at Synchrotron Soleil

    International Nuclear Information System (INIS)

    Renaud, G; Garreau, Y; Betinelli, P; Tournieux, A; Bisou, J; Monteiro, P; Elattaoui, X

    2013-01-01

    Attenuators are commonly used on beamlines to control incident photon flux. Attenuators are mainly controlled by software. In some experimental cases using various diffraction techniques, this architecture is not fast enough to manage high flux variation. The fast attenuation system inserts and extracts filters quickly, allowing very fast beam attenuation at the maximum rate allowed by the filter mechanism and the beam detector response. To build the solution, we used an off-the-shelf CPCI General Purpose board (GPIO) from TEWS that is based on a SPARTAN-3 Xilinx FPGA: We have developed a daughter board and an embedded VHDL program. The logic is dedicated to maintaining incident detector photon flux within an acceptable range for optimized measurements and protecting the X ray detector against over-exposure. This system is part of a continuous scan process. Some low level process logic is also embedded in order to optimize data exchange. During continuous scanning, this process allows each experimental data item collected to be associated with its corresponding photon flux value. This system is in operation on the SIXS beamline and will be soon installed on the DIFFABS beamline. This paper describes the principle and the results obtained with this solution and the possible improvements and perspectives (interfacing more complex detectors such as XPad).

  4. Determining the Structure of Biomaterials Interfaces using Synchrotron-based X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    McBride, M

    2002-01-24

    The purpose of this project is to explore the feasibility of using surface X-ray diffraction (SXRD) to determine the structure of biomineral surfaces in electrolyte solutions and of the adsorbed layer of acidic amino acids that are believed to play a central role in the control of biomineral formation and function. The work is a critical component in the development of an integrated picture of the physical and chemical basis for deposition and dissolution at solid-liquid interfaces in biological systems, and brings a new and very powerful surface-sensitive capability to LLNL. We have chosen as our model systems calcium carbonate and calcium phosphate in aspartic and glutamic acid-bearing solutions. The calcium compounds are ubiquitous among biomineral structures, both those that are beneficial such as bones and teeth, and those that are pathological such as kidney stones, while the two acidic amino acids--both as simple and poly-amino acids--are the dominant constituents of protein mixtures implicated in the control of biomineralization. The goals of the work are: (1) to determine the surface structure of pure calcium phosphate and calcium carbonate surfaces in aqueous solution using SXRD; (2) to determine how those surfaces are modified by the presence of aspartic and glutamic acid, both as the simple amino acids and as poly-aspartate and poly-glutamate and (3) to model the interactions of acidic amino acids with calcite.

  5. X-ray lithography using wiggler and undulator synchrotron-radiation sources

    International Nuclear Information System (INIS)

    Neureuther, A.R.; Kim, K.J.; Thompson, A.C.; Hoyer, E.

    1983-08-01

    A systems design approach is used to identify feasible options for wiggler and undulator beam lines for x-ray lithography in the 0.5 to 0.2 μm linewidth region over 5 cm by 5 cm fields. Typical parameters from the Wiggler and Undulator in the Advanced Light Source designed at the Lawrence Berkeley Laboratory are used as examples. Moving from the conventional wavelengths of 4 to 9 A to very soft wavelengths around 15 A is shown to be very promising. The mask absorber thickness can be reduced a factor of three so that 0.2 μm features can be made with a 1:1 mask aspect ratio. The mask heating limited exposure time is also reduced a factor of three to 3 sec/cm 2 . However, extremely thin beam line windows (1/4 mil Be) and mask supports (1 μm Si) must be used. A wiggler beam line design using a small slit window at a scanning mirror appears feasible. A unconventional, windowless differentially pumped beam line with dual deflecting mirrors could be used with an undulator source

  6. Structural Studies of Bleached Melanin by Synchrotron Small-angle X-ray Scattering¶

    Energy Technology Data Exchange (ETDEWEB)

    Littrell, Kenneth C.; Gallas, James M.; Zajac, Gerry W.; Thiyagarajan, Pappannan

    2003-01-01

    Small-angle X-ray scattering was used to measure the effects of chemical bleaching on the size and morphology of tyrosine-derived synthetic melanin dispersed in aqueous media. The average size as measured by the radius of gyration of the melanin particles in solution, at neutral to mildly basic pH, decreases from 16.5 to 12.5 angstroms with increased bleaching. The melanin particles exhibit scattering characteristic of sheet-like structures with a thickness of approximately 11 angstroms at all but the highest levels of bleaching. The scattering data are well described by the form factor for scattering from a pancake-like circular cylinder. These data are consistent with the hypothesis that unbleached melanin, at neutral to mildly basic pH, is a planar aggregate of 6- to 10-nm-sized melanin protomolecules, hydrogen bonded through their quinone and phenolic perimeters. The observed decrease in melanin particle size with increased bleaching is interpreted as evidence for deaggregation, most probably the result of oxidative disruption of hydrogen bonds and an increase in the number of charged, carboxylic acid groups, whereby the melanin aggregates disassociate into units composed of decreasing numbers of protomolecules.

  7. Soft X-ray synchrotron radiation spectroscopy study of molecule-based nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Lee, E. S.; Kim, D. H.; Kang, J. S.; Kim, P. [The Catholic University of Korea, Bucheon (Korea, Republic of); Kim, K. H. [Korea University, Jochiwon (Korea, Republic of); Baik, J. Y.; Shin, H. J. [POSTECH, Pohang (Korea, Republic of)

    2014-11-15

    The electronic structures of molecule-based nanoparticles, such as biomineralized Helicobacter pylori ferritin (Hpf), Heme, and RbCo[Fe(CN){sub 6}]H{sub 2}O (RbCoFe) Prussian blue analogue, have been investigated by employing photoemission spectroscopy and soft X-ray absorption spectroscopy. Fe ions are found to be nearly trivalent in Hpf and Heme nanoparticles, which provides evidence that the amount of magnetite (Fe{sub 3}O{sub 4}) should be negligible in the Hpf core and that the biomineralization of Fe oxides in the high-Fe-bound-state Hpf core arises from a hematite-like formation. On the other hand, Fe ions are nearly divalent and Co ions are Co{sup 2+}-Co{sup 3+} mixed-valent in RbCoFe. Therefore this finding suggests that the mechanism of the photo-induced transition in RbCoFe Prussian blue analogue is not a simple spin-state transition of Fe{sup 2+}-Co{sup 3+} → Fe{sup 3+}-Co{sup 2+}. It is likely that Co{sup 2+} ions have the high-spin configuration while Fe{sup 2+} ions have the low-spin configuration.

  8. A high-energy-resolution resonant inelastic X-ray scattering spectrometer at ID20 of the European Synchrotron Radiation Facility.

    Science.gov (United States)

    Moretti Sala, M; Martel, K; Henriquet, C; Al Zein, A; Simonelli, L; Sahle, Ch J; Gonzalez, H; Lagier, M C; Ponchut, C; Huotari, S; Verbeni, R; Krisch, M; Monaco, G

    2018-03-01

    An end-station for resonant inelastic X-ray scattering and (resonant) X-ray emission spectroscopy at beamline ID20 of ESRF - The European Synchrotron is presented. The spectrometer hosts five crystal analysers in Rowland geometry for large solid angle collection and is mounted on a rotatable arm for scattering in both the horizontal and vertical planes. The spectrometer is optimized for high-energy-resolution applications, including partial fluorescence yield or high-energy-resolution fluorescence detected X-ray absorption spectroscopy and the study of elementary electronic excitations in solids. In addition, it can be used for non-resonant inelastic X-ray scattering measurements of valence electron excitations.

  9. 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

    Lithium ion battery technology is the heart in operating modern technology devices such as mobile phones and laptops. However, as our society is moving towards the utilization of sustainable energy sources, batteries can be foreseen to become an even more important part of the energy infrastructure...... 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...

  10. On The Design For A Versatile Imaging And Hard X-ray Beamline At the Australian Synchrotron: Implementation of In-Line Phase-Contrast Imaging

    International Nuclear Information System (INIS)

    Wilkins, S.W.; Lewis, R.A.; Siu, K.K.-W.; Nesterets, Y.; Mayo, S.C.; Parry, D.J.; Stevenson, A.W.; Garrett, R.F.; Nugent, K.A.

    2004-01-01

    We outline key design features for a versatile imaging and hard X-ray beamline for operation at the Australian Synchrotron. Special attention is paid to the implementation of in-line phase-contrast imaging using both the plane-wave and spherical-wave cases

  11. Synchrotron-based X-ray Fluorescence Microscopy in Conjunction with Nanoindentation to Study Molecular-Scale Interactions of Phenol–Formaldehyde in Wood Cell Walls

    Science.gov (United States)

    Joseph E. Jakes; Christopher G. Hunt; Daniel J. Yelle; Linda Lorenz; Kolby Hirth; Sophie-Charlotte Gleber; Stefan Vogt; Warren Grigsby; Charles R. Frihart

    2015-01-01

    Understanding and controlling molecular-scale interactions between adhesives and wood polymers are critical to accelerate the development of improved adhesives for advanced wood-based materials. The submicrometer resolution of synchrotron-based X-ray fluorescence microscopy (XFM) was found capable of mapping and quantifying infiltration of Br-labeled phenol−...

  12. Workshop on the coupling of synchrotron radiation IR and X-rays with tip based scanning probe microscopies X-TIP

    Energy Technology Data Exchange (ETDEWEB)

    Comin, F.; Martinez-Criado, G.; Mundboth, K.; Susini, J. [European Synchrotron Radiation Facility (ESRF), 38 - Grenoble (France); Purans, J.; Sammelselg, V. [Tartu Univ. (Estonia); Chevrier, J.; Huant, S. [Universite Joseph-Fourier, Grenoble I, LEPES, 38 (France); Hamilton, B. [School of Electrical Engineering and Electronics, Manchester (United Kingdom); Saito, A. [Osaka Univ., RIKEN/SPring8 (Japan); Dhez, O. [OGG, INFM/CNR, 38 - Grenoble (France); Brocklesby, W.S. [Southampton Univ., Optoelectronics Research Centre (United Kingdom); Alvarez-Prado, L.M. [Ovieado, Dept. de Fisica (Spain); Kuzmin, A. [Institute of Solid State Physics - Riga (Latvia); Pailharey, D. [CRMC-N - CNRS, 13 - Marseille (France); Tonneau, D. [CRMCN - Faculte des sciences de Luminy, 13 - Marseille (France); Chretien, P. [Laboratoire de Genie Electrique de Paris, 75 - Paris (France); Cricenti, A. [ISM-CNR, Rome (Italy); DeWilde, Y. [ESPCI, 75 - Paris (France)

    2005-07-01

    The coupling of scanning probe microscopy (SPM) with synchrotron radiation is attracting increasing attention from nano-science community. By combining these 2 tools one can visualize, for example, the sample nano-structure prior to any X-ray characterization. Coupled with focusing devices or independently, SPM can provide spatial resolution below the optical limits. Furthermore, the possibility of employing SPM to manipulate nano-objects under X-ray beams is another exciting perspective. This document gathers the transparencies of 6 of the presentations made at the workshop: 1) the combination of atomic force microscopy and X-ray beam - experimental set-up and objectives; 2) the combination of scanning probe microscope and X-rays for detection of electrons; 3) towards soft X-ray scanning microscopy using tapered capillaries and laser-based high harmonic sources; 4) near-field magneto-optical microscopy; 5) near-field scanning optical microscopy - a brief overview -; and 6) from aperture-less near-field optical microscopy to infra-red near-field night vision. 4 posters entitled: 1) development of laboratory setup for X-ray/AFM experiments, 2) towards X-ray diffraction on single islands, 3) nano-XEOL using near-field detection, and 4) local collection with a STM tip of photoelectrons emitted by a surface irradiated by visible of UV laser beam, are included in the document.

  13. X-ray phase-contrast CT imaging of the acupoints based on synchrotron radiation

    International Nuclear Information System (INIS)

    Chenglin, Liu; Xiaohua, Wang; Hua, Xu; Fang, Liu; Ruishan, Dang; Dongming, Zhang; Xinyi, Zhang; Honglan, Xie; Tiqiao, Xiao

    2014-01-01

    In this paper, the morphology of the acupuncture point (abbreviated as acupoint hereafter) or tissue where there were no acupoints in the fractional rabbit hind limb was studied by in-line phase contrast CT imaging (PCI-CT) methods based on synchrotron radiation. The density of micro-vessels was calculated for tissues with acupoints or without acupoints. Differences between acupoints area and non-acupoint areas determined by the density of the micro-vessels propose a strong evidence of the existence of acupoints. Our results showed that there were two significantly higher densities of the micro-vessels, where two acupoints were located, respectively. In addition, there were large numbers of involutedly microvascular structure in the acupoint areas. Nevertheless, in non-acupoints area, the microvascular structure was relatively simple and flat

  14. X-ray phase-contrast CT imaging of the acupoints based on synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Chenglin, Liu, E-mail: lclyctc@163.com [Physics Department of Yancheng Teachers’ College, Yancheng 224051 (China); Xiaohua, Wang; Hua, Xu [Physics Department of Yancheng Teachers’ College, Yancheng 224051 (China); Fang, Liu; Ruishan, Dang [Anatomy Department of Second Military Medical University, Shanghai 200433 (China); Dongming, Zhang; Xinyi, Zhang [Synchrotron Radiation Research Center of Fudan University, Shanghai 200433 (China); Honglan, Xie; Tiqiao, Xiao [Shanghai Synchrotron Radiation Facility of Shanghai Institute of Applied Physics, CAS, Shanghai 201800 (China)

    2014-10-15

    In this paper, the morphology of the acupuncture point (abbreviated as acupoint hereafter) or tissue where there were no acupoints in the fractional rabbit hind limb was studied by in-line phase contrast CT imaging (PCI-CT) methods based on synchrotron radiation. The density of micro-vessels was calculated for tissues with acupoints or without acupoints. Differences between acupoints area and non-acupoint areas determined by the density of the micro-vessels propose a strong evidence of the existence of acupoints. Our results showed that there were two significantly higher densities of the micro-vessels, where two acupoints were located, respectively. In addition, there were large numbers of involutedly microvascular structure in the acupoint areas. Nevertheless, in non-acupoints area, the microvascular structure was relatively simple and flat.

  15. 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

    Sodium layered oxides with mixed transition metals have received significant attention as positive electrode candidates for sodium-ion batteries due to high reversible capacity. Sodium layered oxides would be more promising candidates than lithium-compounds in terms of high stability of MO2 slabs...... after extraction of Na induced from larger ionic size of Na. In addition, rich crystal chemistry for sodium layered compounds is available since larger Na+ ion is stable in more spacious prismatic site as compared to Li+ ion. In view of this, the phase transformation of layered compounds during......-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...

  16. X-ray imaging by partially coherent synchrotron light. Application to metallic alloys, tooth dentin and natural rock

    International Nuclear Information System (INIS)

    Zabler, Simon Andreas

    2007-01-01

    The hard spectrum which is available on the BAMline at Berlin's synchrotron BESSY offers the rare opportunity to perform high-resolution X-ray imaging experiments with a partially coherent beam. This thesis work reports on the development of a new tomography system, including Fresnel-propagated imaging, and its application to three specific materials science problems from the fields of engineering materials, biology and earth science. Static and dynamic 2D and 3D images were recorded from a variety of aluminum-based alloys. Coarsening of particle agglomerates (at high solid volume fraction) in liquid solution, as well as rheological properties of semi-solid alloys are thus characterized. Dentin is characterized by a quasi-parallel arrangement of micrometer-sized tubules. This work shows how high-resolution 3D images of water-immersed tooth dentin are recorded, and detailed simulations of the optical wave propagation reveal that Fresnel-images contain additional information about the dense cuff of peritubular dentin surrounding the tubules. The cuff thickness can be extrapolated from the interference fringes that form the propagated images of tubules. Absorption and Fresnel-propagated X-ray tomography are applied to measure samples of different rocks before and after mechanical compression nondestructively. In a first approach, limestone and greywacke are investigated, representing two sedimentary rocks of different grain size. Basalt and granite are tested in a second approach to compare different rock types. Development of cracks is observed in all materials, leading to fracture when increasing mechanical load is applied. In this work, relatively small mm-sized samples are used in order to test a classical fracture model wherein micro-flaws initiate the formation of larger cracks. For the first time, Fresnel-propagated imaging is applied to rock samples, highlighting micrometer-sized intergranular porosity as well as different material phases. The latter is shown

  17. X-ray Synchrotron Microtomography of a silicified Jurassic Cheirolepidiaceae (Conifer cone: histology and morphology of Pararaucaria collinsonae sp. nov.

    Directory of Open Access Journals (Sweden)

    David C. Steart

    2014-10-01

    Full Text Available We document a new species of ovulate cone (Pararaucaria collinsonae on the basis of silicified fossils from the Late Jurassic Purbeck Limestone Group of southern England (Tithonian Stage: ca. 145 million years. Our description principally relies on the anatomy of the ovuliferous scales, revealed through X-ray synchrotron microtomography (SRXMT performed at the Diamond Light Source (UK. This study represents the first application of SRXMT to macro-scale silicified plant fossils, and demonstrates the significant advantages of this approach, which can resolve cellular structure over lab-based X-ray computed microtomography (XMT. The method enabled us to characterize tissues and precisely demarcate their boundaries, elucidating organ shape, and thus allowing an accurate assessment of affinities. The cones are broadly spherical (ca. 1.3 cm diameter, and are structured around a central axis with helically arranged bract/scale complexes, each of which bares a single ovule. A three-lobed ovuliferous scale and ovules enclosed within pocket-forming tissue, demonstrate an affinity with Cheirolepidiaceae. Details of vascular sclerenchyma bundles, integument structure, and the number and attachment of the ovules indicate greatest similarity to P. patagonica and P. carrii. This fossil develops our understanding of the dominant tree element of the Purbeck Fossil Forest, providing the first evidence for ovulate cheirolepidiaceous cones in Europe. Alongside recent discoveries in North America, this significantly extends the known palaeogeographic range of Pararaucaria, supporting a mid-palaeolatitudinal distribution in both Gondwana and Laurasia during the Late Jurassic. Palaeoclimatic interpretations derived from contemporaneous floras, climate sensitive sediments, and general circulation climate models indicate that Pararaucaria was a constituent of low diversity floras in semi-arid Mediterranean-type environments.

  18. X-ray Synchrotron Microtomography of a silicified Jurassic Cheirolepidiaceae (Conifer) cone: histology and morphology of Pararaucaria collinsonae sp. nov.

    Science.gov (United States)

    Steart, David C; Spencer, Alan R T; Garwood, Russell J; Hilton, Jason; Munt, Martin C; Needham, John; Kenrick, Paul

    2014-01-01

    We document a new species of ovulate cone (Pararaucaria collinsonae) on the basis of silicified fossils from the Late Jurassic Purbeck Limestone Group of southern England (Tithonian Stage: ca. 145 million years). Our description principally relies on the anatomy of the ovuliferous scales, revealed through X-ray synchrotron microtomography (SRXMT) performed at the Diamond Light Source (UK). This study represents the first application of SRXMT to macro-scale silicified plant fossils, and demonstrates the significant advantages of this approach, which can resolve cellular structure over lab-based X-ray computed microtomography (XMT). The method enabled us to characterize tissues and precisely demarcate their boundaries, elucidating organ shape, and thus allowing an accurate assessment of affinities. The cones are broadly spherical (ca. 1.3 cm diameter), and are structured around a central axis with helically arranged bract/scale complexes, each of which bares a single ovule. A three-lobed ovuliferous scale and ovules enclosed within pocket-forming tissue, demonstrate an affinity with Cheirolepidiaceae. Details of vascular sclerenchyma bundles, integument structure, and the number and attachment of the ovules indicate greatest similarity to P. patagonica and P. carrii. This fossil develops our understanding of the dominant tree element of the Purbeck Fossil Forest, providing the first evidence for ovulate cheirolepidiaceous cones in Europe. Alongside recent discoveries in North America, this significantly extends the known palaeogeographic range of Pararaucaria, supporting a mid-palaeolatitudinal distribution in both Gondwana and Laurasia during the Late Jurassic. Palaeoclimatic interpretations derived from contemporaneous floras, climate sensitive sediments, and general circulation climate models indicate that Pararaucaria was a constituent of low diversity floras in semi-arid Mediterranean-type environments.

  19. X-ray imaging by partially coherent synchrotron light. Application to metallic alloys, tooth dentin and natural rock

    Energy Technology Data Exchange (ETDEWEB)

    Zabler, Simon Andreas

    2007-10-09

    The hard spectrum which is available on the BAMline at Berlin's synchrotron BESSY offers the rare opportunity to perform high-resolution X-ray imaging experiments with a partially coherent beam. This thesis work reports on the development of a new tomography system, including Fresnel-propagated imaging, and its application to three specific materials science problems from the fields of engineering materials, biology and earth science. Static and dynamic 2D and 3D images were recorded from a variety of aluminum-based alloys. Coarsening of particle agglomerates (at high solid volume fraction) in liquid solution, as well as rheological properties of semi-solid alloys are thus characterized. Dentin is characterized by a quasi-parallel arrangement of micrometer-sized tubules. This work shows how high-resolution 3D images of water-immersed tooth dentin are recorded, and detailed simulations of the optical wave propagation reveal that Fresnel-images contain additional information about the dense cuff of peritubular dentin surrounding the tubules. The cuff thickness can be extrapolated from the interference fringes that form the propagated images of tubules. Absorption and Fresnel-propagated X-ray tomography are applied to measure samples of different rocks before and after mechanical compression nondestructively. In a first approach, limestone and greywacke are investigated, representing two sedimentary rocks of different grain size. Basalt and granite are tested in a second approach to compare different rock types. Development of cracks is observed in all materials, leading to fracture when increasing mechanical load is applied. In this work, relatively small mm-sized samples are used in order to test a classical fracture model wherein micro-flaws initiate the formation of larger cracks. For the first time, Fresnel-propagated imaging is applied to rock samples, highlighting micrometer-sized intergranular porosity as well as different material phases. The latter is

  20. The zinc distribution in prostate tissues using X-ray microfluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Leitao, Roberta G.; Anjos, Marcelino J.; Canellas, Catarine G.L.; Pereira, Marcelo O.; Pereira, Gabriela R.; Lopes, Ricardo T.

    2009-01-01

    Many elements play an essential role in a number of biological processes as activators or inhibitors of cellular and enzymatic activity. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in case of selected diseases. Zinc concentration in a prostate gland is much higher than that in other human tissues. The high concentration of zinc in the prostate suggests that zinc may play a role in prostate health. The aim of this work was to study the elemental distribution for Zinc in prostate tissues from patterns of relative fluorescence intensities. The measurements were performed in standard geometry of 45 deg incidence, exciting with a white beam and using a conventional system collimation orthogonal slits) in the XRF beam line at the Synchrotron Light National Laboratory (Campinas, Brazil). The prostate glands were cut into pieces (slice) with thickness of 0.5 mm. The results showed the zinc distribution was not uniform for different zones of the prostate analyzed. (author)

  1. Elemental distribution in brain of wistar rats by X-ray microfluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Lab. de Instrumentacao Nuclear]. E-mail: renata@lin.ufrj.br; Anjos, Marcelino J. dos; Oliveira, Luis F. de [Universidade do Estado, Rio de Janeiro, RJ (Brazil). Inst. de Fisica]. E-mail: marcelin@lin.ufrj.br; Carmo, Maria da Graca T. do [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Nutricao]. E-mail: tcarmo@editema.com.br; Rocha, Monica S. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Dept. de Farmacologia]. E-mail: mrocha@farmaco.ufrj.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fec.unicamp.br; Correa Junior, Jose D.; Martinez, Ana Maria B. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Dept. de Histologia]. E-mail: martinez@histo.ufrj.br

    2005-07-01

    The main goal of this research is to study the changes in the elemental distribution in brain rats, due the knowledge of the spatial distribution and the local concentration of trace elements in tissues have great importance since trace elements are involved in many biological functions of living organisms. For perform this research, Wistar rats with different ages (3, 48 and 72 weeks) were used. The microfluorescence measurements were carried out in a standard geometry of 45 deg/45 deg, exciting with a white beam and using a conventional system collimation (orthogonal slits) in the XRF beamline at the Synchrotron Light National Laboratory (Campinas, Brazil). The following elements were studied: P, S, Cl, K, Ca, Fe, and Zn. Among these elements, Fe and Zn are related with Parkinson and Alzheimer diseases, respectively. By the elemental maps, we can observe that the distribution of zinc was more pronounced in the hippocampus area, the distribution of iron was more conspicuous in the cortical region and bellows the thalamus and, moreover potassium and chlorine distributions were more present in the cortical area. Although, the small statistic, we can view that almost all measured elements are present in lower intensity in brains of rats with 3 weeks, and are usually the same for the other ages studied. (author)

  2. Analysis of wood microstructure by synchrotron radiation-based x-ray microtomography (SRμCT)

    Science.gov (United States)

    Lautner, Silke; Beckmann, Felix

    2012-10-01

    Wood is a versatile tissue complex composed of different cell types such as tracheids, fibers, vessels and parenchyma cells, that each fulfills specific tasks within the woody body of a tree. However, even within a tree genus wood structure can differ significantly due to either biotic or abiotic stress factors occurring during the growth season, or due to cultivar specific growth characteristics. Typical tools for structural analysis of wood so far are scanning electron microscopy (SEM) and light microscopy, allowing measurements of sectional planes. However, the detection of boundary surfaces between neighboring cells and interconnectivity can only be observed in a restricted dimension. In our investigations at DESY, Hamburg, we applied SRμCT for characterization of small wood samples of poplar (Populus trichocarpa) to gain a three dimensional image of a small scale sample that allows us to visualize size, volume, form and interconnectivity of the cells in a non-destructive way. Dependent on sample size, high resolution of micro-structure can be gained. This technique is appropriate to calculate volumes, e.g. of water transported in vessel cells. Since it is possible to reconstruct the vessel network within a stem section, effects of wounding or other environmental stresses on the xylem structure in general, and particularly on the water transport system, might be detected and visualized in 3D by synchrotron radiation-based microtomography. Hence this method is a most promising tool for future investigations in the field of plant physiology.

  3. Elemental mapping by synchrotron radiation X-Ray microfluorescence in cellular spheroid of prostate tumor cells

    Energy Technology Data Exchange (ETDEWEB)

    Leitao, R.G.; Anjos, M.J.; Lopes, R.T., E-mail: roberta@lin.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear; Santos, C.A.N. [Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMETRO), Duque de Caxias, RJ (Brazil). Lab. de Biotecnologia; Palumbo Junior, A.; Souza, P.A.V.R.; Nasciutti, L.E. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Ciencias Biomedicas; Pereira, G.R. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Lab. de Ensaios Nao Destrutivos, Corrosao e Soldagem

    2013-08-15

    Prostate cancer is the sixth most common type of cancer and the third most common in males in Western industrialized countries. Cellular spheroid serves as excellent physiologic tumor models as they mimic avascular tumors and micrometastases. Trace elements play a significant role in biological processes. They are capable of affecting human health by competing with essential elements for available binding sites and by the activation or inhibition of reactions between metabolic enzymes. It is well known that zinc levels in the peripheral zone of dorsal and lateral lobes of the prostate are almost 10 times higher than in other soft tissues. Prostate tumor cells were isolated of the prostate tissue samples that were collected from patients submitted to surgery. The measurements were performed in XRF beam line at the Synchrotron Light National Laboratory (LNLS) in Campinas, Brazil. The results showed that all elements were heterogeneously distributed in different areas of the spheroids analyzed. P, S and Cl showed similar elemental distribution in all the samples analyzed while K, Ca, Fe, and Cu showed different elemental distribution. In all spheroids analyzed, Zn presented more intense distributions in the central region of the spheroid. The relationship between the function of Zn in the secretory epithelial cells and the carcinogenic process suggests that more studies on elemental mapping in spheroids are necessary. (author)

  4. National synchrotron light source user's manual: Guide to the VUV and x-ray beamlines: Third edition

    International Nuclear Information System (INIS)

    Gmuer, N.F.; Thomlinson, W.; White-DePace, S.

    1989-01-01

    This report contains information on the following topics: A Word on the Writing of Beamline Descriptions; Beamline Equipment Utilization for General Users; the Vacuum Ultraviolet (VUV) Storage Ring and Beamlines; VUV Beamline Descriptions--An Explanation; VUV Beamline Descriptions; X-Ray Storage Ring and Beamlines; X-Ray Beamline Descriptions--An Explanation; and X-Ray Beamline Descriptions

  5. National synchrotron light source user's manual: Guide to the VUV and x-ray beamlines: Third edition

    Energy Technology Data Exchange (ETDEWEB)

    Gmuer, N.F.; Thomlinson, W.; White-DePace, S.

    1989-01-01

    This report contains information on the following topics: A Word on the Writing of Beamline Descriptions; Beamline Equipment Utilization for General Users; the Vacuum Ultraviolet (VUV) Storage Ring and Beamlines; VUV Beamline Descriptions--An Explanation; VUV Beamline Descriptions; X-Ray Storage Ring and Beamlines; X-Ray Beamline Descriptions--An Explanation; and X-Ray Beamline Descriptions.

  6. Possibilities and limitations of synchrotron X-ray powder diffraction with double crystal and double multilayer monochromators for microscopic speciation studies

    Energy Technology Data Exchange (ETDEWEB)

    De Nolf, Wout [Department of Chemistry, University of Antwerp, Universiteitsplein 1, B-2610, Antwerpen (Wilrijk) (Belgium)], E-mail: wout.denolf@ua.ac.be; Jaroszewicz, Jakub [Department of Chemistry, University of Antwerp, Universiteitsplein 1, B-2610, Antwerpen (Wilrijk) (Belgium); Terzano, Roberto [Dipartimento di Biologia e Chimica Agro-forestale ed Ambientale, Via Amendola 165/A, I-70126, University of Bari, Bari (Italy); Lind, Ole Christian; Salbu, Brit [Isotope Laboratory, Norwegian University of Life Sciences, PO Box 5003, N-1432 As (Norway); Vekemans, Bart [Department of Analytical Chemistry, Ghent University, Krijgslaan 281 S12, B-9000 Gent (Belgium); Janssens, Koen [Department of Chemistry, University of Antwerp, Universiteitsplein 1, B-2610, Antwerpen (Wilrijk) (Belgium); Falkenberg, Gerald [HASYLAB at DESY, Beamline L, Notkestraat 85, D-22603, Hamburg (Germany)

    2009-08-15

    The performance of a combined microbeam X-ray fluorescence/X-ray powder diffraction (XRF/XRPD) measurement station at Hamburger Synchrotronstrahlungslabor (HASYLAB) Beamline L is discussed in comparison to that at European Synchrotron Radiation Facility (ESRF) ID18F/ID22. The angular resolution in the X-ray diffractograms is documented when different combinations of X-ray source, optics and X-ray diffraction detectors are employed. Typical angular resolution values in the range 0.3-0.5 deg. are obtained at the bending magnet source when a 'pink' beam form of excitation is employed. A similar setup at European Synchrotron Radiation Facility beamlines ID18F and ID22 allows to reach angular resolution values of 0.1-0.15 deg. In order to document the possibilities and limitations for speciation of metals in environmental materials by means of Hamburger Synchrotronstrahlungslabor Beamline L X-ray fluorescence/X-ray powder diffraction setup, two case studies are discussed, one involved in the identification of the crystal phases in which heavy metals such as chromium, iron, barium and lead are present in polluted soils of an industrial site (Val Basento, Italy) and another involved in the speciation of uranium in depleted uranium particles (Ceja Mountains, Kosovo). In the former case, the angular resolution is sufficient to allow identification of most crystalline phases present while in the latter case, it is necessary to dispose of an angular resolution of ca. 0.2 deg. to distinguish between different forms of oxidized uranium.

  7. Synchrotron measurements of local microstructure and residual strains in ductile cast iron

    DEFF Research Database (Denmark)

    Zhang, Yubin; Andriollo, Tito; Fæster, Søren

    2017-01-01

    The local microstructure and distribution of thermally induced residual strains in ferrite matrix grains around an individual spherical graphite nodule in ductile cast iron (DCI) were measured using a synchrotron X-ray micro-diffraction technique. It is found that the matrix grains are deformed, ...

  8. Optical design of an x-ray absorption spectroscopy beamline at Indus-2 synchrotron radiation source

    International Nuclear Information System (INIS)

    Das, N.C.; Jha, S.N.; Roy, A.P.

    1999-10-01

    Details of optical design of EXAFS beamline at Indus-2 SRS, under development at CAT, Indore, have been discussed in this report. This beamline will cover the photon energy range of 5 keV to 20 keV and will use a bent crystal of Si(111) having 2d value equal to 6.2709 A. It will accept a horizontal divergence of 1.5 mrad. The heart of the beamline is the bent crystal polychromator which will disperse and focus the synchrotron beam at the experimental sample position. The transmitted radiation from the sample will be, subsequently, detected by a position sensitive detector (CCD type). The detector length is 25 mm. Assuming a suitable value for the distance between the source and the crystal, we have computed several geometrical parameters of the beamline, such as, Bragg angle, crystal length, crystal radius, crystal to sample distance, sample to detector distance, etc. for three different photon energies, namely, 5 keV, 10 keV, and 20 keV. The band passes around these photon energies are 0.3 keV, 1 keV and 2 keV respectively. It has been found that computed geometrical parameters are well within acceptable limits. An extensive ray tracing work was done using the software program SHADOW to evaluate the imaging properties of the beamline. It was established that the image spot size at the sample position improved substantially when the crystal is changed from spherical cylinder shape to elliptic cylinder shape. From the ray intensity plots, the average resolution of the crystal bender was estimated to be 1 eV per channel. Finally based on the optical layout of the beamline, a schematic mechanical layout of the beamline has been prepared. (author)

  9. Surface modification of PTFE sheet by synchrotron radiation in the soft X-ray region

    International Nuclear Information System (INIS)

    Kato, Y.; Kanda, K.; Haruyama, Y.; Matsui, S.

    2004-01-01

    Full text: The surface properties of poly (tetrafluoroethylene) (PTFE) are changed by the exposure to synchrotron radiation (SR). We succeeded in controlling the wettability of the PTFE surface from hydrophobic to hydrophilic by varying the substrate temperature during the SR irradiation and found that the wettability was ascribable to microstructure and chemical composition of surface.In these previous works, oxygen atoms were found to inhabit on the hydrophobic surface of PTFE. In this study, we investigated the surface modification of PTFE from the SR exposure experiment under the O 2 gas atmosphere. The SR exposure to the PTFE sheet was carried out at beamline 6 (BL6) of the New- SUBARU. The PTFE sheet was irradiated to the white beam, ranging 50-1000 eV at BL6 at room temperature. The gas cell was mounted at the irradiation chamber. The O 2 gas pressure in the gas cell can be maintained at about 0.20 Pa during the SR exposure using 5mm φ hole window. The wettability of PTFE surface was evaluated by the contact angle of a small water drop. Contact angle was measured with the water drop of 1 μl using the contact angle meter. Fig.1 shows the SR dose dependence of contact angle of PTFE surface under the O 2 gas atmosphere and under the vacuum. Contact angle decreased monotonically with SR dose. The decrease rate of contact angle of the PTFE surface irradiated under the O 2 gas atmosphere was larger than that of the PTFE surface irradiated without O 2 gas. Therefore, the combination of O atom to the PTFE surface was enhanced by the O 2 gas in the reaction region. These results suggested that the bonding of O atom on the hydrophobic PTFE surface is dominantly produced in the sample chamber during SR irradiation, but not in the air atmosphere after the SR irradiation

  10. Synchrotron x-ray microtomography of the interior microstructure of chocolate

    Science.gov (United States)

    Lügger, Svenja K.; Wilde, Fabian; Dülger, Nihan; Reinke, Lennart M.; Kozhar, Sergii; Beckmann, Felix; Greving, Imke; Vieira, Josélio; Heinrich, Stefan; Palzer, Stefan

    2016-10-01

    The structure of chocolate, a multicomponent food product, was analyzed using microtomography. Chocolate consists of a semi-solid cocoa butter matrix and a dense network of suspended particles. A detailed analysis of the microstructure is needed to understand mass transport phenomena. Transport of lipids from e.g. a filling or liquid cocoa butter is responsible for major problems in the confectionery industry such as formation of chocolate bloom, which is the formation of visible white spots or a grayish haze on the chocolate surface and leads to consumer rejections and thus large sales losses for the confectionery industry. In this study it was possible to visualize the inner structure of chocolate and clearly distinguish the particles from the continuous phase by taking advantage of the high density contrast of synchrotron radiation. Consequently, particle arrangement and cracks within the sample were made visible. The cracks are several micrometers thick and propagate throughout the entire sample. Images of pure cocoa butter, chocolate without any particles, did not show any cracks and thus confirmed that cracks are a result of embedded particles. They arise during the manufacturing process. Thus, the solidification process, a critical manufacturing step, was simulated with finite element methods in order to understand crack formation during this step. The simulation showed that cracks arise because of significant contraction of cocoa butter, the matrix phase, without any major change of volume of the suspended particles. Tempering of the chocolate mass prior to solidification is another critical step for a good product quality. We found that samples which solidified in an uncontrolled manner are less homogeneous than tempered samples. In summary, our study visualized for the first time the inner microstructure of tempered and untempered cocoa butter as well as chocolate without sample destruction and revealed cracks, which might act as transport pathways.

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

    International Nuclear Information System (INIS)

    Yoo, C.S.

    1997-01-01

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

  12. Evaluation of heavy metals in atmospheric emissions from automotive industry by total reflection X-ray fluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Weber Neto, Jose, E-mail: silvana@fec.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Saneamento e Ambiente; Vives, Ana Elisa Sirito de, E-mail: aesvives@unimep.b [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo

    2009-07-01

    This study had as goal to determine heavy metals and other elements (Ba, Br, Ca, Pb, Cl, Cr, Sr, Fe, Mn, Ni, K, Si, Ti and Zn) in atmospheric pollutants generated by an automotive industry located in the city of Engenheiro Coelho, state of Sao Paulo, Brazil. The sampling and sample preparation procedures were based on methods established by the Company of Sanitation and Technology (CETESB L9.234) and also by the Environmental Protection Agency (EPA - Method 29). The analysis was performed at XRF Beamline (D09B-XRF) in the Synchrotron Light Source Laboratory (Campinas/SP). A white beam of synchrotron radiation was used for sample and standard excitation which were irradiated by 100 seconds. For X-ray lines detection, a Ge (HP) detector with 150 eV of resolution at 5.9 keV was employed. For zinc, iron, barium, calcium and potassium, the values obtained were in the range of 30 mg/Nm{sup 3} and, for other elements, the concentrations were approximately 1 mg/Nm{sup 3}. The sum of As, Be, Co, Cr, Cu, Mn, Ni, Pb, Sb, Se, Sn, Te and Zn concentration was compared with the limits established by CONAMA 264/1999 and SEMA 041/2002 resolutions (7.0 mg/Nm{sup 3}) and it was observed that, for all samples, sums are higher than the permissive value mainly due to the high concentration of zinc. Detection limits for SR-TXRF technique were 0.10 mug/Nm{sup 3} for Pb and 0.02 mug/Nm{sup 3} for Zn. (author)

  13. Synchrotron X-Ray Charge-Density Study of Coordination Polymer (Mn(HCOO)2(H2O)2)∞

    International Nuclear Information System (INIS)

    Poulsen, Rasmus D.; Jorgensen, Mads R.V.; Overgaard, Jacob; Larsen, Finn K.; Morgenroth, Wolfgang; Graber, Timothy; Chen, Yu-Sheng; Iversen, Bo B.

    2007-01-01

    Three high-quality single-crystal X-ray diffraction data sets have been measured under very different conditions on a structurally simple, but magnetically complex, coordination polymer, (Mn(HCOO) 2 (H 2 O) 2 )∞ (1). The first data set is a conventional 100(2) K Mo Kα data set, the second is a very high resolution 100(2) K data set measured on a second-generation synchrotron source, while the third data set was measured with a tiny crystal on a high brilliance third-generation synchrotron source at 16(2) K. Furthermore, the magnetic susceptibility (χ) and the heat capacity (C p ) have been measured from 2 to 300 K on pressed powder. The charge density of 1 was determined from multipole modeling of the experimental structure factors, and overall there is good agreement between the densities obtained separately from the three data sets. When considering the fine density features, the two 100 K data sets agree well with each other, but show small differences to the 16 K data set. Comparison with ab initio theory suggests that the 16 K APS data set provides the most accurate density. Topological analysis of the metal-ligand bonding, experimental 3d orbital populations on the Mn atoms, and Bader atomic charges indicate quite ionic, high-spin metal atoms. This picture is supported by the effective moment estimated from the magnetization measurements (5.840(2)μ B ), but it is at variance with earlier spin density measurements from polarized neutron diffraction. The magnetic ordering originates from superexchange involving covalent interactions with the ligands, and non-ionic effects are observed in the static deformation density maps as well as in plots of the valence shell charge concentrations. Overall, the present study provides a benchmark charge density that can be used in comparison with future metal formate dihydrate charge densities.

  14. Synchrotron X-ray charge-density study of coordination polymer [Mn(HCOO)2(H2O)2]infinity.

    Science.gov (United States)

    Poulsen, Rasmus D; Jørgensen, Mads R V; Overgaard, Jacob; Larsen, Finn K; Morgenroth, Wolfgang; Graber, Timothy; Chen, Yu-Sheng; Iversen, Bo B

    2007-01-01

    Three high-quality single-crystal X-ray diffraction data sets have been measured under very different conditions on a structurally simple, but magnetically complex, coordination polymer, [Mn(HCOO)(2)(H(2)O)(2)](infinity) (1). The first data set is a conventional 100(2) K Mo(Kalpha) data set, the second is a very high resolution 100(2) K data set measured on a second-generation synchrotron source, while the third data set was measured with a tiny crystal on a high brilliance third-generation synchrotron source at 16(2) K. Furthermore, the magnetic susceptibility (chi) and the heat capacity (C(p)) have been measured from 2 to 300 K on pressed powder. The charge density of 1 was determined from multipole modeling of the experimental structure factors, and overall there is good agreement between the densities obtained separately from the three data sets. When considering the fine density features, the two 100 K data sets agree well with each other, but show small differences to the 16 K data set. Comparison with ab initio theory suggests that the 16 K APS data set provides the most accurate density. Topological analysis of the metal-ligand bonding, experimental 3d orbital populations on the Mn atoms, and Bader atomic charges indicate quite ionic, high-spin metal atoms. This picture is supported by the effective moment estimated from the magnetization measurements (5.840(2) mu(B)), but it is at variance with earlier spin density measurements from polarized neutron diffraction. The magnetic ordering originates from superexchange involving covalent interactions with the ligands, and non-ionic effects are observed in the static deformation density maps as well as in plots of the valence shell charge concentrations. Overall, the present study provides a benchmark charge density that can be used in comparison with future metal formate dihydrate charge densities.

  15. Investigation of Essential Element Distribution in the Equine Metacarpophalangeal Joint using a Synchrotron Radiation Micro X-Ray Fluorescence Technique

    Science.gov (United States)

    Kaabar, Wejdan; Gundogdu, O.; Tzaphlidou, M.; Janousch, M.; Attenburrow, D.; Bradley, D. A.

    2008-05-01

    In articular cartilage, Ca, P, K and S are among some of the well known co-factors of the metalloproteinases enzymatic family, the latter playing a pivotal role in the growth and degeneration of the collagenous bone-cartilage interface of articulating joints. Current study forms part of a larger investigation concerning the distribution of these and other key elements in such media. For the purpose of evaluating these low atomic number elements (Z⩽20), use was made of the capabilities of the LUCIA Station, located at the synchrotron facility of the Paul Scherrer Institute (PSI). Using an incident radiation energy of 4.06 keV, a synchrotron radiation micro x-ray fluorescence (SR-μXRF) technique was applied in examining the distribution of the essential elements Ca, P, K and S in the bone-cartilage interface of both healthy and diseased (osteoarthritic) areas of an equine metacarpophalangeal joint. The SR-μXRF mappings and line profile patterns have revealed remarkable changes in both the pattern and absolute distributions of these elements, agreeing with the findings of others. The elemental presence shown in the individual area scans encompassing the lesion each reflect the visibly abraded outer surface of the cartilage and change in shape of the bone surface. One of the area scans for the bone-cartilage interface shows a marked change in both the pattern and absolute elemental presence for all three elements compared to that observed at two other scan sites. The observation of change in bone cartilage composition around the surface of the articulating joint is thought to be novel, the variation being almost certainly due to the differing weight-bearing role of the subchondral bone at each location.

  16. Phase transformations in Ni/Ti multilayers investigated by synchrotron radiation-based x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cavaleiro, A.J., E-mail: andre.cavaleiro@dem.uc.pt [CEMUC, Department of Mechanical Engineering, University of Coimbra, R. Luís Reis Santos, 3030-788 Coimbra (Portugal); Ramos, A.S. [CEMUC, Department of Mechanical Engineering, University of Coimbra, R. Luís Reis Santos, 3030-788 Coimbra (Portugal); Martins, R.M.S. [CENIMAT/I3N, Department of Materials Science, Faculty of Sciences and Technology, University Nova de Lisboa, 2829-516 Caparica (Portugal); Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); LATR/IST/CTN – Campus Tecnológico e Nuclear, Estrada Nacional 10 ao km 139.7, 2695-066 Bobadela LRS (Portugal); Fernandes, F.M. Braz [CENIMAT/I3N, Department of Materials Science, Faculty of Sciences and Technology, University Nova de Lisboa, 2829-516 Caparica (Portugal); Morgiel, J. [Institute of Metallurgy and Materials Science, Polish Academy of Sciences, Reymonta 25, 30-059 Cracow (Poland); Baehtz, C. [Helmholtz Zentrum Dresden Rossendorf HZDR, Institute of Ion Beam Physics and Materials Research, D-01314 Dresden (Germany); Vieira, M.T. [CEMUC, Department of Mechanical Engineering, University of Coimbra, R. Luís Reis Santos, 3030-788 Coimbra (Portugal)

    2015-10-15

    X-ray diffraction using synchrotron radiation was used for real-time investigation of the phase evolution of Ni/Ti multilayer thin films during annealing. These multilayers were deposited onto Ti–6Al–4V substrates by dc magnetron sputtering from pure Ni and Ti targets. The deposition parameters were adjusted in order to obtain a near equiatomic chemical composition and modulation periods (Λ) below 25 nm. Along the entire thickness of the films, well-defined structures with alternate Ni- and Ti-rich layers are observed, even for Λ = 4 nm. In this case, a halo characteristic of an amorphous structure is obtained, while for Λ of 12 and 25 nm the as-deposited thin films are nanocrystalline being possible to identify the (111) Ni and (002) Ti diffraction peaks. The nanolayered structure vanishes during annealing due to interdiffusion followed by reaction. The reaction between Ni and Ti to produce NiTi in the cubic B2 structure occurs in a short delay of time and within a narrow temperature range. For Λ of 25, 12 and 4 nm, the reaction temperature is close to 320, 350 and 385 °C, respectively. For higher temperatures, in addition to the austenitic phase, the NiTi{sub 2} phase is identified. The diffusion of Ti from the substrate and Ni towards the substrate could favour the precipitation of NiTi{sub 2}. - Highlights: • Alternate Ni- and Ti-rich layers are observed, even for short periods. • Phase evolution was studied using synchrotron radiation XRD during annealing. • Ni and Ti reacted at ∼300–400 °C to form B2–NiTi in a single step. • The higher the period the lower the reaction temperature. • At higher temperatures NiTi{sub 2} was detected due to Ni diffusion towards Ti{sub 6}Al{sub 4}V.

  17. Evaluation of heavy metals in atmospheric emissions from automotive industry by total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Moreira, Silvana; Weber Neto, Jose; Vives, Ana Elisa Sirito de

    2009-01-01

    This study had as goal to determine heavy metals and other elements (Ba, Br, Ca, Pb, Cl, Cr, Sr, Fe, Mn, Ni, K, Si, Ti and Zn) in atmospheric pollutants generated by an automotive industry located in the city of Engenheiro Coelho, state of Sao Paulo, Brazil. The sampling and sample preparation procedures were based on methods established by the Company of Sanitation and Technology (CETESB L9.234) and also by the Environmental Protection Agency (EPA - Method 29). The analysis was performed at XRF Beamline (D09B-XRF) in the Synchrotron Light Source Laboratory (Campinas/SP). A white beam of synchrotron radiation was used for sample and standard excitation which were irradiated by 100 seconds. For X-ray lines detection, a Ge (HP) detector with 150 eV of resolution at 5.9 keV was employed. For zinc, iron, barium, calcium and potassium, the values obtained were in the range of 30 mg/Nm 3 and, for other elements, the concentrations were approximately 1 mg/Nm 3 . The sum of As, Be, Co, Cr, Cu, Mn, Ni, Pb, Sb, Se, Sn, Te and Zn concentration was compared with the limits established by CONAMA 264/1999 and SEMA 041/2002 resolutions (7.0 mg/Nm 3 ) and it was observed that, for all samples, sums are higher than the permissive value mainly due to the high concentration of zinc. Detection limits for SR-TXRF technique were 0.10 μg/Nm 3 for Pb and 0.02 μg/Nm 3 for Zn. (author)

  18. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Prilliman, Stephen Gerald [Univ. of California, Berkeley, CA (United States)

    2003-01-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe2O3) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the γ to the α structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the α structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced α phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the α phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition

  19. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    International Nuclear Information System (INIS)

    Prilliman, Gerald Stephen

    2003-01-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe 2 O 3 ) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the γ to the α structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the α structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced α phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the α phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition that must be overridden with pressure

  20. Incremental distribution of strontium and zinc in great ape and fossil hominin cementum using synchrotron X-ray fluorescence mapping.

    Science.gov (United States)

    Dean, Christopher; Le Cabec, Adeline; Spiers, Kathryn; Zhang, Yi; Garrevoet, Jan

    2018-01-01

    Cementum and the incremental markings it contains have been widely studied as a means of ageing animals and retrieving information about diet and nutrition. The distribution of trace elements in great ape and fossil hominin cementum has not been studied previously. Synchrotron X-ray fluorescence (SXRF) enables rapid scanning of large tissue areas with high resolution of elemental distributions. First, we used SXRF to map calcium, phosphorus, strontium and zinc distributions in great ape dentine and cementum. At higher resolution, we compared zinc and strontium distributions in cellular and acellular cementum in regions where clear incremental markings were expressed. We then mapped trace element distributions in fossil hominin dentine and cementum from the 1.55-1.65 million year old site of Koobi Fora, Kenya. Zinc, in particular, is a precise marker of cementum increments in great apes, and is retained in fossil hominin cementum, but does not correspond well with the more diffuse fluctuations observed in strontium distribution. Cementum is unusual among mineralized tissues in retaining so much zinc. This is known to reduce the acid solubility of hydroxyapatite and so may confer resistance to resorption by osteoclasts in the dynamic remodelling environment of the periodontal ligament and alveolar bone. © 2018 The Author(s).

  1. Localization of iron in rice grain using synchrotron X-ray fluorescence microscopy and high resolution secondary ion mass spectrometry

    KAUST Repository

    Kyriacou, Bianca

    2014-03-01

    Cereal crops accumulate low levels of iron (Fe) of which only a small fraction (5-10%) is bioavailable in human diets. Extensive co-localization of Fe in outer grain tissues with phytic acid, a strong chelator of metal ions, results in the formation of insoluble complexes that cannot be digested by humans. Here we describe the use of synchrotron X-ray fluorescence microscopy (XFM) and high resolution secondary ion mass spectrometry (NanoSIMS) to map the distribution of Fe, zinc (Zn), phosphorus (P) and other elements in the aleurone and subaleurone layers of mature grain from wild-type and an Fe-enriched line of rice (Oryza sativa L.). The results obtained from both XFM and NanoSIMS indicated that most Fe was co-localized with P (indicative of phytic acid) in the aleurone layer but that a small amount of Fe, often present as "hotspots", extended further into the subaleurone and outer endosperm in a pattern that was not co-localized with P. We hypothesize that Fe in subaleurone and outer endosperm layers of rice grain could be bound to low molecular weight chelators such as nicotianamine and/or deoxymugineic acid. © 2014.

  2. Hydration process for calcium-aluminate cement within EVA emulsion by SPring-8 synchrotron radiation x-ray diffraction method

    International Nuclear Information System (INIS)

    Kotera, Masaru; Matsuda, Ikuyo; Miyashita, Keiko; Adachi, Nobuyuki; Tamura, Hisayuki

    2005-01-01

    Polymer-modified mortars which consist of a polymer emulsion and cement materials have been widely developed in the construction materials fields. Forming process of the polymer-modified cement membrane simultaneously involves evaporation of water within the polymer emulsion and hydration of cement. It is important for the polymer-modified cement paste that the hydrate crystal of cement is generating by the hydration during the setting process under existence of the polymer emulsion. In this study, hydration process for calcium-aluminate cement under existence of poly (ethylene-vinyl acetate) (EVA) emulsion (polymer-cement ratio=100%) was investigated by X-ray diffraction method using synchrotron radiation (SPring-8). The diffraction peaks of calcium aluminate (CA) disappeared after the hardening, on the other hand, the peaks of hydrate crystals of calcium-aluminate cement (C 2 AH 8 and C 3 AH 6 ) could be observed. This polymer-modified cement paste hydrated using the water within the polymer emulsion. The hydration of C 2 AH 8 from CA started at around 300 min, and then C 3 AH 6 hydrate crystal increased after 700 min at ambient temperature. This implies that the conversion from C 2 AH 8 to C 3 AH 6 occurred to be more stable phase. The setting temperature affected the reaction rate. In case of hydration at 35degC, the start time of the hydration for calcium-aluminate cement was quicker than that in the ambient temperature four or more times. (author)

  3. Synchrotron Radiation X-Ray Phase-Contrast Tomography Visualizes Microvasculature Changes in Mice Brains after Ischemic Injury

    Directory of Open Access Journals (Sweden)

    Peng Miao

    2016-01-01

    Full Text Available Imaging brain microvasculature is important in plasticity studies of cerebrovascular diseases. Applying contrast agents, traditional μCT and μMRI methods gain imaging contrast for vasculature. The aim of this study is to develop a synchrotron radiation X-ray inline phase-contrast tomography (SRXPCT method for imaging the intact mouse brain (microvasculature in high resolution (~3.7 μm without contrast agent. A specific preparation protocol was proposed to enhance the phase contrast of brain vasculature by using density difference over gas-tissue interface. The CT imaging system was developed and optimized to obtain 3D brain vasculature of adult male C57BL/6 mice. The SRXPCT method was further applied to investigate the microvasculature changes in mouse brains (n=14 after 14-day reperfusion from transient middle cerebral artery occlusion (tMCAO. 3D reconstructions of brain microvasculature demonstrated that the branching radius ratio (post- to preinjury of small vessels (radius < 7.4 μm in the injury group was significantly smaller than that in the sham group (p<0.05. This result revealed the active angiogenesis in the recovery brain after stroke. As a high-resolution and contrast-agent-free method, the SRXPCT method demonstrates higher potential in investigations of functional plasticity in cerebrovascular diseases.

  4. Synchrotron X-ray diffraction studies of phase transitions in physisorbed monolayers of rare gases on graphite

    International Nuclear Information System (INIS)

    Bohr, J.

    1984-01-01

    This study is an investigation of phase transition in monoatomic layers adsorbed on graphite. Such effects can be considered physical realizations of two-dimensional systems. The experimental technique used is synchrotron X-ray diffraction. Systems which have been investigated include the commensurate-incommensurate phase transition in krypton monolayer. By adjusting the spreading pressure in the krypton layer by means of a coadsorbent deuterium gas it has been unambiguously demonstrated that at low temperatures the phase transition is of first order. A melting study of incommensurate argon monolayers demonstrates an experimental verification of the possibility for having a continuous melting transition in two-dimensions. Mixtures of two-components have been investigated for their phases. No (chemical) order-disorder transition is seen. A discussion is given on this lack of a chemical order. This lack is utilized to study the commensurate-incommensurate phase transition driven by average particle size. Finally, a special low-temperature phase is identified in a xenon monlayer which is diluted with freon. (Auth.)

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

    Science.gov (United States)

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

    2015-03-01

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

  6. In situ and real-time analysis of the growth and interaction of equiaxed grains by synchrotron X- ray radiography

    Science.gov (United States)

    Bogno, A.; Nguyen-Thi, H.; Billia, B.; Reinhart, G.; Mangelinck-Noël, N.; Bergeon, N.; Schenk, T.; Baruchel, J.

    2012-01-01

    The phenomena involved during equiaxed growth are dynamic, so that in situ and real-time investigation by X-ray imaging is compulsory to fully analyse the microstructure formation. The experiments on Al - 10 wt% Cu alloy of this paper are carried out at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France). Equiaxed growth was achieved in nearly isothermal conditions and continuously monitored from the very early stages of solidification to an asymptotic state. First, measurements of dendrite arms velocity for a same grain showed slight differences in the early stages of the growth. This effect is attributed to a gravity-related "self - poisoning" of the grain. Then, the propagation of primary dendrite arms was analysed and two successive growth regimes were observed. First, due to the relative distance with neighbour grains, each grain could be considered as isolated (i.e. growing freely) and tip growth rate gradually increased. In a subsequent phase, tip growth rate slowly decreased towards zero, due to the proximity of neighbouring grains. Using an image analysis technique, we were able to measure the solute profiles in the liquid phase between interacting arms. These measurements confirmed that solutal impingement is responsible for stopping the grain growth.

  7. Simulation of AZ-PN100 resist pattern fluctuation in X-ray lithography, including synchrotron beam polarization

    International Nuclear Information System (INIS)

    Scheckler, E.W.; Ogawa, Taro; Tanaka, Toshihiko; Takeda, Eiji; Oizumi, Hiroaki.

    1993-01-01

    A new simulation model for nanometer-scale pattern fluctuation in X-ray lithography is presented and applied to a study of AZ-PN100 negative chemical amplification resist. The exposure simulation considers polarized photons from a synchrotron radiation (SR) source. Monte Carlo simulation of Auger and photoelectron generation is followed by electron scattering simulation to determine the deposited energy distribution at the nanometer scale, including beam polarization effects. An acid-catalyst random walk model simulates the post-exposure bake (PEB) step. Fourier transform infrared (FTIR) spectroscopy and developed resist thickness measurements are used to fit PEB and rate models for AZ-PN100. A polymer removal model for development simulation predicts the macroscopic resist shape and pattern roughness. The simulated 3σ linewidth variation is in excess of 24 nm. Simulation also shows a detrimental effect if the beam polarization is perpendicular to the line. Simulation assuming a theoretical ideal exposure yields a 50 nm minimum line for standard process conditions. (author)

  8. P3HT/PCBM polymer thin films studied by synchrotron-based grazing incidence X-ray diffraction

    International Nuclear Information System (INIS)

    Yang Yingguo; Zhengguan Haojie; Ji Gengwu; Feng Shanglei; Li Xiaolong; Gao Xingyu

    2014-01-01

    Background: The microstructures of P3HT (poly(3-hexyl-thiophene)) in P3HT/PCBM ([6, 6]-phenyl C61-butyric acid methyl ester) thin films play a key role in governing the performance of organic solar cells (OSCs) based on these films. Purpose: We aim to study the self-organization of P3HT in the P3HT/PCBM thin films annealed at different temperatures. Methods: Using different incidence angles, information about the microstructures of P3HT at different depths in these films was obtained by synchrotron based grazing incidence X-ray diffraction (GIXRD). Results: It is shown that the crystalline structure of P3HT has been substantially improved by thermal annealing. One dimensional GIXRD clearly indicates that P3HT edge-on structures in the inner layers have been improved with their number increased in comparison with those at the surface and the interface layers. In addition, thermal annealing also helps the formation of P3HT face-on structures in the films, as evidenced by 2 dimensional GIXRD. Conclusion: The improved structures in these films lead to more charge transport channels formed to improve the carrier mobility, which in turn helps the improvement of OSCs. Thus, the present GIXRD results will improve the understanding of annealing effects at different depths of the P3HT/PCBM thin films for enhanced OSCs devices. (authors)

  9. Analysis of residual stress in metal-inert-gas-welded Al-2024 using neutron and synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Ganguly, S.; Stelmukh, V.; Edwards, L.; Fitzpatrick, M.E.

    2008-01-01

    A combination of neutron and synchrotron X-ray diffraction was used to measure and map the full three-dimensional state of residual stress across the cross-section in coupon samples of metal-inert-gas (MIG)-welded 2024 aluminium alloy. Samples were analysed both as-welded and following a post-welding skim which served to remove the weld flash and reduce the plate thickness. The profile of the residual stress and its evolution following skimming has been accurately characterized. The longitudinal direction shows the highest residual stress, approaching 300 MPa in tension. The skimming treatment did not change the peak stress, but the overall profile of stress was altered: this is slightly unexpected as machining away stressed material would generally be expected to reduce the peak residual stress. The results are discussed in terms of the generation of stress during welding and its evolution during skimming. Finally a comparison is made with the stress generated in the as-welded and skimmed conditions of a variable polarity plasma arc (VPPA)-welded specimen of similar dimensions, to show the effects of different weld processes on the residual stress generated. The stress measurement in the VPPA sample was carried out under near identical experimental conditions

  10. Experimental determination of bulk modulus of 14Å tobermorite using high pressure synchrotron X-ray diffraction

    KAUST Repository

    Oh, Jae Eun

    2012-02-01

    Using a diamond anvil cell, 14 Å tobermorite, a structural analogue of calcium silicate hydrates (C-S-H), was examined by high-pressure synchrotron X-ray diffraction up to 4.8 GPa under hydrostatic conditions. The bulk modulus of 14 Å tobermorite was calculated, K o = 47 GPa. Comparison of the current results with previous high pressure studies on C-S-H(I) indicates that: (1) the compression behavior of the lattice parameters a and b of 14 Å tobermorite and C-S-H(I) are very similar, implying that both materials may have very similar Ca-O layers, and also implying that an introduction of structural defects into the Ca-O layers may not substantially change in-plane incompressibility of the ab plane of 14 Å tobermorite; and (2) the bulk modulus values of 14 Å tobermorite and C-S-H(I) are dominated by the incompressibility of the lattice parameter c, which is directly related to the interlayer spacing composed of dreierketten silicate chains, interlayer Ca, and water molecules. © 2011 Elsevier Ltd. All rights reserved.

  11. In situ synchrotron radiation X-ray diffraction studies on molecular aggregation structure of nylon 12 films during bulge testing.

    Science.gov (United States)

    Kojio, Ken; Nagano, Chigusa; Fujimoto, Aya; Nozaki, Shuhei; Yokomachi, Kazutoshi; Kamitani, Kazutaka; Watanabe, Hirohmi; Takahara, Atsushi

    2018-02-28

    It is desirable to establish a method for evaluating mechanical properties, such as modulus and strength, of micrometer and sub-micrometer thick polymer films. Bulge tests, where bulge deformation is imposed on films by the pressure of an inert gas, are suitable for satisfying this demand. However, very few studies on polymer films exist in the literature. In this study, bulge testing equipment for in situ synchrotron radiation wide-angle X-ray diffraction (WAXD) measurements is designed and used to study the relationship between the molecular aggregation structure and the mechanical properties of a crystalline nylon 12 (Ny12) film during bulge testing. Isothermally crystallized and quenched Ny12 films exhibited stress-strain curves similar to those obtained by conventional uniaxial elongation. In situ WAXD measurements during bulge testing revealed that the lattice extension of the crystallites is clearly dependent on crystallinity. Concretely, crystallites in the isothermally crystallized film show higher elastic properties than those in the quenched one. The results of the molecular aggregation structure, including the crystal structure and the amorphous chain surrounding the crystallites, of the films during bulge deformation firstly obtained in this study must be useful for designing toughened polymer films.

  12. Microstructural investigation using synchrotron radiation X-ray microtomography reveals taste-masking mechanism of acetaminophen microspheres.

    Science.gov (United States)

    Guo, Zhen; Yin, Xianzhen; Liu, Congbiao; Wu, Li; Zhu, Weifeng; Shao, Qun; York, Peter; Patterson, Laurence; Zhang, Jiwen

    2016-02-29

    The structure of solid drug delivery systems has considerable influence on drug release behaviors from particles and granules and also impacts other properties relevant to release characteristics such as taste. In this study, lipid-based microspheres of acetaminophen were prepared to mask the undesirable taste of drug and therefore to identify the optimal formulation for drug release. Synchrotron radiation X-ray computed microtomography (SR-μCT) was used to investigate the fine structural architectures of microspheres non-destructively at different sampling times during drug release test, which were simultaneously determined to quantitatively correlate the structural data with drug release behaviors. The results demonstrated that the polymeric formulation component, namely, cationic polymethacrylate (Eudragit E100), was the key factor to mask the bitter taste of acetaminophen by inhibiting immediate drug release thereby reducing the interaction intensity of the bitter material with the oral cavity taste buds. The structure and morphology of the microspheres were found to be influenced by the shape and particle size of the drug, which was also an important factor for taste-masking performance. The quantitative analysis generated detailed structural information which was correlated well with drug release behaviors. Thus, SR-μCT has been proved as a powerful tool to investigate the fine microstructure of particles and provides a new approach in the design of particles for taste masking. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Tests of small X-ray Active Matrix Pixel Sensor prototypes at the National Synchrotron Light Source

    Science.gov (United States)

    Carini, G. A.; Chen, W.; Dragone, A.; Fried, J.; Jakoncic, J.; Kuczweski, A.; Li, Z.; Mead, J.; Michta, R.; Pratte, J.-F.; Rehak, P.; Siddons, D. P.

    2009-03-01

    X-ray Active Matrix Pixel Sensors (XAMPS) were designed and fabricated at Brookhaven National Laboratory. Devices based on J-FET technology were produced on 100 mm high-resistivity silicon, typically 400 μm-thick. The prototypes are square matrices with n rows and n columns with n = 16, 32, 64, 128, 256, 512. Each pixel of the matrix is 90 × 90 μm2 and contains a JFET switch to control the charge readout. The XAMPS is a position sensitive ionization detector made on high resistivity silicon. It consists of a pixel array detector with integrated switches. Pixels are isolated from each other by a potential barrier and the device is fully depleted by applying a high voltage bias to the junction on the entrance window of the sensor. The small features of the design presented some technological challenges fully addressed during this production. The first prototypes were tested at the National Synchrotron Light Source (NSLS) with a monochromatic beam of 8 keV and millisecond readout and exhibit good performances at room temperature.

  14. Tests of small X-ray Active Matrix Pixel Sensor prototypes at the National Synchrotron Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Carini, G A; Chen, W; Fried, J; Jakoncic, J; Kuczweski, A; Li, Z; Mead, J; Michta, R; Pratte, J-F; Rehak, P; Siddons, D P [Brookhaven National Laboratory, Upton, 11973 NY (United States); Dragone, A [SLAC National Accelerator Center, Menlo Park, 94025 CA (United States)], E-mail: carini@bnl.gov

    2009-03-15

    X-ray Active Matrix Pixel Sensors (XAMPS) were designed and fabricated at Brookhaven National Laboratory. Devices based on J-FET technology were produced on 100 mm high-resistivity silicon, typically 400 {mu}m-thick. The prototypes are square matrices with n rows and n columns with n = 16, 32, 64, 128, 256, 512. Each pixel of the matrix is 90 x 90 {mu}m{sup 2} and contains a JFET switch to control the charge readout. The XAMPS is a position sensitive ionization detector made on high resistivity silicon. It consists of a pixel array detector with integrated switches. Pixels are isolated from each other by a potential barrier and the device is fully depleted by applying a high voltage bias to the junction on the entrance window of the sensor. The small features of the design presented some technological challenges fully addressed during this production. The first prototypes were tested at the National Synchrotron Light Source (NSLS) with a monochromatic beam of 8 keV and millisecond readout and exhibit good performances at room temperature.

  15. Dynamics of water intercalation fronts in a nano-layered synthetic silicate: A synchrotron X-ray scattering study

    International Nuclear Information System (INIS)

    Lovoll, G.; Sandnes, B.; Meheust, Y.; Maloy, K.J.; Fossum, J.O.; Silva, G.J. da; Mundim, M.S.P.; Droppa, R. Jr.; Fonseca, D.M.

    2005-01-01

    We performed synchrotron X-ray scattering studies of the dynamics of the water intercalation front in a Na-Fluorohectorite clay. Like other smectite clays, fluorohectorite particles can swell due to intercalation of successive water layers. Monitoring the intensities of Bragg peaks of the known 1- and 2-water-layer hydration states at different positions in the sample enabled spatial and temporal measurement of the proportions of the different hydration states. From experiments with controlled temperature and an imposed humidity gradient on a quasi one-dimensional powder sample, we were able to localize the intercalation front and demonstrate that the width of this front was smaller than 2 mm after penetrating 9 mm into the sample. The speed at which the intercalation front advanced through the sample during the diffusion process was shown to decrease with time. The diffraction signature of random water intercalation in the vicinity of the intercalation front also provided information on the changes in the water content of the mesopores around clay particles

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

    Science.gov (United States)

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

    2011-03-01

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

  17. Simultaneous structural enhancement of powder diffraction spectra obtained by X-ray, neutron and synchrotron diffraction studies

    International Nuclear Information System (INIS)

    Maichle, J.K.

    1988-01-01

    The novel method for the enhancement of structural data is explained, and is applied for the first time for a simultaneous analysis and evaluation of neutron and synchrotron diffraction data obtained for the superconductor BaPb 0.75 Bi 0.25 O 3 . This substance can be specified in the measured temperature range between 2 K and 310 K to belong to the monoclinic space group I 2/m, and thus is determined to be in a distorted perovskite cell ahead of (a≅b≅√2 a 0 ; c≅2a 0 ). The oxygen octaeders are for the most part tilted around the (x.1/4.1/4)-axis. The simultaneous evaluation of several X-ray diffraction data sets of the high-T c superconductor YBa 2 Cu 3 O 7±z confirms the orthorhombic symmetry with space group P mmm, YBa 2 Cu 3 O 7±z likewise is in a distorted perovskite cell ahead of (a≅b≅a 0 ; c≅3a 0 ). At low temperatures, however, a saddle-shaped distortion of the oxygen group, hitherto believed to be plane, is found in the plane (x.y.0.37). (orig.) [de

  18. [Metallic Elemental Analysis of Tibetan Herbal Medicines and Tibetan Medicine Preparations by Synchrotron Radiation X-Ray Fluorescence].

    Science.gov (United States)

    Yang, Hong-xia; Li Cen; Du, Yu-zhi; Wei, Li-xin

    2015-06-01

    To discuss the relationship between metallic element and disease through determine the elementals in Tibetan Herbal Medicines and Tibetan Medicine Preparations that have obvious effect on hepatobiliary diseases by Synchrotron Radiation X-ray Source, then to reveal the substance foundation of pharmacological action. The results show that all the Tibetan Herbal Medicines used in the experiment have the 9 kinds of metallic elements of potassium(K), calcium(Ca), titanium(Ti), vanadium(V), chromium(Cr), manganese(Mn), ferrum(Fe), zinc(Zn) and lead(Pb), the content of the elements are in the ppb or ppm level though the element constitute and the content have obvious difference. Tibetan Medicine Preparations have another 6 kinds of metallic elements of nickel(Ni), copper(Cu), rubidium(Rb), mercury(Hg), cobalt(Co), gallium(Ga) and 1 kind of nonmetallic elements of arsenic(As) when compare with Herbal Medicines, and the element constitute and the content also have obvious difference. Take advantage of SR-XRF, the test gets the basic data of elements of Tibetan Herbal Medicines and Preparations, supply the scientific support to discuss the interaction of pharmacological mechanism and the metallic elements, and find the suitability of the technique for the metallic elements detection in Tibetan Medicines.

  19. PRELIMINARY RESULTS IN SYNCHROTRON X-RAY DIFFRACTION MEASUREMENTS OF RUBBER COMPOSITES STRUCTURE BEFORE AND AFTER EXPOSURE TO HYDROGEN

    Directory of Open Access Journals (Sweden)

    Francesca Cosmi

    2011-05-01

    Full Text Available In future years, fuel cells are expected to represent a promising technology as a source of heat and electricity in buildings and of electrical power for vehicles, since fossil fuels are exhausting and significantly degrade air quality. It is well known that, when exposed to a hydrogen environment, hydrogen embrittlerment may affect materials such as iron and steel. But these are not the only materials that are used for hydrogen equipment. In particular, the rubber materials used for O–rings that seal high pressure hydrogen gas equipment show problems of internal fracture, called blister fracture, when the gas is rapidly decompressed. As many different kinds of fillers can be used, in this work we started to investigate the influence of the type of filler on the rubber composites structure, by means of X-ray diffraction measurements performed at the Elettra synchrotron radiation facility in Trieste. In this preliminary study, three kinds of samples were analyzed before and after exposure to hydrogen: Sulphur vulcanized EPDM, Peroxide vulcanized EPDM and Sulphur vulcanized NBR. While Peroxide vulcanized samples did not show significant differences in the diffraction pattern, changes could be detected in the cristalline form of Sulfure vulcanized rubber.

  20. Trace elemental analysis of drugs of abuse using synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF).

    Science.gov (United States)

    Muratsu, Seiji; Ninomiya, Toshio; Kagoshima, Yasushi; Matsui, Junji

    2002-09-01

    Synchrotron radiation total reflection X-ray fluorescence spectroscopy (SR-TXRF) was utilized to analyze various trace elements in small amounts of drugs of abuse. Sample amounts of 1 microL solutions containing 10 microg of drugs (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, cocaine, and heroin) were spotted on silicon wafers for direct analysis. In addition, a leaflet of marijuana was set directly on a silicon wafer, and opium in the form of a soft lump was smeared on another silicon wafer for analysis. In these experiments, about 10 pg of contaminant elements could be detected. For example, in a seized methamphetamine sample, iodine was found, which could be indicative of synthetic route. In seized 3,4-methylenedioxymethamphetamine samples, variable amounts of phosphorus, calcium, sulfur, and potassium were found, which could not be detected in a control 3,4-methylenedioxymethamphetamine sample. For marijuana and opium, two spectral patterns were obtained that were far different from each other and could be easily discriminated. Using SR-TXRF, pg amounts of each trace element in 10 microg of various drugs can be easily detected, which is not the case either for a standard TXRF experimental system or for other elemental analysis techniques.