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Sample records for 3d x-ray diffraction

  1. A method based on diffraction theory for predicting 3D focusing performance of compound refractive X-ray lenses

    Zichun Le; Kai Liu; Jingqiu Liang

    2005-01-01

    A method based on the diffraction theory for estimating the three-dimensional (3D) focusing performance of the compound refractive X-ray lenses is presented in this paper. As a special application, the 3D X-ray intensity distribution near the focus is derived for a plano-concave compound refractive X-ray lens.Moreover, the computer codes are developed and some results of 3D focusing performance for a compound refractive X-ray lens with Si material are shown and discussed.

  2. New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging

    Ludwig, W.; King, A.; Reischig, P.;

    2009-01-01

    Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes...... and crystallographic orientations for certain categories of polycrystalline materials. Direct visualisation of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques may be possible, but is restricted to specific...... material systems. A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain...

  3. New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging

    Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes and crystallographic orientations for certain categories of polycrystalline materials. Direct visualisation of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques may be possible, but is restricted to specific material systems. A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape, crystallographic orientation and local attenuation coefficient distribution. The technique applies to the larger range of plastically undeformed, polycrystalline mono-phase materials, provided some conditions on grain size and texture are fulfilled. The straightforward combination with high-resolution microtomography opens interesting new possibilities for the observation of microstructure related damage and deformation mechanisms in these materials.

  4. New insights into single-grain mechanical behavior from temperature-dependent 3-D coherent X-ray diffraction

    Coherent X-ray diffraction is able to yield non-destructively 3-D strain maps with unprecedented resolution in small isolated crystals. In this work we have used this technique to investigate the mechanical behavior of a single grain within a Au polycrystalline film. The 111 Bragg reflection from a 1250×950×475 nm single grain has been successfully measured in three dimensions during thermomechanical loading. From these 3-D reciprocal space maps the displacement field is obtained through a specific phase-retrieval procedure. The uz(x,y,z) component of the displacement field component is deduced as a function of temperature with a high spatial resolution of 17×17×22 nm within the single grain. This displacement field is discussed with respect to grain-to-grain interactions in the supported metal film. This study opens important perspectives for the evaluation of mechanical properties of polycrystals via coherent X-ray diffraction

  5. X-Ray Diffraction.

    Smith, D. K.; Smith, K. L.

    1980-01-01

    Reviews applications in research and analytical characterization of compounds and materials in the field of X-ray diffraction, emphasizing new developments in applications and instrumentation in both single crystal and powder diffraction. Cites 414 references. (CS)

  6. Characterization of 3D Trench PZT Capacitors for High Density FRAM Devices by Synchrotron X-ray Micro-diffraction

    Shin, Sangmin; Han, Hee; Park, Yong Jun; Choi, Jae-Young; Park, Youngsoo; Baik, Sunggi

    2007-01-01

    3D trench PbZrxTi1-xO3 (PZT) capacitors for 256 Mbit 1T-1C FRAM devices were characterized by synchrotron X-ray micro-diffraction at Pohang Light Source. Three layes, Ir/PZT/Ir were deposited on SiO2 trench holes with different widths ranging from 180 nm to 810 nm and 400 nm in depth by ALD and MOCVD. Each hole is separated from neighboring holes by 200 nm. The cross sectional TEM analysis for the trenches revealed that the PZT layers were consisted of columnar grains at the trench entrance and changes to polycrystalline granular grains at the lower part of the trench. The transition from columnar to granular grains was dependent on the trench size. The smaller trenches were favorable to granular grain formation. High resolution synchrotron X-ray diffraction analysis was performed to determine the crystal structure of each region. The beam was focused to about 500 μm and the diffraction patterns were obtained from a single trench. Only the peaks corresponding to ferroelectric tetragonal phases are observed for the trenches larger than 670 nm, which consist of fully columnar grains. However, the trenches smaller than 670 nm showed the peaks corresponding the pyrochlore phases, which suggested that the granular grains are of pyrochlore phases and non-ferroelectric.

  7. Characterization of 3D Trench PZT Capacitors for High Density FRAM Devices by Synchrotron X-ray Micro-diffraction

    3D trench PbZrxTi1-xO3 (PZT) capacitors for 256 Mbit 1T-1C FRAM devices were characterized by synchrotron X-ray micro-diffraction at Pohang Light Source. Three layers, Ir/PZT/Ir were deposited on SiO2 trench holes with different widths ranging from 180 nm to 810 nm and 400 nm in depth by ALD and MOCVD. Each hole is separated from neighboring holes by 200 nm. The cross sectional TEM analysis for the trenches revealed that the PZT layers were consisted of columnar grains at the trench entrance and changes to polycrystalline granular grains at the lower part of the trench. The transition from columnar to granular grains was dependent on the trench size. The smaller trenches were favorable to granular grain formation. High resolution synchrotron X-ray diffraction analysis was performed to determine the crystal structure of each region. The beam was focused to about 500 μm and the diffraction patterns were obtained from a single trench. Only the peaks corresponding to ferroelectric tetragonal phases are observed for the trenches larger than 670 nm, which consist of fully columnar grains. However, the trenches smaller than 670 nm showed the peaks corresponding the pyrochlore phases, which suggested that the granular grains are of pyrochlore phases and non-ferroelectric

  8. Stability of dislocation structures in copper towards stress relaxation investigated by high angular resolution 3D X-ray diffraction

    Jakobsen, Bo; Poulsen, Henning Friis; Lienert, Ulrich;

    2009-01-01

    A 300 µm thick tensile specimen of OFHC copper is subjected to a tensile loading sequence and deformed to a maximal strain of 3.11%. Using the novel three-dimensional X-ray diffraction method High angular resolution 3DXRD', the evolution of the microstructure within a deeply embedded grain is cha...

  9. X-ray diffraction

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  10. X-ray diffraction

    The seventh edition of Philips' Review of literature on X-ray diffraction begins with a list of conference proceedings on the subject, organised by the Philips' organisation at regular intervals in various European countries. This is followed by a list of bulletins. The bibliography is divided according to the equipment (cameras, diffractometers, monochromators) and its applications. The applications are subdivided into sections for high/low temperature and pressure, effects due to the equipment, small angle scattering and a part for stress, texture and phase analyses of metals and quantitative analysis of minerals

  11. Interface Orientation Distribution during Grain Growth in Bulk SrTiO3 Measured by Means of 3D X-Ray Diffraction Contrast Tomography

    Syha, Melanie; Rheinheimer, Wolfgang; Bäurer, Michael;

    2012-01-01

    interface normal distribution clearly shows a preference for (100) oriented interfaces in the selected grains when annealed at 1600°C. This observation can be connected to existent interfacial energy estimations resulting from capillarity vector reconstructions. © 2012 Materials Research Society.......3D x-ray diffraction contrast tomography (DCT) is a non-destructive technique for the determination of grain shape and crystallography in polycrystalline bulk materials. Using this technique, a strontium titanate specimen was repeatedly measured between annealing steps.. A systematic analysis of...

  12. X-ray diffraction apparatus

    The invention provides an x-ray diffraction apparatus permitting the rotation of the divergence sit in conjunction with the rotation of the x-ray irradiated specimen, whereby the dimensions of the x-ray irradiated portion of the specimen remain substantially constant during the rotation of the specimen. In a preferred embodiment, the divergence slit is connected to a structural element linked with a second structural element connected to the specimen such that the divergence slit rotates at a lower angular speed than the specimen

  13. 3-D growth of a short fatigue crack within a polycrystalline microstructure studied using combined diffraction and phase-contrast X-ray tomography

    Herbig, M.; King, Andrew; Reischig, Peter;

    2011-01-01

    X-ray diffraction contrast tomography is a recently developed, non-destructive synchrotron imaging technique which characterizes microstructure and grain orientation in polycrystalline materials in three dimensions. By combining it with propagation-based phase-contrast tomography it is possible t...... beta titanium alloy Ti 21S that allows for visualization and analysis of the growth rate and crystallographic orientation of the fracture surface....

  14. Submicron X-ray diffraction

    At the Advanced Light Source in Berkeley the authors have instrumented a beam line that is devoted exclusively to x-ray micro diffraction problems. By micro diffraction they mean those classes of problems in Physics and Materials Science that require x-ray beam sizes in the sub-micron range. The beam line has a unity magnification toroidal mirror that produces a 50 by 200 micron focus just inside an x-ray hutch at the position of an x-y slit. The beam path in the hutch consists of source defining slits, a four bounce Ge or Si monochromator, followed by elliptically bent Kirkpatrick-Baez mirror pair which focuses the beam from the slits to sub micron dimensions (0.8 x 0.8 microns). An important feature of this arrangement is the ability to switch between white and monochromatic beams that are essential for characterizing crystals or crystal grains in the sub-micron range. Since sample rotation is fixed they have facilities for precision translation of the specimen to allow them to scan different crystal regions or grains. The sample stage rests on a state of the art six-circle diffractometer equipped with encoders in the main rotation stages calibrated to a second of arc. The detector is a 4K x 4K CCD (Bruker) with a 9 x 9 cm view area mounted on a detector arm that can be positioned around the sample. The detector itself can also be positioned to better than 1 micron along the detector arm. Using this facility they have been able to measure the orientation structure of single grains of passivated or buried Al interconnect test structures. Such structures or their equivalents are important in connecting individual components on integrated circuits. Their sub-micron dimensions result in very high current densities that can result in interconnect failures. The variation in sub-grain structure in a single grain is rich in detail. They have obtained detailed maps of misorientations in single grains using white beam Laue diffraction patterns From these they have been

  15. X-ray topography and multiple diffraction

    A short summary on X-ray topography, which is based on the dynamical theory of X-ray diffraction, is made. The applications and properties related to the use of the multiple diffraction technique are analized and discussed. (L.C.)

  16. X-Ray Diffractive Optics

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  17. Two-dimensional x-ray diffraction

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  18. X-ray diffraction imaging and analysis

    The first papers dealing with the very important application of x-ray diffraction to crystal structure analysis were also published in 1912 by W.L. Bragg, while a student at Cambridge. Bragg performed an analysis of the Laue diffraction pattern of zinc blend and determined the correct structure of the crystal lattice. There have been many practical applications for x-ray diffraction techniques. Historically conventional x-ray machines were used as generators and film used as the recording medium. Prior to 1966, all attempts to directly image x-ray diffraction patterns used a large format x-ray image intensifier tube of the same type as conventionally used for medical and industrial fluoroscopy. Since the 1960's numerous electro-optical systems have been developed which are far better suited for real-time viewing and recording of x-ray diffraction patterns. Modern x-ray diffraction imaging systems incorporating rotating anode and pulsed x-ray generators, synchrotron x-ray sources, and optimized electro-optical systems have been used to orient single crystals, to study crystal lattice rotation accompanying plastic deformation, to measure the rate of grain boundary migration during recrystallization annealing of cold-worked metals, to determine the physical state of exploding metals, to rapidly measure residual stress (strain), to study the dynamics of structural phase transitions in ferroelectric crystals, to monitor the amorphous to crystalline phase transformation of rapidly solidified metals, and to record topographic images of lattice defects in quartz, gallium arsenide and nickel alloy turbine blade crystals

  19. 3D Rotational X-Ray guidance for surgical interventions

    Kraats, Everine Brenda van de

    2005-01-01

    The research described in this thesis is aimed at increasing the accuracy and decreasing the invasiveness of surgical procedures, with a focus on spine procedures, by using a combination of multi-modality images, computer-assisted navigation, intraoperative 3D rotational X-ray (3DRX) imaging, and mi

  20. Diffraction enhanced x-ray imaging

    Diffraction enhanced imaging (DEI) is a new x-ray radiographic imaging modality using synchrotron x-rays which produces images of thick absorbing objects that are almost completely free of scatter. They show dramatically improved contrast over standard imaging applied to the same phantoms. The contrast is based not only on attenuation but also the refraction and diffraction properties of the sample. The diffraction component and the apparent absorption component (absorption plus extinction contrast) can each be determined independently. This imaging method may improve the image quality for medical applications such as mammography

  1. Soft x-ray resonant magnetic diffraction.

    Wilkins, S. B.; Hatton, P. D.; Roper, M.D.; Prabhakaran, D.; Boothroyd, A. T.

    2003-01-01

    We have conducted the first soft x-ray diffraction experiments from a bulk single crystal, studying the bilayer manganite La22xSr12xMn2O7 with x 0:475 in which we were able to access the (002) Bragg reflection using soft x rays. The Bragg reflection displays a strong resonant enhancement at the LIII and LII manganese absorption edges. We demonstrate that the resonant enhancement of the magnetic diffraction of the (001) is extremely large, indeed so large that it exceeds that of t...

  2. Single Particle X-ray Diffractive Imaging

    Bogan, M J; Benner, W H; Boutet, S; Rohner, U; Frank, M; Seibert, M; Maia, F; Barty, A; Bajt, S; Riot, V; Woods, B; Marchesini, S; Hau-Riege, S P; Svenda, M; Marklund, E; Spiller, E; Hajdu, J; Chapman, H N

    2007-10-01

    In nanotechnology, strategies for the creation and manipulation of nanoparticles in the gas phase are critically important for surface modification and substrate-free characterization. Recent coherent diffractive imaging with intense femtosecond X-ray pulses has verified the capability of single-shot imaging of nanoscale objects at sub-optical resolutions beyond the radiation-induced damage threshold. By intercepting electrospray-generated particles with a single 15 femtosecond soft-X-ray pulse, we demonstrate diffractive imaging of a nanoscale specimen in free flight for the first time, an important step toward imaging uncrystallized biomolecules.

  3. The Dynamical Theory of X Ray Diffraction

    Balchin, A. A.; Whitehouse, C. R.

    1974-01-01

    Summarizes the Darwin theory of x-ray diffraction in thin crystals or crystals with a mosaic texture and its modified application to crystals with three-dimensional electrostatic dipoles. Indicates that the dynamical theory is brought into its present relevance by the improvement of single crystal growth techniques. (CC)

  4. Advanced X-ray diffractive optics

    Vila-Comamala, J; Jefimovs, K; Sarkar, S S; Solak, H H; Guzenko, V A; Stampanoni, M; Marone, F; Raabe, J; Tzvetkov, G; Grolimund, D; Borca, C N; David, C [Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Pilvi, T; Ritala, M [Department of Chemistry, FIN-00014 University of Helsinki (Finland); Fink, R H [Friedrich-Alexander Universitaet, D-91058 Erlangen (Germany); Kaulich, B, E-mail: joan.vila@psi.c [ELETTRA Sincrotrone, I-34012 Basovizza (Italy)

    2009-09-01

    X-ray microscopy greatly benefits from the advances in x-ray optics. At the Paul Scherrer Institut, developments in x-ray diffractive optics include the manufacture and optimization of Fresnel zone plates (FZPs) and diffractive optical elements for both soft and hard x-ray regimes. In particular, we demonstrate here a novel method for the production of ultra-high resolution FZPs. This technique is based on the deposition of a zone plate material (iridium) onto the sidewalls of a prepatterned template structure (silicon) by atomic layer deposition. This approach overcomes the limitations due to electron-beam writing of dense patterns in FZP fabrication and provides a clear route to push the resolution into sub-10 nm regime. A FZP fabricated by this method was used to resolve test structures with 12 nm lines and spaces at the scanning transmission x-ray microscope of the PolLux beamline of the Swiss Light Source at 1.2 keV photon energy.

  5. X-ray energy dispersive diffraction

    X-ray energy dispersive diffraction is used mainly for structural characterization of polycrystalline powders and amorphous materials. One of the important features of it is the fixed scattering angle facilitating in particular studies of materials in special environments (e.g., high pressure, high and low temperature). There are two versions of X-ray energy dispersive diffraction. In one - called XED - an incident 'white' beam is used and the spectral distribution of the diffracted photons is analyzed by means of a solid state detector. Its important feature is the simultaneous appearance of all reflections. In the other version - called monochromator scan method (MSM) - the incident beam is monochromatic and its wavelength is changed stepwise by rotating the crystal monochromator. (orig.)

  6. Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2016-08-09

    A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

  7. Basic of X-ray diffraction

    Giacovazzo, C. [Bari Univ. (Italy). Dip. Geomineralogico

    1996-09-01

    The basic concepts of X-ray diffraction may be more easily understood if it is made preliminary use of a mathematical background. In these pages the authors will first define the delta function and its use for the representation of a lattice. Then the concepts of Fourier transform and convolution are given. At the end of this talk one should realize that a crystal is the convolution of the lattice with a function representing the content of the unit cell.

  8. X-ray diffraction contrast tomography (DCT) system, and an X-ray diffraction contrast tomography (DCT) method

    2012-01-01

    Source: US2012008736A An X-ray diffraction contrast tomography system (DCT) comprising a laboratory X-ray source (2), a staging device (5) rotating a polycrystalline material sample in the direct path of the X-ray beam, a first X-ray detector (6) detecting the direct X-ray beam being transmitted...

  9. 3D synchrotron x-ray microtomography of paint samples

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

    2009-07-01

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

  10. Glancing angle synchrotron X-ray diffraction

    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. Glancing angle synchrotron X-ray diffraction

    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.

  12. X-Ray Diffraction on NIF

    Eggert, J H; Wark, J

    2012-02-15

    The National Ignition Facility (NIF) is currently a 192 beam, 1.6 MJ laser. NIF Ramp-Compression Experiments have already made the relevant exo-planet pressure range from 1 to 50 Mbar accessible. We Proposed to Study Carbon Phases by X-Ray Diffraction on NIF. Just a few years ago, ultra-high pressure phase diagrams for materials were very 'simple'. New experiments and theories point out surprising and decidedly complex behavior at the highest pressures considered. High pressures phases of aluminum are also predicted to be complex. Recent metadynamics survey of carbon proposed a dynamic pathway among multiple phases. We need to develop diagnostics and techniques to explore this new regime of highly compressed matter science. X-Ray Diffraction - Understand the phase diagram/EOS/strength/texture of materials to 10's of Mbar. Strategy and physics goals: (1) Powder diffraction; (2) Begin with diamond; (3) Continue with metals etc.; (4) Explore phase diagrams; (5) Develop liquid diffraction; and (6) Reduce background/improve resolution.

  13. 3D -Ray Diffraction Microscopy

    Poulsen, Henning Friis; Schmidt, Søren; Juul Jensen, Dorte;

    2014-01-01

    Three-dimensional X-ray diffraction (3DXRD) microscopy is a fast and non-destructive structural characterization technique aimed at the study of individual crystalline elements (grains or subgrains) within mm-sized polycrystalline specimens. It is based on two principles: the use of highly penetr...

  14. Microstresses and x-ray diffraction

    Drahokoupil, J.; Čerňanský, Marian; Ganev, N.; Kolařík, K.; Pala, Z.

    Ostrava: VŠB - TU, 2008 - (Fuxa, J.; Macura, F.; Halama, R.), s. 94-98 ISBN 978-80-248-1774-3. [Experimental Stress Analysis 2008 /46./. Horní Bečva (CZ), 02.06.2008-05.06.2008] R&D Projects: GA ČR GA106/07/0805 Institutional research plan: CEZ:AV0Z10100520 Keywords : microstress and macrostress * shot peening * x-ray diffraction * depth distribution Subject RIV: BM - Solid Matter Physics ; Magnetism

  15. Study of 3-D stress development in parent and twin pairs of a hexagonal close-packed polycrystal: Part I – in-situ three-dimensional synchrotron X-ray diffraction measurement

    High anisotropy in the elastic and plastic properties of hexagonal close-packed (hcp) structured metals not only results in drastic stress variation across grain boundaries, but also heterogeneous distributions within grains. Understanding the mechanism of load sharing between different grains becomes more complicated when deformation twinning plays a significant role in accommodating an externally applied load. In this paper, a comprehensive study of stress development in a coarse grained strongly textured hcp polycrystal Zircaloy-2, is given using three-dimensional X-ray diffraction (3DXRD) microscopy. In-situ uniaxial straining was carried out at seven steps up to 2.7% in the macroscopic direction that favors twin formation, while center-of-mass position, crystallographic orientation, elastic strain, stress, and relative volume of each grain were measured. This information was used to reconstruct the 3D microstructure and statistically study neighborhood effects on the load sharing. The investigated volume of the sample contained 6132 grains initially, yet as a result of twin formation, 9724 grains were measured in the same volume at the last loading step. It is shown that the most favored (highest Schmid factor) twin variant contributes the most to the twin number fraction; however, if the measured local stress within each grain is used for the calculation of Schmid factor, the contribution of other variants is relatively independent of Schmid factor

  16. Towards magnetic 3D x-ray imaging

    Fischer, Peter; Streubel, R.; Im, M.-Y.; Parkinson, D.; Hong, J.-I.; Schmidt, O. G.; Makarov, D.

    2014-03-01

    Mesoscale phenomena in magnetism will add essential parameters to improve speed, size and energy efficiency of spin driven devices. Multidimensional visualization techniques will be crucial to achieve mesoscience goals. Magnetic tomography is of large interest to understand e.g. interfaces in magnetic multilayers, the inner structure of magnetic nanocrystals, nanowires or the functionality of artificial 3D magnetic nanostructures. We have developed tomographic capabilities with magnetic full-field soft X-ray microscopy combining X-MCD as element specific magnetic contrast mechanism, high spatial and temporal resolution due to the Fresnel zone plate optics. At beamline 6.1.2 at the ALS (Berkeley CA) a new rotation stage allows recording an angular series (up to 360 deg) of high precision 2D projection images. Applying state-of-the-art reconstruction algorithms it is possible to retrieve the full 3D structure. We will present results on prototypic rolled-up Ni and Co/Pt tubes and glass capillaries coated with magnetic films and compare to other 3D imaging approaches e.g. in electron microscopy. Supported by BES MSD DOE Contract No. DE-AC02-05-CH11231 and ERC under the EU FP7 program (grant agreement No. 306277).

  17. X-ray tomography: Biological cells in 3-D at better than 50 nm resolution

    Full text: X-ray microscopy can be used to image whole, hydrated, specimens with a spatial resolution 5-10 times better than that obtained using visible light microscopy. X-ray imaging at photon energies below the K- absorption edge of oxygen, referred to as the water window, exploits the strong natural contrast for organic material embedded in a mostly water matrix. With a transmission X-ray microscope using Fresnel zone plate optics, specimens up to 10 microns thick can be examined. The highest X-ray transmission in hydrated samples is obtained at a wavelength of 2.4 nm but, due to the low numerical aperture of zone plate lenses operated in st order diffraction mode the structures resolved are much larger than the X-ray wavelength. Because of the low NA of X-ray lenses (NA=0.05), combined with the effect of polychromatic illumination and a wavelength dependant focal length, the effective depth of ld is large (6-10 microns). The experiments presented here were performed at the Advanced Light Source using the full ld transmission X-ray microscope, XM-1. This microscope employs a bend magnet X-ray source and zone plate condenser and objective lenses. The condenser zone plate acts as a monochromator and the X-ray images are recorded directly on a cooled, back-thinned 1024x1024 pixel CCD camera. The sample holder was a rotationally symmetric glass tube; the region containing the sample was 10 microns in diameter with a wall thickness of 200 nm. Live yeast cells were loaded into the tube, rapidly frozen by a blast of liquid nitrogen-cooled helium gas, and maintained at 140 deg C by a steady flow of cold helium. The image sequence spanned 180 deg and consisted of 45 images spaced by 4 deg. The images were aligned to a common axis and computed tomographic reconstruction was used to obtain the 3-D X-ray linear absorption coefficient. Volume rendering and animation of reconstructed data was performed using the 3-D program, Amira. Acquisition time for 90 images was 3 min

  18. X-ray imaging of laser produced plasmas by a compound 3D x-ray lens

    Pilot scheme for the study of plasma under extreme condition is implemented using a compound 3D X-ray lens. Hard X-ray image of laser plasma produced by irradiating of copper foil by intense laser pulse was recorded using this lens

  19. X-ray high-resolution diffraction using refractive lenses

    Drakopoulos, Michael; Snigirev, Anatoly; Snigireva, Irina; Schilling, Jörg

    2005-01-01

    Refractive x-ray lenses have recently been applied for imaging and scanning microscopy with hard x rays. We report the application of refractive lenses in an optical scheme for high-resolution x-ray diffraction, performed at a high brilliance synchrotron radiation source. An experimental proof of principle and a theoretical discussion are presented. In particular, we observe the x-ray diffraction pattern from a two-dimensional photonic crystal with 4.2 µm periodicity, which normally is employ...

  20. Application of the probability theory in predicting 3D focusing behaviors of compound X-ray refractive lenses

    Zichun Le; Xinjian Zhao; Jingqiu Liang; Yaping Sun; Kai Liu; Ming Zhang; Shuqin Guo; Bisheng Quan

    2005-01-01

    A theoretical method based on the diffractive theory is used for predicting three-dimensional (3D) focusing performances of the compound X-rays refractive lenses (CRLs). However, the derivation of the 3D intensity distribution near focus for the X-ray refractive lenses is quite complicated. In this paper, we introduce a simple theoretical method that is based on the first and second moments in the theory of probability. As an example, the 3D focusing performance of a CRL with Si material is predicted. Moreover, the results are compared with those obtained by the diffractive theory. It is shown that the method introduced in this paper is accurate enough.

  1. X-ray diffraction in phase characterisation

    Full text: The technique of X-ray diffraction (XRD) began in 1912 when von Laue discovered that crystalline materials interact with X-rays in a manner that reveals the underlying structure of the phase(s) present in the sample. Initially, the method was only used for the determination of crystal structure, but more recent developments have seen its application in a number of areas. 1) Phase identification; the positions of the lines in an XRD pattern are determined by the crystal symmetry, the unit cell dimensions and the wavelength used to collect the data while their intensities are proportional to the type and location of the atom within the unit cell. The arrangement of lines in a diffraction pattern serves as a 'finger-print' for the phase allowing it to be identified in pure or multi-phase samples. 2)Crystallite size and strain; decreasing crystallite size and increasing micro-strain both have the effect of increasing the observed peak widths in a diffraction pattern. However, since the effect of size and strain vary differently as function of diffraction angle (secθ and tanθ respectively), it is possible to determine the size and strain components using wide range diffraction data. 3)Crystal structure refinement; the advent of the Rietveld method in the late 1960's allowed the refinement of known (or partially known) crystal structures without the need to decompose the pattern into individual peak intensities. The method relies on (i) calculating a diffraction from a model which includes the crystal structure, pattern background and peak width and shape, (ii) comparing the calculated pattern with the observed data, and (iii) minimising the difference between the calculated and observed patterns by varying the model in a least-squares minimisation process. 4) Phase quantification; the strength of XRD lies in the fact that it is one of the few techniques that is sensitive to the phases present in the sample. Since an XRD pattern is produced by the crystal

  2. Oscillation photography applied to resonant x-ray diffraction

    Inami, T [Synchrotron Radiation Research Unit, Japan Atomic Energy Agency, Hyogo 679-5148 (Japan); Toyokawa, H [Japan Synchrotron Radiation Research Institute, Hyogo 679-5198 (Japan); Terada, N; Kitazawa, H, E-mail: inami@spring8.or.j [National Institute for Materials Science, Tsukuba 305-0047 (Japan)

    2009-03-01

    Recently, resonant x-ray diffraction has been used for detecting charge, magnetic and multipole orders. In practice, however, this technique surveys only a small portion of the reciprocal space. In this study, we applied oscillation photography to resonant x-ray diffraction. For a test sample, we explored nearly a whole Brillouin zone and successfully observed resonant peaks. This feasibility study indicates that oscillation photography is useful for expanding observable areas and enhances the capability of resonant x-ray diffraction.

  3. X-ray diffraction from shock-loaded polycrystals

    Swift, Damian C.

    2007-01-01

    X-ray diffraction was demonstrated from shock-compressed polycrystalline metal on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25 to 125 microns thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, and the beam was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray ...

  4. Advanced X-ray diffractive optics

    Vila-Comamala, J.; Jefimovs, K.; Pilvi, T.; Ritala, M; Sarkar, S S; Solak, H H; Guzenko, V.A.; Stampanoni, M.; Marone, F.; J. Raabe; G. Tzvetkov; Fink, R H; Grolimund, D.; Borca, C.N.; Kaulich, B

    2009-01-01

    X-ray microscopy greatly bene�ts from the advances in x-ray optics. At the Paul Scherrer Institut, developments in x-ray di�ractive optics include the manufacture and optimization of Fresnel zone plates (FZPs) and di�ractive optical elements for both soft and hard x-ray regimes. In particular, we demonstrate here a novel method for the production of ultra-high resolution FZPs. This technique is based on the deposition of a zone plate material (iridium) onto the sidewalls of a p...

  5. Measuring the 3D shape of X-ray clusters

    Samsing, Johan; Hansen, Steen H

    2012-01-01

    Observations and numerical simulations of galaxy clusters strongly indicate that the hot intracluster x-ray emitting gas is not spherically symmetric. In many earlier studies spherical symmetry has been assumed partly because of limited data quality, however new deep observations and instrumental designs will make it possible to go beyond that assumption. Measuring the temperature and density profiles are of interest when observing the x-ray gas, however the spatial shape of the gas itself also carries very useful information. For example, it is believed that the x-ray gas shape in the inner parts of galaxy clusters is greatly affected by feedback mechanisms, cooling and rotation, and measuring this shape can therefore indirectly provide information on these mechanisms. In this paper we present a novel method to measure the three-dimensional shape of the intracluster x-ray emitting gas. We can measure the shape from the x-ray observations only, i.e. the method does not require combination with independent mea...

  6. Development of a 3-D x-ray system

    Evans, J P O

    1993-01-01

    major departure has been the introduction of a dual energy linear x-ray detector array which will allow, in general, the discrimination between organic and inorganic substances. The second design is a compromise between ease of visual inspection for human observers and optimum three-dimensional co-ordinate measurement capability. The system is part of an on going research programme into the possibility of introducing psychological depth cues into the resultant x-ray images. The research presented in this thesis was initiated to enhance the visual interpretation of complex x-ray images, specifically in response to problems encountered in the routine screening of freight by HM. Customs and Excise. This phase of the work culminated in the development of the first experimental machine. During this work the security industry was starting to adopt a new type of x-ray detector, namely the dual energy x-ray sensor. The Department of Transport made available funding to the Police Scientific Development Branch (P.S.D.B...

  7. Mammography spectrum measurement using an x-ray diffraction device

    The use of a diffraction spectrometer developed by Deslattes for the determination of mammographic kV is extended to the measurement of accurate, relative x-ray spectra. Raw x-ray spectra (photon fluence versus energy) are determined by passing an x-ray beam through a bent quartz diffraction crystal, and the diffracted x-rays are detected by an x-ray intensifying screen coupled to a charge coupled device. Two nonlinear correction procedures, one operating on the energy axis and the other operating on the fluence axis, are described and performed on measured x-ray spectra. The corrected x-ray spectra are compared against tabulated x-ray spectra measured under nearly identical conditions. Results indicate that the current device is capable of producing accurate relative x-ray spectral measurements in the energy region from 12 keV to 40 keV, which represents most of the screen-film mammography energy range. Twelve keV is the low-energy cut-off, due to the design geometry of the device. The spectrometer was also used to determine the energy-dependent x-ray mass attenuation coefficients for aluminium, with excellent results in the 12-30 keV range. Additional utility of the device for accurately determining the attenuation characteristics of various normal and abnormal breast tissues and phantom substitutes is anticipated. (author)

  8. Energy-dispersive X-ray diffraction mapping on a benchtop X-ray fluorescence system

    Lane, DW; Nyombi, A; Shackel, J

    2014-01-01

    A method for energy-dispersive X-ray diffraction mapping is presented, using a conventional low-power benchtop X-ray fluorescence spectrometer, the Seiko Instruments SEA6000VX. Hyper spectral X-ray maps with a 10µm step size were collected from polished metal surfaces, sectioned Bi, Pb and steel shot gun pellets. Candidate diffraction lines were identified by eliminating those that matched a characteristic line for an element and those predicted for escape peaks, sum peaks, and Rayleigh and C...

  9. Thin film characterisation by advanced X-ray diffraction techniques

    The Fifth School on X-ray diffraction from polycrystalline materials was devoted to thin film characterization by advanced X-ray diffraction techniques. Twenty contributions are contained in this volume; all twenty are recorded in the INIS Database. X-ray diffraction is known to be a powerful analytical tool for characterizing materials and understanding their structural features. The aim of these articles is to illustrate the fundamental contribution of modern diffraction techniques (grazing incidence, surface analysis, standing waves, etc.) to the characterization of thin and ultra-thin films, which have become important in many advanced technologies

  10. Femtosecond x-ray diffraction: experiments and limits

    Wark, Justin S.; Allen, A. M.; Ansbro, P. C.; Bucksbaum, Philip H.; Chang, Zenghu; DeCamp, Mark F.; Falcone, Roger W.; Heimann, Philip A.; Johnson, S. L.; Kang, Inuk; Kapteyn, Henry C.; Larsson, Jorgen; Lee, Richard W.; Lindenberg, Aaron; Merlin, Roberto D.; Missalla, Thomas; Naylor, G.; Padmore, Howard A.; Reis, David A.; Scheidt, K.; Sjoegren, Anders; Sondhauss, P. C.; Wulff, Michael

    2001-01-01

    Although the realisation of femtosecond X-ray free electron laser (FEL) X-ray pulses is still some time away, X-ray diffraction experiments within the sub-picosecond domain are already being performed using both synchrotron and laser- plasma based X-ray sources. Within this paper we summarise the current status of some of these experiments which, to date, have mainly concentrated on observing non-thermal melt and coherent phonons in laser-irradiated semiconductors. Furthermore, with the advent of FEL sources, X-ray pulse lengths may soon be sufficiently short that the finite response time of monochromators may themselves place fundamental limits on achievable temporal resolution. A brief review of time-dependent X-ray diffraction relevant to such effects is presented.

  11. Magnetic X-ray diffraction from samarium

    Watson, D. [School of Physics and Space Research, University of Birmingham, Birmingham B15 2TT (United Kingdom); Forgan, E.M. [School of Physics and Space Research, University of Birmingham, Birmingham B15 2TT (United Kingdom); Stirling, W.G. [Department of Physics, University of Keele, Keele, Staffs ST5 5BG (United Kingdom); Nuttall, W.J. [Department of Physics, University of Keele, Keele, Staffs ST5 5BG (United Kingdom); Perry, S.C. [Department of Physics, University of Keele, Keele, Staffs ST5 5BG (United Kingdom); Costa, M.M.R. [Physics Department, Universidade de Coimbra, 3000 Coimbra (Portugal); Fort, D. [School of Metallurgy and Materials, University of Birmingham, Birmingham B15 2TT (United Kingdom)

    1995-02-09

    We report X-ray scattering observations on antiferromagnetic samarium, using the NSLS synchrotron source. We have made new observations of the absorption-corrected energy dependence and temperature variation of the resonantly enhanced magnetic signal from the hexagonal sites near the L{sub III} edge. ((orig.)).

  12. Amorphous silica studied by high energy x-ray diffraction

    Poulsen, H.F.; Neuefeind, J.; Neumann, H.B.;

    1995-01-01

    The use of hard X-rays (60-300 keV) for diffraction studies of disordered materials has several advantages: higher resolution in direct space, smaller correction terms, removal of truncation effects, the possibility for operating in extreme environments and for direct comparison between X-ray and...

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

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

    1988-01-01

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

  14. X-ray diffraction pattern and deformation texture of beeswax

    Schoening, F.R.L. (University of the Witwatersrand, Johannesburg (South Africa). Dept. of Physics)

    1980-06-01

    The x-ray diffraction pattern of beeswax shows paraffin-like spacings which have been attributed to monoesters, and long spacings which have been attributed to diesters and hydrocarbons. The d-values and line intensities are given. Optical and x-ray observations of deformed specimens indicate that the molecular axes tend to lie perpendicular to the direction of elongation.

  15. 2D and 3D Refraction Based X-ray Imaging Suitable for Clinical and Pathological Diagnosis

    Ando, Masami; Bando, Hiroko; Chen, Zhihua; Chikaura, Yoshinori; Choi, Chang-Hyuk; Endo, Tokiko; Esumi, Hiroyasu; Gang, Li; Hashimoto, Eiko; Hirano, Keiichi; Hyodo, Kazuyuki; Ichihara, Shu; Jheon, SangHoon; Kim, HongTae; Kim, JongKi; Kimura, Tatsuro; Lee, ChangHyun; Maksimenko, Anton; Ohbayashi, Chiho; Park, SungHwan; Shimao, Daisuke; Sugiyama, Hiroshi; Tang, Jintian; Ueno, Ei; Yamasaki, Katsuhito; Yuasa, Tetsuya

    2007-01-01

    The first observation of micro papillary (MP) breast cancer by x-ray dark-field imaging (XDFI) and the first observation of the 3D x-ray internal structure of another breast cancer, ductal carcinoma in-situ (DCIS), are reported. The specimen size for the sheet-shaped MP was 26 mm × 22 mm × 2.8 mm, and that for the rod-shaped DCIS was 3.6 mm in diameter and 4.7 mm in height. The experiment was performed at the Photon Factory, KEK: High Energy Accelerator Research Organization. We achieved a high-contrast x-ray image by adopting a thickness-controlled transmission-type angular analyzer that allows only refraction components from the object for 2D imaging. This provides a high-contrast image of cancer-cell nests, cancer cells and stroma. For x-ray 3D imaging, a new algorithm due to the refraction for x-ray CT was created. The angular information was acquired by x-ray optics diffraction-enhanced imaging (DEI). The number of data was 900 for each reconstruction. A reconstructed CT image may include ductus lactiferi, micro calcification and the breast gland. This modality has the possibility to open up a new clinical and pathological diagnosis using x-ray, offering more precise inspection and detection of early signs of breast cancer.

  16. 2D and 3D Refraction Based X-ray Imaging Suitable for Clinical and Pathological Diagnosis

    The first observation of micro papillary (MP) breast cancer by x-ray dark-field imaging (XDFI) and the first observation of the 3D x-ray internal structure of another breast cancer, ductal carcinoma in-situ (DCIS), are reported. The specimen size for the sheet-shaped MP was 26 mm x 22 mm x 2.8 mm, and that for the rod-shaped DCIS was 3.6 mm in diameter and 4.7 mm in height. The experiment was performed at the Photon Factory, KEK: High Energy Accelerator Research Organization. We achieved a high-contrast x-ray image by adopting a thickness-controlled transmission-type angular analyzer that allows only refraction components from the object for 2D imaging. This provides a high-contrast image of cancer-cell nests, cancer cells and stroma. For x-ray 3D imaging, a new algorithm due to the refraction for x-ray CT was created. The angular information was acquired by x-ray optics diffraction-enhanced imaging (DEI). The number of data was 900 for each reconstruction. A reconstructed CT image may include ductus lactiferi, micro calcification and the breast gland. This modality has the possibility to open up a new clinical and pathological diagnosis using x-ray, offering more precise inspection and detection of early signs of breast cancer

  17. Characterization of Metalloproteins and Biomaterials by X-ray Absorption Spectroscopy and X-ray Diffraction

    Frankær, Christian Grundahl

    and R6) were solved by single crystal X-ray diffraction (XRD) to 1.40 Å, 1.30 Å and 1.80 Å resolution, respectively. The zinc coordination in each conformation was studied by XAS including both extended X-ray absorption fine structure (EXAFS) spectroscopy and X-ray absorption near edge structure...... the zinc coordination in the T3-sites, in particular. Furthermore, XANES spectra for the zinc sites in T6 and R6 insulin were successfully calculated using finite difference methods, and the bond distances and angles were optimized from a quantitative XANES analysis. T6 insulin was furthermore...

  18. X-ray wavefront modeling of Bragg diffraction from crystals

    Sutter, John P.

    2011-09-01

    The diffraction of an X-ray wavefront from a slightly distorted crystal can be modeled by the Takagi-Taupin theory, an extension of the well-known dynamical diffraction theory for perfect crystals. Maxwell's equations applied to a perturbed periodic medium yield two coupled differential equations in the incident and diffracted amplitude. These equations are discretized for numerical calculation into the determination of the two amplitudes on the points of an integration mesh, beginning with the incident amplitudes at the crystal's top surface. The result is a set of diffracted amplitudes on the top surface (in the Bragg geometry) or the bottom surface (in the Laue geometry), forming a wavefront that in turn can be propagated through free space using the Fresnel- Huygens equations. The performance of the Diamond Light Source I20 dispersive spectrometer has here been simulated using this method. Methods are shown for transforming displacements calculated by finite element analysis into local lattice distortions, and for efficiently performing 3-D linear interpolations from these onto the Takagi-Taupin integration mesh, allowing this method to be extended to crystals under thermal load or novel mechanical bender designs.

  19. Simulating X-ray diffraction of textured films

    Breiby, Dag W.; Bunk, Oliver; Andreasen, Jens Wenzel;

    2008-01-01

    Computationally efficient simulations of grazing-incidence X-ray diffraction (GIXD) are discussed, with particular attention given to textured thin polycrystalline films on supporting substrates. A computer program has been developed for simulating scattering from thin films exhibiting varying...

  20. X-ray diffraction radiation in conditions of Cherenkov effect

    Tishchenko, A. A.; Potylitsyn, A. P.; Strikhanov, M. N.

    2006-01-01

    X-ray diffraction radiation from ultra-relativistic electrons moving near an absorbing target is considered. The emission yield is found to increase significantly in conditions of Cherenkov effect. (c) 2006 Elsevier B.V. All rights reserved.

  1. Thin film characterisation by advanced X-ray diffraction techniques

    Cappuccio, G.; Terranova, M.L. [eds.] [INFN, Laboratori Nazionali di Frascati, Rome (Italy)

    1996-09-01

    This report described the papers presented at the 5. School on X-ray diffraction from polycrystalline materials held at Frascati (Rome) in 2-5 October 1996. A separate abstract was prepared for each of the papers.

  2. 3D contrast-enhanced MR portography and direct X-ray portography: a correlation study

    Objective: To evaluate the accuracy of 3D contrast-enhanced MR portography (3D CEMRP) by correlating with direct X-ray portography. Methods: Twenty-six patients underwent 3D CEMRP study. The findings of 3D CEMRP including the patency of the portal vein and its intrahepatic left and right branches, as well as collaterals were evaluated and compared with those from direct x-ray portography. Causes of disagreement between the two methods were analyzed. Results: The main portal vein appearance was accordant with 3D CEMRP and direct x-ray portography in all cases. For intrahepatic portal veins, the results agreed in 21 patients but disagreed in 5. In one patient with a huge tumor in right liver, the right posterior portal vein was classified as occluded at 3D CEMRP, but displaced and diffusely narrowed at direct x-ray portography. The findings of left intrahepatic portal vein were discordant in three patients with hepatocelluar carcinoma in the left lobe. 3D CE MRP demonstrated complete occlusion of the left portal veins, whereas direct x-ray portography showed proximal narrowing and distal occlusion. In another patient with hepatocelluar carcinoma, a small non-occlusive thrombus involving the sagittal segment of the left portal vein was seen on MRP but not on direct x-ray portography. With demonstration of portosystemic collaterals, 3D CEMRP showed results similar to those of X-ray portography, except one recanalized para-umbilical vein was excluded from the limited scan coverage. Conclusion: 3D CE MRP correlated well with direct x-ray portography in most cases. Compared with direct portography, 3D CEMRP had limitation in distinguishing narrowing of an intrahepatic portal vein from occlusion. But it showed advantage in demonstrating small thrombus within portal vein. (authors)

  3. High energy X-ray diffraction

    from the sample within the angular acceptance given by the experimental setup. Due to the use of high energy x-rays bulk investigations of several mm thick Al plates are possible. The depth resolution is achieved by the use of a spiral slit. Simply spoken, it consists of twelve equidistant concentric spiral apertures cut into a WC plate. All paths through the 2 mm thick plate lie on cones, which have one common apex (i.e. the focal point of the slit system; here 50 mm). The azimuth selective depth resolved signal is recorded with an online image plate scanner. The technique permitted to map for the first time, non-destructively and depth resolved, the material composition and strain distribution in the weld zone. The results presented here relate to a FSW between AA2024 (single phase Al alloy) and AlSi10Mg (an alloy containing 10 wt.-% Si distributed in the form of Si particles in an Al matrix). The peak intensities from the Si phase can be used as an indicator for the mixing of the two welding partners since Si is only contained in the AlSi10Mg. The result from this evaluation is shown in figure 2a. For a better comprehension the welding tool is shown schematically. The grey shaded area corresponds to the position of the tool pin that was plunged into the material during the weld process. It can be observed that a significant amount of AA2024 is protruding about 5 mm in the AlSi10Mg side, while the AlSi10Mg material is dominant close to the weld centre. Large tensile strains of up to 1500x10-6 are observed in longitudinal direction. In transverse direction the residual strains are largely compressive. Furthermore the strain is rather homogeneous in depth. Only close to the anvil side of the plate (i.e. opposite the tool side) variations in depth occur. This could be explained by the different heat and material flow close to the anvil and around the tool tip. Future measurements over larger regions will in addition concentrate on the determination of the complete depth

  4. DIFFRACTION LIMIT OF THE X-RAY REFRACTIVE LENSES

    Jaskevich, Y. R.; Kravchenko, O. I.; Chembrovsky, A. G.

    2013-01-01

    A compound X-ray lenses is an array of microlenses with a common axis. The resolution limited by aberration and by diffraction. Aberration can be corrected by shaping refractive surfaces for the experiment geometry. Due to the small value of refractive index the ideal shape of the surface is similar to the parabola. Diffraction limit comes from single slit theory based on absorption aperture of the compound refractive lenses. X-rays passing through lenses form Airy pattern. The size ...

  5. Synchrotron x-ray diffraction study of liquid surfaces

    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. X-ray diffraction microscopy based on refractive optics

    Roth, Thomas; Snigireva, Irina; Snigirev, Anatoly

    2014-01-01

    We describe a diffraction microscopy technique based on refractive optics to study structural variations in crystals. The X-ray beam diffracted by a crystal was magnified by beryllium parabolic refractive lenses on a 2D X-ray camera. The microscopy setup was integrated into the 6-circle Huber diffractometer at the ESRF beamline ID06. Our setup allowed to visualize structural imperfections with a resolution of approximately 1 micrometer. The configuration, however, can easily be adapted for sub-micrometer resolution.

  7. X-ray diffraction identification of clay minerals by microcomputer

    The identification of clay minerals by X-ray powder diffraction are done by searching an unknown pattern with a file of standard X-ray diffraction patterns. For this searching done by hand is necessary a long time. This paper shows a program in ''Basic'' language to be utilized in microcomputers for the math of the unknown pattern, using the high velocity of comparison of the microcomputer. A few minutes are used for the match. (author)

  8. 3D Reconstruction from X-ray Fluoroscopy for Clinical Veterinary Medicine using Differential Volume Rendering

    Khongsomboon, Khamphong; Hamamoto, Kazuhiko; Kondo, Shozo

    3D reconstruction from ordinary X-ray equipment which is not CT or MRI is required in clinical veterinary medicine. Authors have already proposed a 3D reconstruction technique from X-ray photograph to present bone structure. Although the reconstruction is useful for veterinary medicine, the thechnique has two problems. One is about exposure of X-ray and the other is about data acquisition process. An x-ray equipment which is not special one but can solve the problems is X-ray fluoroscopy. Therefore, in this paper, we propose a method for 3D-reconstruction from X-ray fluoroscopy for clinical veterinary medicine. Fluoroscopy is usually used to observe a movement of organ or to identify a position of organ for surgery by weak X-ray intensity. Since fluoroscopy can output a observed result as movie, the previous two problems which are caused by use of X-ray photograph can be solved. However, a new problem arises due to weak X-ray intensity. Although fluoroscopy can present information of not only bone structure but soft tissues, the contrast is very low and it is very difficult to recognize some soft tissues. It is very useful to be able to observe not only bone structure but soft tissues clearly by ordinary X-ray equipment in the field of clinical veterinary medicine. To solve this problem, this paper proposes a new method to determine opacity in volume rendering process. The opacity is determined according to 3D differential coefficient of 3D reconstruction. This differential volume rendering can present a 3D structure image of multiple organs volumetrically and clearly for clinical veterinary medicine. This paper shows results of simulation and experimental investigation of small dog and evaluation by veterinarians.

  9. 3D reconstruction from X-ray fluoroscopy for clinical veterinary medicine using differential volume rendering

    3D reconstruction from ordinary X-ray equipment which is not CT or MRI is required in clinical veterinary medicine. Authors have already proposed a 3D reconstruction technique from X-ray photograph to present bone structure. Although the reconstruction is useful for veterinary medicine, the technique has two problems. One is about exposure of X-ray and the other is about data acquisition process. An x-ray equipment which is not special one but can solve the problems is X-ray fluoroscopy. Therefore, in this paper, we propose a method for 3D-reconstruction from X-ray fluoroscopy for clinical veterinary medicine. Fluoroscopy is usually used to observe a movement of organ or to identify a position of organ for surgery by weak X-ray intensity. Since fluoroscopy can output a observed result as movie, the previous two problems which are caused by use of X-ray photograph can be solved. However, a new problem arises due to weak X-ray intensity. Although fluoroscopy can present information of not only bone structure but soft tissues, the contrast is very low and it is very difficult to recognize some soft tissues. It is very useful to be able to observe not only bone structure but soft tissues clearly by ordinary X-ray equipment in the field of clinical veterinary medicine. To solve this problem, this paper proposes a new method to determine opacity in volume rendering process. The opacity is determined according to 3D differential coefficient of 3D reconstruction. This differential volume rendering can present a 3D structure image of multiple organs volumetrically and clearly for clinical veterinary medicine. This paper shows results of simulation and experimental investigation of small dog and evaluation by veterinarians. (author)

  10. High-resolution ab initio Three-dimensional X-ray Diffraction Microscopy

    Chapman, H N; Barty, A; Marchesini, S; Noy, A; Cui, C; Howells, M R; Rosen, R; He, H; Spence, J H; Weierstall, U; Beetz, T; Jacobsen, C; Shapiro, D

    2005-08-19

    Coherent X-ray diffraction microscopy is a method of imaging non-periodic isolated objects at resolutions only limited, in principle, by the largest scattering angles recorded. We demonstrate X-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the 3D diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a non-periodic object. We also construct 2D images of thick objects with infinite depth of focus (without loss of transverse spatial resolution). These methods can be used to image biological and materials science samples at high resolution using X-ray undulator radiation, and establishes the techniques to be used in atomic-resolution ultrafast imaging at X-ray free-electron laser sources.

  11. 'Magnetic field'. X-ray diffraction

    The major subject of this paper is X-ray diffraction experiments in magnetic field using synchrotron radiation X-rays. This paper firstly introduces the basic experimental methods of X-ray diffraction, and then, the X-ray diffraction experiments in magnetic field that are carried out in Japan using four kinds of magnets such as permanent magnet, electromagnet, superconducting magnet, and pulsed high magnetic field magnet. Then, it introduces the following cases: (1) resonant X-ray diffraction experiment in magnetic field where the ordered state of electric dipole and magnetic octupole were observed in cerium hexaboride (CeB6) using a superconducting magnet, (2) ordered state of electric quadrupole of CeB6 using an electromagnet, and (3) pulsed magnetic field X-ray diffraction experiment that captured the change of lattice constant due to valence transition in the magnetic field application of Yb ions in YbInCu4 using a pulsed magnet. (A.O.)

  12. Statistical skull models from 3D X-ray images

    Berar, M; Bailly, G; Payan, Y; Berar, Maxime; Desvignes, Michel; Payan, Yohan

    2006-01-01

    We present 2 statistical models of the skull and mandible built upon an elastic registration method of 3D meshes. The aim of this work is to relate degrees of freedom of skull anatomy, as static relations are of main interest for anthropology and legal medicine. Statistical models can effectively provide reconstructions together with statistical precision. In our applications, patient-specific meshes of the skull and the mandible are high-density meshes, extracted from 3D CT scans. All our patient-specific meshes are registrated in a subject-shared reference system using our 3D-to-3D elastic matching algorithm. Registration is based upon the minimization of a distance between the high density mesh and a shared low density mesh, defined on the vertexes, in a multi resolution approach. A Principal Component analysis is performed on the normalised registrated data to build a statistical linear model of the skull and mandible shape variation. The accuracy of the reconstruction is under the millimetre in the shape...

  13. 3D diffraction tomography for visualization of contrast media

    Pai, Vinay M.; Stein, Ashley; Kozlowski, Megan; George, Ashvin; Kopace, Rael; Bennett, Eric; Auxier, Julie A.; Wen, Han

    2011-03-01

    In x-ray CT, the ability to selectively isolate a contrast agent signal from the surrounding soft tissue and bone can greatly enhance contrast visibility and enable quantification of contrast concentration. We present here a 3D diffraction tomography implementation for selectively retaining volumetric diffraction signal from contrast agent particles that are within a banded size range while suppressing the background signal from soft tissue and bone. For this purpose, we developed a CT implementation of a single-shot x-ray diffraction imaging technique utilizing gratings. This technique yields both diffraction and absorption images from a single grating-modulated projection image through analysis in the spatial frequency domain. A solution of iron oxide nano-particles, having very different x-ray diffraction properties from tissue, was injected into ex vivo chicken wing and in vivo rat specimens respectively and imaged in a 3D diffraction CT setup. Following parallel beam reconstruction, it is noted that while the soft tissue, bone and contrast media are observed in the absorption volume reconstruction, only the contrast media is observed in the diffraction volume reconstruction. This 3D diffraction tomographic reconstruction permits the visualization and quantification of the contrast agent isolated from the soft tissue and bone background.

  14. X-ray characterization by energy-resolved powder diffraction

    Cheung, G.; Hooker, S. M.

    2016-08-01

    A method for single-shot, nondestructive characterization of broadband x-ray beams, based on energy-resolved powder diffraction, is described. Monte-Carlo simulations are used to simulate data for x-ray beams in the keV range with parameters similar to those generated by betatron oscillations in a laser-driven plasma accelerator. The retrieved x-ray spectra are found to be in excellent agreement with those of the input beams for realistic numbers of incident photons. It is demonstrated that the angular divergence of the x rays can be deduced from the deviation of the detected photons from the Debye-Scherrer rings which would be produced by a parallel beam. It is shown that the angular divergence can be measured as a function of the photon energy, yielding the angularly resolved spectrum of the input x-ray beam.

  15. Spectroscopic imaging, diffraction, and holography with x-ray photoemission

    X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimental fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons

  16. X-ray diffraction microtomography using synchrotron radiation

    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...

  17. X-ray diffraction crystallography. Introduction, examples and solved problems

    Waseda, Yoshio; Shinoda, Kozo [Tohoku Univ., Sendai (Japan). Inst. of Multidisciplinary Research for Advanced Materials; Matsubara, Eiichiro [Kyoto Univ. (Japan). Dept. of Materials Science and Engineering

    2011-07-01

    X-ray diffraction crystallography for powder samples is a well-established and widely used method. It is applied to materials characterization to reveal the atomic scale structure of various substances in a variety of states. The book deals with fundamental properties of X-rays, geometry analysis of crystals, X-ray scattering and diffraction in polycrystalline samples and its application to the determination of the crystal structure. The reciprocal lattice and integrated diffraction intensity from crystals and symmetry analysis of crystals are explained. To learn the method of X-ray diffraction crystallography well and to be able to cope with the given subject, a certain number of exercises is presented in the book to calculate specific values for typical examples. This is particularly important for beginners in X-ray diffraction crystallography. One aim of this book is to offer guidance to solving the problems of 90 typical substances. For further convenience, 100 supplementary exercises are also provided with solutions. Some essential points with basic equations are summarized in each chapter, together with some relevant physical constants and the atomic scattering factors of the elements. (orig.)

  18. Coherent X-ray diffraction studies of mesoscopic materials

    Shabalin, Anatoly

    2015-12-15

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  19. Coherent X-ray diffraction studies of mesoscopic materials

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  20. Analytic 3D Imaging of Mammalian Nucleus at Nanoscale Using Coherent X-Rays and Optical Fluorescence Microscopy

    Song, Changyong; Takagi, Masatoshi; Park, Jaehyun; Xu, Rui; Gallagher-Jones, Marcus; Imamoto, Naoko; Ishikawa, Tetsuya

    2014-01-01

    Despite the notable progress that has been made with nano-bio imaging probes, quantitative nanoscale imaging of multistructured specimens such as mammalian cells remains challenging due to their inherent structural complexity. Here, we successfully performed three-dimensional (3D) imaging of mammalian nuclei by combining coherent x-ray diffraction microscopy, explicitly visualizing nuclear substructures at several tens of nanometer resolution, and optical fluorescence microscopy, cross confir...

  1. X-ray powder diffraction from solid deuterium

    Kawamura, H; Umemoto, S; Takemura, K; Ohishi, Y; Shimomura, O

    2002-01-01

    X-ray powder diffraction from solid deuterium was first observed under high pressure at SPring-8. At pressures up to 62 GPa and room temperature, three diffraction lines (100, 002, 101) of the hcp lattice were observed. The derived cell volume and the c/a ratio were consistent with single-crystal data. At 83 K and 94 GPa, three diffraction lines were also obtained and assigned to the hcp lattice.

  2. Photoluminescence and X-ray Diffraction of Distributed Bragg Reflector

    LI Lin; LI Yong-da; LIU Wen-li; LU Bin; JU Guo-xian; ZHANG Yong-ming; HAO Yong-qin; SU Wei; ZHONG Jing-chang

    2004-01-01

    Spectral and structural characteristics of distributed Bragg reflector (DBR) in vertical-cavity surface-emitting lasers were studied with photoluminescence and double- crystal X- ray diffraction measurement. The expected high quality epitaxial DBR structure was verified. In the X- ray double- crystal rocking curves of DBR the zeroth- order peak, the first and second order satellite peaks were measured.Splitting of diffraction peak appeared in the rocking curves was analyzed. The effects of introduced deep energy levels on the structural perfection and optical properties were discussed.

  3. 3D contrast-enhanced MR portography and direct X-ray portography: a correlation study

    Our objective was to compare 3D contrast-enhanced MR portography (3D CE MRP) on a 1.5-T MR imager with direct X-ray portography. Twenty-six consecutive patients underwent 3D CE MRP with in-plane resolution of 1.4 or 1.8 mm, and direct X-ray portography. The findings of these two methods were evaluated and compared. The main portal vein (PV), right PV with its anterior and posterior segmental branches, and left PV including its sagittal segment were shown clearly without diagnostic problem in all cases on MRP. The main PV appearance was accordant with MRP and X-ray. For intrahepatic PVs, the results agreed in 21 patients but disagreed in 5 patients. In 1 patient with a huge tumor in right liver, the right posterior PV was classified as occluded at MRP, but diffusely narrowed at X-ray. The findings of left intrahepatic PV were discordant in 3 patients with hepatocelluar carcinoma in the left lobe. The MRP demonstrated complete occlusion of the left PVs, whereas X-ray showed proximal narrowing and distal occlusion. In another patient with hepatocelluar carcinoma, a small non-occlusive thrombus involving the sagittal segment of the left PV was seen on MRP but not on X-ray. With demonstration of varices and portosystemic shunts, MRP showed results similar to those of X-ray, except one recanalized para-umbilical vein was excluded from the field of view at MRP due to the patient's limited ability of breathholding. The 3D CE MRP correlated well with direct X-ray portography in most cases, it was limited in distinguishing narrowing of an intrahepatic PV from occlusion, but it showed advantage in demonstrating small thrombus within PV. (orig.)

  4. 3D Hydrodynamic & Radiative Transfer Models of X-ray Emission from Colliding Wind Binaries

    Russell, Christopher M P; Owocki, Stanley P; Corcoran, Michael F; Hamaguchi, Kenji; Sugawara, Yasuharu

    2014-01-01

    Colliding wind binaries (CWBs) are unique laboratories for X-ray astrophysics. The massive stars in these systems possess powerful stellar winds with speeds up to $\\sim$3000 km s$^{-1}$, and their collision leads to hot plasma (up to $\\sim10^8$K) that emit thermal X-rays (up to $\\sim$10 keV). Many X-ray telescopes have observed CWBs, including Suzaku, and our work aims to model these X-ray observations. We use 3D smoothed particle hydrodynamics (SPH) to model the wind-wind interaction, and then perform 3D radiative transfer to compute the emergent X-ray flux, which is folded through X-ray telescopes' response functions to compare directly with observations. In these proceedings, we present our models of Suzaku observations of the multi-year-period, highly eccentric systems $\\eta$ Carinae and WR 140. The models reproduce the observations well away from periastron passage, but only $\\eta$ Carinae's X-ray spectrum is reproduced at periastron; the WR 140 model produces too much flux during this more complicated p...

  5. X-Ray Diffraction Project Final Report, Fiscal Year 2006

    An x-ray diffraction diagnostic system was developed for determining real-time shock-driven lattice parameter shifts in single crystals at the gas gun at TA-IV at Sandia National Laboratories (SNL). The signal-to-noise ratio and resolution of the system were measured using imaging plates as the detector and by varying the slit width. This report includes tests of the x-ray diffraction system using a phosphor coupled to a charge-coupled device (CCD) camera by a coherent fiber-optic bundle. The system timing delay was measured with a newly installed transistor-transistor logic (TTL) bypass designed to reduce the x-ray delay time. The axial misalignment of the Bragg planes was determined with respect to the optical axis for a set of eight LiF [lithium fluoride] crystals provided by SNL to determine their suitability for gas gun experiments

  6. Single-shot 3D structure determination of nanocrystals with femtosecond X-ray free electron laser pulses

    Xu, Rui; Song, Changyong; Rodriguez, Jose A; Huang, Zhifeng; Chen, Chien-Chun; Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Kim, Sangsoo; Kim, Sunam; Suzuki, Akihiro; Takayama, Yuki; Oroguchi, Tomotaka; Takahashi, Yukio; Fan, Jiadong; Zou, Yunfei; Hatsui, Takaki; Inubushi, Yuichi; Kameshima, Takashi; Yonekura, Koji; Tono, Kensuke; Togashi, Tadashi; Sato, Takahiro; Yamamoto, Masaki; Nakasako, Masayoshi; Yabashi, Makina; Ishikawa, Tetsuya; Miao, Jianwei

    2013-01-01

    Coherent diffraction imaging (CDI) using synchrotron radiation, X-ray free electron lasers (X-FELs), high harmonic generation, soft X-ray lasers, and optical lasers has found broad applications across several disciplines. An active research direction in CDI is to determine the structure of single particles with intense, femtosecond X-FEL pulses based on diffraction-before-destruction scheme. However, single-shot 3D structure determination has not been experimentally realized yet. Here we report the first experimental demonstration of single-shot 3D structure determination of individual nanocrystals using ~10 femtosecond X-FEL pulses. Coherent diffraction patterns are collected from high-index-faceted nanocrystals, each struck by a single X-FEL pulse. Taking advantage of the symmetry of the nanocrystal, we reconstruct the 3D structure of each nanocrystal from a single-shot diffraction pattern at ~5.5 nm resolution. As symmetry exists in many nanocrystals and virus particles, this method can be applied to 3D st...

  7. Coherent diffraction imaging using focused hard X-rays

    Kim, Sunam; Kim, Sangsoo; Lee, Su Yong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Marathe, Shashidhara; Song, Changyong; Gallagher-Jones, Marcus; Kang, Hyon Chol

    2016-05-01

    A quantitative height profile image of a silicon nano-trench structure was obtained via coherent diffraction imaging (CDI) utilizing focused X-rays at a photon energy of 5.5 keV. The ability to optimize the spatial coherence and the photon flux density of a focused X-ray beam was the key technique for achieving such technical progress at a given X-ray photon flux. This was achieved by investigating the tunability of the focused beam's optical properties and performing a CDI experiment with the focused X-rays. The relationship between the focused X-rays' optical properties ( e.g., photon flux density and spatial coherence length) and the incident beam's size, which can be tuned by adjusting the slits in front of the Fresnel zone plate (FZP) was elucidated. We also obtained a quantitative image of a nano-trench sample produced via the reconstruction process of CDI, which utilizes carefully tuned, focused X-rays.

  8. Evaluation of a new method for stenosis quantification from 3D x-ray angiography images

    Betting, Fabienne; Moris, Gilles; Knoplioch, Jerome; Trousset, Yves L.; Sureda, Francisco; Launay, Laurent

    2001-05-01

    A new method for stenosis quantification from 3D X-ray angiography images has been evaluated on both phantom and clinical data. On phantoms, for the parts larger or equal to 3 mm, the standard deviation of the measurement error has always found to be less or equal to 0.4 mm, and the maximum measurement error less than 0.17 mm. No clear relationship has been observed between the performances of the quantification method and the acquisition FoV. On clinical data, the 3D quantification method proved to be more robust to vessel bifurcations than its 3D equivalent. On a total of 15 clinical cases, the differences between 2D and 3D quantification were always less than 0.7 mm. The conclusion is that stenosis quantification from 3D X-4ay angiography images is an attractive alternative to quantification from 2D X-ray images.

  9. The three dimensional X-ray diffraction technique

    Juul Jensen, Dorte; Poulsen, Henning Friis

    2012-01-01

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials...

  10. Theory of time-resolved inelastic x-ray diffraction

    Lorenz, Ulf; Møller, Klaus Braagaard; Henriksen, Niels Engholm

    2010-01-01

    Starting from a general theory of time-resolved x-ray scattering, we derive a convenient expression for the diffraction signal based on a careful analysis of the relevant inelastic scattering processes. We demonstrate that the resulting inelastic limit applies to a wider variety of experimental c...

  11. X-ray diffraction study of directionally grown perylene crystallites

    Breiby, Dag W.; Lemke, H. T.; Hammershøj, P.;

    2008-01-01

    Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel...

  12. X-Ray diffraction Investigation of Electrochemically Deposited Copper

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

    2004-01-01

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

  13. X-Ray Diffraction Simulation Using Laser Pointers and Printers.

    Johnson, Neil E.

    2001-01-01

    Uses a laser pointer to demonstrate the analogy between optical and X-ray diffraction and a laser printer with 600 or 1200 dot resolution to create and modify arrays, print them on transparencies, and illuminate them with laser pointers. Includes 14 references. (Author/YDS)

  14. Computer Simulation and X-ray Diffraction of Nanocrystals

    2001-01-01

    X-ray diffraction of structure in nanocrystalline α-Fe and Cu was studied by atomistic simulation. Atomic position equilibrium was reached by using molecular dynamics method to simulate nanocrystalline structure with Finnis potentials to model interatomic interactions. lt was found that the boundary component exhibits short-range order, and the distortion in crystalline component increases with the decrease of grain size.

  15. A Practical Method of Simulating X-Ray Diffraction

    Brisse, F.; Sundararajan, P. R.

    1975-01-01

    Describes an experiment in which the beam of X-rays is simulated through the use of a laser as a monochromatic light source and the crystal is replaced by photographically prepared masks. A strong diffraction pattern as large as 20 cm. can be obtained. (GS)

  16. Diffraction of X-ray pulse in crystals

    Baryshevsky, V. G.

    1999-01-01

    The X-ray radiation delay law dependence on the diffraction asymmetry parameters is analyzed. It is shown that the use of subpicosecond pulses allows to observe the time delay of pulse in crystal phenomenon and to investigate the delay law experimentally. It is also shown that pulse delay law depends on the quanta polarization.

  17. X-ray diffraction pattern of powder rhenium semiheptaoxide

    The X-ray diffraction pattern of Re2O7 powder at 110-115 deg C under the conditions excluding absorption of the air moisture by the sample is obtained. Rhombic lattice parameters a=12.52; b=15.26; c=5.45 A are calculated

  18. Oxygen precipitation studied by x-ray diffraction techniques

    Meduňa, M.; Caha, O.; Růžička, J.; Bernatová, S.; Svoboda, Milan; Buršík, Jiří

    178 -179, - (2011), s. 325-330. ISSN 1012-0394 R&D Projects: GA ČR(CZ) GA202/09/1013 Institutional research plan: CEZ:AV0Z20410507 Keywords : Czochralski silicon * oxygen precipitates * x-ray Laue diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism

  19. Powder X-ray diffraction study af alkali alanates

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...

  20. Fusion bonding of Si wafers investigated by x ray diffraction

    Weichel, Steen; Grey, Francois; Rasmussen, Kurt;

    2000-01-01

    The interface structure of bonded Si(001) wafers with twist angle 6.5 degrees is studied as a function of annealing temperature. An ordered structure is observed in x-ray diffraction by monitoring a satellite reflection due to the periodic modulation near the interface, which results from the for...

  1. Single-Shot Femtosecond X-ray Diffraction from Randomly Oriented Ellipsoidal Nanoparticles

    Coherent diffractive imaging of single particles using the single-shot 'diffract and destroy' approach with an x-ray free electron laser (FEL) was recently demonstrated. A high-resolution low-noise coherent diffraction pattern, representative of the object before it turns into a plasma and explodes, results from the interaction of the FEL with the particle. Iterative phase retrieval algorithms are used to reconstruct two-dimensional projection images of the object from the recorded intensities alone. Here we describe the first single-shot diffraction data set that mimics the data proposed for obtaining 3D structure from identical particles. Ellipsoidal iron oxide nanoparticles (250 nm x 50 nm) were aerosolized and injected through an aerodynamic lens stack into a soft x-ray FEL. Particle orientation was not controlled with this injection method. We observed that, at the instant the x-ray pulse interacts with the particle, a snapshot of the particle's orientation is encoded in the diffraction pattern. The results give credence to one of the technical concepts of imaging individual nanometer and subnanometer-sized objects such as single molecules or larger clusters of molecules using hard x-ray FELs and will be used to help develop robust algorithms for determining particle orientations and 3D structure.

  2. Theory of time-resolved inelastic x-ray diffraction

    Lorenz, Ulf; Møller, Klaus Braagaard; Henriksen, Niels Engholm

    2010-01-01

    Starting from a general theory of time-resolved x-ray scattering, we derive a convenient expression for the diffraction signal based on a careful analysis of the relevant inelastic scattering processes. We demonstrate that the resulting inelastic limit applies to a wider variety of experimental conditions than similar, previously derived formulas, and it directly allows the application of selection rules when interpreting diffraction signals. Furthermore, we present a simple extension to syst...

  3. Diffraction enhanced X-ray imaging of mammals crystalline lens

    Crystalline lenses are transparent biological materials where the organization of the lens fibers can also be affected by changes at molecular level, and therefore the structure and morphology of the tissue can be correlated to the loss of transparency of the lens. In this work, internal structure of mammal lenses regarding the long-range ordering of the fibers are investigated by diffraction enhanced X-ray imaging (DEI) radiography. Moreover, DEI and absorption X-ray synchrotron radiographs for healthy and cataractous crystalline lenses are compared. Significant differences in healthy and cataractous crystalline lenses are observed

  4. Diffraction enhanced X-ray imaging of mammals crystalline lens

    Antunes, A. [Departamento de Fisica Aplicada, USP, CP 66318, 05315-970 Sao Paulo, SP (Brazil)]. E-mail: antunes@if.usp.br; Hoennicke, M.G. [LORXI, Departamento de Fisica, Universidade Federal do Parana, Curitiba (Brazil); Safatle, A.M.V. [Faculdade de Medicina Veterinaria e Zootecnia, USP, 05508-900 Sao Paulo, SP (Brazil); Cusatis, C. [LORXI, Departamento de Fisica, Universidade Federal do Parana, Curitiba (Brazil); Moraes Barros, P.S. [Faculdade de Medicina Veterinaria e Zootecnia, USP, 05508-900 Sao Paulo, SP (Brazil); Morelhao, S.L. [Departamento de Fisica Aplicada, USP, CP 66318, 05315-970 Sao Paulo, SP (Brazil)

    2005-08-15

    Crystalline lenses are transparent biological materials where the organization of the lens fibers can also be affected by changes at molecular level, and therefore the structure and morphology of the tissue can be correlated to the loss of transparency of the lens. In this work, internal structure of mammal lenses regarding the long-range ordering of the fibers are investigated by diffraction enhanced X-ray imaging (DEI) radiography. Moreover, DEI and absorption X-ray synchrotron radiographs for healthy and cataractous crystalline lenses are compared. Significant differences in healthy and cataractous crystalline lenses are observed.

  5. Determination of organic crystal structures by X ray powder diffraction

    McBride, L

    2000-01-01

    The crystal structure of Ibuprofen has been solved from synchrotron X-ray powder diffraction data using a genetic algorithm (GA). The performance of the GA is improved by incorporating prior chemical information in the form of hard limits on the values that can be taken by the flexible torsion angles within the molecule. Powder X-ray diffraction data were collected for the anti-convulsant compounds remacemide, remacemide nitrate and remacemide acetate at 130 K on BM 16 at the X-ray European Synchrotron Radiation Facility (ESRF) at Grenoble. High quality crystal structures were obtained using data collected to a resolution of typically 1.5 A. The structure determinations were performed using a simulated annealing (SA) method and constrained Rietveld refinements for the structures converged to chi sup 2 values of 1.64, 1.84 and 1.76 for the free base, nitrate and acetate respectively. The previously unknown crystal structure of the drug famotidine Form B has been solved using X-ray powder diffraction data colle...

  6. MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

    Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

    2013-01-01

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  7. X-ray magnetic diffraction of ferromagnets with synchrotron radiation

    Ito, M

    2002-01-01

    X-ray magnetic diffraction experiment of ferromagnets that utilizes elliptically polarized synchrotron radiation is presented. First we have reviewed shortly historical backgrounds and theoretical aspects of the experiment. We have presented how the magnetic form factors are measured and are separated into the spin-moment component and the orbital-moment component in this experiment. Peculiar features of the polarization factor of this experiment have been explained. We have introduced two examples of the experiment. One is the measurement of the spin-magnetic form factor of SmAl sub 2 with white X-rays from a bending magnet at the Photon Factory. The other is the measurement of the orbital-magnetic form factor of Holmium Iron Garnets with monochromatic X-rays from an undulator at the SPring-8. Finally we summarize the article and show some future prospects of this experiment. (author)

  8. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  9. Characterisation of the deformation mechanisms in hcp metals by combined use of X-ray imaging and diffraction techniques

    Nervo, Laura

    2015-01-01

    We envisage a fundamental study of the physical mechanisms (dislocation slip versus deformation twinning) involved in plastic deformation of hexagonal close-packed (HCP) metals like titanium and magnesium. A novel combination of X-ray imaging and diffraction techniques, termed X-ray diffraction contrast tomography (DCT), will be used to investigate details of the deformation process in the bulk of polycrystalline specimen. DCT provides access to the position, 3D shape, (average) orientation a...

  10. 3D ablation catheter localisation using individual C-arm x-ray projections

    Haase, C.; Schäfer, D.; Dössel, O.; Grass, M.

    2014-11-01

    Cardiac ablation procedures during electrophysiology interventions are performed under x-ray guidance with a C-arm imaging system. Some procedures require catheter navigation in complex anatomies like the left atrium. Navigation aids like 3D road maps and external tracking systems may be used to facilitate catheter navigation. As an alternative to external tracking a fully automatic method is presented here that enables the calculation of the 3D location of the ablation catheter from individual 2D x-ray projections. The method registers a high resolution, deformable 3D attenuation model of the catheter to a 2D x-ray projection. The 3D localization is based on the divergent beam projection of the catheter. On an individual projection, the catheter tip is detected in 2D by image filtering and a template matching method. The deformable 3D catheter model is adapted using the projection geometry provided by the C-arm system and 2D similarity measures for an accurate 2D/3D registration. Prior to the tracking and registration procedure, the deformable 3D attenuation model is automatically extracted from a separate 3D cone beam CT reconstruction of the device. The method can hence be applied to various cardiac ablation catheters. In a simulation study of a virtual ablation procedure with realistic background, noise, scatter and motion blur an average 3D registration accuracy of 3.8 mm is reached for the catheter tip. In this study four different types of ablation catheters were used. Experiments using measured C-arm fluoroscopy projections of a catheter in a RSD phantom deliver an average 3D accuracy of 4.5 mm.

  11. Development of 2D, pseudo 3D and 3D x-ray imaging for early diagnosis of breast cancer and rheumatoid arthritis

    By using plane-wave x-rays with synchrotron radiation refraction-based x-ray medical imaging can be used to visualize soft tissue, as reported in this paper. This method comprises two-dimensional (2D) x-ray dark-field imaging (XDFI), the tomosynthesis of pseudo 3D (sliced) x-ray imaging by the adoption of XDFI and 3D x-ray imaging by utilizing a newly devised algorithm. We aim to make contribution to the early diagnosis of breast cancer, which is a major cancer among women, and rheumatoid arthritises which cannot be detected in its early stages. (author)

  12. Three-dimensional coherent X-ray diffraction imaging of a whole, frozen-hydrated cell

    Rodriguez, Jose A; Chen, Chien-Chun; Huang, Zhifeng; Jiang, Huaidong; Raines, Kevin S; Nam, Daewoong; Chen, Allan L; Pryor, A J; Wiegart, Lutz; Song, Changyong; Madsen, Anders; Chushkin, Yuriy; Zontone, Federico; Bradley, Peter J; Miao, Jianwei

    2014-01-01

    A structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffraction imaging (cryo-CDI) could bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, we report for the first time 3D cryo-CDI of a whole, frozen-hydrated cell - in this case a Neospora caninum tachyzoite - using 8 keV X-rays. Our 3D reconstruction reveals the surface and internal morphology of the cell, including its complex, polarized sub-cellular architecture with a 3D resolution of ~75-100 nm, which is presently limited by the coherent X-ray flux and detector size. Given the imminent improvement in the coherent X-ray flux at the facilities worldwide, our work forecasts the possibility of routine 3D imaging of frozen-hydrated cells with spatial resolutions in the tens of nanometres.

  13. 3-D Multiphase Segmentation of X-Ray Micro Computed Tomography Data of Geologic Materials

    Tuller, M.; Kulkarni, R.; Fink, W.

    2011-12-01

    Advancements of noninvasive imaging methods such as X-Ray Computed Tomography (CT) led to a recent surge of applications in Geoscience. While substantial efforts and resources have been devoted to advance CT technology and micro-scale analysis, the development of a stable 3-D multiphase image segmentation method applicable to large datasets is lacking. To eliminate the need for wet/dry or dual energy scans, image alignment, and subtraction analysis, commonly applied in synchrotron X-Ray micro CT, a segmentation method based on a Bayesian Markov Random Field (MRF) framework amenable to true 3-D multiphase processing was developed and evaluated. Furthermore, several heuristic and deterministic combinatorial optimization schemes required to solve the labeling problem of the MRF image model were implemented and tested for computational efficiency and their impact on segmentation results. Test results for natural and artificial porous media datasets demonstrate great potential of the MRF image model for 3-D multiphase segmentation.

  14. Element-specific X-ray phase tomography of 3D structures at the nanoscale.

    Donnelly, Claire; Guizar-Sicairos, Manuel; Scagnoli, Valerio; Holler, Mirko; Huthwelker, Thomas; Menzel, Andreas; Vartiainen, Ismo; Müller, Elisabeth; Kirk, Eugenie; Gliga, Sebastian; Raabe, Jörg; Heyderman, Laura J

    2015-03-20

    Recent advances in fabrication techniques to create mesoscopic 3D structures have led to significant developments in a variety of fields including biology, photonics, and magnetism. Further progress in these areas benefits from their full quantitative and structural characterization. We present resonant ptychographic tomography, combining quantitative hard x-ray phase imaging and resonant elastic scattering to achieve ab initio element-specific 3D characterization of a cobalt-coated artificial buckyball polymer scaffold at the nanoscale. By performing ptychographic x-ray tomography at and far from the Co K edge, we are able to locate and quantify the Co layer in our sample to a 3D spatial resolution of 25 nm. With a quantitative determination of the electron density we can determine that the Co layer is oxidized, which is confirmed with microfluorescence experiments. PMID:25839287

  15. X-ray scattering in the elastic regime as source for 3D imaging reconstruction technique

    Kocifaj, Miroslav; Mego, Michal

    2015-11-01

    X-ray beams propagate across a target object before they are projected onto a regularly spaced array of detectors to produce a routine X-ray image. A 3D attenuation coefficient distribution is obtained by tomographic reconstruction where scattering is usually regarded as a source of parasitic signals which increase the level of electromagnetic noise that is difficult to eliminate. However, the elastically scattered radiation could be a valuable source of information, because it can provide a 3D topology of electron densities and thus contribute significantly to the optical characterization of the scanned object. The scattering and attenuation data form a complementary base for concurrent retrieval of both electron density and attenuation coefficient distributions. In this paper we developed the 3D reconstruction method that combines both data inputs and produces better image resolution compared to traditional technology.

  16. Focal construct geometry for high intensity energy dispersive x-ray diffraction based on x-ray capillary optics.

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi; Jiang, Bowen; Zhu, Yu

    2016-03-14

    We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis. PMID:26979685

  17. Focal construct geometry for high intensity energy dispersive x-ray diffraction based on x-ray capillary optics

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi; Jiang, Bowen; Zhu, Yu

    2016-03-01

    We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis.

  18. X-ray diffraction from single GaAs nanowires

    Biermanns, Andreas

    2012-11-12

    In recent years, developments in X-ray focussing optics have allowed to produce highly intense, coherent X-ray beams with spot sizes in the range of 100 nm and below. Together with the development of new experimental stations, X-ray diffraction techniques can now be applied to study single nanometer-sized objects. In the present work, X-ray diffraction is applied to study different aspects of the epitaxial growth of GaAs nanowires. Besides conventional diffraction methods, which employ X-ray beams with dimensions of several tens of {mu}m, special emphasis lies on the use of nanodiffraction methods which allow to study single nanowires in their as-grown state without further preparation. In particular, coherent X-ray diffraction is applied to measure simultaneously the 3-dimensional shape and lattice parameters of GaAs nanowires grown by metal-organic vapor phase epitaxy. It is observed that due to a high density of zinc-blende rotational twins within the nanowires, their lattice parameter deviates systematically from the bulk zinc-blende phase. In a second step, the initial stage in the growth of GaAs nanowires on Si (1 1 1) surfaces is studied. This nanowires, obtained by Ga-assisted growth in molecular beam epitaxy, grow predominantly in the cubic zinc-blende structure, but contain inclusions of the hexagonal wurtzite phase close to their bottom interface. Using nanodiffraction methods, the position of the different structural units along the growth axis is determined. Because the GaAs lattice is 4% larger than silicon, these nanowires release their lattice mismatch by the inclusion of dislocations at the interface. Whereas NWs with diameters below 50 nm are free of strain, a rough interface structure in nanowires with diameters above 100 nm prevents a complete plastic relaxation, leading to a residual strain at the interface that decays elastically along the growth direction. Finally, measurements on GaAs-core/InAs-shell nanowire heterostructures are presented

  19. 3D Radio and X-Ray Modeling and Data Analysis Software: Revealing Flare Complexity

    Nita, Gelu M; Kuznetsov, Alexey A; Kontar, Eduard P; Gary, Dale E

    2014-01-01

    We have undertaken a major enhancement of our IDL-based simulation tools developed earlier for modeling microwave and X-ray emission. The object-based architecture provides an interactive graphical user interface that allows the user to import photospheric magnetic field maps and perform magnetic field extrapolations to almost instantly generate 3D magnetic field models, to investigate the magnetic topology of these models by interactively creating magnetic field lines and associated magnetic flux tubes, to populate the flux tubes with user-defined nonuniform thermal plasma and anisotropic, nonuniform, nonthermal electron distributions; to investigate the spatial and spectral properties of radio and X-ray emission calculated from the model, and to compare the model-derived images and spectra with observational data. The application integrates shared-object libraries containing fast gyrosynchrotron emission codes developed in FORTRAN and C++, soft and hard X-ray codes developed in IDL, a FORTRAN-based potentia...

  20. Lattice rotations of individual bulk grains. Part 1: 3D X-ray characterization

    Poulsen, H.F.; Margulies, L.; Schmidt, S.;

    2003-01-01

    Three-dimensional X-ray diffraction has been applied to characterise the plastic deformation of individualgrains deeply embedded in a 99.6% pure aluminium specimen. The specimen is 4 mm thick with an average grain size of 75 μm. The average latticerotation for each grain as well as the degree of...

  1. 3D localization of electrophysiology catheters from a single x-ray cone-beam projection

    Purpose: X-ray images allow the visualization of percutaneous devices such as catheters in real time but inherently lack depth information. The provision of 3D localization of these devices from cone beam x-ray projections would be advantageous for interventions such as electrophysiology (EP), whereby the operator needs to return a device to the same anatomical locations during the procedure. A method to achieve real-time 3D single view localization (SVL) of an object of known geometry from a single x-ray image is presented. SVL exploits the change in the magnification of an object as its distance from the x-ray source is varied. The x-ray projection of an object of interest is compared to a synthetic x-ray projection of a model of said object as its pose is varied. Methods: SVL was tested with a 3 mm spherical marker and an electrophysiology catheter. The effect of x-ray acquisition parameters on SVL was investigated. An independent reference localization method was developed to compare results when imaging a catheter translated via a computer controlled three-axes stage. SVL was also performed on clinical fluoroscopy image sequences. A commercial navigation system was used in some clinical image sequences for comparison. Results: SVL estimates exhibited little change as x-ray acquisition parameters were varied. The reproducibility of catheter position estimates in phantoms denoted by the standard deviations, (σx, σy, σz) = (0.099 mm,  0.093 mm,  2.2 mm), where x and y are parallel to the detector plane and z is the distance from the x-ray source. Position estimates (x, y, z) exhibited a 4% systematic error (underestimation) when compared to the reference method. The authors demonstrated that EP catheters can be tracked in clinical fluoroscopic images. Conclusions: It has been shown that EP catheters can be localized in real time in phantoms and clinical images at fluoroscopic exposure rates. Further work is required to characterize performance in clinical

  2. 3D localization of electrophysiology catheters from a single x-ray cone-beam projection

    Robert, Normand, E-mail: normand.robert@sri.utoronto.ca; Polack, George G.; Sethi, Benu; Rowlands, John A. [Physical Sciences, Sunnybrook Research Institute, 2075 Bayview Avenue, Toronto, Ontario M4N 3M5 (Canada); Crystal, Eugene [Division of Cardiology, Sunnybrook Health Sciences Centre, 2075 Bayview Avenue, Toronto, Ontario M4N 3M5 (Canada)

    2015-10-15

    Purpose: X-ray images allow the visualization of percutaneous devices such as catheters in real time but inherently lack depth information. The provision of 3D localization of these devices from cone beam x-ray projections would be advantageous for interventions such as electrophysiology (EP), whereby the operator needs to return a device to the same anatomical locations during the procedure. A method to achieve real-time 3D single view localization (SVL) of an object of known geometry from a single x-ray image is presented. SVL exploits the change in the magnification of an object as its distance from the x-ray source is varied. The x-ray projection of an object of interest is compared to a synthetic x-ray projection of a model of said object as its pose is varied. Methods: SVL was tested with a 3 mm spherical marker and an electrophysiology catheter. The effect of x-ray acquisition parameters on SVL was investigated. An independent reference localization method was developed to compare results when imaging a catheter translated via a computer controlled three-axes stage. SVL was also performed on clinical fluoroscopy image sequences. A commercial navigation system was used in some clinical image sequences for comparison. Results: SVL estimates exhibited little change as x-ray acquisition parameters were varied. The reproducibility of catheter position estimates in phantoms denoted by the standard deviations, (σ{sub x}, σ{sub y}, σ{sub z}) = (0.099 mm,  0.093 mm,  2.2 mm), where x and y are parallel to the detector plane and z is the distance from the x-ray source. Position estimates (x, y, z) exhibited a 4% systematic error (underestimation) when compared to the reference method. The authors demonstrated that EP catheters can be tracked in clinical fluoroscopic images. Conclusions: It has been shown that EP catheters can be localized in real time in phantoms and clinical images at fluoroscopic exposure rates. Further work is required to characterize

  3. X-ray and neutron diffraction studies of chalcocite oxidation

    Full text: The mineral chalcocite (Cu2S), which is often found in the enriched zone of sulphide deposits, is an important source of copper. The oxidation behaviour of chalcocite is of interest in terms of the mineral exploration technology and also for understanding the behaviour of the mineral under roasting conditions. Recently, the oxidation of chalcocite was the subject of a study by Dunn et al (1994) involving the use of thermal analysis, scanning electron microscopy, electron probe microanalysis, powder x-ray diffraction (XRD) and Fourier transform spectroscopy. The study indicated that the following transformations are likely to occur: at 430-490 deg C, partial conversion of Cu2S to Cu2O and CuSO4 via Cu1.96S and Cu1.80S; at 490-590 deg C, further conversion of Cu2S to Cu2O, CuO CuSO4 and CuSO4; and at 590-820 deg C, Cu2O, CuO CuSO4 and CuSO4 to CuO. In this study, the oxidation of chalcocite was analysed from a crystallographic perspective. Ambient x-ray diffraction and in-situ neutron diffraction were used to determine the phases present, at various temperatures, as oxidation progressed. Ambient x-ray experiments involved heating chalcocite powder in an air stream, to a target temperature, cooling it to room temperature in a nitrogen stream, and analysing by Bragg-Brentano x-ray powder diffractometry. In situ neutron experiments consisted of, powdered chalcocite being heated in an air stream to various target temperatures, and then held in a nitrogen stream at the given temperature while Medium Resolution Powder Diffractometry (EPD) was performed. Rietveld modelling of the x-ray and neutron data was used to confirm the phase identifications made by search/match analysis, and to then map the variations in phase levels with temperature as the oxidation progresses through various phase transformations. The talk will consider the results obtained from the study with particular reference to the identification of previously undetected phases, and the differences

  4. X-ray diffraction at Bragg angles around π/2

    X-ray diffraction at Bragg angles around π/2 is studied from the theoretical and experimental points of view. The proposed corrections to the dynamical theory in the θβ ≅ π/2 cases, has been reviewed showing the equivalence between two formalisms leading to a corrected expression for the dependence of the angular parameter y with the angle of incidence. An expression for y valid in the conventional and θ β ≅ π/2 cases has been obtained. A general expression for Bragg law and for energy resolution after a Bragg diffraction was also deduced. (author)

  5. Nano structured materials studied by coherent X-ray diffraction

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  6. Nano structured materials studied by coherent X-ray diffraction

    Gulden, Johannes

    2013-03-15

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  7. 3D global estimation and augmented reality visualization of intra-operative X-ray dose.

    Rodas, Nicolas Loy; Padoy, Nicolas

    2014-01-01

    The growing use of image-guided minimally-invasive surgical procedures is confronting clinicians and surgical staff with new radiation exposure risks from X-ray imaging devices. The accurate estimation of intra-operative radiation exposure can increase staff awareness of radiation exposure risks and enable the implementation of well-adapted safety measures. The current surgical practice of wearing a single dosimeter at chest level to measure radiation exposure does not provide a sufficiently accurate estimation of radiation absorption throughout the body. In this paper, we propose an approach that combines data from wireless dosimeters with the simulation of radiation propagation in order to provide a global radiation risk map in the area near the X-ray device. We use a multi-camera RGBD system to obtain a 3D point cloud reconstruction of the room. The positions of the table, C-arm and clinician are then used 1) to simulate the propagation of radiation in a real-world setup and 2) to overlay the resulting 3D risk-map onto the scene in an augmented reality manner. By using real-time wireless dosimeters in our system, we can both calibrate the simulation and validate its accuracy at specific locations in real-time. We demonstrate our system in an operating room equipped with a robotised X-ray imaging device and validate the radiation simulation on several X-ray acquisition setups. PMID:25333145

  8. Design and fabrication of micro X-ray diffraction system

    Park, Yang Soon; Han, Sun Ho; Kim, Jong Goo; Jee, Kwang Yong

    2006-10-15

    It has been observed that microstructure changes occur at the pellet periphery(rim) of the fuel at very high burn-up. Despite its narrow range (below some hundreds microns in depth), this peripheral region(rim) determines the behaviour of nuclear fuel. To determine lattice parameter with XRD at intervals as small as 30-50 {mu} m in radial direction of irradiated fuel samples, a micro X-ray diffraction system was designed and fabricated. This report describes the micro X-ray diffraction system consisted of an X-ray microbeam alignment system and a sample micro translation system, its characterization, and its performance test through the analysis for the micro region of some specimens. This system will be set in a radiation shielded glove box, and then used for analysis of lattice parameter change and the phase change at intervals as small as 30-50 {mu} m in radial direction of the rim of an irradiated fuel sample and a fuel cladding.

  9. Gamma/x-ray linear pushbroom stereo for 3D cargo inspection

    Zhu, Zhigang; Hu, Yu-Chi

    2006-05-01

    For evaluating the contents of trucks, containers, cargo, and passenger vehicles by a non-intrusive gamma-ray or X-ray imaging system to determine the possible presence of contraband, three-dimensional (3D) measurements could provide more information than 2D measurements. In this paper, a linear pushbroom scanning model is built for such a commonly used gamma-ray or x-ray cargo inspection system. Accurate 3D measurements of the objects inside a cargo can be obtained by using two such scanning systems with different scanning angles to construct a pushbroom stereo system. A simple but robust calibration method is proposed to find the important parameters of the linear pushbroom sensors. Then, a fast and automated stereo matching algorithm based on free-form deformable registration is developed to obtain 3D measurements of the objects under inspection. A user interface is designed for 3D visualization of the objects in interests. Experimental results of sensor calibration, stereo matching, 3D measurements and visualization of a 3D cargo container and the objects inside, are presented.

  10. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    Robert M. Lawrence

    2015-07-01

    Full Text Available Serial femtosecond crystallography (SFX using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ∼700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  11. New developments for 3D CT at high X-ray energy

    CT is well suited both for measurements and for flaw detection in cast metal products which as a rule have a complex shape and internal caverns. Currently available tomographs for 3D scanning of large objects still have shortcomings. Line detectors - normally operated with a 450 kV X-ray source - are slow. Systems with detector panels normally have 225 kV microfocus tubes which provide insufficient power. The microfocus tube cannot be replaced by a 450 kV tube as scattered radiation at higher energies will considerably reduce the image quality of the tomograms. In the context of European research projects during the past few years, Empa developed new methods for faster data acquisition with line detector systems and correction of scattered radiation for CT with conical beams and with panel detectors. The contribution outlines the state of the art and also presents new trends, especially for fast 3D volume scanning with high X-ray energy

  12. Crystallite size determination by x-ray diffraction

    Full text: Particle sizing problem arises in many fields of science, technology and material production. Methods based on X-ray diffraction lines broadening cover size interval of 10-100 nm and are well documented. Larger crystallites demonstrate no line broadening and require alternative methods for size determination. When crystallites are relatively large (10-500 mkm) and a small volume of the sample is irradiated the diffraction pattern exhibits discrete spots instead of continuous diffraction lines. We base our approach on the linear correlation between average crystallite's size and diffraction spots dimensions which is valid for crystallite size above 5 mkm. Thus the aim of this work is to extract the crystallite size distribution function from the analysis of the spot size distribution

  13. NDE of spacecraft materials using 3D Compton backscatter x-ray imaging

    Burke, E. R.; Grubsky, V.; Romanov, V.; Shoemaker, K.

    2016-02-01

    We present the results of testing of the NDE performance of a Compton Imaging Tomography (CIT) system for single-sided, penetrating 3D inspection. The system was recently developed by Physical Optics Corporation (POC) and delivered to NASA for testing and evaluation. The CIT technology is based on 3D structure mapping by collecting the information on density profiles in multiple object cross sections through hard x-ray Compton backscatter imaging. The individual cross sections are processed and fused together in software, generating a 3D map of the density profile of the object which can then be analyzed slice-by-slice in x, y, or z directions. The developed CIT scanner is based on a 200-kV x-ray source, flat-panel x-ray detector (FPD), and apodized x-ray imaging optics. The CIT technology is particularly well suited to the NDE of lightweight aerospace materials, such as the thermal protection system (TPS) ceramic and composite materials, micrometeoroid and orbital debris (MMOD) shielding, spacecraft pressure walls, inflatable habitat structures, composite overwrapped pressure vessels (COPVs), and aluminum honeycomb materials. The current system provides 3D localization of defects and features with field of view 20x12x8 cm3 and spatial resolution ˜2 mm. In this paper, we review several aerospace NDE applications of the CIT technology, with particular emphasis on TPS. Based on the analysis of the testing results, we provide recommendations for continued development on TPS applications that can benefit the most from the unique capabilities of this new NDE technology.

  14. Bone histomorphometric quantification by X-ray phase contrast and transmission 3D SR microcomputed tomography

    Full text: Conventional histomorphometry is an important method for quantitative evaluation of bone microstructure. X-ray computed tomography is a noninvasive technique, which can be used to evaluate histomorphometric indices. In this technique, the output 3D images are used to quantify the whole sample, differently from the conventional one, in which the quantification is performed in 2D slices and extrapolated for 3D case. Looking for better resolutions and visualization of soft tissues, X-ray phase contrast imaging technique was developed. The objective of this work was to perform histomorphometric quantification of human cancellous bone using 3D synchrotron X ray computed microtomography, using two distinct techniques: transmission and phase contrast, in order to compare the results and evaluate the viability of applying the same methodology of quantification for both technique. All experiments were performed at the ELETTRA Synchrotron Light Laboratory in Trieste (Italy). MicroCT data sets were collected using the CT set-up on the SYRMEP (Synchrotron Radiation for Medical Physics) beamline. Results showed that there is a better correlation between histomorphometric parameters of both techniques when morphological filters had been used. However, using these filters, some important information given by phase contrast are lost and they shall be explored by new techniques of quantification

  15. 3D X-ray microscopy: image formation, tomography and instrumentation

    Selin, Mårten

    2016-01-01

    Tomography in soft X-ray microscopy is an emerging technique for obtaining quantitative 3D structural information about cells. One of its strengths, compared with other techniques, is that it can image intact cells in their near-native state at a few 10 nm’s resolution, without staining. However, the methods for reconstructing 3D-data rely on algorithms that assume projection data, which the images are generally not due to the imaging systems’ limited depth of focus. To bring out the full pot...

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

    In situ investigations into the P/T field of C60 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure

  17. X-ray Mirage Diffraction and Its Interference Fringes

    Fukamachi, Tomoe; Kawamura, Takaaki

    When the dispersion angle of X-rays in a perfect crystal is large, interference fringes are observed between the beams in the Bragg-Laue mode and Bragg-Bragg-Laue mode in the emitted beams from the lateral surface. If the crystal is weakly bent, X-rays propagate along a path of hyperbolic form and are diffracted from the incident surface, which is called mirage diffraction. Under the condition, mirage interference fringes between two mirage diffraction beams are observed not only from the incident surface but also from the lateral surface. Two approaches are proposed to determine strain parameters in the bent crystal by using the mirage interference fringes from the incident surface or the lateral surface. In one approach, the third peak of the mirage interference fringes is used. In the other, the region is used where no direct beam reaches to the lateral surface. The resultant strain parameters determined by the two approaches show excellent agreement. Some characteristics and advantages of using mirage interference fringes are discussed.

  18. Automation of a Guinier camera for X-ray diffraction

    The automation of a Guinier X-ray diffraction camera is discussed. The photographic plate in the conventional setup has been replaced by a curved proportional counter (CPC) which has an electronic readout system. As a result the recording time has been reduced from a few hours to a few minutes. The construction and optimum dimensions of the CPC are discussed and the most essential parts of the readout electronics are highlighted. A linewidth of 200 μm FWHM and an accuracy of 30 μm are achieved. 45 refs.; 53 figs.; 4 tabs

  19. Resonant X-ray diffraction: Basic theoretical principles

    We present the main steps governing the theory of resonant X-ray diffraction (RXD). We focus on the derivation of the anomalous scattering amplitude from perturbation theory and starting from the low-energy expansion of the Dirac Hamiltonian. We give the main ingredients of the multipolar expansion in term of electric and magnetic transitions. We also show the expansion in terms of scattering tensors of the material. We end by giving the RXD formula necessary to simulate in practice this spectroscopy. (authors)

  20. Structural science using neutron and x-ray diffraction

    I was awarded a prize by The Japanese Society for Neutron Science at 2009. The main topic of the title is the contribution to the structural science using neutron and x-ray. Special emphasis was adopted for the development of instrumentations. In this paper, the idea of structural science is given, and the importance of the crystal and magnetic structures for material properties will be discussed. Starting from my personal history for development of instrumentations on diffraction studies, I will touch the scientific results. At the last part, future development on this field will be overlooked. (author)

  1. X-Ray Diffraction of Heterogeneous Solid Hydrogen - Oral Presentation

    Levitan, Abraham [SLAC National Accelerator Lab., Menlo Park, CA (United States)

    2015-08-24

    Angularly resolved x-ray diffraction at 5.5 keV establishes the structure of a 5 μm diameter solid hydrogen jet, providing a foundation for analysis of hydrogen in a warm dense matter state. The jet was composed of approximately 65% ± 5% HCP and 35% ± 5% FCC by volume with an average crystallite size on the order of hundreds of nanometers. Broadening in the angularly resolved spectrum provided strong evidence for anisotropic strain up to approximately 3 % in the HCP lattice. Finally, we found no evidence for orientational ordering of the crystal domains.

  2. Ultrafast X-Ray Diffraction of Heterogeneous Solid Hydrogen

    Levitan, Abraham [Olin College of Engineering, Needham, MA (United States)

    2015-08-19

    Angularly resolved x-ray diffraction at 5.5 keV establishes the structure of a 5 µm diameter solid hydrogen jet, providing a foundation for analysis of hydrogen in a warm dense matter state. The jet was composed of approximately 65 % ± 5% HCP and 35 % ± 5% FCC by volume with an average crystallite size on the order of hundreds of nanometers. Broadening in the angularly resolved spectrum provided strong evidence for anisotropic strain up to approximately 3 % in the HCP lattice. Finally, we found no evidence for orientational ordering of the crystal domains.

  3. The three dimensional X-ray diffraction technique

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials are sketched. Examples of the use of the technique are given and future trends and developments are suggested. The primary aim of the paper is to give 3DXRD novices an easy introduction to the technique and to describe a way from a dream to reality and new results.

  4. The three dimensional X-ray diffraction technique

    Jensen, D. Juul, E-mail: doje@dtu.dk [Danish Chinese Center for Nanometals, Materials Science and Advanced Characterization Section, Department of Wind Energy, Technical University of Denmark, Riso Campus (Denmark); Poulsen, H.F. [Department of Physics, Technical University of Denmark, Lyngby Campus (Denmark)

    2012-10-15

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials are sketched. Examples of the use of the technique are given and future trends and developments are suggested. The primary aim of the paper is to give 3DXRD novices an easy introduction to the technique and to describe a way from a dream to reality and new results.

  5. Ab initio structure determination via powder X-ray diffraction

    Digamber G Porob; T N Guru Row

    2001-10-01

    Structure determination by powder X-ray diffraction data has gone through a recent surge since it has become important to get to the structural information of materials which do not yield good quality single crystals. Although the method of structure completion when once the starting model is provided is facile through the Rietveld refinement technique, the structure solution ab initio os still not push-button technology. In this article a survey of the recent development in this area is provided with an illustration of the structure determination of -NaBi3V2O10.

  6. X-ray diffraction analysis of InAs nanowires

    Semiconductor nanowires have attracted great interest as building blocks for future electronic and optoelectronic devices. The variability of the growth process opens the opportunity to control and combine the various properties tailoring for specific application. It was shown that the electrical and optical characteristics of the nanowires are strongly connected with their structure. Despite intensive research in this field, the growth process is still not fully understood. In particular, extensive real structure investigations are required. Most of the reports dedicated on the structural researches are based on the results of scanning electron microscopy (SEM) or transmission electron microscopy (TEM). SEM provides an image of the surface with nanostructures and is mainly used to describe the morphology of the sample, but it does not bring information about the internal structure, phase composition and defect structure. At the same time, the internal structure can be examined by TEM down to atomic scale. TEM image of good quality are very expensive due to the efforts in sample preparation and in localisation of a single object. All these aspects make the statistical structural analysis difficult. In the present work, X-ray diffraction analysis has been applied for structural investigation of InAs nanowires grown by different techniques. Using various X-ray diffraction geometries, the nanowire systems were investigated in terms of the lattice parameters, phase composition, strains and displacement fields and stacking defects. In particular, realizing grazing incidence diffraction and controlling the penetration depth of X-ray beam, we characterized sample series grown by Au-assisted metal organic phase epitaxy on GaAs [111]B substrate with different growth time. According to the results of SEM and X-ray investigations, a model of the growth process has been proposed. A more detailed analysis was performed on InAs nanowires grown by molecular beam epitaxy (MBE) on

  7. Diffraction peaks restoration and extraction in energy dispersive X-ray diffraction

    This paper proposes a method to restore energy dispersive X-ray diffraction (EDXRD) spectra and to extract diffraction peaks. It follows a maximum a posteriori approach using a physical model of the formation of the EDXRD data to remove blur caused by both the detector and the coarse angular resolution of X-ray tube based EDXRD setup. It separates peaks due to the diffraction by crystalline material from a continuous background. Tested on real data (graphite and NaCl), our algorithm achieved to detect diffraction peaks with a good precision (about 1 keV depending on the peak position) even at high energy where very few photons were measured.

  8. Characterization of Brazilian asphalt using X-ray diffraction

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. The X ray diffraction can give valuable information over the characteristics of a material. Thus, the X-ray diffraction (XRD) method was employed to investigate parameters that characterize and differentiate asphalt groups (Boscan, CAP20, CAP40, CAP50/60, CAP50/70 and CAP85/100). The scattering measurements were carried out in θ-2θ reflection geometry using a powder diffractometer Shimadzu XRD-6000 at the Nuclear Instrumentation Laboratory, Brazil. Scans were typically done from 8 deg to 28 deg every 0.05. The parameters analyzed were: FWHM, peak area, peak center, peak height, left half width and right half width. Thus, in this study, scattering profiles from different asphalt groups were carefully measured in order to establish characteristic signatures of these materials. The results indicate that by using three parameters (peak centroid, peak area and peak intensity) it is possible to characterize and differentiate the asphalt. (author)

  9. X-ray diffraction line profile analysis of nanocrystalline graphite

    The structure evolution to nanocrystalline graphite produced by ball milling in n-dodecane has been studied by Fourier analysis of broadened X-ray diffraction line profiles according to double-Voigt method. The Fourier analysis gave size and strain distributions of the coherently diffracting domains (X-ray crystallite size) and root-mean-square-strain (rmss) and their average values. The precursor graphite was defined by average crystal sizes of about hundreds of nanometers, measured along the in-plane and out-of-plane directions, and low rmss value of 0.38 x 10-3. During milling, the average crystallite sizes of graphite decreased to about 6 and 43 nm along the out-of-plane and in-plane directions, respectively. Correspondingly, the rmss of milled graphite increased to 6.54 x 10-3. Analysis of the out-of-plane to in-plane crystallite size ratios showed that the crystallites became progressively thinner and flatter. A linear relationship between rmss and reciprocal crystallite size along the stacking axis revealed that size of disordered boundary regions gradually increased at the expense of ordered crystalline regions. A model describing crystalline-nanocrystalline transformation of graphite along different crystallographic axis was formulated and used to discuss the experimental data. It was concluded that a distortion-controlled process is responsible for the crystalline-nanocrystalline transformation of graphite milled in n-dodecane

  10. Microstructure analysis of nanocrystalline powders by X-ray diffraction

    The use of X-ray diffraction line profile analysis for the study of nanocrystalline powders is described. The fundamentals of the theory are presented in terms of crystallite/domain size, size distribution, lattice distortion, dislocations density and stacking faults. Line profile parameters and the methods of pattern fitting introduced to overcome the diffraction-line overlap problem are discussed. The approaches based of the integral breadth of the measured line profiles and the Fourier method are discussed. In addition, simplified approaches are also commented. Representative examples are selected to illustrate various cases of microstructure, such as nanomaterials with strain-free spherical nano crystallites, strain-free crystallites with anisotropic crystallite shape, anisotropic crystallites with microstrains and spherical crystallites with dislocation densities and crystallite size distributions. (author)

  11. Application of 3D X-ray CT data sets to finite element analysis

    Finite Element Modeling (FEM) is becoming more important as industry drives toward concurrent engineering. A fundamental hindrance to fully exploiting the power of FEM is the human effort required to acquire complex part geometry, particularly as-built geometry, as a FEM mesh. Many Quantitative Non Destructive Evaluation (QNDE) techniques that produce three-dimensional (3D) data sets provide a substantial reduction in the effort required to apply FEM to as-built parts. This paper describes progress at LLNL on the application of 3D X-ray computed tomography (CT) data sets to more rapidly produce high-quality FEM meshes of complex, as-built geometries. Issues related to the volume segmentation of the 3D CT data as well as the use of this segmented data to tailor generic hexahedral FEM meshes to part specific geometries are discussed. The application of these techniques to FEM analysis in the medical field is reported here

  12. Quantification of rutile in anatase by X-ray diffraction

    Nowadays the discovering of new and better materials required in all areas of the industry has been lead to the human being to introduce him to this small and great world. The crystalline materials, have properties markedly directional. When it is necessary to realize a quantitative analysis to these materials the task is not easy. The main objective of this work is the research of a real problem, its solution and perfecting of a technique involving the theoretical and experimental principles which allow the quantification of crystalline phases. The chapter 1 treats about the study of crystalline state during the last century, by means of the X-ray diffraction technique. The chapter 2 studies the nature and production of X-rays, the chapter 3 expounds the principles of the diffraction technique which to carry out when it is satisfied the Bragg law studying the powder diffraction method and its applications. In the chapter 4 it is explained how the intensities of the beams diffracted are determined by the atoms positions inside of the elemental cell of the crystal. The properties of the crystalline samples of anatase and rutile are described in the chapter 5. The results of this last analysis are the information which will be processed by means of the auxiliary software: Diffrac AT, Axum and Peakfit as well as the TAFOR and CUANTI software describing this part with more detail in the chapters 6 and 7 where it is mentioned step by step the function of each software until to reach the quantification of crystalline phases, objective of this work. Finally, in the chapter 8 there are a results analysis and conclusions. The contribution of this work is for those learned institutions of limited resources which can tackle in this way the characterization of materials. (Author)

  13. Fabrication of large area X-ray diffraction grating for X-ray phase imaging

    X-ray lithography, which uses highly directional synchrotron radiation, is one of the technologies that can be used for fabricating micrometer-sized structures. In X-ray lithography, the accuracy of the fabricated structure depends largely on the accuracy of the X-ray mask. Since X-ray radiation is highly directional, a micro-fabrication technology that produces un-tapered and high aspect ratio highly absorbent structures on a low absorbent membrane is required. Conventionally, a resin material is used as the support membrane for large area X-ray masks. However, resin membranes have the disadvantage that they can sag after several cycles of X-ray exposure due to the heat generated by the X-rays. Therefore, we proposed and used thin carbon wafers for the membrane material because carbon has an extremely small thermal expansion coefficient. We fabricated new carbon membrane X-ray masks, and these results of X-ray lithography demonstrate the superior performance.

  14. Probing Local Mineralogy in 3D with Dual Energy X-Ray Microscopy

    Gelb, J.; Yun, S.; Doerr, D.; Hunter, L.; Johnson, B.; Merkle, A.; Fahey, K.

    2013-12-01

    In recent years, 3D imaging of rock microstructures has become routine practice for determining pore-scale properties in the geosciences. X-Ray imaging techniques, such as X-Ray Microscopy (XRM), have demonstrated several unique capabilities: namely, the ability to characterize the same sample across a range of length scales and REVs (from millimeters to nanometers), and to perform these characterizations on the same sample over a range of times/treatments (e.g., to observe fluid transporting through the pore networks in a flow cell). While the XRM technique is a popular choice for structural (i.e., pore) characterization, historically it has provided little mineralogical information. This means that resulting simulations are either based on pore structure alone, or rely on correlative chemical mapping techniques for compositionally-sensitive models. Recent advancements in XRM techniques are now enabling compositional sensitivity for a variety of geological sample types. By collecting high-resolution 3D tomography data sets at two different source settings (energies), results may be mixed together to enhance the appearance (contrast) of specific materials. This approach is proving beneficial, for example, to mining applications to locate and identify precious metals, as well as for oil & gas applications to map local hydrophobicity. Here, we will introduce the technique of dual energy X-Ray microscopy, showing how it extends the capabilities of traditional XRM techniques, affording the same high resolution structural information while adding 3D compositional data. Application examples will be shown to illustrate its effectiveness at both the single to sub-micron length scale for mining applications as well as at the 150 nm length scale for shale rock analysis.

  15. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface Project

    National Aeronautics and Space Administration — We propose to develop a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for analysis of mineralogical composition of regolith,...

  16. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface Project

    National Aeronautics and Space Administration — We propose to develop LUNA, a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for mineralogical analysis of regolith, rock...

  17. X-Ray Diffraction and X-Ray Fluorescent Analyses of Prehistoric Pottery Shards from Ulu Kelantan

    Zuliskandar Ramli; Nik H.S.N. Abdul Rahman; Adnan Jusoh; Yunus Sauman

    2011-01-01

    Problem statement: X-Ray Diffraction (XRD) and X-Ray Fluorescent (XRF) were used in order to obtain mineralogical and elemental composition of seven pottery shards that have been unearthed during the excavation at Peraling Cave and Cha Cave in Ulu Kelantan, Malaysia. Approach: Peraling Cave and Cha Cave were prehistoric sites dating from 10, 000 BC which were inhabited by Hoabinhian people and then continuously used by people of Neolithic culture around 3000 BC. Results: Mineralogical and ele...

  18. 3D numerical model of the Omega Nebula (M17): simulated thermal X-ray emission

    Reyes-Iturbide, J; Rosado, M; Rodríguez-Gónzalez, A; González, R F; Esquivel, A

    2009-01-01

    We present 3D hydrodynamical simulations of the superbubble M17, also known as the Omega nebula, carried out with the adaptive grid code yguazu'-a, which includes radiative cooling. The superbubble is modelled considering the winds of 11 individual stars from the open cluster inside the nebula (NGC 6618), for which there are estimates of the mass loss rates and terminal velocities based on their spectral types. These stars are located inside a dense interstellar medium, and they are bounded by two dense molecular clouds. We carried out three numerical models of this scenario, considering different line of sight positions of the stars (the position in the plane of the sky is known, thus fixed). Synthetic thermal X-ray emission maps are calculated from the numerical models and compared with ROSAT observations of this astrophysical object. Our models reproduce successfully both the observed X-ray morphology and the total X-ray luminosity, without taking into account thermal conduction effects.

  19. A 3D kinematics measurement of knee joint using X-ray projection images

    Most of previous studies about joint kinematic analysis using X-ray image needed totally clear outline bones. However, to obtain the clear outline is not easy in clinical because X-ray image of knee often overlaps with bones. In this study, the method of kinetic analysis that uses the outline, which was not totally clear, was proposed. In order to achieve the aim, P type Fourier Descriptor that can be used in an open curve was applied. And, the library database was preliminary selected using feature vectors which were based on shape feature, initial point and terminal point of the outline. After an outline of the object was divided in three parts, template pattern matching was performed. In results, the standard deviation of errors of patella were θx=1.00±0.84 deg, θy=0.55±0.65 deg and θz=0.62±0.12 deg. As to femur, tibia and patella, a part of divided outlines influenced the accuracy of our proposal method. This result shows that, even if all outline of bone is not clear on X-ray image, 3D kinematic analysis can be carried out. (author)

  20. The first X-ray diffraction measurements on Mars

    Bish, David; Blake, David; Vaniman, David; Sarrazin, Philippe; Bristow, Thomas; Achilles, Cherie; Dera, Przemyslaw; Chipera, Steve; Crisp, Joy; Downs, R. T.; Farmer, Jack; Gailhanou, Marc; Ming, Doug; Morookian, John Michael; Morris, Richard; Morrison, Shaunna; Rampe, Elizabeth; Treiman, Allan; Yen, Albert

    2014-01-01

    The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component. PMID:25485131

  1. [Diffraction gratings used in x-ray spectroscopy]: Final report

    This subcontract was initiated in order to facilitate the development at MIT of technologies for fabricating the very fine diffraction grating required in x-ray spectroscopy at Lawrence Livermore Laboratory (LLL). These gratings are generally gold transmission gratings with spatial periods of 200 nm or less. The major focus of our efforts was to develop a means of fabricating gratings of 100 nm period. We explored two approaches: e-beam fabrication of x-ray lithography masks, and achromatic holographic lithography. This work was pursued by Erik Anderson as a major component of his Ph.D. thesis. Erik was successful in both the e-beam and holographic approaches. However, the e-beam method proved to be highly impractical: exposure times of about 115 days would be required to cover an area of 1 cm2. The achromatic holography, on the other hand, should be capable of exposing areas well in excess of 1 cm2 in times under 1 hour. Moreover, 100 nm-period gratings produced by achromatic holography are coherent over their entire area whereas gratings produced by e-beam lithography are coherent only over areas /approximately/100 μm. The remainder of this report consists of portions excerpted from Erik Anderson's thesis. These contain all the details of our work on 100 nm period gratings. 26 refs., 17 figs

  2. Understanding Plasticity and Fracture in Aluminum Alloys and their Composites by 3D X-ray Synchrotron Tomography and Microdiffraction

    Hruby, Peter

    differential-aperture X-ray structural microscopy (DAXM), from which peak-broadening characteristics were quantified. Plasticity, as determined by the broadening of diffracted peaks, was mapped in 3D. Two-dimensional (2D) maps of plasticity were directly compared to the corresponding tomography slices. A 3D representation of the plastic zone surrounding the fatigue crack was generated by superimposing the mapped plasticity on the 3D crack profile.

  3. Development of confocal 3D X-ray fluorescence instrument and its applications to micro depth profiling

    We have developed a confocal micro X-ray fluorescence instrument. Two independent X-ray tubes of Mo and Cr targets were installed to this instrument. Two polycapillary full X-ray lenses were attached to two X-ray tubes, and a polycapillary half X-ray lens was also attached to the X-ray detector (silicon drift detector, SDD). Finally, three focus spots of three lenses were adjusted at a common position. By using this confocal micro X-ray fluorescence instrument, depth profiling for layered samples were performed. It was found that depth resolution depended on energy of X-ray fluorescence that was measured. In addition, X-ray elemental maps were determined at different depths for an agar sample including metal fragments of Cu, Ti and Au. The elemental maps showed actual distributions of metal fragments in the agar, indicating that the confocal micro X-ray fluorescence is a feasible technique for non-destructive depth analysis and 3D X-ray fluorescence analysis. (author)

  4. Powder X-ray diffraction laboratory, Reston, Virginia

    Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

    2014-01-01

    The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

  5. Special properties of X-ray diffraction on carbon onions

    The kinematic theory of X-ray diffraction was applied to the study of the most intense Bragg's reflection observed for carbon onions. It was shown that the agreement with experimental data was attained using a convolution of a Lorentzian contour with regard to the distribution of onion sizes and of an asymmetric contour taking into account the fluctuations of intershell distances inside the particle. It can be assumed that the observed scatter in intershell distances indicates a nonequilibrium state of the internal configuration of onion shells. It appeared to be possible to estimate not only the average onion size, which exceeds the average size of pristine nanodiamonds that are used for onion preparation by annealing, but their size distribution function as well

  6. Quantitative biological imaging by ptychographic X-ray diffraction microscopy

    Giewekemeyer, Klaus; Kalbfleisch, Sebastian; Beerlink, Andre; Salditt, Tim [Institut fuer Roentgenphysik, Georg-August-Universitaet Goettingen (Germany); Thibault, Pierre; Dierolf, Martin; Pfeiffer, Franz [Department Physik (E17), Technische Universitaet Muenchen, Garching (Germany); Kewish, Cameron M. [Paul Scherrer Institut, Villigen PSI (Switzerland)

    2010-07-01

    Mesoscopic structures with specific functions are abundant in many cellular systems and have been well characterized by electron microscopy in the past. However, the quantitative study of the three-dimensional structure and density of subcellular components remains a difficult problem. In this contribution we show how these limitations could be overcome in the future by the application of recently introduced and now rapidly evolving coherent X-ray imaging techniques for quantitative biological imaging on the nanoscale. More specifically, we report on a recent scanning (ptychographic) diffraction experiment on unstained and unsliced freeze-dried cells of the bacterium Deinococcus radiourans using only a pinhole as beam defining optical element. As a result quantitative density projections well below optical resolution have been achieved.

  7. Magnetoelastic effect in holmium studied by X-ray diffraction

    X-ray diffraction measurements have been performed on a single crystal sample of the rare earth metal holmium. The temperature and magnetic field dependence of the c-lattice parameter was studied in detail below the Neel temperature of 132K. Magnetic structural phase transitions were observed as a change in the c-lattice parameter. In addition, lattice modulations induced by the magnetic structure were investigated by observing satellite reflections. A model based on the exchange magnetostriction can explain these magnetostrictive behaviors. The magnetic structures which were used in the analysis were reproduced by the self-consistent mean field calculation. The model has explained the temperature and magnetic field dependence of the c-lattice parameter, as well as the behaviors of the wave number and the amplitude of the lattice modulation. (author)

  8. A new theory for X-ray diffraction

    By considering the scattering distributed throughout space, there is an intensity enhancement at the Bragg angle even when the Bragg condition is not satisfied. This leads to an alternative explanation for the diffraction from powders and small crystals. This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the ‘Bragg position’ even if the ‘Bragg condition’ is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many ‘Bragg positions’. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on ‘Bragg-type’ scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the ‘background’. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models

  9. Precise rotational alignment of x-ray transmission diffraction gratings

    Gold transmission diffraction gratings used for x-ray spectroscopy must sometimes be rotationally aligned to the axis of a diagnostic instrument to within sub-milliradian accuracy. We have fabricated transmission diffraction gratings with high line-densities (grating period of 200 and 300 nm) using uv holographic and x-ray lithography. Since the submicron features of the gratings are not optically visible, precision alignment is time consuming and difficult to verify in situ. We have developed a technique to write an optically visible alignment pattern onto these gratings using a scanning electron microscope (SEM). At high magnification (15000 X) several submicron lines of the grating are observable in the SEM, making it possible to write an alignment pattern parallel to the grating lines in an electron-beam-sensitive coating that overlays the grating. We create an alignment pattern by following a 1-cm-long grating line using the SEM's joystick-controlled translation stage. By following the same grating line we are assured the traveled direction of the SEM electron beam is parallel to the grating to better than 10 μradian. The electron-beam-exposed line-width can be large (5 to 15 μm wide) depending on the SEM magnification, and is therefore optically visible. The exposed pattern is eventually made a permanent feature of the grating by ion beam etching or gold electroplating. The pattern can be used to accurately align the grating to the axis of a diagnostic instrument. More importantly, the alignment of the grating can be quickly verified in situ

  10. 3D X-rays application for precision measurement of the cell structure of extruded polystyrene

    Lim, J. Y.; Kim, K. Y.; Shin, H. S.; Yeom, S.; Lee, S. E.

    2015-12-01

    While the thermal performance of existing insulation materials have been determined by blister gases, the thermal performance of future insulation materials will be dependent on the cell size and independent foam content as we use eco-friendly blister gases with a higher thermal conductivity. However, with the current technology we are only able to guess the whole cell size and independent foam content through SEM applied 2D fragmentary scanning but are still far from the level of accurate cell structure data extraction. Under this situation, we utilized X-ray CT scanned 3D images to identify and shape the cell structure and proposed a method of inferring the whole distribution and independent foam content as accurately as possible. According to X-ray CT scanning images and SEM images, the shape was similar but according to tracer applied CT scanning images, the cell size distribution was 380∼400 pm within the range of the general insulation diameter distribution which had the highest reliability. As for extrusion foaming polystyrene, we need additional image processing to identify the independent foam content as its density is too low. So, it is recommended to raise the 3D cell structure completeness of XPS by improving the scanning accuracy.

  11. Nanostructured diffractive optical devices for soft X-ray microscopes

    Hambach, D; Schneider, G

    2001-01-01

    The new transmission X-ray microscope (TXM) installed at the BESSY II electron storage ring uses an off-axis transmission zone plate (OTZ) as diffractive and focusing element of the condenser-monochromator setup. A high resolution micro-zone plate (MZP) forms a magnified image on a CCD-detector. Both, the OTZ with an active area of up to 24 mm sup 2 and the MZP with zone widths as small as 25 nm are generated by a process including electron beam lithography (EBL), dry etching and subsequent electroplating of nickel on top of silicon membrane substrates with about 100-150 nm thickness. The combination of a larger zone width and the usage of nickel zone structures allows to increase the diffraction efficiency of the condenser element at least by a factor of 3 compared to the earlier used KZP7 condenser zone plate in the TXM at BESSY I. Groove diffraction efficiencies of 21.6% and 14.7% were measured for MZP objectives with 40 and 25 nm outermost zone width, respectively.

  12. X-ray diffraction study of glucomannans and their acetates

    Crystalline polymorphs of four glucomannans with a different mannose/glucose ratio from 1.5 to 4.0 and their acetyl derivatives was studied by X-ray diffraction measurements. The glucomannans showed an amorphous or similar crystal structure (Mannan I or Mannan II polymorph) of β-1,4-d-mannan depending on their mannose content, indicating the occurrence of isomorphous replacement of mannose by glucose during glucomannan crystallization. When these glucomannans were annealed, however, Konjac glucomannan (mannose/glucose ratio = 1.6) showed a different powder pattern from both Mannans I and II. The fiber pattern of the annealed Konjac glucomannan indicated that it took an extended two-fold helical structure. Among the acetylated glucomannans, Higanbana glucomannan with a high mannose content (mannose/glucose = 4.0) showed a similar diffraction pattern to that of β-1,4-d-mannan triacetate, indicating that the isomorphous replacement also occurred in the acetyl derivative. However, glucomannan triacetate with a low mannose content (1.5 or 1.6) showed a different crystalline form from that of mannan triacetate. The fiber diffraction pattern of Konjac glucomannan acetate suggested that it took a three-fold helix

  13. Diffracted X-ray tracking for monitoring intramolecular motion in individual protein molecules using broad band X-ray

    Ichiyanagi, Kouhei; Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Hoshisashi, Kentaro; Jae-won, Chang; Tokue, Maki; Matsushita, Yufuku; Nishijima, Masaki; Inoue, Yoshihisa; Senba, Yasunori; Ohashi, Haruhiko; Ohta, Noboru; Yagi, Naoto; Sasaki, Yuji C.

    2013-10-01

    Diffracted X-ray tracking (DXT) enables the tilting and twisting motions of single protein molecules to be monitored with micro- to milliradian resolution using a highly brilliant X-ray source with a wide energy bandwidth. We have developed a technique to monitor single molecules using gold nanocrystals attached to individual protein molecules using the BL28B2 beamline at SPring-8. In this paper we present the installation of a single toroidal X-ray mirror at BL28B2 to focus X-rays in an energy range of 10-20 keV (△E/E = 82% for an X-ray with a wide energy bandwidth). With this beamline we tracked diffraction spots from gold nanocrystals over a wide angle range than that using quasi-monochromatic X-rays. Application of the wide angle DXT technique to biological systems enabled us to observe the on-site motions of single protein molecules that have been functionalized in vivo. We further extend the capability of DXT by observing the fractional tilting and twisting motions of inner proteins under various conditions. As a proof of this methodology and to determine instrumental performance the intramolecular motions of a human serum albumin complex with 2-anthracenecarboxylic acid was investigated using the BL28B2 beamline. The random tilting and twisting intramolecular motions are shown to be directly linked to the movement of individual protein molecules in the buffer solution.

  14. Diffracted X-ray tracking for monitoring intramolecular motion in individual protein molecules using broad band X-ray

    Diffracted X-ray tracking (DXT) enables the tilting and twisting motions of single protein molecules to be monitored with micro- to milliradian resolution using a highly brilliant X-ray source with a wide energy bandwidth. We have developed a technique to monitor single molecules using gold nanocrystals attached to individual protein molecules using the BL28B2 beamline at SPring-8. In this paper we present the installation of a single toroidal X-ray mirror at BL28B2 to focus X-rays in an energy range of 10–20 keV (△E/E = 82% for an X-ray with a wide energy bandwidth). With this beamline we tracked diffraction spots from gold nanocrystals over a wide angle range than that using quasi-monochromatic X-rays. Application of the wide angle DXT technique to biological systems enabled us to observe the on-site motions of single protein molecules that have been functionalized in vivo. We further extend the capability of DXT by observing the fractional tilting and twisting motions of inner proteins under various conditions. As a proof of this methodology and to determine instrumental performance the intramolecular motions of a human serum albumin complex with 2-anthracenecarboxylic acid was investigated using the BL28B2 beamline. The random tilting and twisting intramolecular motions are shown to be directly linked to the movement of individual protein molecules in the buffer solution

  15. Three-dimensional coherent X-ray diffraction imaging of a whole, frozen-hydrated cell

    Rodriguez, Jose A.; Xu, Rui; Chen, Chien-Chun; Huang, Zhifeng; Jiang, Huaidong; Raines, Kevin S.; Nam, Daewoong; Chen, Allan L.; Pryor, A J; Wiegart, Lutz; Song, Changyong; Madsen, Anders; Chushkin, Yuriy; Zontone, Federico; Bradley, Peter J.

    2014-01-01

    A structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffraction imaging (cryo-CDI) could bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, we report for the first time 3D cryo-CDI of a whole, frozen-hydrated cell - in this case a Neospora caninum tachyzoite - usi...

  16. TU-F-BRF-04: Registration of 3D Transesophageal Echocardiography and X-Ray Fluoroscopy Using An Inverse Geometry X-Ray System

    Purpose: To develop a method for the fusion of 3D echocardiography and Scanning-Beam Digital X-ray (SBDX) fluoroscopy to assist with catheter device and soft tissue visualization during interventional procedures. Methods: SBDX is a technology for low-dose inverse geometry x-ray fluoroscopy that performs digital tomosynthesis at multiple planes in real time. In this study, transesophageal echocardiography (TEE) images were fused with SBDX images by estimating the 3D position and orientation (the “pose”) of the TEE probe within the x-ray coordinate system and then spatially transforming the TEE image data to match this pose. An initial pose estimate was obtained through tomosynthesis-based 3D localization of points along the probe perimeter. Position and angle estimates were then iteratively refined by comparing simulated projections of a 3D probe model against SBDX x-ray images. Algorithm performance was quantified by imaging a TEE probe in different known orientations and locations within the x-ray field (0-30 degree tilt angle, up to 50 mm translation). Fused 3D TEE/SBDX imaging was demonstrated by imaging a tissue-mimicking polyvinyl alcohol cylindrical cavity as a catheter was navigated along the cavity axis. Results: Detected changes in probe tilt angle agreed with the known changes to within 1.2 degrees. For a 50 mm translation along the source-detector axis, the detected translation was 50.3 mm. Errors for in-plane translations ranged from 0.1 to 0.9 mm. In a fused 3D TEE/SBDX display, the catheter device was well visualized and coincident with the device shadow in the TEE images. The TEE images portrayed phantom boundaries that were not evident under x-ray. Conclusion: Registration of soft tissue anatomy derived from TEE imaging and device imaging from SBDX x-ray fluoroscopy is feasible. The simultaneous 3D visualization of these two modalities may be useful in interventional procedures involving the navigation of devices to soft tissue anatomy

  17. TU-F-BRF-04: Registration of 3D Transesophageal Echocardiography and X-Ray Fluoroscopy Using An Inverse Geometry X-Ray System

    Speidel, M; Hatt, C; Tomkowiak, M; Raval, A [University of Wisconsin, Madison, WI (United States); Funk, T [Triple Ring Technologies, Inc., Newark, CA (United States)

    2014-06-15

    Purpose: To develop a method for the fusion of 3D echocardiography and Scanning-Beam Digital X-ray (SBDX) fluoroscopy to assist with catheter device and soft tissue visualization during interventional procedures. Methods: SBDX is a technology for low-dose inverse geometry x-ray fluoroscopy that performs digital tomosynthesis at multiple planes in real time. In this study, transesophageal echocardiography (TEE) images were fused with SBDX images by estimating the 3D position and orientation (the “pose”) of the TEE probe within the x-ray coordinate system and then spatially transforming the TEE image data to match this pose. An initial pose estimate was obtained through tomosynthesis-based 3D localization of points along the probe perimeter. Position and angle estimates were then iteratively refined by comparing simulated projections of a 3D probe model against SBDX x-ray images. Algorithm performance was quantified by imaging a TEE probe in different known orientations and locations within the x-ray field (0-30 degree tilt angle, up to 50 mm translation). Fused 3D TEE/SBDX imaging was demonstrated by imaging a tissue-mimicking polyvinyl alcohol cylindrical cavity as a catheter was navigated along the cavity axis. Results: Detected changes in probe tilt angle agreed with the known changes to within 1.2 degrees. For a 50 mm translation along the source-detector axis, the detected translation was 50.3 mm. Errors for in-plane translations ranged from 0.1 to 0.9 mm. In a fused 3D TEE/SBDX display, the catheter device was well visualized and coincident with the device shadow in the TEE images. The TEE images portrayed phantom boundaries that were not evident under x-ray. Conclusion: Registration of soft tissue anatomy derived from TEE imaging and device imaging from SBDX x-ray fluoroscopy is feasible. The simultaneous 3D visualization of these two modalities may be useful in interventional procedures involving the navigation of devices to soft tissue anatomy.

  18. Ultrafast time-resolved X-ray diffraction using an optimized laser-plasma based X-ray source

    Femtosecond X-ray pulses are invaluable tools to investigate the structural dynamics triggered by a femtosecond laser pulse. These ultrashort X-ray pulses can be provided by lab-sized laser-produced plasma X-ray sources. This thesis is dedicated to optimizing the X-ray emission from the X-ray source at the University of Duisburg-Essen and using this source to investigate ultrafast structural dynamics in laser excited materials. For these purposes, detailed investigations on how the laser intensities, target thicknesses, angles of incidence and different pre-pulse/pre-plasma conditions affecting the emission of Kα-photons from Cu and Ti targets were performed. The outcomes from these studies are applied to optimize the X-ray production of the existing X-ray source for time resolved X-ray diffraction (TRXD) experiments. In the mean time, in order to improve the measurement sensitivity/accuracy, and automatize and speed up the experimental procedures, several other improvements have been implemented in the experimental setup for TRXD experiments. These improvements of the setup are essential to achieve the results of the three TRXD experiments discussed in this thesis. In the first experiment, Debye-Waller effect in a thin laser-excited Au film was observed. The drop of measured diffraction signal with a decay time constant of 4.3±1 ps was measured for high excitation fluences. This result is in good agreement with previous experimental results as well as the Two-Temperature Model (TTM) calculations at high fluences. The second experiment extends the studies of coherent optical phonons in laser-excited Bi to a higher excitation fluence range that has not been investigated previously. Large amplitude coherent atomic motion and a complete softening of the A1g phonon mode were observed. These observations represents conclusive experimental evidence that the Peierls distortion, which defines the equilibrium structure of Bi, vanishes and the material is transformed into

  19. An autonomous CZT module for X-ray diffraction imaging

    We present the development of a CZT-based detection module dedicated to X-ray diffraction imaging. This kind of application requires a good energy and spatial resolution in order to resolve Bragg peaks. In a first part, we present the detector configuration used and dimensioning constraints. As the input energy range is comprised between 20 and 150 keV, we use 5 mm thick high resistivity CZT crystals. The 660 mm2 detection area is segmented on both sides into 192 anodes and 12 cathodes. Signals from both sides are read jointly in order to perform multi parametric event corrections (depth of interaction, charge sharing, induction sharing). In order to be integrated easily inside an X-ray imaging system, the system has been conceived to be completely autonomous: it is powered by a single 12 V supply and is interfaced with the external system by Ethernet for communication and RS485 for synchronization. In a second part, we describe the system readout architecture and then the implementation of the data processing. An FPGA circuit embeds a digital processing chain that carries out readout ASIC interfacing and advanced multi parametric data corrections. Gain, offset but also depth of interaction and charge sharing are corrected on the flow. Incoming events from different channels are clustered together by comparing their location and time of occurrence. The FPGA also embeds a processor running an operating system that controls the system, carries out all calibrations, automated tests and acquisitions. Eventually, we show the results obtained and demonstrate the relative influence of depth of interaction and charge sharing. Homogeneity of detector behavior is also discussed and the reproducibility of the performance between modules is presented. The average energy resolution at 25 C is 2.4 % FWHM at 122 keV and 3.8 % FWHM at 60 keV and the average efficiency is 73 %. (authors)

  20. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; Nelson, Johanna; Shapiro, David; Stewart, Andrew; Turner, Joshua; Jacobsen, Chris

    2009-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite n...

  1. Tomography of a Cryo-immobilized Yeast Cell Using Ptychographic Coherent X-Ray Diffractive Imaging

    Giewekemeyer, Klaus; Hackenberger, Claudia; Aquila, Andrew; Wilke, R. N.; Groves, Matthew; Jordanova, R.; Lamzin, V. S.; Borchers, G.; Saksl, K.; Zozulya, A.V.; Sprung, M.; Adrian P. Mancuso

    2015-01-01

    The structural investigation of noncrystalline, soft biological matter using x-rays is of rapidly increasing interest. Large-scale x-ray sources, such as synchrotrons and x-ray free electron lasers, are becoming ever brighter and make the study of such weakly scattering materials more feasible. Variants of coherent diffractive imaging (CDI) are particularly attractive, as the absence of an objective lens between sample and detector ensures that no x-ray photons scattered by a sample are lost ...

  2. X-ray color imaging with 3D sensitive voxel detector

    X-ray imaging is today widely used in a broad range of applications. Nevertheless some limitations are represented by the inability to distinguish between a thick layer of low Z material and a thin layer of high Z material, and by the beam hardening, where the incident X-ray spectrum is modified as the beam traverses the sample. Such effects cause problems in many applications (e.g. CT reconstruction) generating artifacts and worsening the spatial resolution. This work presents a new technique allowing spectral sensitivity using a new 3D voxel detector based on the Timepix pixel detector. The device is designed as a layered stack of several Timepix sensors. The readout chip is thinned down to reduce the amount of insensitive absorbing material. Every single layers in the stack act as a filter, i.e. each stack layer visualizes a different part of the spectrum attenuated by the object giving further information about the object composition. The comparison of attenuation levels observed in different detector layers can be used to estimate the extent of the beam hardening effect in the imaged object and thus point out differences in the material composition.

  3. Multi-contrast 3D X-ray imaging of porous and composite materials

    Grating-based X-ray computed tomography allows for simultaneous and nondestructive determination of the full X-ray complex index of refraction and the scattering coefficient distribution inside an object in three dimensions. Its multi-contrast capabilities combined with a high resolution of a few micrometers make it a suitable tool for assessing multiple phases inside porous and composite materials such as concrete. Here, we present quantitative results of a proof-of-principle experiment performed on a concrete sample. Thanks to the complementarity of the contrast channels, more concrete phases could be distinguished than in conventional attenuation-based imaging. The phase-contrast reconstruction shows high contrast between the hardened cement paste and the aggregates and thus allows easy 3D segmentation. Thanks to the dark-field image, micro-cracks inside the coarse aggregates are visible. We believe that these results are extremely interesting in the field of porous and composite materials studies because of unique information provided by grating interferometry in a non-destructive way

  4. Multi-contrast 3D X-ray imaging of porous and composite materials

    Sarapata, Adrian; Herzen, Julia [Lehrstuhl für Biomedizinische Physik, Physik-Department and Institut für Medizintechnik, Technische Universität München, 85748 Garching (Germany); Ruiz-Yaniz, Maite [Lehrstuhl für Biomedizinische Physik, Physik-Department and Institut für Medizintechnik, Technische Universität München, 85748 Garching (Germany); European Synchrotron Radiation Facility, 38000 Grenoble (France); Zanette, Irene [Lehrstuhl für Biomedizinische Physik, Physik-Department and Institut für Medizintechnik, Technische Universität München, 85748 Garching (Germany); Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0QX (United Kingdom); Rack, Alexander [European Synchrotron Radiation Facility, 38000 Grenoble (France); Pfeiffer, Franz [Lehrstuhl für Biomedizinische Physik, Physik-Department and Institut für Medizintechnik, Technische Universität München, 85748 Garching (Germany); Institut für Diagnostische und Interventionelle Radiologie, Klinikum rechts der Isar, Technische Universität München, 81675 München (Germany)

    2015-04-13

    Grating-based X-ray computed tomography allows for simultaneous and nondestructive determination of the full X-ray complex index of refraction and the scattering coefficient distribution inside an object in three dimensions. Its multi-contrast capabilities combined with a high resolution of a few micrometers make it a suitable tool for assessing multiple phases inside porous and composite materials such as concrete. Here, we present quantitative results of a proof-of-principle experiment performed on a concrete sample. Thanks to the complementarity of the contrast channels, more concrete phases could be distinguished than in conventional attenuation-based imaging. The phase-contrast reconstruction shows high contrast between the hardened cement paste and the aggregates and thus allows easy 3D segmentation. Thanks to the dark-field image, micro-cracks inside the coarse aggregates are visible. We believe that these results are extremely interesting in the field of porous and composite materials studies because of unique information provided by grating interferometry in a non-destructive way.

  5. Registration of 2D x-ray images to 3D MRI by generating pseudo-CT data

    van der Bom, M. J.; Pluim, J. P. W.; Gounis, M. J.; van de Kraats, E. B.; Sprinkhuizen, S. M.; Timmer, J.; Homan, R.; Bartels, L. W.

    2011-02-01

    Spatial and soft tissue information provided by magnetic resonance imaging can be very valuable during image-guided procedures, where usually only real-time two-dimensional (2D) x-ray images are available. Registration of 2D x-ray images to three-dimensional (3D) magnetic resonance imaging (MRI) data, acquired prior to the procedure, can provide optimal information to guide the procedure. However, registering x-ray images to MRI data is not a trivial task because of their fundamental difference in tissue contrast. This paper presents a technique that generates pseudo-computed tomography (CT) data from multi-spectral MRI acquisitions which is sufficiently similar to real CT data to enable registration of x-ray to MRI with comparable accuracy as registration of x-ray to CT. The method is based on a k-nearest-neighbors (kNN)-regression strategy which labels voxels of MRI data with CT Hounsfield Units. The regression method uses multi-spectral MRI intensities and intensity gradients as features to discriminate between various tissue types. The efficacy of using pseudo-CT data for registration of x-ray to MRI was tested on ex vivo animal data. 2D-3D registration experiments using CT and pseudo-CT data of multiple subjects were performed with a commonly used 2D-3D registration algorithm. On average, the median target registration error for registration of two x-ray images to MRI data was approximately 1 mm larger than for x-ray to CT registration. The authors have shown that pseudo-CT data generated from multi-spectral MRI facilitate registration of MRI to x-ray images. From the experiments it could be concluded that the accuracy achieved was comparable to that of registering x-ray images to CT data.

  6. X-ray diffraction analysis of residual stress in zirconia dental composites

    Allahkarami, Masoud

    Dental restoration ceramic is a complex system to be characterized. Beside its essential biocompatibility, and pleasant appearance, it requires being mechanically strong in a catastrophic loading environment. Any design is restricted with geometry boundary and material property limits. Inspired by natural teeth, a multilayer ceramic is a smart way of achieving an enhanced restoration. Bi-layers of zirconia core covered by porcelain are known as one of the best multilayer restorations. Residual stresses may be introduced into a bi-layer dental ceramic restoration during its entire manufacturing process due to thermal expansion and elastic property mismatch. It is impossible to achieve a free of residual stresses bi-layer zirconia-porcelain restoration. The idea is to take the advantage of residual stress in design in such a way to prevent the crack initiation and progression. The hypothesis is a compressive residual stress at external contact surface would be enabling the restoration to endure a greater tensile stress. Optimizing the layers thickness, manufacturing process, and validating 3D simulations require development of new techniques of thickness, residual stresses and phase transformation measurement. In the present work, a combined mirco-tomography and finite element based method were adapted for thickness measurement. Two new 2D X-ray diffraction based techniques were adapted for phase transformation area mapping and combined phase transformation and residual stress measurement. Concerning the complex geometry of crown, an efficient method for X-ray diffraction data collection mapping on a given curved surface was developed. Finally a novel method for 3D dimensional x-ray diffraction data collection and visualization were introduced.

  7. Two digital X-ray imaging systems for applications in X-ray diffraction

    Two digital X-ray imaging systems developed at the Rutherford Appleton Laboratory are described:- the Mark I and the Mark II. Both use a bidimensionally sensitive Multiwire proportional counter as the basic X-ray image transducer coupled to a digital microcomputer system. The Mark I system provides the advantages of high speed, high sensitivity digital imaging directly into the computer with the potential for software control of the sample orientation and environment. The Mark II system adds the novel features of signal averaging and multi-frame exposures. (author)

  8. Preliminary Investigation: 2D-3D Registration of MR and X-ray Cardiac Images Using Catheter Constraints

    Truong, Michael V.N.; Aslam, Abdullah; Rinaldi, Christopher Aldo; Razavi, Reza; Penney, Graeme P.; Rhode, Kawal

    2009-01-01

    Cardiac catheterization procedures are routinely guided by X-ray fluoroscopy but suffer from poor soft-tissue contrast and a lack of depth information. These procedures often employ pre-operative magnetic resonance or computed tomography imaging for treatment planning due to their excellent soft-tissue contrast and 3D imaging capabilities. We developed a 2D-3D image registration method to consolidate the advantages of both modalities by overlaying the 3D images onto the X-ray. Our method uses...

  9. X-Ray Nanofocus CT: Visualising Of Internal 3D-Structures With Submicrometer Resolution

    Weinekoetter, Christian

    2008-09-01

    High-resolution X-ray Computed Tomography (CT) allows the visualization and failure analysis of the internal micro structure of objects—even if they have complicated 3D-structures where 2D X-ray microscopy would give unclear information. During the past several years, computed tomography has progressed to higher resolution and quicker reconstruction of the 3D-volume. Most recently it even allows a three-dimensional look into the inside of materials with submicron resolution. With the use of nanofocus® tube technology, nanoCT®-systems are pushing forward into application fields that were exclusive to high cost and rare available synchrotron techniques. The study was performed with the new nanotom, a very compact laboratory system which allows the analysis of samples up to 120 mm in diameter and weighing up to 1 kg with exceptional voxel-resolution down to nanoCT-examinations e.g. of synthetic materials, metals, ceramics, composite materials, mineral and organic samples. There are a few physical effects influencing the CT quality, such as beam-hardening within the sample or ring-artefacts, which can not be completely avoided. To optimize the quality of high resolution 3D volumes, the nanotom® includes a variety of effective software tools to reduce ring-artefacts and correct beam hardenings or drift effects which occurred during data acquisition. The resulting CT volume data set can be displayed in various ways, for example by virtual slicing and sectional views in any direction of the volume. By the fact that this requires only a mouse click, this technique will substitute destructive mechanical slicing and cutting in many applications. The initial CT results obtained with the nanotom® demonstrate that it is now possible to analyze the three-dimensional micro structure of materials and small objects with submicrometer resolution. Any internal difference in material, density or porosity within a sample can be visualized and data like distances can be measured

  10. X-ray diffraction study of synthetic tetraborates and hexaborates

    The results of the X-ray diffraction of the tetraborates (NH3CH2CH2NH3)(B4O5(OH)4), (NH4)(Co(NH3)5H2O)(B4O5(OH)4)2x5H2O and of the hexaborates Ni(H2O)4(B6O)(OH)6xH2O (triclinic and monoclinic modification). (NH4)2{Co(H2O)2(B6O7(OH)6)2}x2H2O, (Ni(H2O)6){Ni(B6O7(OH)3(OCH3)3)2}, Co(H2O)3(B6O7(OH)6)x1.5C2H5OH and Ni(H2O)3(B6O7(OH)6)xC2H5OH have been reviewed. The crystal solvates isostructural to the latter compound - nickel hexaborates containing propyl and allyl alcohols, acetone and methyl ethyl ketone have been studied

  11. Investigation of kidney stones by X-ray diffraction method

    Muakthong, D.

    2005-01-01

    Full Text Available An investigation of 39 male kidney stone samples and 11 female kidney stone samples obtained from Songklanakarind Hospital, Hat Yai, Songkhla was carried out. Most samples were obtained from patients ages over 40 years. By means of X-ray diffraction (XRD, kidney stones can be classified according to their structure and composition into 3 groups is 1. uric acid (C5H4N4O3 and ammonium acid urate (C5H7N5O3 2. oxalates; whewelite (C2CaO4!H2O CaC2O4!H2O and weddellite (C2CaO4!2H2O 3. phosphates; struvite (NH4MgPO4!6H2O and calcium phosphate hydrate (Ca3(PO42!xH2O. External and internal environments such as occupation, dietary habits, lack of water-drinking etc. are the major factors for kidney stone formation. Results from this study are very useful for the patients to prevent recrystallization of kidney stones by avoiding some elements or some organic compounds which are main components of kidney stones formed in the human urinary system.

  12. A magnetic x-ray diffraction investigation of gadolinium selenide

    Costa, M.M.R.; Almeida, M.J.M. de [Departamento de Fisica, Universidade de Coimbra, Coimbra (Portugal); Nuttall, W.J.; Stirling, W.G. [Department of Physics, Keele University, Keele, Staffs (United Kingdom); Tang, C.C. [Daresbury Laboratory, Warrington, Cheshire (United Kingdom); Forsyth, J.B. [Rutherford Appleton Laboratory, Chilton, Oxon (United Kingdom); Cooper, M.J. [Department of Physics, University of Warwick, Coventry (United Kingdom)

    1996-04-01

    A single-crystal synchrotron radiation study of gadolinium selenide has been made in the temperature range 15-100 K. GdSe has the rocksalt structure and becomes antiferromagnetic below a reported Neel temperature of 65 K. At 15 K, magnetic reflections are observed at G+T with modulation wavevector T={l_brace}1/2:1/2:1/2{r_brace} propagating from reciprocal lattice point G. This is achieved by exploiting the resonant enhancement in the vicinity of the Gd L{sub II} and L{sub III} edges. Similar enhancements are observed at the two edges, with the maximum effect occurring approximately 3 eV above the absorption edge. The temperature dependence of the intensity of the magnetic reflections indicates a Neel temperature of 63(1) K. These measurements, together with high-resolution studies of the fundamental reflections (T=0), contribute further evidence of magnetic or structural changes in the sample at 37(1) K. Our observations are discussed and compared with previous x-ray diffraction and magnetic susceptibility measurements. (author)

  13. Federated repositories of X-ray diffraction images.

    Androulakis, Steve; Schmidberger, Jason; Bate, Mark A; DeGori, Ross; Beitz, Anthony; Keong, Cyrus; Cameron, Bob; McGowan, Sheena; Porter, Corrine J; Harrison, Andrew; Hunter, Jane; Martin, Jennifer L; Kobe, Bostjan; Dobson, Renwick C J; Parker, Michael W; Whisstock, James C; Gray, Joan; Treloar, Andrew; Groenewegen, David; Dickson, Neil; Buckle, Ashley M

    2008-07-01

    There is a pressing need for the archiving and curation of raw X-ray diffraction data. This information is critical for validation, methods development and improvement of archived structures. However, the relatively large size of these data sets has presented challenges for storage in a single worldwide repository such as the Protein Data Bank archive. This problem can be avoided by using a federated approach, where each institution utilizes its institutional repository for storage, with a discovery service overlaid. Institutional repositories are relatively stable and adequately funded, ensuring persistence. Here, a simple repository solution is described, utilizing Fedora open-source database software and data-annotation and deposition tools that can be deployed at any site cheaply and easily. Data sets and associated metadata from federated repositories are given a unique and persistent handle, providing a simple mechanism for search and retrieval via web interfaces. In addition to ensuring that valuable data is not lost, the provision of raw data has several uses for the crystallographic community. Most importantly, structure determination can only be truly repeated or verified when the raw data are available. Moreover, the availability of raw data is extremely useful for the development of improved methods of image analysis and data processing. PMID:18566516

  14. X-ray diffraction analysis of mudstone from nw sudan

    This study deals with the theoretical and experimental aspects of the x-ray diffraction technique (XRD). The XRD technique is used to investigate fine structure of matter, and it is most efficient method for the determination of the mineralogical composition of rocks. The XRD technique is used also to investigate the clay mineralogical of mud-stones of the Nubian sandstones of north western Sudan. The XRD results revealed that the mud-stone samples are composed, in decreasing abundance's of kaolinite, smectite, chlorite and illite. Non-clay minerals reported include quartz, feldspars and geothite. Kaolinite dominates in most of samples with percentages ranging between 78-96%. Smectite comes second in abundance and ranges between 10-24%, followed by chlorite and illite which showed the lowest abundance's. The dominance of kaolinite over smectite indicates that intense chemical weathering and leaching occurred under warm humid climate interrupted by dry periods. Most probably these clay minerals were produced by inheritance and partly by neo formation. The variation of the chemical composition of these mud stones is due basically to differences in clay mineralogy which was controlled by source rock geology, weathering physicochemical behavior of elements, local environment and climatic condition in the past. (Author)

  15. Neutron and x-ray diffraction studies in cement

    Full text: Phase quantification of cement is difficult due to the complexity of phases, and cement composition is complicated by the polymorphic modifications of these phases. Only three of the seven polymorphs of the main component of cement, tricalcium silicate, have their structures fully determined, although more polymorphs are likely to be present There has been an increase in the use of Rietveld refinement for the analysis of cement in recent years, and an advantage of the method is the ability to define the tricalcium silicate form. It is usual to include a polymorph of tricalcium silicate in each of the three crystal systems encountered when beginning a refinement, and then exclude those not found. Care must be taken not to allow one crystal system to alter itself to compensate for another. Using synchrotron x-ray diffraction data, refinement of some atomic positions in a tricalcium silicate form resulted in a 24.5% improvement in the fits of the phase. An investigation using neutron data also showed significant improvement in the rb values for two polymorph of tricalcium silicate in a clinker sample, and also showed slight deviation in the phase quantification results obtained

  16. X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

    The Guinier - Haegg focusing camera is discussed with reference to its use as an instrument for rapid phase analysis. An actual camera and the alignment procedure employed in its setting up are described. The results obtained with the instrument are compared with those obtained with Debye - Scherrer cameras and powder diffractometers. Exposure times of 15 - 30 minutes with compounds of simple structure are roughly one-sixth of those required for Debye - Scherrer patterns. Coupled with the lower background resulting from the use of a monochromatic X-ray beam, the shorter exposure time gives a ten-fold increase in sensitivity for the detection of minor phases as compared with the Debye - Scherrer camera. Attention is paid to the precautions taken to obtain reliable Bragg angles from Guinier - Haegg film measurements, with particular reference to calibration procedures. The evaluation of unit cell parameters from Guinier - Haegg data is discussed together with the application of tests for the presence of angle-dependent systematic errors. It is concluded that with proper calibration procedures and least squares treatment of the data, accuracies of the order of 0.005% are attainable. A compilation of diffraction data for a number of compounds examined in the Active Central Laboratory at Studsvik is presented to exemplify the scope of this type of powder camera

  17. X-ray diffraction and X-ray absorption spectroscopic analyses for intercalative nanohybrids with low crystallinity

    Dae-Hwan Park

    2016-03-01

    Full Text Available Intercalation reactions can be achieved through ion-exchange, pillaring, and exfoliation–reassembling reactions to explore new intercalation compounds with desired electronic, electrochemical, and optical functions. Such intercalative nanohybrids with lamellar or porous structure have received much attention due to their potential applications such as catalysts, electrodes, selective adsorbents, stabilizing agents, and even drug delivery systems. In this review, we briefly introduce and highlight X-ray diffraction and X-ray absorption spectroscopy studies on the intercalative nanohybrids to understand their intracrystalline and electronic structures along with physicochemical functions.

  18. Local ISM 3D Distribution and Soft X-ray Background Inferences for Nearby Hot Gas

    Puspitarini, L.; Lallement, R.; Snowden, Steven L.; Vergely, J.-L.; Snowden, S.

    2014-01-01

    Three-dimensional (3D) interstellar medium (ISM) maps can be used to locate not only interstellar (IS) clouds, but also IS bubbles between the clouds that are blown by stellar winds and supernovae, and are filled by hot gas. To demonstrate this, and to derive a clearer picture of the local ISM, we compare our recent 3D IS dust distribution maps to the ROSAT diffuse Xray background maps after removal of heliospheric emission. In the Galactic plane, there is a good correspondence between the locations and extents of the mapped nearby cavities and the soft (0.25 keV) background emission distribution, showing that most of these nearby cavities contribute to this soft X-ray emission. Assuming a constant dust to gas ratio and homogeneous 106 K hot gas filling the cavities, we modeled in a simple way the 0.25 keV surface brightness along the Galactic plane as seen from the Sun, taking into account the absorption by the mapped clouds. The data-model comparison favors the existence of hot gas in the solar neighborhood, the so-called Local Bubble (LB). The inferred mean pressure in the local cavities is found to be approx.9,400/cu cm K, in agreement with previous studies, providing a validation test for the method. On the other hand, the model overestimates the emission from the huge cavities located in the third quadrant. Using CaII absorption data, we show that the dust to CaII ratio is very small in those regions, implying the presence of a large quantity of lower temperature (non-X-ray emitting) ionized gas and as a consequence a reduction of the volume filled by hot gas, explaining at least part of the discrepancy. In the meridian plane, the two main brightness enhancements coincide well with the LB's most elongated parts and chimneys connecting the LB to the halo, but no particular nearby cavity is found towards the enhancement in the direction of the bright North Polar Spur (NPS) at high latitude. We searched in the 3D maps for the source regions of the higher energy

  19. Coherent convergent-beam time-resolved X-ray diffraction

    Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

    2014-01-01

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic ...

  20. 3-d chemical imaging using angle-scan nanotomography in a soft X-ray scanning transmission X-ray microscope

    Three-dimensional chemical mapping using angle scan nanotomography in a soft X-ray scanning transmission X-ray microscope (STXM) has been used to investigate the spatial distributions of a low density polyacrylate polyelectrolyte ionomer inside submicron sized polystyrene microspheres. Acquisition of tomograms at multiple photon energies provides true, quantifiable 3-d chemical sensitivity. Both pre-O 1s and C 1s results are shown. The study reveals aspects of the 3-d distribution of the polyelectrolyte that were inferred indirectly or had not been known prior to this study. The potential and challenges for extension of the technique to studies of other polymeric and to biological systems is discussed. (orig.)

  1. Transmission x-ray diffraction of undisturbed soil microfabrics obtained by microdrilling in thin sections

    Denaix, L.; Oort, van F.; Pernes, M.; Jongmans, A.G.

    1999-01-01

    Clay mineralogical studies by X-ray diffraction performed on extracted <2-μm fractions do not always represent all clay mineral constituents present in the soil. In this work, transmission X-ray diffraction (TXRD) was applied to undisturbed microsamples of optically homogeneous mineral soil fabrics

  2. Diffuse X-ray diffraction by a crystal of an aging alloy

    The theory of the diffusive X-ray diffraction is considered on the generalized model of the aging alloy structure. The formula for calculating the distribution of the X-ray diffusive diffraction intensity for such model is deduced. This formula allows to obtain the theoretical distribution of the diffusive scattering intensity for different specific model

  3. A Computer Program for Calculation of Calibration Curves for Quantitative X-Ray Diffraction Analysis.

    Blanchard, Frank N.

    1980-01-01

    Describes a FORTRAN IV program written to supplement a laboratory exercise dealing with quantitative x-ray diffraction analysis of mixtures of polycrystalline phases in an introductory course in x-ray diffraction. Gives an example of the use of the program and compares calculated and observed calibration data. (Author/GS)

  4. X-Ray Diffraction and the Discovery of the Structure of DNA

    Crouse, David T.

    2007-01-01

    A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

  5. Characterization of Gas-Solid Reactions using In Situ Powder X-ray Diffraction

    Møller, Kasper Trans; Hansen, Bjarne Rosenlund Søndertoft; Dippel, Ann-Christin;

    2014-01-01

    X-ray diffraction is a superior technique for structural characterization of crystalline matter. Here we review the use of in situ powder X-ray diffraction (PXD) mainly for real-time studies of solid/gas reactions, data analysis and the extraction of valuable knowledge of structural, chemical...

  6. Complementing high-throughput X-ray powder diffraction data with quantum-chemical calculations

    Naelapaa, Kaisa; van de Streek, Jacco; Rantanen, Jukka;

    2012-01-01

    single crystals or bulk samples of sufficient quantity to carry out high-quality X-ray diffraction measurements. This process could be made more efficient by a robust procedure for crystal structure determination directly from high-throughput X-ray powder diffraction (XRPD) data. Quantum...

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

    Ludwig, Wolfgang; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, Erik Mejdal; Proudhon, H.; Buffiere, J.Y.

    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......-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 at...... the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms....

  8. X-RAY DIFFRACTION STUDY OF A PANCHAVAKTRA RAS

    B. Srinivasulu*, P. Bhadra Dev, P.H.C. Murthy

    2012-06-01

    Full Text Available Analytical monitoring of Pharmaceutical products is necessary to ensure its safety and efficacy throughout all phases of the drug. A systematic approach should be adapted to the presentation and evaluation of stable information, which should include, as necessary, physical, chemical, biological and microbiological test characteristics. Indian System of Medicine (ISM frequently uses metal/mineral drugs. It is mandatory to standardize the preparatory procedures. For the Pharmaceutical standardization, three batches of the Panchavaktra ras were prepared and analytical study of final product carried out. Panchavaktra ras consist equal parts of Parada (Mercury, Gandhaka (Sulphur, Tankana (Borax Pippali (Piper longum L. and Marica (Piper nigrum L., and Mardhana (Grinding was done carefully with sufficient quantity of juice of Datura metel leaves for 24 hours and a final product was obtained in the form of Vati (tablet form. It is one of the formulations mentioned in Amavata (Rheumatoid Arthritis disease. The final products were subjected to Powder X-Ray Diffraction (XRD studies and values of XRD peaks of particular Panchavaktra ras were observed. This study revealed that high peaks of HgS (Metacinnabar, free S (Sulfur, Chabazite (Ca- exchanged, dehydrated Ca (structure- Rhombohedral in the final products. The structural and chemical characterization of the HgS (Metacinnabar found as cubic, free S (Sulphur as Orthorhombic in all the samples. The 50% strongest peaks of HgS were present at 2-Theta scale between 26-31, 43-44, 51-55, 70-72 degrees. This paper points out the importance of XRD, as a standard tool for further studies and research of Herbo-mineral formulations.

  9. Moving-Article X-Ray Imaging System and Method for 3-D Image Generation

    Fernandez, Kenneth R. (Inventor)

    2012-01-01

    An x-ray imaging system and method for a moving article are provided for an article moved along a linear direction of travel while the article is exposed to non-overlapping x-ray beams. A plurality of parallel linear sensor arrays are disposed in the x-ray beams after they pass through the article. More specifically, a first half of the plurality are disposed in a first of the x-ray beams while a second half of the plurality are disposed in a second of the x-ray beams. Each of the parallel linear sensor arrays is oriented perpendicular to the linear direction of travel. Each of the parallel linear sensor arrays in the first half is matched to a corresponding one of the parallel linear sensor arrays in the second half in terms of an angular position in the first of the x-ray beams and the second of the x-ray beams, respectively.

  10. 3D X-Ray imaging of bone tissue from micro to nano scale and associated inverse problems

    Peyrin, F.; Toma, A; Sixou, B.; Denis, L.; Wang, L.(Universität Bochum, Institut für Experimentalphysik, Bochum, 44780, Germany); WEBER,L; Langer, M. (Marco); Cloetens, P.

    2015-01-01

    Imaging bone tissue from the organ to the cellular level is a major goal in bone research to understand, diagnose and predict bone fragility associated to bone disease such as osteoporosis. In this presentation, we show that X-ray CT is particularly well adapted to image bone in 3D up to the nanometer scale. After recalling the principles of 3D CT, we describe advances in bone CT imaging and the needs in associated inverse problems. Clinical X-ray CT is daily used to image skeletal tissue at ...

  11. 3D X-ray CT and diffusion measurements to assess tortuosity and constrictivity in a sedimentary rock

    Takahashi, Hiroaki; Seida, Yoshimi; Yui, Mikazu

    2015-01-01

    A high-resolution, three-dimensional (3D) image of the interior of the sedimentary rock was obtained by means of nano-focus X-ray computer tomography (X-ray CT). Using computational methods to analyze the 3D microstructure of the rock, we presented the tortuosity and geometrical constrictivity. We also presented results on the tritiated water (HTO) diffusion tests and a mercury intrusion porosimetry (MIP) test performed on the rock. We have compared these results to understand the dominant...

  12. Qualitative analysis of powder x-ray diffraction data

    methods of considering significant lines such as with the Hanawalt, Fink and alphabetical index; computer based search-match based on FOM and the more recent graphically based full pattern methods of phase identification. No single approach is foolproof. a range of techniques is recommended if a high level of success is required. Copyright (1999) Australian X-ray Analytical Association Inc

  13. 3D RECONSTRUCTION FROM MULTI-VIEW MEDICAL X-RAY IMAGES – REVIEW AND EVALUATION OF EXISTING METHODS

    S. Hosseinian

    2015-12-01

    Full Text Available The 3D concept is extremely important in clinical studies of human body. Accurate 3D models of bony structures are currently required in clinical routine for diagnosis, patient follow-up, surgical planning, computer assisted surgery and biomechanical applications. However, 3D conventional medical imaging techniques such as computed tomography (CT scan and magnetic resonance imaging (MRI have serious limitations such as using in non-weight-bearing positions, costs and high radiation dose(for CT. Therefore, 3D reconstruction methods from biplanar X-ray images have been taken into consideration as reliable alternative methods in order to achieve accurate 3D models with low dose radiation in weight-bearing positions. Different methods have been offered for 3D reconstruction from X-ray images using photogrammetry which should be assessed. In this paper, after demonstrating the principles of 3D reconstruction from X-ray images, different existing methods of 3D reconstruction of bony structures from radiographs are classified and evaluated with various metrics and their advantages and disadvantages are mentioned. Finally, a comparison has been done on the presented methods with respect to several metrics such as accuracy, reconstruction time and their applications. With regards to the research, each method has several advantages and disadvantages which should be considered for a specific application.

  14. Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer

    Electrochemical in operando X-ray diffraction (XRD) is a powerful method to analyze structural changes of energy storage materials while inserting/de-inserting charge carriers, such as Li- or Na-ions, into/from a host structure. The design of an XRD in operando cell is presented, which enables the use of thin (6 μm) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na0.7MnO2 and Na2.55V6O16 ⋅ 0.6H2O

  15. Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer.

    Hartung, Steffen; Bucher, Nicolas; Bucher, Ramona; Srinivasan, Madhavi

    2015-08-01

    Electrochemical in operando X-ray diffraction (XRD) is a powerful method to analyze structural changes of energy storage materials while inserting/de-inserting charge carriers, such as Li- or Na-ions, into/from a host structure. The design of an XRD in operando cell is presented, which enables the use of thin (6 μm) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na(0.7)MnO2 and Na(2.55)V6O16 ⋅ 0.6H2O. PMID:26329242

  16. Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer

    Hartung, Steffen; Bucher, Nicolas; Bucher, Ramona; Srinivasan, Madhavi

    2015-08-01

    Electrochemical in operando X-ray diffraction (XRD) is a powerful method to analyze structural changes of energy storage materials while inserting/de-inserting charge carriers, such as Li- or Na-ions, into/from a host structure. The design of an XRD in operando cell is presented, which enables the use of thin (6 μm) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na0.7MnO2 and Na2.55V6O16 ṡ 0.6H2O.

  17. Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer

    Hartung, Steffen; Bucher, Nicolas [TUM CREATE, Singapore 138602 (Singapore); Technical University of Munich, Garching 85748 (Germany); School of Materials Science and Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Bucher, Ramona [TUM CREATE, Singapore 138602 (Singapore); Srinivasan, Madhavi [TUM CREATE, Singapore 138602 (Singapore); School of Materials Science and Engineering, Nanyang Technological University, Singapore 639798 (Singapore)

    2015-08-15

    Electrochemical in operando X-ray diffraction (XRD) is a powerful method to analyze structural changes of energy storage materials while inserting/de-inserting charge carriers, such as Li- or Na-ions, into/from a host structure. The design of an XRD in operando cell is presented, which enables the use of thin (6 μm) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na{sub 0.7}MnO{sub 2} and Na{sub 2.55}V{sub 6}O{sub 16} ⋅ 0.6H{sub 2}O.

  18. Non-destructive analysis of micro texture and grain boundary character from X-ray diffraction contrast tomography

    Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting new possibilities for mapping 3D grain shapes and crystallographic orientations in different classes of polycrystalline materials. X-ray diffraction contrast tomography (DCT) is a monochromatic beam imaging technique combining the principles of X-ray micro-tomography and three-dimensional X-ray diffraction microscopy (3DXRD). DCT provides simultaneous access to 3D grain shape, crystallographic orientation and attenuation coefficient distribution at the micrometer length scale. The microtexture of the material can be quantified in more detail by post-processing of the volume data provided by DCT. In particular one can determine the local crystallographic habit plane of the grain boundary by analysing the surface normal of the grain boundary with respect to the crystal orientation. The resulting five parameter description of the character of individual grain boundaries could previously be produced only by destructive characterization techniques. Statistical analysis of this kind of data can be expected to provide new insight into various physico-chemical processes, driven by the grain boundary energy (corrosion, coarsening).

  19. Two digital X-ray imaging systems for applications in X-ray diffraction

    Two digital X-ray imaging systems developed at the Rutherford Appleton Laboratory are described: the Mark I and the Mark II. Both use a bidimensionally sensitive multiwire proportional counter (MWPC) as the basic X-ray image transducer coupled, in the case of the Mark I to a Digital LSI 11-23 microcomputer system via CAMAC, and in the case of the Mark II to a Digital LSI 11-73 microcomputer system via custom-built data acquisition hardware mounted directly on the Q-bus of the microcomputer. The Mark I system provides the advantages of high speed, high sensitivity digital imaging directly into the computer with the potential for software control of the sample orientation and environment. The Mark II system adds the novel features of signal averaging and multiframe exposures. The dedicated digital memories have a resolution of 512x512 pixels of 16 bits, matching well to the spatial resolution of the xenon-filled MWPC (0.5 mm fwhm over an aperture of 200 mm x 200 mm). A 512x512x4 bit video graphics system displays the images in grey scales or colour. (orig.)

  20. Sloped irradiation techniques in deep x-ray lithography for 3D shaping of microstructures

    Feiertag, Gregor; Ehrfeld, Wolfgang; Lehr, Heinz; Schmidt, Martin

    1997-07-01

    Deep x-ray lithography (DXRL) makes use of synchrotron radiation (SR) to transfer an absorber pattern from a mask into a thick resist layer. For most applications the direction of the SR beam is perpendicular to the mask and the resist plane. Subsequent replication techniques, e.g. electroforming, moulding or hot embossing, convert the resist relief obtained after development into micromechanical, microfluidic or micro- optical elements made from metals, polymers or ceramic materials. This process sequence is well known as the LIGA technique. The normal shadow printing process is complemented and enhanced by advanced techniques, e.g. by tilting the mask and the resist with respect to the SR beam or aligned multiple exposures to produce step-like structures. In this paper a technology for the fabrication of multidirectional inclined microstructures applying multiple tilted DXRL will be presented. Instead of one exposure with the mask/substrate assembly perpendicular to the SR beam, irradiation is performed several times applying tilt and rotational angles of the mask/substrate assembly relative to the SR beam. A huge variety of 3-D structures can be obtained using this technique. Some possible applications will be discussed.

  1. Single order X-ray diffraction with binary sinusoidal transmission grating

    Cao, Leifeng

    2013-10-01

    All existing x-ray dispersive devices including crystals, multilayers and diffraction gratings generate spectra in multiple orders, whereas soft x-ray spectroscopy applications usually require only the first order spectrum. The other diffraction orders can overlap and contaminate the first order spectrum of interest. In this letter we describe how an axis-symmetrically-distributed sinusoidal-shaped aperture with binary transmittance values can be used to disperse x-rays and with a superior diffraction pattern where, along its symmetry axis, all higher-order diffractions can be effectively suppressed. Hence this sophisticated dispersive element generates pure soft x-ray spectra in the first diffraction order, free from interference from higher diffraction orders.

  2. Measurement of thickness of thin films by the X-ray diffraction method

    X-ray diffraction method can be used to measure the thickness of thin films (coatings). The principle and the experimental details of the x-ray diffraction methods are described. The intensities of the diffracted beams are derived assuming a random orientation of the crystallites in the diffracting medium. Consequently, the expressions are not valid when the sample has preferred orientation. To check the performance of the method, thicknesses of nickel deposits on mild steel plates were determined by the x-ray diffraction method and the results compared with those obtained by the weighing method and metallographic examination. The weighing method which gives an accuracy of +- 0.1 micron is taken as the standard. The x-ray diffraction methods and the metallographic examinations give values within +- 1 micron of the value obtained by the weighing method. (author)

  3. Application of relativistic scattering theory of x rays to diffraction anomalous fine structure in Cu

    Arola, E.; Strange, Paul

    1998-01-01

    We apply our recent first-principles formalism of magnetic scattering of circularly polarized x rays to a single Cu crystal. We demonstrate the ability of our formalism to interpret the crystalline environment related near-edge fine structure features in the resonant x-ray scattering spectra at the Cu K absorption edge. We find good agreement between the computed and measured diffraction anomalous fine structure features of the x-ray scattering spectra.

  4. Ptychographic coherent x-ray diffractive imaging in the water window

    Giewekemeyer, K.; Beckers, M.; Gorniak, T.; Grunze, M.; Salditt, T.; Rosenhahn, A.

    2011-01-01

    Coherent x-ray diffractive microscopy enables full reconstruction of the complex transmission function of an isolated object to diffraction-limited resolution without relying on any optical elements between the sample and detector. In combination with ptychography, also specimens of unlimited lateral extension can be imaged. Here we report on an application of ptychographic coherent diffractive imaging (PCDI) in the soft x-ray regime, more precisely in the so-called water wi...

  5. Direct assessment of 3D foot bone kinematics using biplanar X-ray fluoroscopy and an automatic model registration method

    Ito, Kohta; Hosoda, Koh; Shimizu, Masahiro; Ikemoto, Shuhei; Kume, Shinnosuke; Nagura, Takeo; Imanishi, Nobuaki; Aiso, Sadakazu; Jinzaki, Masahiro; Ogihara, Naomichi

    2015-01-01

    Background Quantifying detailed 3-dimensional (3D) kinematics of the foot in contact with the ground during locomotion is crucial for understanding the biomechanical functions of the complex musculoskeletal structure of the foot. Biplanar X-ray fluoroscopic systems and model-based registration techniques have recently been employed to capture and visualise 3D foot bone movements in vivo, but such techniques have generally been performed manually. In the present study, we developed an automati...

  6. Structural Investigations of Nanowires Using X-Ray Diffraction

    Stankevic, Tomas

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

  7. [X-ray diffraction experiments with condenser matter

    This report discusses research on the following topics: high-Tc superconductors; The response of crystal to an applied electric field; quasicrystals; surface structure and kinetics of surface layer formation; EXAFS studies of superconductors and heterostructures; effect of iron on the crystal structure of perovskite; x-ray detector development; and SAXS experiments

  8. X-ray powder diffraction in forensic practice

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

    Roč. 13, č. 3 (2006), s. 153-155. ISSN 1210-8529 R&D Projects: GA MV RN20052005001 Institutional research plan: CEZ:AV0Z40320502 Keywords : X-ray powder microdiffraction * pigments * forensic practice Subject RIV: CA - Inorganic Chemistry

  9. 3D Nanoscale Chemical Imaging of the Distribution of Aluminum Coordination Environments in Zeolites with Soft X-Ray Microscopy

    Aramburo, Luis R.; Liu, Yijin; Tyliszczak, Tolek; de Groot, Frank M. F.; Andrews, Joy C.; Weckhuysen, Bert M.

    2013-01-01

    Here, we present the first nanoscale chemical imaging study revealing the spatial distribution of the amount and coordination environment of aluminum in zeolite materials with 3D scanning transmission X-ray microscopy (STXM). For this purpose, we have focused on two showcase samples involving the in

  10. Computed X-ray powder diffraction patterns for ultrasmall zeolite crystals

    Theoretical X-ray diffraction patterns have been calculated for powders of very small faujasite (FAU) and ZSM-5 (MFI) crystallites. These calculated patterns give the first realistic picture of the expected appearance of X-ray powder diffraction patterns of ultrasmall crystals of these well known commercial zeolites. The X-ray patterns were calculated using SKIP -small-crystal interference program - a program originally written to assist in the interpretation of X-ray diffraction patterns of synthetic zeolites and layered materials. The results are somewhat surprising in that they suggest that the crystallite size of faujasite must fall to below 4-5 unit cells before the resulting pattern diverges significantly from the asymptotic pattern. In contrast, the calculated X-ray pattern of ten-unit-cell ZSM-5 crystallites is scarcely recognizable. (orig.)

  11. Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; Lima, Enju; Marchesini, Stefano; Miao, Huijie; Neiman, Aaron M.; Shapiro, David; Steinbrener, Jan; Stewart, Andrew; Turner, Joshua J.; Jacobsen, Chris

    2009-01-01

    We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below −170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstr...

  12. Characterization of diffraction gratings by use of a tabletop soft-x-ray laser

    We have demonstrated the use of a high-repetition-rate 46.9-mm tabletop laser to characterize diffraction gratings designed for grazing-incidence operation in the soft-x-ray spectral region. The efficiencies for various diffraction orders were measured as a function of angle of incidence and compared with the results of model simulations. This measurement technique provides benchmarks with which to improve electromagnetic codes used in the design of soft-x-ray diffraction gratings. The results illustrate the potential of compact tabletop soft-x-ray lasers for use as a new tool for characterization of short-wavelength optics at the manufacturer's site

  13. Temperature-dependent vibrational spectroscopic and X-ray diffraction investigation of nanosized nickel chromite

    Matulková, Irena; Holec, Petr; Němec, Ivan; Kitazawa, Hideaki; Furubayashi, Takao; Vejpravová, Jana

    2015-06-01

    The nanocrystalline nickel chromite (NiCr2O4) with particle size of ∼20 nm was prepared by auto-combustion method. The nanocrystals were characterized by powder X-ray diffraction, vibrational spectroscopy and magnetic measurements. The expected structural phase transitions (cubic-tetragonal-orthorhombic) were studied by methods of temperature-dependent X-ray powder diffraction and vibrational spectroscopy. The evolution of the Raman spectra and X-ray diffraction patterns collected from 350 K down to 4 K confirmed the cubic-to-tetragonal distortion at ∼250 K, whereas the tetragonal-to-orthorhombic transition was not confirmed in the nanocrystalline sample.

  14. Review - X-ray diffraction measurements in high magnetic fields and at high temperatures

    Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

    2009-01-01

    Full Text Available A system was developed measuring x-ray powder diffraction in high magnetic fields up to 5 T and at temperatures from 283 to 473 K. The stability of the temperature is within 1 K over 6 h. In order to examine the ability of the system, the high-field x-ray diffraction measurements were carried out for Si and a Ni-based ferromagnetic shape-memory alloy. The results show that the x-ray powder diffraction measurements in high magnetic fields and at high temperatures are useful for materials research.

  15. X-ray Diffraction Study of Single-base Propellant Ageing

    2001-01-01

    Ageing of single-base propellants, extending over a storage period of more than 50 years, was investigated by X-ray diffraction analysis. X-ray degree of crystallinity and interplanar spacing were determined. Analysed was the effect of nitrogen content, degree of substitution (DOS) and diphenylamine (DPA) content on structural changes in propellants.

  16. On the theory of time-resolved x-ray diffraction

    Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2008-01-01

    We derive the basic theoretical formulation for X-ray diffraction with pulsed fields, using a fully quantized description of light and matter. Relevant time scales are discussed for coherent as well as incoherent X-ray pulses, and we provide expressions to be used for calculation...

  17. Influence of conversion material morphology on electrochemistry studied with operando X-ray tomography and diffraction.

    Villevieille, Claire; Ebner, Martin; Gómez-Cámer, Juan Luis; Marone, Federica; Novák, Petr; Wood, Vanessa

    2015-03-11

    X-ray diffraction and X-ray tomography are performed on intermetallic particles undergoing lithiation in a porous electrode. Differences between ensemble phase evolution and that at a single-particle level are explored. It is found that all particles evidence core-shell lithiation; however, particles with internal porosity are more mechanically robust and exhibit less fracture. PMID:25619158

  18. Microprocessor-based system for automatic X-ray diffraction and fluorescence

    A data acquisition and processing device appropriate for X-ray analysis and goniometer control was built. The Z-80 based system as well as the whole architeture is described. The advantages and new possibilities of the automated instrument as compared to the traditional ones are listed. The X-ray diffraction and fluorescence techniques can take advantage of the automation. (Author)

  19. The x-ray diffraction pattern and deformation texture of beeswax

    The x-ray diffraction pattern of beeswax shows paraffin-like spacings which have been attributed to monoesters, and long spacings which have been attributed to diesters and hydrocarbons. The d-values and line intensities are given. Optical and x-ray observations of deformed specimens indicate that the molecular axes tend to lie perpendicular to the direction of elongation

  20. Electrochemical discharge of nanocrystalline magnetite: structure analysis using X-ray diffraction and X-ray absorption spectroscopy.

    Menard, Melissa C; Takeuchi, Kenneth J; Marschilok, Amy C; Takeuchi, Esther S

    2013-11-14

    Magnetite (Fe3O4) is an abundant, low cost, environmentally benign material with potential application in batteries. Recently, low temperature coprecipitation methods have enabled preparation of a series of nanocrystalline magnetite samples with a range of crystallite sizes. Electrochemical cells based on Li/Fe3O4 show a linear increase in capacity with decreasing crystallite size at voltages ≥1.2 V where a 2× capacity improvement relative to commercial (26.2 nm) magnetite is observed. In this report, a combination of X-ray powder diffraction (XRD) and X-ray absorption spectroscopy (XAS) is used to measure magnetite structural changes occurring upon electrochemical reduction, with parent Fe3O4 crystallite size as a variable. Notably, XAS provides evidence of metallic iron formation at high levels of electrochemical reduction. PMID:24077019

  1. Analysis of a 3D imaging device by reconstruction from cone beam X ray radiographs

    The aim of our study is to analyse the principle of a 3D imaging device which attempts to restore the local density on a cuberill from a set of digital radiographs taken around the object. We have to use a ponctual radiation source to localize the acquisition lines. Therefore the attenuation measurements are modelled by the cone beam X ray transform. In the analysis of the inverse problem, we work out two inversion diagrams which compute the original function, the image of the object, by a sequence of transforms. The theoretical and algorithmical difficulty comes from the fact that, even in the simple case of a circular acquisition trajectory, the cone-shaped geometry prohibits splitting the problem into a superposition of reconstructions in two dimensions. We describe a novel theoretical framework based on the Radon transform. In this new representation space, it becomes possible by a rebinning operation to redistribute the integral values associated to planes from the coordinates system linked to source positions to the spherical coordinates system of the domain. To ensure this shift of space, we have established two formulas, the first approximate but leading to faster processing, related to the Radon transform, the second exact, related to the first derivative of the Radon transform. The inversion of these transforms completes the reconstruction. We state a theorem where we present the hypothesis under which the exact diagram does restore the original function. These are not verified for a circular trajectory, owing to a shadow zone in the Radon domain associated to the planes which intersect the object but not the trajectory. We propose either to restore the missing information or to use an oscillating trajectory

  2. Fully 3D-Integrated Pixel Detectors for X-Rays

    Deptuch, Grzegorz W. [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Gabriella, Carini [SLAC National Accelerator Lab., Menlo Park, CA (United States); Enquist, Paul [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Grybos, Pawel [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Holm, Scott [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Lipton, Ronald [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Maj, Piotr [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Patti, Robert [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Siddons, David Peter [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Szczygiel, Robert [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States); Yarema, Raymond [Fermi National Accelerator Lab. (FNAL), Batavia, IL (United States)

    2016-01-01

    The vertically integrated photon imaging chip (VIPIC1) pixel detector is a stack consisting of a 500-μm-thick silicon sensor, a two-tier 34-μm-thick integrated circuit, and a host printed circuit board (PCB). The integrated circuit tiers were bonded using the direct bonding technology with copper, and each tier features 1-μm-diameter through-silicon vias that were used for connections to the sensor on one side, and to the host PCB on the other side. The 80-μm-pixel-pitch sensor was the direct bonding technology with nickel bonded to the integrated circuit. The stack was mounted on the board using Sn–Pb balls placed on a 320-μm pitch, yielding an entirely wire-bond-less structure. The analog front-end features a pulse response peaking at below 250 ns, and the power consumption per pixel is 25 μW. We successful completed the 3-D integration and have reported here. Additionally, all pixels in the matrix of 64 × 64 pixels were responding on well-bonded devices. Correct operation of the sparsified readout, allowing a single 153-ns bunch timing resolution, was confirmed in the tests on a synchrotron beam of 10-keV X-rays. An equivalent noise charge of 36.2 e- rms and a conversion gain of 69.5 μV/e- with 2.6 e- rms and 2.7 μV/e- rms pixel-to-pixel variations, respectively, were measured.

  3. Ultrafast structural dynamics studied by kilohertz time-resolved x-ray diffraction

    郭鑫; 江舟亚; 陈龙; 陈黎明; 辛建国; 陈洁

    2015-01-01

    Ultrashort multi-keV x-ray pulses are generated by electron plasma produced by the irradiation of femtosecond pulses on metals. These sub-picosecond x-ray pulses have extended the field of x-ray spectroscopy into the femtosecond time domain. However, pulse-to-pulse instability and long data acquisition time restrict the application of ultrashort x-ray systems operating at low repetition rates. Here we report on the performance of a femtosecond laser plasma-induced hard x-ray source that operates at 1-kHz repetition rate, and provides a flux of 2.0 × 1010 photons/s of Cu Kα radiation. Using this system for time-resolved x-ray diffraction experiments, we record in real time, the transient processes and structural changes induced by the interaction of 400-nm femtosecond pulse with the surface of a 200-nm thick Au (111) single crystal.

  4. X-Ray Diffraction Determination of Stresses in Thin Films

    Vreeland, T.; Dommann, A.; Tsai, C.-J.; Nicolet, M-A.

    1988-01-01

    This paper presents the methodology employed in the determination of the stress tensor for thin crystalline films using x-ray rocking curves. Use of the same equipment for the determination of the average stress in poly- or non-crystalline thin films attached to a crystalline substrate is also discussed. In this case the lattice curvature of the substrate is determined by measurement of the shift In the Bragg peak with lateral position in the substrate. Strains in single crystal layers may...

  5. 3D Ultrastructural organization of whole Chlamydomonas reinhardtii cells studied by nanoscale soft x-ray tomography.

    Eric Hummel

    Full Text Available The complex architecture of their structural elements and compartments is a hallmark of eukaryotic cells. The creation of high resolution models of whole cells has been limited by the relatively low resolution of conventional light microscopes and the requirement for ultrathin sections in transmission electron microscopy. We used soft x-ray tomography to study the 3D ultrastructural organization of whole cells of the unicellular green alga Chlamydomonas reinhardtii at unprecedented spatial resolution. Intact frozen hydrated cells were imaged using the natural x-ray absorption contrast of the sample without any staining. We applied different fiducial-based and fiducial-less alignment procedures for the 3D reconstructions. The reconstructed 3D volumes of the cells show features down to 30 nm in size. The whole cell tomograms reveal ultrastructural details such as nuclear envelope membranes, thylakoids, basal apparatus, and flagellar microtubule doublets. In addition, the x-ray tomograms provide quantitative data from the cell architecture. Therefore, nanoscale soft x-ray tomography is a new valuable tool for numerous qualitative and quantitative applications in plant cell biology.

  6. Precision measurement of the $3d \\to 2p$ x-ray energy in kaonic $^4$He

    Okada, S; Bhang, H; Cargnelli, M; Chiba, J; Choi, Seonho; Curceanu, C; Fukuda, Y; Hanaki, T; Hayano, R S; Iio, M; Ishikawa, T; Ishimoto, S; Ishiwatari, T; Itahashi, K; Iwai, M; Iwasaki, M; Juhász, B; Kienle, P; Marton, J; Matsuda, Y; Ohnishi, H; Outa, H; Sato, M; Schmid, P; Suzuki, S; Suzuki, T; Tatsuno, H; Tomono, D; Widmann, E; Yamazaki, T; Yim, H; Zmeskal, J

    2007-01-01

    We have measured the Balmer-series x-rays of kaonic $^4$He atoms using novel large-area silicon drift x-ray detectors in order to study the low-energy $\\bar{K}$-nucleus strong interaction. The energy of the $3d \\to 2p$ transition was determined to be 6467 $\\pm$ 3 (stat) $\\pm$ 2 (syst) eV. The resulting strong-interaction energy-level shift is in agreement with theoretical calculations, thus eliminating a long-standing discrepancy between theory and experiment.

  7. Precision measurement of the 3 d → 2 p x-ray energy in kaonic 4He

    Okada, S.; Beer, G.; Bhang, H.; Cargnelli, M.; Chiba, J.; Choi, Seonho; Curceanu, C.; Fukuda, Y.; Hanaki, T.; Hayano, R. S.; Iio, M.; Ishikawa, T.; Ishimoto, S.; Ishiwatari, T.; Itahashi, K.; Iwai, M.; Iwasaki, M.; Juhász, B.; Kienle, P.; Marton, J.; Matsuda, Y.; Ohnishi, H.; Outa, H.; Sato, M.; Schmid, P.; Suzuki, S.; Suzuki, T.; Tatsuno, H.; Tomono, D.; Widmann, E.; Yamazaki, T.; Yim, H.; Zmeskal, J.

    2007-09-01

    We have measured the Balmer-series x-rays of kaonic 4He atoms using novel large-area silicon drift x-ray detectors in order to study the low-energy Kbar-nucleus strong interaction. The energy of the 3 d → 2 p transition was determined to be 6467 ± 3 (stat) ± 2 (syst) eV. The resulting strong-interaction energy-level shift is in agreement with theoretical calculations, thus eliminating a long-standing discrepancy between theory and experiment.

  8. Precision measurement of the 3d{yields}2p x-ray energy in kaonic {sup 4}He

    Okada, S. [RIKEN Nishina Center, RIKEN, Saitama 351-0198 (Japan)], E-mail: sokada@riken.jp; Beer, G. [Department of Physics and Astronomy, University of Victoria, British Columbia V8W 3P6 (Canada); Bhang, H. [Department of Physics, Seoul National University, Seoul 151-742 (Korea, Republic of); Cargnelli, M. [Stefan Meyer Institut fuer subatomare Physik, Austrian Academy of Sciences, A-1090 Vienna (Austria); Chiba, J. [Department of Physics, Tokyo University of Science, Chiba 278-8510 (Japan); Choi, Seonho [Department of Physics, Seoul National University, Seoul 151-742 (Korea, Republic of); Curceanu, C. [Laboratori Nazionali di Frascati, INFN, I-00044 Frascati (Italy); Fukuda, Y. [Department of Physics, Tokyo Institute of Technology, Tokyo 152-8551 (Japan); Hanaki, T. [Department of Physics, Tokyo University of Science, Chiba 278-8510 (Japan); Hayano, R.S. [Department of Physics, University of Tokyo, Tokyo 113-0033 (Japan); Iio, M. [RIKEN Nishina Center, RIKEN, Saitama 351-0198 (Japan); Ishikawa, T. [Department of Physics, University of Tokyo, Tokyo 113-0033 (Japan); Ishimoto, S. [High Energy Accelerator Research Organization (KEK), Ibaraki 305-0801 (Japan); Ishiwatari, T. [Stefan Meyer Institut fuer subatomare Physik, Austrian Academy of Sciences, A-1090 Vienna (Austria); Itahashi, K. [RIKEN Nishina Center, RIKEN, Saitama 351-0198 (Japan); Iwai, M. [High Energy Accelerator Research Organization (KEK), Ibaraki 305-0801 (Japan); Iwasaki, M. [RIKEN Nishina Center, RIKEN, Saitama 351-0198 (Japan); Department of Physics, Tokyo Institute of Technology, Tokyo 152-8551 (Japan); Juhasz, B. [Stefan Meyer Institut fuer subatomare Physik, Austrian Academy of Sciences, A-1090 Vienna (Austria); Kienle, P. [Stefan Meyer Institut fuer subatomare Physik, Austrian Academy of Sciences, A-1090 Vienna (Austria); Physik Department, Technische Universitaet Muenchen, D-85748 Garching (Germany)] (and others)

    2007-09-27

    We have measured the Balmer-series x-rays of kaonic {sup 4}He atoms using novel large-area silicon drift x-ray detectors in order to study the low-energy K-bar -nucleus strong interaction. The energy of the 3d{yields}2p transition was determined to be 6467{+-}3(stat){+-}2(syst) eV. The resulting strong-interaction energy-level shift is in agreement with theoretical calculations, thus eliminating a long-standing discrepancy between theory and experiment.

  9. Powder Handling Device for X-ray Diffraction Analysis with Minimal Sample Preparation Project

    National Aeronautics and Space Administration — This project consists in developing a Vibrating Powder Handling System for planetary X-Ray Diffraction instruments. The principle of this novel sample handling...

  10. Crystallization and preliminary X-ray diffraction studies of infectious bronchitis virus nonstructural protein 9

    Ma, Yanlin; Chen, Cheng; Wei, Lei; Yang, Qingzhu; Liao, Ming; Li, Xuemei

    2010-01-01

    The gene segment encoding avian infectious bronchitis virus nonstructural protein 9 has been cloned and expressed in Escherichia coli. The protein has been crystallized and the crystals diffracted X-rays to 2.44 Å resolution.

  11. Powder Handling Device for X-ray Diffraction Analysis with Minimal Sample Preparation Project

    National Aeronautics and Space Administration — This project consists of developing a Vibrating Sample Holder (VSH) for planetary X-Ray Diffraction (XRD) instruments. The principle of this novel sample handling...

  12. State-of-the-art and problems of X-ray diffraction analysis of biomacromolecules

    The state-of-the-art of X-ray diffraction studies of biomacromolecules is briefly characterized, and the challenge imposed by science is discussed. These studies are characterized by a wide scope and extensive use. This field of science is of great interest and is developed in many countries. The main purpose is to solve practical problems in medicine consisting in the design of drugs against various diseases. X-ray diffraction analysis of enzymes brought the pharmaceutical industry to a new level, thus allowing the rational design of drugs against formerly untreatable diseases. Modern X-ray diffraction studies of biomacromolecules laid the basis for a new science called structural biology. This method allows one to solve fundamental problems of physical chemistry for a new state of matter existing in living systems. Here, science poses numerous problems in analysis of X-ray diffraction data on biological macromolecules. Many of theses problems are in their infancy

  13. Application of imaging plate to micro-beam X-ray diffraction

    A new type of integrating area detector system with high sensitivity and high spatial resolution was recently developed for diagnostic radiography. In this detector system, a two dimensional X-ray image is temporarily stored as a distribution of F-centers in a photostimulable phosphor screen called the imaging plate (IP). The image in the IP is then read out by measuring the intensity of fluorescence which is stimulated by a focused He-Ne laser beam scanning the surface of the phosphor screen. The residual X-ray image in the IP can be erased simply by exposing it to a large dose of visible light and the IP can be used repeatedly. The detector has 100% detective quantum efficiency for 0-20 keV X-ray, a spatial resolution better than 0.15mm(fwhm), a dynamic range of 105 and no counting rate limitation. The exposure time can be shorten to 1/20-1/60 in comparison with the use of the X-ray film. In this study, we examined the possibility of the IP for the X-ray studies on the mechanical behaviour of materials by using the back-reflection X-ray technique. An exposure time of more than 30 minutes would be required for a conventional high sensitivity X-ray film in the case of αFe(211) diffraction by Cr-Kα X-rays. When the imaging plates were used in place of the film under the same X-ray condition, we could obtain visually similar patterns by exposing the time of less than 90 seconds. These diffraction patterns can be precisely analyzed with the help of the image processing analyzer. We conclude that this detector system is usable in almost the same way as an X-ray film. Especially, this will be more powerful means in the field of micro-beam X-ray diffraction. (author)

  14. The structure of tellurite glass: A combined NMR, neutron diffraction, and x-ray diffraction study

    McLaughlin, J. C.; Tagg, S. L.; Zwanzier, J. W.; Shastri, S. D.; Haeffner, D. R.

    2000-04-04

    Models are presented of sodium tellurite glasses in the composition range (Na{sub 2}0){sub x}-(TeO{sub 2}){sub 1{minus}x}. 0.1 < x < 0.3. The models combine self-consistently data from three different and complementary sources: sodium-23 nuclear magnetic resonance (NMR), neutron diffraction, and x-ray diffraction. The models were generated using the Reverse Monte Carlo algorithm, modified to include NMR data in addition to diffraction data. The presence in the models of all five tellurite polyhedra consistent with the Te{sup +4} oxidation state were found to be necessary to achieve agreement with the data. The distribution of polyhedra among these types varied from a predominance of highly bridged species at low sodium content, to polyhedra with one or zero bridging oxygen at high sodium content. The models indicate that the sodium cations themselves form sodium oxide clusters particularly at the x = 0.2 composition.

  15. Development of a novel apparatus for experiments in soft X-ray diffraction imaging and diffraction tomography

    We report the development of a novel experimental chamber for experiments in soft x-ray diffraction tomography, diffraction imaging of single biological objects, and magnetic speckle imaging. The chamber will allow for acquisition of nearly full three-dimensional diffraction data sets as well as high magnification zone plate images of holograms for the diffraction tomography experiment. (authors)

  16. Dynamical diffraction theory for the parametric X-rays and coherent bremsstrahlung

    Feranchuk, Ilya D.; Lugovskaya, O.; Ulyanenkov, A.

    2005-01-01

    The various mechanisms of X-ray radiation from relativistically charged particles in a crystal are analyzed from a common point of view, based on quantum electrodynamics in a medium. Parametric X-rays (PXR), diffraction radiation (DR) and coherent bremsstrahlung (CB) lead to different contributions to the amplitude of the radiation process but because of their interference they cannot be considered separately in the radiation intensity. The role of the dynamical diffraction effect...

  17. Influence of X-ray Powder Diffraction Instrument Error on Crystalline Structure Analysis

    HUANG Qing-Ming; YU Jian-Chang; WANG Yun-Min; WU Wan-Guo

    2005-01-01

    Standard mica was used to correct the X-ray powder diffraction instrument error and mathematic methods were employed to find the correction equation. By analyzing mullite sample and comparing the corrected and uncorrected analysis results we found the former is obviously more reasonable. So the conclusion is that the X-ray powder diffraction instrument error greatly affects the crystalline structure analysis, and the above method is convenient and effective for the correction of instrument error.

  18. Structural characterization of thin-film cadmium stearate by X-ray diffraction technique

    X-ray diffraction measurement were carried out on thin films of cadmium stearate using an X-ray diffractometer at Unit Tenaga Nuklear. Structure characteristic obtained from the measured diffraction pattern are compared with that of thin films of manganese stearate reported earlier by Pomerantz et. al. Some of the structural similarities (such as inter-planar spacing) and differences (such as the absence of subsidiary peak between Bragg peaks) are found and discussed

  19. Flash X-Ray Diffraction System for Ultrafast Temperature and Phase Transition Measurements

    A novel ultrafast diagnostic for determining bulk temperature and phase transitions for polycrystalline metal objects has been developed. The diagnostic consists of a 38-stage Marx bank with a cable-coupled X-ray diode that produces a 35-ns pulse of mostly 0.71 (angstrom) monochromatic X rays, and a P-43 fluor coupled to a cooled charge-coupled device camera by a coherent fiber-optic bundle for detection of scattered X rays. The X-ray beam is collimated to a 1o divergence in the scattering plane with the combination of a 1.5-mm tungsten pinhole and a 1.5-mm diameter molybdenum anode. The X-ray diode, in a needle-and-washer configuration, is heavily shielded in all directions other than the collimated beam. The X-ray diode has a sealed reentrant system, which allows the X rays to be produced inside a vacuum containment vessel, close to the sample under study. The direct correlation between the solid-state structure and the coherent X-ray diffraction pattern from a metal surface allows an unequivocal determination of a phase transition. This correlation has been tested in the laboratory with samples of indium and tin. For both metals, diffraction lines were observed at temperatures just below the melt temperature, along with background consisting of Compton scattering and sample fluorescence. Upon melt, the diffraction lines were observed to disappear; however, the background from Compton scattering and sample fluorescence remained. Flash X-ray diffraction also enables direct ultrafast measurements of the bulk temperature of the sample under study. According to the Debye-Waller theory, the diffracted line intensity reduces as the temperature of the sample increases. The amplitude of the reduced diffracted signal also depends on the Debye temperature of the sample, the scattering angle of the diffracted X rays, and the X-ray wavelength. The feasibility of using the Debye-Waller theory for flash X-ray diffraction measurements of the bulk temperature is currently being

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

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

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

  1. Neutron and X-ray diffraction from modulated structures

    This thesis describes X-ray and neutron scattering experiments performed on two examples of modulated structures. After an introduction to the subject of modulated structures, the thesis is divided in three parts. A single crystal elastic neutron scattering experiment between 4.2 and 115 Κ has been performed and four-circle X-ray data have been collected at 8 Κ for the monoclinic low-temperature phase of the layered perovskite PAMC. The results from the neutron scattering experiment indicate that magnetoelastic effects influence the ordering of the crystal. The X-ray experiments have made it possible to determine the crystal structure in the low-temperature phase. The superspace group is P21/b(β-30)Os, with β = 1/3. A small-angle neutron scattering experiment has been performed on the magnetic structure of manganese silicide. When a magnetic field is applied, the modulation vectors turn towards the field direction, showing domain growth and diverging peak widths as they approach the field direction. Phase 'A' is established to have the modulation vectors directed perpendicular to the field direction. Cooling in zero field shows increasing peak widths at low temperatures, indicating a lock-in transition below the lowest reached temperature. To be able to analyse the data of the magnetic order in MnSi, and analytical calculation of the three dimensional resolution function for a small-angle neutron scattering spectrometer has been performed. The calculation is done by application of a combination of phase space analysis and Gaussian approximations for the neutron distribution as well as for the transmission functions of the different apertures. A finite mosaic spread of the crystal and finite correlation widths of the Bragg reflections have been included in the cross section. (au) (3 tabs., 48 ills., 100 refs.)

  2. A Bayesian approach to real-time 3D tumor localization via monoscopic x-ray imaging during treatment delivery

    Purpose: Monoscopic x-ray imaging with on-board kV devices is an attractive approach for real-time image guidance in modern radiation therapy such as VMAT or IMRT, but it falls short in providing reliable information along the direction of imaging x-ray. By effectively taking consideration of projection data at prior times and/or angles through a Bayesian formalism, the authors develop an algorithm for real-time and full 3D tumor localization with a single x-ray imager during treatment delivery. Methods: First, a prior probability density function is constructed using the 2D tumor locations on the projection images acquired during patient setup. Whenever an x-ray image is acquired during the treatment delivery, the corresponding 2D tumor location on the imager is used to update the likelihood function. The unresolved third dimension is obtained by maximizing the posterior probability distribution. The algorithm can also be used in a retrospective fashion when all the projection images during the treatment delivery are used for 3D localization purposes. The algorithm does not involve complex optimization of any model parameter and therefore can be used in a ''plug-and-play'' fashion. The authors validated the algorithm using (1) simulated 3D linear and elliptic motion and (2) 3D tumor motion trajectories of a lung and a pancreas patient reproduced by a physical phantom. Continuous kV images were acquired over a full gantry rotation with the Varian TrueBeam on-board imaging system. Three scenarios were considered: fluoroscopic setup, cone beam CT setup, and retrospective analysis. Results: For the simulation study, the RMS 3D localization error is 1.2 and 2.4 mm for the linear and elliptic motions, respectively. For the phantom experiments, the 3D localization error is < 1 mm on average and < 1.5 mm at 95th percentile in the lung and pancreas cases for all three scenarios. The difference in 3D localization error for different scenarios is small and is not

  3. Twin robotic x-ray system for 2D radiographic and 3D cone-beam CT imaging

    Fieselmann, Andreas; Steinbrener, Jan; Jerebko, Anna K.; Voigt, Johannes M.; Scholz, Rosemarie; Ritschl, Ludwig; Mertelmeier, Thomas

    2016-03-01

    In this work, we provide an initial characterization of a novel twin robotic X-ray system. This system is equipped with two motor-driven telescopic arms carrying X-ray tube and flat-panel detector, respectively. 2D radiographs and fluoroscopic image sequences can be obtained from different viewing angles. Projection data for 3D cone-beam CT reconstruction can be acquired during simultaneous movement of the arms along dedicated scanning trajectories. We provide an initial evaluation of the 3D image quality based on phantom scans and clinical images. Furthermore, initial evaluation of patient dose is conducted. The results show that the system delivers high image quality for a range of medical applications. In particular, high spatial resolution enables adequate visualization of bone structures. This system allows 3D X-ray scanning of patients in standing and weight-bearing position. It could enable new 2D/3D imaging workflows in musculoskeletal imaging and improve diagnosis of musculoskeletal disorders.

  4. X-ray and Neutron Diffraction in the Study of Organic Crystalline Hydrates

    Katharina Fucke

    2010-07-01

    Full Text Available A review. Diffraction methods are a powerful tool to investigate the crystal structure of organic compounds in general and their hydrates in particular. The laboratory standard technique of single crystal X-ray diffraction gives information about the molecular conformation, packing and hydrogen bonding in the crystal structure, while powder X-ray diffraction on bulk material can trace hydration/dehydration processes and phase transitions under non-ambient conditions. Neutron diffraction is a valuable complementary technique to X-ray diffraction and gives highly accurate hydrogen atom positions due to the interaction of the radiation with the atomic nuclei. Although not yet often applied to organic hydrates, neutron single crystal and neutron powder diffraction give precise structural data on hydrogen bonding networks which will help explain why hydrates form in the first place.

  5. X-ray diffraction study of surface-layer structure in parallel grazing rays

    An x-ray diffraction method is described for study of thin polycrystalline and amorphous films and surface layers in an extremely asymmetrical diffraction system in parallel grazing rays using a DRON-3.0 diffractometer. The minimum grazing angles correspond to diffraction under conditions of total external reflection and a layer depth of ∼ 2.5-8 nm

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

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

    2007-06-26

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

  7. Phase and intensity control through diffractive optical elements in X-ray microscopy

    Diffractive optics now plays a major role in optical systems for the extreme ultraviolet and X-ray region. For example, zone plates in their different appearances are widely used for focusing X-rays, as monochromatizing condenser optics, and for high resolution imaging, particularly in X-ray microscopy. The idea in this paper is based upon a more general approach to solve optical problems by transforming a given light distribution or wave as input into the desired waveform on the output of a single X-ray optical component. In this paper we present the design, fabrication and use of novel phase diffractive optical elements (DOEs) that, besides simple focusing, can perform new optical functions in the range of X-rays. Using our own code, we calculated and fabricated through e-beam and X-ray lithography high-resolution DOEs that can generate a constant intensity on a plane (top-hat DOE) or focus a monochromatic X-ray beam into multiple spots. The possibility to introduce a specified phase shift between the generated spots, which can increase the image contrast, is demonstrated by experimental results obtained from computer simulations and experiments performed between 3 and 7.2 keV in both full-field and scanning X-ray microscopy at the ID21 beamline of the European Synchrotron Radiation Facility (ESRF)

  8. 3D-CT imaging using characteristic X-rays and visible lights produced by ion micro-beam bombardment

    Ishii, K.; Matsuyama, S.; Yamazaki, H.; Watanabe, Y.; Kawamura, Y.; Yamaguchi, T.; Momose, G.; Kikuchi, Y.; Terakawa, A.; Galster, W.

    2006-08-01

    We improved the spatial resolution of a 3D-CT imaging system consisting of a micro-beam and an X-ray CCD camera of 1 mega pixels (Hamamatsu photonics C8800X), whose element size is 8 μm × 8 μm providing an image size of 8 mm × 8 mm. A small ant of ∼6 mm body length was placed in a small tube, rotated by a stepping motor, and a spatial resolution of 4 μm for X-ray micron-CT using characteristic Ti-K-X-rays (4.558 keV) produced by 3 MeV proton micro-beams was obtained. We applied the X-ray micron-CT to a small ant's head and obtained the fine structures of the head's interior. Because the CCD is sensitive to visible light, we also examined the capability of light micron-CT using visible red light from an Al2O3(Cr) ruby scintillator and applied the micron-CT to a small red tick. Though the red tick is highly transparent to Ti-K-X-rays, visible red light does not penetrate through the red tick. The most serious problem was dispersion of lights due to Thomson scattering resulting in obscure projection images.

  9. Phase Sensitive X-Ray Diffraction Imaging Study of Protein Crystals

    Hu, Z. W.

    2003-01-01

    The study of defects and growth of protein crystals is of importance in providing a fundamental understanding of this important category of systems and the rationale for crystallization of better ordered crystals for structural determination and drug design. Yet, as a result of the extremely weak scattering power of x-rays in protein and other biological macromolecular crystals, the extinction lengths for those crystals are extremely large and, roughly speaking, of the order of millimeters on average compared to the scale of micrometers for most small molecular crystals. This has significant implication for x-ray diffraction and imaging study of protein crystals, and presents an interesting challenge to currently available x-ray analytical techniques. We proposed that coherence-based phase sensitive x-ray diffraction imaging could provide a way to augment defect contrast in x-ray diffraction images of weakly diffracting biological macromolecular crystals. I shall examine the principles and ideas behind this approach and compare it to other available x-ray topography and diffraction methods. I shall then present some recent experimental results in two model protein systems-cubic apofemtin and tetragonal lysozyme crystals to demonstrate the capability of the coherence-based imaging method in mapping point defects, dislocations, and the degree of perfection of biological macromolecular crystals with extreme sensitivity. While further work is under way, it is intended to show that the observed new features have yielded important information on protein crystal perfection and nucleation and growth mechanism otherwise unobtainable.

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

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  11. Application of high magnification to 3D x-ray computed tomography

    A system was previously described for direct three-dimensional x-ray computed tomography which embodies both a means of performing reconstruction from cone-beam projection data and a means of acquiring such data. After replacing the microfocus source the system resolution under standard conditions is now determined primarily by the spatial resolution of the x-ray image intensifier which serves as the two dimensional detector. To more fully exploit the potential of the x-ray source and to bypass the limits of the detection system the use of high geometric magnification was explored. Initial findings are presented for both a conventional full-field configuration and a configuration in which only a limited volume of a sample can be reconstructed. The results indicate the utility of combining aspects of microradiography with those of computed tomography

  12. Applications of synchrotron x-ray diffraction topography to fractography

    Fractographs have been taken using a variety of probes each of which produces different types of information. Methods which have been used to examine fracture surfaces include: (a) optical microscopy, particularly interference contrast methods, (b) scanning electron microscopy (SEM), (c) SEM with electron channelling, (d) SEM with selected-area electron channelling, (e) Berg-Barrett (B-B) topography, and now (f) synchrotron x-radiation fractography (SXRF). This review concentrated on the role that x-ray methods can play in such studies. In particular, the ability to nondestructively assess the subsurface microstructure associated with the fracture to depths of the order of 5 to 10 μm becomes an important attribute for observations of a large class of semi-brittle metals, semiconductors and ceramics

  13. 3D Ultrastructural Organization of Whole Chlamydomonas reinhardtii Cells Studied by Nanoscale Soft X-Ray Tomography

    Hummel, Eric; Guttmann, Peter; Werner, Stephan; Tarek, Basel; SCHNEIDER, Gerd; Kunz, Michael; Frangakis, Achilleas S.; Westermann, Benedikt

    2012-01-01

    The complex architecture of their structural elements and compartments is a hallmark of eukaryotic cells. The creation of high resolution models of whole cells has been limited by the relatively low resolution of conventional light microscopes and the requirement for ultrathin sections in transmission electron microscopy. We used soft x-ray tomography to study the 3D ultrastructural organization of whole cells of the unicellular green alga Chlamydomonas reinhardtii at unprecedented spatial re...

  14. 3D ultrastructural organization of whole Chlamydomonas reinhardtii cells studied by nanoscale soft x-ray tomography

    Hummel, Eric; Guttmann, Peter; Werner, Stephan; Tarek, Basel; SCHNEIDER, Gerd; Kunz, Michael; Frangakis, Achilleas S.; Westermann, Benedikt

    2012-01-01

    The complex architecture of their structural elements and compartments is a hallmark of eukaryotic cells. The creation of high resolution models of whole cells has been limited by the relatively low resolution of conventional light microscopes and the requirement for ultrathin sections in transmission electron microscopy. We used soft x-ray tomography to study the 3D ultrastructural organization of whole cells of the unicellular green alga Chlamydomonas reinhardtii at unprecedented spatial re...

  15. Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

    Frank, Matthias [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Carlson, David B. [Univ. of California, Davis, CA (United States); Hunter, Mark [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Williams, Garth J. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Messerschmidt, Marc [Univ. of California, Davis, CA (United States); Zatsepin, Nadia A. [Arizona State Univ., Tempe, AZ (United States); Barty, Anton [Univ. of Hamburg (Germany); Benner, Henry [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Chu, Kaiqin [Center for Biophotonics, Sacramento, CA (United States); Graf, Alexander [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hau-Riege, Stefan [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Kirian, Rick [Univ. of Hamburg (Germany); Padeste, Celestino [Paul Scherrer Inst., Villigen (Switzerland); Pardini, Tommaso [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Pedrini, Bill [Paul Scherrer Inst., Villigen (Switzerland); Segelke, Brent [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Seibert, M. M. [Univ. of California, Davis, CA (United States); Spence, John C. [Arizona State Univ., Tempe, AZ (United States); Tsai, Ching-Ju [Paul Scherrer Inst., Villigen (Switzerland); Lane, Steve M. [Center for Biophotonics, Sacramento, CA (United States); Li, Xiao-Dan [Paul Scherrer Inst., Villigen (Switzerland); Schertler, Gebhard [Paul Scherrer Inst., Villigen (Switzerland); Boutet, Sebastien [Univ. of California, Davis, CA (United States); Coleman, Matthew A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Evans, James E. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Univ. of California, Davis, CA (United States)

    2014-02-28

    Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  16. Precipitation in silicon wafers after high temperature preanneal studied by X-ray diffraction methods

    We have investigated oxygen precipitation in Czochralski silicon wafers focusing on influence of nucleation temperature and high temperature pre-anneal during common three step treatment. Thick Si wafers were studied mainly by x-ray diffraction in Laue transmission geometry using Mo x-ray tube, but were also compared to reciprocal space maps obtained in Bragg reflection geometry. The analysis of measured diffraction scans in Laue geometry was performed by means of Takagi equations and statistical dynamical theory of diffraction. From the simulated Laue diffraction curves we find the size of the individual defect area and the fraction of strain area volume in the wafer. The results obtained from x-ray diffraction were compared to loss of interstitial oxygen according to infrared absorption spectroscopy and the size of SiO2 precipitate core was estimated. These techniques are in agreement with transmission electron microscopy images.

  17. Measurement of grain size of polycrystalline materials with confocal energy dispersive micro-X-ray diffraction technology based on polycapillary X-ray optics

    The confocal energy dispersive micro-X-ray diffraction (EDMXRD) based on polycapillary X-ray optics was used to determine the grain size of polycrystalline materials. The grain size of a metallographic specimen of nickel base alloy was measured by using the confocal EDMXRD. The experimental results demonstrated that the confocal EDMXRD had potential applications in measuring large grain size

  18. Characterization of a 20-nm hard x-ray focus by ptychographic coherent diffractive imaging

    Vila-Comamala, Joan; Diaz, Ana; Guizar-Sicairos, Manuel; Gorelick, Sergey; Guzenko, Vitaliy A.; Karvinen, Petri; Kewish, Cameron M.; Färm, Elina; Ritala, Mikko; Mantion, Alexandre; Bunk, Oliver; Menzel, Andreas; David, Christian

    2011-09-01

    Recent advances in the fabrication of diffractive X-ray optics have boosted hard X-ray microscopy into spatial resolutions of 30 nm and below. Here, we demonstrate the fabrication of zone-doubled Fresnel zone plates for multi-keV photon energies (4-12 keV) with outermost zone widths down to 20 nm. However, the characterization of such elements is not straightforward using conventional methods such as knife edge scans on well-characterized test objects. To overcome this limitation, we have used ptychographic coherent diffractive imaging to characterize a 20 nm-wide X-ray focus produced by a zone-doubled Fresnel zone plate at a photon energy of 6.2 keV. An ordinary scanning transmission X-ray microscope was modified to acquire the ptychographic data from a strongly scattering test object. The ptychographic algorithms allowed for the reconstruction of the image of the test object as well as for the reconstruction of the focused hard X-ray beam waist, with high spatial resolution and dynamic range. This method yields a full description of the focusing performance of the Fresnel zone plate and we demonstrate the usefulness ptychographic coherent diffractive imaging for metrology and alignment of nanofocusing diffractive X-ray lenses.

  19. Measurements of transient electron density distributions by femtosecond X-ray diffraction

    This thesis concerns measurements of transient charge density maps by femtosecond X-ray diffraction. Different X-ray diffraction methods will be considered, particularly with regard to their application in femtosecond X-ray diffraction. The rotation method is commonly used in stationary X-ray diffraction. In the work in hand an X-ray diffraction experiment is demonstrated, which combines the method with ultrafast X-ray pulses. This experiment is the first implementation which makes use of the rotation method to map transient intensities of a multitude of Bragg reflections. As a prototype material Bismuth is used, which previously was studied frequently by femtosecond X-ray diffraction by measuring Bragg reflections successively. The experimental results of the present work are compared with the literature data. In the second part a powder-diffraction experiment will be presented, which is used to study the dynamics of the electron-density distribution on ultrafast time scales. The experiment investigates a transition metal complex after photoexcitation of the metal to ligand charge transfer state. Besides expected results, i. e. the change of the bond length between the metal and the ligand and the transfer of electronic charge from the metal to the ligand, a strong contribution of the anion to the charge transfer was found. Furthermore, the charge transfer has predominantly a cooperative character. That is, the excitation of a single complex causes an alteration of the charge density of several neighboring units. The results show that more than 30 transition-metal complexes and 60 anions contribute to the charge transfer. This collective response is a consequence of the strong coulomb interactions of the densely packed ions.

  20. Automated materials discrimination using 3D dual energy X ray images

    Wang, T W

    2002-01-01

    The ability of a human observer to identify an explosive device concealed in complex arrangements of objects routinely encountered in the 2D x-ray screening of passenger baggage at airports is often problematic. Standard dual-energy x-ray techniques enable colour encoding of the resultant images in terms of organic, inorganic and metal substances. This transmission imaging technique produces colour information computed from a high-energy x-ray signal and a low energy x-ray signal (80keV

  1. Development of a CZT spectroscopic 3D imager prototype for hard X ray astronomy

    Auricchio, N.; Caroli, E.; Basili, A.; Schiavone, F.; Stephen, J. B.; Milano, L.; Benassi, G.; Zambelli, N.; Zappettini, A.; Del Sordo, S.; Moscatelli, F.; Budtz-Jørgensen, Carl; Kuvvetli, Irfan; Curado da Silva, R. M.

    The development of focusing optics based on wide band Laue lenses operating from ∼60 keV up to several hundreds of keV is particularly challenging. This type of hard X-ray or gamma ray optics requires a high performance focal plane detector in order to exploit to the best its intrinsic capabiliti...

  2. 3D nanoscale imaging of biological samples with laboratory-based soft X-ray sources

    Dehlinger, Aurélie; Blechschmidt, Anne; Grötzsch, Daniel; Jung, Robert; Kanngießer, Birgit; Seim, Christian; Stiel, Holger

    2015-09-01

    In microscopy, where the theoretical resolution limit depends on the wavelength of the probing light, radiation in the soft X-ray regime can be used to analyze samples that cannot be resolved with visible light microscopes. In the case of soft X-ray microscopy in the water-window, the energy range of the radiation lies between the absorption edges of carbon (at 284 eV, 4.36 nm) and oxygen (543 eV, 2.34 nm). As a result, carbon-based structures, such as biological samples, posses a strong absorption, whereas e.g. water is more transparent to this radiation. Microscopy in the water-window, therefore, allows the structural investigation of aqueous samples with resolutions of a few tens of nanometers and a penetration depth of up to 10μm. The development of highly brilliant laser-produced plasma-sources has enabled the transfer of Xray microscopy, that was formerly bound to synchrotron sources, to the laboratory, which opens the access of this method to a broader scientific community. The Laboratory Transmission X-ray Microscope at the Berlin Laboratory for innovative X-ray technologies (BLiX) runs with a laser produced nitrogen plasma that emits radiation in the soft X-ray regime. The mentioned high penetration depth can be exploited to analyze biological samples in their natural state and with several projection angles. The obtained tomogram is the key to a more precise and global analysis of samples originating from various fields of life science.

  3. In situ analysis of electrocrystallization process of metal electrodeposition with confocal energy dispersive X-ray diffraction based on polycapillary X-ray optics

    The confocal energy dispersive X-ray diffraction (EDXRD) based on a polycapillary focusing X-ray lens (PFXRL) in excitation channel and a polycapillary parallel X-ray lens (PPXRL) in detection channel was presented to study the electrocrystallization process of metal electrodeposition. The input focal spot of the PPXRL and the output focal spot of the PFXRL was adjusted in a confocal configuration, and only the X-rays from the volume overlapped by the two foci could be accordingly detected by the detector. The experimental results demonstrated the confocal EDXRD could be used to in situ real-time analysis of electrochemical crystal growth process

  4. In situ analysis of electrocrystallization process of metal electrodeposition with confocal energy dispersive X-ray diffraction based on polycapillary X-ray optics

    Li, Fangzuo; Liu, Zhiguo [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Sun, Tianxi, E-mail: stx@bnu.edu.cn [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Yang, Chaolin; Sun, Weiyuan; Sun, Xuepeng [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Ma, Yongzhong [Center for Disease Control and Prevention of Beijing, Beijing 100013 (China); Ding, Xunliang [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

    2015-06-11

    The confocal energy dispersive X-ray diffraction (EDXRD) based on a polycapillary focusing X-ray lens (PFXRL) in excitation channel and a polycapillary parallel X-ray lens (PPXRL) in detection channel was presented to study the electrocrystallization process of metal electrodeposition. The input focal spot of the PPXRL and the output focal spot of the PFXRL was adjusted in a confocal configuration, and only the X-rays from the volume overlapped by the two foci could be accordingly detected by the detector. The experimental results demonstrated the confocal EDXRD could be used to in situ real-time analysis of electrochemical crystal growth process.

  5. A CCD area detector for X-ray diffraction under high pressure for rotating anode source

    Amar Sinha; Alka B Garg; V Vijayakumar; B K Godwal; S K Sikka

    2000-04-01

    Details of a two-dimensional X-ray area detector developed using a charge coupled device, a image intensifier and a fibre optic taper are given. The detector system is especially optimized for angle dispersive X-ray diffraction set up using rotating anode generator as X-ray source. The performance of this detector was tested by successfully carrying out powder X-ray diffraction measurements on various materials such as intermetallics AuIn2, AuGa2, high material Pd and low scatterer adamantane (C10H16) at ambient conditions. Its utility for quick detection of phase transitions at high pressures with diamond anvil cell is demonstrated by reproducing the known pressure induced structural transitions in RbI, KI and a new structural phase transition in AuGa2 above 10 GPa. Various softwares have also been developed to analyze data from this detector.

  6. A cooled avalanche photodiode detector for X-ray magnetic diffraction experiments

    Kishimoto, S; Ito, M

    2001-01-01

    A cooled avalanche photodiode (APD) detector was developed for X-ray magnetic diffraction experiments. A stack of four silicon APDs was cooled down to 243 K by a thermoelectric cooler. The energy widths of 0.89 and 1.55 keV (FWHM) were obtained for 8.05 keV X-rays at 1x10 sup 6 s sup - sup 1 and for 16.53 keV X-rays at 2x10 sup 6 s sup - sup 1 , respectively. Test measurements of X-ray magnetic diffraction were executed using a terbium single crystal and white synchrotron radiation. A peak width of (1 0 3) reflection (5.4 keV) was roughly three times wider than that with a high-purity germanium detector.

  7. New X-Ray Tomography Method Based on the 3D Radon Transform Compatible with Anisotropic Sources

    Vassholz, M.; Koberstein-Schwarz, B.; Ruhlandt, A.; Krenkel, M.; Salditt, T.

    2016-02-01

    In this work, we propose a novel computed tomography (CT) approach for three-dimensional (3D) object reconstruction, based on a generalized tomographic geometry with two-dimensional angular sampling (two angular degrees of freedom). The reconstruction is based on the 3D radon transform and is compatible with anisotropic beam conditions. This allows isotropic 3D imaging with a source, which can be extended along one direction for increased flux, while high resolution is achieved by a small source size only in the orthogonal direction. This novel scheme for analytical CT is demonstrated by numerical simulations and proof-of-concept experiments. In this way high resolution and coherence along a single direction determines the reconstruction quality of the entire 3D data set, opening up, for example, new opportunities to achieve nanoscale resolution and/or phase contrast with low brilliance sources such as laboratory x-ray or neutron sources.

  8. X-ray diffraction studies of NbTe2 single crystal

    Neha Bhatt; Rajiv Vaidya; S G Patel; A R Jani

    2004-02-01

    NbTe2 is a member of transition metal dichalcogenide (TMDC) group. Single crystals of niobium ditelluride (NbTe2) have been grown by a chemical vapour transport technique using iodine as transporting agent. The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size for a number of reflections has been calculated using Scherrer’s formula.

  9. Metal layer Bragg-Fresnel lenses for diffraction focusing of hard x-rays

    A thin-film Bragg-Fresnel lens (BFL) was developed for diffractive focusing of hard x-rays into submicron to nanometer spots for scanning x-ray spectromicroscopy. The lens is made of metal-layer Fresnel zones deposited on an x-ray reflective substrate. The use of a high-density lens structure reduces the thickness of the lens and simplifies the fabrication process. Linear and elliptical lenses made of a 200-nm-thick Au film were fabricated using e-beam lithography and a metal deposition process. The focusing capabilities of the Au layer BFLs were demonstrated at the Advanced Photon Source

  10. The 3D microscopic 'signature' of strain within glacial sediments revealed using X-ray computed microtomography

    Tarplee, Mark F. V.; van der Meer, Jaap J. M.; Davis, Graham R.

    2011-11-01

    sample evidence indicates that complex, polyphase (brittle/ductile) deformation histories are common in such diamictic soft sediments and that the local (micro-scale) environment (composition, structure, shear forces and effective pressure) controls rheology. The sediment void ratio is a key indicator of strain. Three of the samples are tentatively placed at different points on the strain cycle for subglacially deforming soft sediment, based on their void ratio, characteristics and distribution. It has been demonstrated that μCT offers significant potential for elucidating glacial soft sediment kinematics. The ability of the technique to both test a variety of hypotheses pertaining to mechanisms operating within the subglacial environment and evaluate efforts to replicate those processes under controlled, laboratory conditions is therefore discussed along with solutions to the problems encountered within this project. μCT also permits the seamless linking of analytical techniques applied at the hand specimen (mm), micromorphological (μm-mm), scanning electron microscopy and X-ray diffraction/fluorescence (nm-μm) scales and the archiving, duplication and dissemination of sample volumetric 3D data.

  11. Takagi-Taupin Description of X-ray Dynamical Diffraction from Diffractive Optics with Large Numerical Aperture

    Yan, Hanfei; Maser, Jorg; Macrander, Albert; Shen, Qun; Vogt, Stefan; Stephenson, Brian; Kang, Hyon Chol

    2007-01-01

    We present a formalism of x-ray dynamical diffraction from volume diffractive optics with large numerical aperture and high aspect ratio, in an analogy to the Takagi-Taupin equations for strained single crystals. We derive a set of basic equations for dynamical diffraction from volume diffractive optics, which enable us to study the focusing property of these optics with various grating profiles. We study volume diffractive optics that satisfy the Bragg condition to various degrees, namely fl...

  12. Quality experimental and calculated powder x-ray diffraction

    Sullenger, D.B.; Cantrell, J.S.; Beiter, T.A.; Tomlin, D.W.

    1996-08-01

    For several years, we have submitted quality powder XRD patterns to the International Centre for Diffraction Data for inclusion as reference standards in their Powder Diffraction File. The procedure followed is described; examples used are {beta}-UH{sub 3}, {alpha}- BaT{sub 2}, alpha-lithium disilicate ({alpha}-Li{sub 2}Si{sub 2}O{sub 5}), and 2,2`,4,4`,6,6`hexanitroazobenzene-III (HNAB-III).

  13. X-ray, 1H/13C 2D and 3D NMR studies of the structures of davallene and adipedatol, two triterpenes isolated from American Adiantum capillus-veneris

    Two triterpenic compounds Davallene 1 and Adipedatol 2 were isolated from the roots of Mexican Adiantum capillus-veneris (Adiantaceae). The structures of both compounds are discussed on the basis of new 2D and 3D NMR spectroscopic and single crystal X-ray diffraction data. (author)

  14. Device for the characterisation of samples by means of x-ray dispersion or diffraction

    Pons Pons, Ramon

    2011-01-01

    [EN] The invention can be used for the characterisation of samples under controlled environment conditions, such as controlled temperature, pressure, humidity, or in an oxidising, inert, reducing atmosphere, etc., by means of X-ray diffraction/dispersion without requiring the use of specially-adapted sample-holders (6). The device comprises an X-ray source (2), a focusing collimator (3) and a detector (4). The device also comprises two compartments (7) under vacuum, which define a cavity (5) ...

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

    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 15o during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern

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

    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.

  17. Materials identification using a small-scale pixellated x-ray diffraction system

    O’Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

    2016-05-01

    A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

  18. The discovery of X-ray diffraction by crystals and its great impact on science

    In April 1912, Friedrich, Knipping and Laue discovered X-ray diffraction in a CuSO4 crystal. Later, Laue derived the famous Laue equations which explain the diffraction phenomenon. For this, Laue was awarded a Nobel Prize for Physics in 1914. In 1912 W. H. Bragg and W. L. Bragg received news of Laue 's discovery, and from X-ray diffraction experiments in a ZnS crystal they derived the famous Bragg equation. For this work, father and son were together awarded the Nobel Prize for Physics in 1915, To commemorate the 100th anniversary of the discovery of X-ray diffraction, this article reviews the important contributions of the early pioneers and their historic impact on science and technology worldwide. (author)

  19. X-ray diffraction from intact tau aggregates in human brain tissue

    Landahl, Eric C.; Antipova, Olga; Bongaarts, Angela; Barrea, Raul; Berry, Robert; Binder, Lester I.; Irving, Thomas; Orgel, Joseph; Vana, Laurel; Rice, Sarah E.

    2011-09-01

    We describe an instrument to record X-ray diffraction patterns from diseased regions of human brain tissue by combining an in-line visible light fluorescence microscope with an X-ray diffraction microprobe. We use thiazine red fluorescence to specifically label and detect the filamentous tau protein pathology associated with Pick's disease, as several laboratories have done previously. We demonstrate that thiazine red-enhanced regions within the tissue show periodic structure in X-ray diffraction, which is not observed in healthy tissue. One observed periodicity (4.2 Å) is characteristic of cross-beta sheet structure, consistent with previous results from powder diffraction studies performed on purified, dried tau protein.

  20. X-ray diffraction from intact tau aggregates in human brain tissue

    Landahl, Eric C. [DePaul University, Department of Physics, 2219 N. Kenmore Ave., IL 60614, Chicago (United States); Antipova, Olga [Illinois Institute of Technology, Department of Biological Chemical and Physical Sciences, 3101 South Dearborn St., IL 60616, Chicago (United States); Bongaarts, Angela [Northwestern University, Department of Cell and Molecular Biology, 303 E. Chicago Ave., IL 60611, Chicago (United States); Barrea, Raul [Illinois Institute of Technology, Department of Biological Chemical and Physical Sciences, 3101 South Dearborn St., IL 60616, Chicago (United States); Berry, Robert; Binder, Lester I. [Northwestern University, Department of Cell and Molecular Biology, 303 E. Chicago Ave., IL 60611, Chicago (United States); Irving, Thomas; Orgel, Joseph [Illinois Institute of Technology, Department of Biological Chemical and Physical Sciences, 3101 South Dearborn St., IL 60616, Chicago (United States); Vana, Laurel [Northwestern University, Department of Cell and Molecular Biology, 303 E. Chicago Ave., IL 60611, Chicago (United States); Rice, Sarah E., E-mail: s-rice@northwestern.edu [Northwestern University, Department of Cell and Molecular Biology, 303 E. Chicago Ave., IL 60611, Chicago (United States)

    2011-09-01

    We describe an instrument to record X-ray diffraction patterns from diseased regions of human brain tissue by combining an in-line visible light fluorescence microscope with an X-ray diffraction microprobe. We use thiazine red fluorescence to specifically label and detect the filamentous tau protein pathology associated with Pick's disease, as several laboratories have done previously. We demonstrate that thiazine red-enhanced regions within the tissue show periodic structure in X-ray diffraction, which is not observed in healthy tissue. One observed periodicity (4.2 A) is characteristic of cross-beta sheet structure, consistent with previous results from powder diffraction studies performed on purified, dried tau protein.

  1. X-ray diffraction from intact tau aggregates in human brain tissue

    Landahl, Eric C.; Antipova, Olga; Bongaarts, Angela; Barrea, Raul; Berry, Robert; Binder, Lester I.; Irving, Thomas; Orgel, Joseph; Vana, Laurel; Rice, Sarah E. (DePaul); (IIT); (NWU)

    2011-09-15

    We describe an instrument to record X-ray diffraction patterns from diseased regions of human brain tissue by combining an in-line visible light fluorescence microscope with an X-ray diffraction microprobe. We use thiazine red fluorescence to specifically label and detect the filamentous tau protein pathology associated with Pick's disease, as several laboratories have done previously. We demonstrate that thiazine red-enhanced regions within the tissue show periodic structure in X-ray diffraction, which is not observed in healthy tissue. One observed periodicity (4.2 {angstrom}) is characteristic of cross-beta sheet structure, consistent with previous results from powder diffraction studies performed on purified, dried tau protein.

  2. X-Ray Diffraction and X-Ray Fluorescent Analyses of Prehistoric Pottery Shards from Ulu Kelantan

    Zuliskandar Ramli

    2011-01-01

    Full Text Available Problem statement: X-Ray Diffraction (XRD and X-Ray Fluorescent (XRF were used in order to obtain mineralogical and elemental composition of seven pottery shards that have been unearthed during the excavation at Peraling Cave and Cha Cave in Ulu Kelantan, Malaysia. Approach: Peraling Cave and Cha Cave were prehistoric sites dating from 10, 000 BC which were inhabited by Hoabinhian people and then continuously used by people of Neolithic culture around 3000 BC. Results: Mineralogical and elemental analyses were carried out to determine whether the pottery found in the archaeological sites was locally made or trading items. Several clay samples from rivers in Ulu Kelantan such as Perias River, Chai River, Peralon River, Nenggiri River, Betis River and Jenera River were taken to be analysed. Conclusion/Recommendations: Mineralogical and elemental content of the pottery shards showed that the pottery shards did not originate from the Ulu Kelantan area and one of the samples contained clinochlore mineral. Clinochlore forms from the metamorphic and hydrothermal alterations of other iron and magnesium silicate minerals and is usually found in igneus rock and metamorphic rock formation.

  3. X-ray coherent diffraction interpreted through the fractional Fourier transform

    Le Bolloc' h, D., E-mail: lebolloch@lps.u-psud.fr [Laboratoire de Physique des Solides (CNRS-UMR 8502), Bat. 510, Universite Paris-sud, 91405 Orsay Cedex (France); Pinsolle, E.; Sadoc, J.F. [Laboratoire de Physique des Solides (CNRS-UMR 8502), Bat. 510, Universite Paris-sud, 91405 Orsay Cedex (France)

    2012-06-01

    We propose to use the fractional Fourier transform to deal with diffraction of coherent X-ray beams from the Fresnel to the Fraunhofer regime. We will illustrate the benefits of the approach compared to the Fresnel wave propagation theory from situations commonly encountered in diffraction experiments: the successive diffraction of two objects and coherent diffraction of a periodic modulation as a charge density wave, containing or not a phase shift.

  4. X-ray coherent diffraction interpreted through the fractional Fourier transform

    We propose to use the fractional Fourier transform to deal with diffraction of coherent X-ray beams from the Fresnel to the Fraunhofer regime. We will illustrate the benefits of the approach compared to the Fresnel wave propagation theory from situations commonly encountered in diffraction experiments: the successive diffraction of two objects and coherent diffraction of a periodic modulation as a charge density wave, containing or not a phase shift.

  5. Radiation damage free two-color X-ray ghost diffraction with atomic resolution

    Li, Zheng; Chapman, Henry; Shih, Yanhua

    2015-01-01

    The X-ray free electron lasers (XFEL) can enable diffractive structural determination of protein crystals or single molecules that are too small and radiation-sensitive for conventional X-ray analysis. However the electronic form factor could have been modified during the ultrashort X-ray pulse due to photoionization and electron cascade caused by the intense X-ray pulse. For general X-ray imaging techniques, to minimize radiation damage effect is of major concern to ensure faithful reconstruction of the structure. Here we show that a radiation damage free diffraction can be achieved with an atomic spatial resolution, by using X-ray parametric down-conversion (PDC), and two-color biphoton ghost imaging. We illustrate that formation of the diffractive patterns satisfies a condition analogous to the Bragg equation, with a resolution that could be as fine as the lattice length scale of several Angstrom. Because the samples are illuminated by the optical photons of low energy, they can be free of radiation damage...

  6. X-ray diffraction investigation of the sulphur induced 4x1 reconstruction of Ni(110)

    Foss, M.; Feidenhans'l, R.; Nielsen, M.; Findeisen, E.; Buslaps, T.; Johnson, R.L.; Besenbacher, F.; Stensgaard, I.

    1993-01-01

    The atomic structure of the Ni(110)4 x 1-S reconstruction has been determined on the basis of surface X-ray diffraction measurements. An analysis of the in-plane diffraction data shows that the model consists of Ni rows along the [001] direction, two for every 4 x 1 unit cell, corresponding to 0...

  7. Titration of a Solid Acid Monitored by X-Ray Diffraction

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

    An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

  8. X-ray Coherent diffraction interpreted through the fractional Fourier transform

    Bolloc'h, David Le; Sadoc, Jean-Francois

    2011-01-01

    Diffraction of coherent x-ray beams is treated through the Fractionnal Fourier transform. The transformation allow us to deal with coherent diffraction experiments from the Fresnel to the Fraunhofer regime. The analogy with the Huygens-Fresnel theory is first discussed and a generalized uncertainty principle is introduced.

  9. Serial femtosecond X-ray diffraction of 30S ribosomal subunit microcrystals in liquid suspension at ambient temperature using an X-ray free-electron laser

    Serial femtosecond X-ray (SFX) diffraction extending beyond 6 Å resolution using T. thermophilus 30S ribosomal subunit crystals is reported. High-resolution ribosome structures determined by X-ray crystallography have provided important insights into the mechanism of translation. Such studies have thus far relied on large ribosome crystals kept at cryogenic temperatures to reduce radiation damage. Here, the application of serial femtosecond X-ray crystallography (SFX) using an X-ray free-electron laser (XFEL) to obtain diffraction data from ribosome microcrystals in liquid suspension at ambient temperature is described. 30S ribosomal subunit microcrystals diffracted to beyond 6 Å resolution, demonstrating the feasibility of using SFX for ribosome structural studies. The ability to collect diffraction data at near-physiological temperatures promises to provide fundamental insights into the structural dynamics of the ribosome and its functional complexes

  10. Reservoir core porosity in the Resende formation using 3D high-resolution X-ray computed microtomography

    The storage capacity and production of oil are influenced, among other things, by rocks and fluids characteristics. Porosity is one of the most important characteristics to be analyzed in oil industry, mainly in oil prospection because it represents the direct capacity of storage fluids in the rocks. By definition, porosity is the ratio of pore volume to the total bulk volume of the formation, expressed in percentage, being able to be absolute or effective. The aim of this study was to calculate porosity by 3D High-Resolution X-ray Computed Microtomography using core plugs from Resende Formation which were collected in Porto Real, Rio de Janeiro State. This formation is characterized by sandstones and fine conglomerates with associated fine siliciclastic sediments, and the paleoenviroment is interpreted as a braided fluvial system. For acquisitions data, it was used a 3D high resolution microtomography system which has a microfocus X-ray tube (spot size < 5μm) and a 12-bit cooled X-ray camera (CCD fiber-optically coupled to a scintillator) operated at 100 kV and 100 μA. Twenty-two samples taken at different depths from two boreholes were analyzed. A total of 961 slices were performed with a resolution of 14.9 μm. The results demonstrated that μ-CT is a reliable and effective technique. Through the images and data it was possible to quantify the porosity and to view the size and shape of porous. (author)

  11. Analysis of the KROTOS KFC test by coupling X-Ray image analysis and MC3D calculations

    During a hypothetical severe accident sequence in a Pressurized Water Reactor (PWR), the hot molten materials (corium) issuing from the degraded reactor core may generate a steam explosion if they come in contact with water and may damage the structures and threaten the reactor integrity. The SERENA program is an international OECD project that aims at helping the understanding of this phenomenon also called Fuel Coolant Interaction (FCI) by providing data. CEA takes part in this program by performing tests in its KROTOS facility where steam explosions using prototypic corium can be triggered. Data about the different phases in the premixing are extracted from the KROTOS X-Ray radioscopy images by using KIWI software (KROTOS Image analysis of Water-corium Interaction) currently developed by CEA. The MC3D code, developed by IRSN, is a thermal-hydraulic multiphase code mainly dedicated to FCI studies. It is composed of two applications: premixing and explosion. An overall FCI calculation with MC3D requires a premixing calculation followed by an explosion calculation. The present paper proposes an alternative approach in which all the features of the premixing are extracted from the X-Ray pictures using the KIWI software and transferred to an MC3D dataset for a direct simulation of the explosion. The main hypothesis are discussed as well as the first explosion results obtained with MC3D for the KROTOS KFC test. These results are rather encouraging and are analyzed on the basis of comparisons with the experimental data. (authors)

  12. Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

    Liu, Yifei; Manjubala, Inderchand; Roschger, Paul; Schell, Hanna; Duda, Georg N.; Fratzl, Peter

    2010-10-01

    Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

  13. Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

    Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

  14. Analysis of the KROTOS KFC test by coupling X-Ray image analysis and MC3D calculations

    Brayer, C.; Charton, A.; Grishchenko, D.; Fouquart, P.; Bullado, Y.; Compagnon, F.; Correggio, P.; Cassiaut-Louis, N.; Piluso, P. [Commissariat a l' Energie Atomique et Aux Energies Alternatives, CEA Cadarache, DEN, F-13108 Saint-Paul-Les-Durance (France)

    2012-07-01

    During a hypothetical severe accident sequence in a Pressurized Water Reactor (PWR), the hot molten materials (corium) issuing from the degraded reactor core may generate a steam explosion if they come in contact with water and may damage the structures and threaten the reactor integrity. The SERENA program is an international OECD project that aims at helping the understanding of this phenomenon also called Fuel Coolant Interaction (FCI) by providing data. CEA takes part in this program by performing tests in its KROTOS facility where steam explosions using prototypic corium can be triggered. Data about the different phases in the premixing are extracted from the KROTOS X-Ray radioscopy images by using KIWI software (KROTOS Image analysis of Water-corium Interaction) currently developed by CEA. The MC3D code, developed by IRSN, is a thermal-hydraulic multiphase code mainly dedicated to FCI studies. It is composed of two applications: premixing and explosion. An overall FCI calculation with MC3D requires a premixing calculation followed by an explosion calculation. The present paper proposes an alternative approach in which all the features of the premixing are extracted from the X-Ray pictures using the KIWI software and transferred to an MC3D dataset for a direct simulation of the explosion. The main hypothesis are discussed as well as the first explosion results obtained with MC3D for the KROTOS KFC test. These results are rather encouraging and are analyzed on the basis of comparisons with the experimental data. (authors)

  15. Methodology toward 3D micro X-ray fluorescence imaging using an energy dispersive charge-coupled device detector.

    Garrevoet, Jan; Vekemans, Bart; Tack, Pieter; De Samber, Björn; Schmitz, Sylvia; Brenker, Frank E; Falkenberg, Gerald; Vincze, Laszlo

    2014-12-01

    A new three-dimensional (3D) micro X-ray fluorescence (μXRF) methodology based on a novel 2D energy dispersive CCD detector has been developed and evaluated at the P06 beamline of the Petra-III storage ring (DESY) in Hamburg, Germany. This method is based on the illumination of the investigated sample cross-section by a horizontally focused beam (vertical sheet beam) while fluorescent X-rays are detected perpendicularly to the sheet beam by a 2D energy dispersive (ED) CCD detector allowing the collection of 2D cross-sectional elemental images of a certain depth within the sample, limited only by signal self-absorption effects. 3D elemental information is obtained by a linear scan of the sample in the horizontal direction across the vertically oriented sheet beam and combining the detected cross-sectional images into a 3D elemental distribution data set. Results of the 3D μXRF analysis of mineral inclusions in natural deep Earth diamonds are presented to illustrate this new methodology. PMID:25346101

  16. Structure of drug-target proteins determined by both X-ray and neutron diffraction

    Crystallography enables us to obtain accurate atomic positions within proteins. High resolution X-ray crystallography provides information for most of the atoms comprising a protein, with the exception of hydrogens. Neutron diffraction data can provide information of the location of hydrogen atoms to the structural information determined by X-ray crystallography. Here, we show the recent of the structural determination of drug-target proteins, porcine pancreatic elastase (PPE) and human immuno-deficiency virus type-1 protease (HIV-PR) by both X-ray and neutron diffraction. The structure of porcine pancreatic elastase with its potent inhibitor (FR13080) was determined to 0.94A resolution by X-ray diffraction and 1.75 A resolution by neutron diffraction. It was found that there are two characteristic hydrogen bonding interactions in which hydrogen atoms were confirmed. One is located between a catalytic aspartate and histidine, another is involved in the inhibitor recognition site. The structure of HIV-PR with its potent inhibitor (KNI-272) was also determined to 0.93 A resolution by X-ray diffraction and 2.3 A resolution by neutron diffraction. The ionization state of the catalytic residues were clarified to show that Asp125 is protonated and Asp25 is deprotonated. The ionization state and the location of hydrogen atoms of the catalytic residue in HIV-PR were firstly determined by neutron diffraction. Furthermore, collaborative use of both X-ray and neutron to identify the location of ambiguous hydrogen atoms will be shown. (author)

  17. Automated materials discrimination using 3D dual energy X ray images

    The ability of a human observer to identify an explosive device concealed in complex arrangements of objects routinely encountered in the 2D x-ray screening of passenger baggage at airports is often problematic. Standard dual-energy x-ray techniques enable colour encoding of the resultant images in terms of organic, inorganic and metal substances. This transmission imaging technique produces colour information computed from a high-energy x-ray signal and a low energy x-ray signal (80keVeff ≤ 13) to be automatically discriminated from many layers of overlapping substances. This is achieved by applying a basis materials subtraction technique to the data provided by a wavelet image segmentation algorithm. This imaging technique is reliant upon the image data for the masking substances to be discriminated independently of the target material. Further work investigated the extraction of depth data from stereoscopic images to estimate the mass density of the target material. A binocular stereoscopic dual-energy x-ray machine previously developed by the Vision Systems Group at The Nottingham Trent University in collaboration with The Home Office Science and Technology Group provided the image data for the empirical investigation. This machine utilises a novel linear castellated dual-energy x-ray detector recently developed by the Vision Systems Group. This detector array employs half the number of scintillator-photodiode sensors in comparison to a conventional linear dual-energy sensor. The castellated sensor required the development of an image enhancement algorithm to remove the spatial interlace effect in the resultant images prior to the calibration of the system for materials discrimination. To automate the basis materials subtraction technique a wavelet image segmentation and classification algorithm was developed. This enabled overlapping image structures in the x-rayed baggage to be partitioned. A series of experiments was conducted to investigate the

  18. X-ray diffraction line-profile analysis of nanocatalyst Pt/C

    X-ray diffraction line-profile is closely related with microstructure of crystalline material. Under the assumption that crystallite size and microstrain diffraction line-profiles can be approximated with the Voigt function, the method of X-ray diffraction line-profile analysis, used to determine microstructural information of crystallite size and dislocation, is described in detail. With this procedure, nanocatalyst Pt/C produced by glycol synthesis method is investigated by X-ray diffraction line-profile analysis. The lognormal mean of the sample crystallite size is 0.95 nm, and the lognormal variance is 0.37. The crystallite size distribution from X-ray diffraction line-profile analysis is well consistent with transmission electron microscopy observations. The integral breadths of the sample diffraction line-profiles are compared, anisotropic diffraction line broaden- ing is found. If such a phenomenon is caused by the dislocations of Burgers vector 1/2(110), the value of the dislocation density can be calculated. The results show, whether the dislocation character is screw or edge, the order of the dislocation density is about 1015/m2. (authors)

  19. Finding 3D Teeth Positions by Using 2D Uncalibrated Dental X-ray Images

    Sridhar, Bitra; Prasad, Dandey Venkata

    2010-01-01

    In Dental Radiology very often several radiographs (uncalibrated in position) are taken from the same person. The radiographs do not provide the depth details, and there is often requirement of three dimensional (3D) data to achieve better diagnosis by radiologist. The purpose of this project is a step forward to solve needs of dentists for evaluating the degree of severity of teeth cavities by 3D reconstruction implementing the uncalibrated radiographs. The 3D information retrieval from two ...

  20. Laser-wakefield accelerators as hard x-ray sources for 3D medical imaging of human bone.

    Cole, J M; Wood, J C; Lopes, N C; Poder, K; Abel, R L; Alatabi, S; Bryant, J S J; Jin, A; Kneip, S; Mecseki, K; Symes, D R; Mangles, S P D; Najmudin, Z

    2015-01-01

    A bright μm-sized source of hard synchrotron x-rays (critical energy Ecrit > 30 keV) based on the betatron oscillations of laser wakefield accelerated electrons has been developed. The potential of this source for medical imaging was demonstrated by performing micro-computed tomography of a human femoral trabecular bone sample, allowing full 3D reconstruction to a resolution below 50 μm. The use of a 1 cm long wakefield accelerator means that the length of the beamline (excluding the laser) is dominated by the x-ray imaging distances rather than the electron acceleration distances. The source possesses high peak brightness, which allows each image to be recorded with a single exposure and reduces the time required for a full tomographic scan. These properties make this an interesting laboratory source for many tomographic imaging applications. PMID:26283308

  1. Laser-wakefield accelerators as hard x-ray sources for 3D medical imaging of human bone

    Cole, J. M.; Wood, J. C.; Lopes, N. C.; Poder, K.; Abel, R. L.; Alatabi, S.; Bryant, J. S. J.; Jin, A.; Kneip, S.; Mecseki, K.; Symes, D. R.; Mangles, S. P. D.; Najmudin, Z.

    2015-08-01

    A bright μm-sized source of hard synchrotron x-rays (critical energy Ecrit > 30 keV) based on the betatron oscillations of laser wakefield accelerated electrons has been developed. The potential of this source for medical imaging was demonstrated by performing micro-computed tomography of a human femoral trabecular bone sample, allowing full 3D reconstruction to a resolution below 50 μm. The use of a 1 cm long wakefield accelerator means that the length of the beamline (excluding the laser) is dominated by the x-ray imaging distances rather than the electron acceleration distances. The source possesses high peak brightness, which allows each image to be recorded with a single exposure and reduces the time required for a full tomographic scan. These properties make this an interesting laboratory source for many tomographic imaging applications.

  2. Solid-state /sup 13/C NMR and X-ray diffraction of dermatan sulfate

    Winter, W.T.; Taylor, M.G.; Stevens, E.S.; Morris, E.R.; Rees, D.A.

    1986-05-29

    Dermatan sulfate in the solid state has been studied by /sup 13/C CP/MAS nmr and X-ray diffraction in order to establish the ring conformation of the L-iduronate moiety. The solid state nmr spectrum is similar to the solution spectrum obtained previously, indicating that a ring conformation at least approximating to /sup 1/C/sub 4/ predominates in the solid state. X-ray powder diffraction data from the same sample indicate the presence of the 8-fold helix form previously observed by fiber diffraction, and interpreted in terms of a /sup 4/C/sub 1/ ring form. A likely explanation of the results is that a distorted /sup 1/C/sub 4/ L-iduronate ring conformation, not considered in the initial X-ray analysis, may emerge to provide a satisfactory interpretation of all available physical-chemical data.

  3. Solid-state 13C NMR and X-ray diffraction of dermatan sulfate

    Dermatan sulfate in the solid state has been studied by 13C CP/MAS nmr and X-ray diffraction in order to establish the ring conformation of the L-iduronate moiety. The solid state nmr spectrum is similar to the solution spectrum obtained previously, indicating that a ring conformation at least approximating to 1C4 predominates in the solid state. X-ray powder diffraction data from the same sample indicate the presence of the 8-fold helix form previously observed by fiber diffraction, and interpreted in terms of a 4C1 ring form. A likely explanation of the results is that a distorted 1C4 L-iduronate ring conformation, not considered in the initial X-ray analysis, may emerge to provide a satisfactory interpretation of all available physical-chemical data

  4. Submicron X-Ray Diffraction and its Applications to Problems in Materials and Environmental Science

    The availability of high brilliance 3rd generation synchrotron sources together with progress in achromatic focusing optics allow to add submicron spatial resolution to the conventional century-old X-ray diffraction technique. The new capabilities include the possibility to map in-situ, grain orientations, crystalline phase distribution and full strain/stress tensors at a very local level, by combining white and monochromatic X-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron X-ray diffraction techniques at the ALS, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed

  5. Synchrotron X-ray diffraction analysis for quantitative defect evaluation in GaP/Si nanolayers

    In the context of III–V monolithic integration on silicon, synchrotron X-ray diffraction has been employed in this study using a bi-dimensional large area hybrid pixel detector (XPAD third generation) to characterize defects in the GaP layers. Despite a very coherent interface (low plastic relaxation) of GaP/Si, 2 types of defect are detected. Micro-twins contributions are evidenced and quantitatively evaluated from additional reflections analysis. Antiphase domains are evidenced using the Williamson-Hall-like plot method applied to transverse scans extracted directly from single XPAD images taken on specular GaP reflections. - Highlights: ► Antiphase domain evidence and characterization in GaP/Si using X-ray diffraction ► Microtwin evidence and characterization ► Synchrotron diffraction ► Large area X-ray hybrid pixel detector

  6. Synchrotron X-ray diffraction analysis for quantitative defect evaluation in GaP/Si nanolayers

    Nguyen Thanh, T.; Robert, C. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Létoublon, A., E-mail: Antoine.letoublon@insa-rennes.fr [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Cornet, C. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Quinci, T. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); CEA LCP, INES, 50 av. du Lac Léman, Savoie Technolac, 73375 Le Bourget du Lac (France); Giudicelli, E.; Almosni, S. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Boudet, N. [CRG-D2AM, ESRF and Inst. Néel, CNRS-UJF, 25 Av des Martyrs, 38042 Grenoble (France); Ponchet, A. [CEMES, CNRS, Université de Toulouse, 29 rue J. Marvig BP 94347, 31055 Toulouse Cedex 4 (France); Kuyyalil, J. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Danila, M. [National Institute for Research and Development in Microtechnologies (IMT), 126A Erou Iancu Nicolae Street, 077190, Bucharest (Romania); Durand, O.; Bertru, N.; Le Corre, A. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France)

    2013-08-31

    In the context of III–V monolithic integration on silicon, synchrotron X-ray diffraction has been employed in this study using a bi-dimensional large area hybrid pixel detector (XPAD third generation) to characterize defects in the GaP layers. Despite a very coherent interface (low plastic relaxation) of GaP/Si, 2 types of defect are detected. Micro-twins contributions are evidenced and quantitatively evaluated from additional reflections analysis. Antiphase domains are evidenced using the Williamson-Hall-like plot method applied to transverse scans extracted directly from single XPAD images taken on specular GaP reflections. - Highlights: ► Antiphase domain evidence and characterization in GaP/Si using X-ray diffraction ► Microtwin evidence and characterization ► Synchrotron diffraction ► Large area X-ray hybrid pixel detector.

  7. X-ray diffraction from the ripple structures created by femtosecond laser pulses

    In this paper, we present the investigation and characterization of the laser-induced surface structure on an asymmetrically cut InSb crystal. We describe diffraction from the ripple surface and present a theoretical model that can be used to simulate X-ray energy scans. The asymmetrically cut InSb sample was irradiated with short-pulse radiation centred at 800 nm, with fluences ranging from 10 to 80 mJ/cm2. The irradiated sample surface profile was investigated using optical and atomic force microscopy. We have investigated how laser-induced ripples influence the possibility of studying repetitive melting of solids using X-ray diffraction. The main effects arise from variations in local asymmetry angles, which reduce the attenuation length and increase the X-ray diffraction efficiency. (orig.)

  8. Imaging nanoscale lattice variations by machine learning of x-ray diffraction microscopy data

    Laanait, Nouamane; Zhang, Zhan; Schlepütz, Christian M.

    2016-09-01

    We present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional data cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. We demonstrate this ‘big data’ approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate.

  9. Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

    The software suite SITENNO is developed for processing diffraction data collected in coherent X-ray diffraction imaging experiments of non-crystalline particles using an X-ray free-electron laser. Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles

  10. 3D tumor localization through real-time volumetric x-ray imaging for lung cancer radiotherapy

    Li, Ruijiang; Jia, Xun; Gu, Xuejun; Folkerts, Michael; Men, Chunhua; Song, William Y; Jiang, Steve B

    2011-01-01

    Recently we have developed an algorithm for reconstructing volumetric images and extracting 3D tumor motion information from a single x-ray projection. We have demonstrated its feasibility using a digital respiratory phantom with regular breathing patterns. In this work, we present a detailed description and a comprehensive evaluation of the improved algorithm. The algorithm was improved by incorporating respiratory motion prediction. The accuracy and efficiency were then evaluated on 1) a digital respiratory phantom, 2) a physical respiratory phantom, and 3) five lung cancer patients. These evaluation cases include both regular and irregular breathing patterns that are different from the training dataset. For the digital respiratory phantom with regular and irregular breathing, the average 3D tumor localization error is less than 1 mm. On an NVIDIA Tesla C1060 GPU card, the average computation time for 3D tumor localization from each projection ranges between 0.19 and 0.26 seconds, for both regular and irreg...

  11. Note: Application of a pixel-array area detector to simultaneous single crystal x-ray diffraction and x-ray absorption spectroscopy measurements

    X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam

  12. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  13. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    Shymanovich, U.

    2007-11-13

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  14. Nano-structured titanium and aluminium nitride coatings: Study by grazing incidence X-ray diffraction and X-ray absorption and anomalous diffraction

    Tuilier, M.-H., E-mail: marie-helene.tuilier@uha.fr [Universite de Haute Alsace (UHA), Laboratoire Physique et Mecanique Textile (LPMT), EA 4365 -conventionnee au CNRS, Equipe PPMR, F-68093 Mulhouse (France); Pac, M.-J. [Universite de Haute Alsace (UHA), Laboratoire Physique et Mecanique Textile (LPMT), EA 4365 - conventionnee au CNRS, Equipe PPMR, F-68093 Mulhouse (France); Anokhin, D.V. [Universite de Haute Alsace (UHA), CNRS, Institut de Science des Materiaux de Mulhouse (IS2M), LRC 7228, F-68093 Mulhouse (France); Moscow State University, Faculty of Fundamental Physical and Chemical Engineering, 119991, Moscow, GSP-1, 1-51 Leninskie Gory (Russian Federation); Ivanov, D.A. [Universite de Haute Alsace (UHA), CNRS, Institut de Science des Materiaux de Mulhouse (IS2M), LRC 7228, F-68093 Mulhouse (France); Rousselot, C. [Universite de Franche-Comte, FEMTO-ST (UMR CNRS 6174), F-25211 Montbeliard (France); Thiaudiere, D. [Synchrotron Soleil, Saint Aubin, F-91192 Gif sur Yvette (France)

    2012-12-30

    Titanium and aluminium nitride thin films, Ti{sub 1-x}Al{sub x}N (x = 0, x = 0.5, x = 0.68), deposited by reactive magnetron sputtering on silicon substrates are investigated by combining two different X-ray diffraction experiments carried out using synchrotron radiation. Grazing-incidence X-ray diffraction and Ti K-edge diffraction anomalous near edge structure spectroscopy provide information on the micro- and nano-structure of the films respectively, which play a crucial role in the functionality of coatings. The spectroscopic data of Ti{sub 0.50}Al{sub 0.50}N film show that Ti atoms in crystallized domains and grain boundaries are all in octahedral cubic local order, but their growth mode is quite different. It is found that the crystallized part of the Ti{sub 0.50}Al{sub 0.50}N film has a single-crystalline nature, whereas the TiN one presents a fibrillar microstructure. For Ti{sub 0.32}Al{sub 0.68}N film, grazing-incidence X-ray diffraction provides information on the uniaxial texture along the [001] direction of the hexagonal lattice. A sharp Ti K pre-edge peak is observed in diffraction anomalous near edge spectrum that definitely shows that Ti atoms are incorporated in the hexagonal lattice of those fibrillar domains. Moreover, the difference observed between Ti K-edge diffraction anomalous and X-ray absorption pre-edge regions proves that a significant part of Ti atoms is located in nanocrystallites with cubic symmetry outside of the crystallized domains. - Highlights: Black-Right-Pointing-Pointer We study nano and micro-structures of TiN, Ti{sub 0.50}Al{sub 0.50}N and Ti{sub 0.32}Al{sub 0.68}N films. Black-Right-Pointing-Pointer Anomalous diffraction solves the crystallized part regardless of grain boundaries. Black-Right-Pointing-Pointer TiN microstructure is fibrillar, Ti{sub 0.5}Al{sub 0.5}N presents single crystalline domains. Black-Right-Pointing-Pointer For Ti{sub 0.32}Al{sub 0.68}N, Ti atoms are located in nanocrystallites with cubic symmetry

  15. 3-D surface profile measurements of large x-ray synchrotron radiation mirrors using stitching interferometry

    Stitching interferometry, using small-aperture, high-resolution, phase-measuring interferometry, has been proposed for quite some time now as a metrology technique to obtain 3-dimensional profiles of surfaces of oversized optical components and substrates. The aim of this work is to apply this method to the specific case of long grazing-incidence x-ray mirrors, such as those used in beamlines at synchrotron radiation facilities around the world. Both fabrication and characterization of these mirrors would greatly benefit from this technique because it offers the potential for providing measurements with accuracy and resolution better than those obtained using existing noncontact laser profilers, such as the long trace profiler (LTP). Measurement data can be used as feedback for computer-controlled fabrication processes to correct for possible topography errors. The data can also be used for simulating and predicting mirror performance under realistic conditions. A semiautomated stitching system was built and tested at the X-ray Optics Metrology Laboratory of the Advanced Photon Source at Argonne National Laboratory. The initial objective was to achieve a measurement sensitivity on the order of 1 (micro)rad rms. Preliminary tests on a 1 m-long x-ray mirror showed system repeatability of less than 0.6 (micro)rad rms. This value is comparable to that of a conventional LTP. The measurement accuracy was mostly affected by environmental perturbations and system calibration effects. With a fully automated and improved system (to be built in the near future), we expect to achieve measurement sensitivity on the order of 0.0 (micro)rad rms or better. In this paper, after a brief review of basic principles and general technical difficulties and challenges of the stitching technique, a detailed description of the measurement setup is given and preliminary results obtained with it are analyzed and discussed

  16. Controlled molecules for X-ray diffraction experiments at free-electron lasers

    X-ray diffractive imaging is at the very heart of materials science and has been utilized for decades to solve unknown molecular structures. Nowadays, it serves as the key method of structural biology to solve molecular structures of large biological molecules comprising several thousand or even millions of atoms. However, X-ray diffraction from isolated molecules is very weak. Therefore, the regular and periodic arrangement of a huge number of identical copies of a certain molecule of interest within a crystal lattice has been a necessary condition in order to exploit Bragg diffraction of X-rays. This results in a huge increase in scattered signal and a strongly improved signal-to-noise ratio compared to diffraction from non-crystalline samples. The major bottleneck of structural biology is that many of biologically interesting molecules refuse to form crystals of sufficient size to be used at synchrotron X-ray lightsources. However, novel X-ray free-electron lasers (XFELs), which became operational very recently, promise to address this issue. X-ray pulses provided by XFELs are many orders of magnitude more intense than X-ray pulses from a synchrotron source and at the same time as short as only several tens of femtoseconds. Combined with wavelengths in the nm-pm range, XFELs are well-suited to study ultrafast atomic and molecular dynamics. Additionally, the ultrashort pulses can be utilized to circumvent the damage threshold which set a limit to the incident intensity in X-ray diffraction experiments before. At XFELs, though eventually destroying the investigated sample, no significant sample deterioration happens on the ultrashort timescale of the XFEL pulse and the measured diffraction pattern is due to an (almost) unharmed sample. In the framework of this thesis, the approach of utilizing the highly intense XFEL pulses for X-ray diffraction of weakly-scattering non-crystalline samples was taken to the limit of small isolated molecules. X-ray diffraction was

  17. Controlled molecules for X-ray diffraction experiments at free-electron lasers

    Stern, Stephan

    2013-12-15

    X-ray diffractive imaging is at the very heart of materials science and has been utilized for decades to solve unknown molecular structures. Nowadays, it serves as the key method of structural biology to solve molecular structures of large biological molecules comprising several thousand or even millions of atoms. However, X-ray diffraction from isolated molecules is very weak. Therefore, the regular and periodic arrangement of a huge number of identical copies of a certain molecule of interest within a crystal lattice has been a necessary condition in order to exploit Bragg diffraction of X-rays. This results in a huge increase in scattered signal and a strongly improved signal-to-noise ratio compared to diffraction from non-crystalline samples. The major bottleneck of structural biology is that many of biologically interesting molecules refuse to form crystals of sufficient size to be used at synchrotron X-ray lightsources. However, novel X-ray free-electron lasers (XFELs), which became operational very recently, promise to address this issue. X-ray pulses provided by XFELs are many orders of magnitude more intense than X-ray pulses from a synchrotron source and at the same time as short as only several tens of femtoseconds. Combined with wavelengths in the nm-pm range, XFELs are well-suited to study ultrafast atomic and molecular dynamics. Additionally, the ultrashort pulses can be utilized to circumvent the damage threshold which set a limit to the incident intensity in X-ray diffraction experiments before. At XFELs, though eventually destroying the investigated sample, no significant sample deterioration happens on the ultrashort timescale of the XFEL pulse and the measured diffraction pattern is due to an (almost) unharmed sample. In the framework of this thesis, the approach of utilizing the highly intense XFEL pulses for X-ray diffraction of weakly-scattering non-crystalline samples was taken to the limit of small isolated molecules. X-ray diffraction was

  18. High resolution double-sided diffractive optics for hard X-ray microscopy.

    Mohacsi, Istvan; Vartiainen, Ismo; Guizar-Sicairos, Manuel; Karvinen, Petri; Guzenko, Vitaliy A; Müller, Elisabeth; Färm, Elina; Ritala, Mikko; Kewish, Cameron M; Somogyi, Andrea; David, Christian

    2015-01-26

    The fabrication of high aspect ratio metallic nanostructures is crucial for the production of efficient diffractive X-ray optics in the hard X-ray range. We present a novel method to increase their structure height via the double-sided patterning of the support membrane. In transmission, the two Fresnel zone plates on the two sides of the substrate will act as a single zone plate with added structure height. The presented double-sided zone plates with 30 nm smallest zone width offer up to 9.9% focusing efficiency at 9 keV, that results in a factor of two improvement over their previously demonstrated single-sided counterparts. The increase in efficiency paves the way to speed up X-ray microscopy measurements and allows the more efficient utilization of the flux in full-field X-ray microscopy. PMID:25835837

  19. An X-ray diffractometer using mirage diffraction.

    Fukamachi, Tomoe; Jongsukswat, Sukswat; Ju, Dongying; Negishi, Riichirou; Hirano, Keiichi; Kawamura, Takaaki

    2014-08-01

    Some characteristics are reported of a triple-crystal diffractometer with a (+, -, +) setting of Si(220) using mirage diffraction. The first crystal is flat, while the second and third crystals are bent. Basically, the first crystal is used as a collimator, the second as a monochromator and the third as the sample. The third crystal also works as an analyzer. The advantages of this diffractometer are that its setup is easy, its structure is simple, the divergence angle from the second crystal is small and the energy resolution of the third crystal is high, of the order of sub-meV. PMID:25242911

  20. X-ray grazing incidence diffraction from multilayers

    Tixier, S.; Boeni, P.; Swygenhoven, H. van; Horisberger, M. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Grazing incidence scattering geometries using synchrotron radiation have been applied in order to characterise the roughness profiles and the structural coherence of multilayers. The lateral correlation length of the roughness profiles was evaluated using diffuse reflectivity in the `out of plane` geometry. This type of measurement is the only diffuse reflectivity technique allowing large lateral momentum transfer. It is typically suitable for correlation lengths smaller than 1000 A. The lateral structural coherence length of Ni{sub 3}Al/Ni multilayers as a function of the layer thickness was obtained by grazing incidence diffraction (GID). 3 figs., 1 ref.

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

    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...... 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....

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

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

    1998-01-01

    An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

  3. Positional order in Langmuir monolayers: An X-ray diffraction study

    Kaganer, V.M.; Brezesinski, G.; Möhwald, H.;

    1999-01-01

    The structural phase transition from the hexagonal to a distorted-hexagonal (centered rectangular) phase (the LS-S transition) in Langmuir monolayers of octadecanol is studied in a grazing incidence x-ray diffraction experiment. We find algebraic decay of positional correlations, which suggests...... solid-like order in both phases at the distances accessible in the present x-ray diffraction experiment. The transition is accompanied by strong positional disorder, which is evident from the drastic increase of the exponent eta to values eta>2 close to the transition. Remarkably, on approaching...

  4. Determination of densities from chemical composition and X-Ray diffraction

    X-ray diffraction method applied to retained austenite measurements gives volume per cent results, whereas the same kind of measurement made by Moessbauer Effect gives iron percentages. To compare both results one needs to convert the volume % to weight % or vice-versa. This necessitates, among other things, in determining the densities of the α and #betta# phases in the steel being studied. A method for calculating the densities, based on the application of the definition of density to just one unit cell, using X-ray diffraction and chemical results, are described. (Author)

  5. A Least-Squares Method for Unfolding Convolution Products in X-ray Diffraction Line Profiles

    Yokoyama, Fumiyoshi

    1982-01-01

    A deconvolution method for the X-ray diffraction line profile is proposed, which is based on the conventional least-squares method. The true profile is assumed to be a functional form. The numerical values of parameters of the function assumed are determined so that the calculated profile, which is a convolution of the function and the instrumental profile, has a minimum deviation from the observed one. The method is illustrated by analysis of the X-ray powder diffraction profile of sodium ch...

  6. Transmission diffraction-tomography system using a high-energy X-ray tube.

    Garrity, D J; Jenneson, P M; Crook, R; Vincent, S M

    2010-01-01

    A high-energy bench-top energy dispersive X-ray diffraction (EDXRD) system for 3-dimensional mapping of the crystalline structure and phase transformations in steel is described, for which preliminary data and system development are presented here. The use of precision tungsten slit screens with up to 225 keV X-rays allows for diffraction through samples of 304 L austenitic stainless steel of thickness 3-10 mm, while sample positioning is carried out with a precision goniometer and translation stage system. PMID:19962905

  7. X-Ray diffraction study of carriers and deposited metallic catalysts

    Moroz, Ella M.

    1992-02-01

    The possibilities of applying some X-ray diffraction methods in the study of multicomponent highly disperse systems are examined. Such methods include the method based on the radial distribution of atoms (RDA), full-profile X-ray diffraction analysis (FPA), and the method involving the determination of substructural characteristics (MDSC). Examples of the determination of the structural and substructural characteristics of the most important catalyst carriers as well as deposited and non-deposited metallic catalysts are presented. The bibliography includes 129 references.

  8. Crystallization and preliminary X-ray diffraction study of porcine carboxypeptidase B

    Akparov, V. Kh., E-mail: valery@akparov.ru [Scientific Center of Russian Federation Research Institute for Genetics and Selection of Industrial Microorganisms (Russian Federation); Timofeev, V. I., E-mail: inna@ns.crys.ras.ru; Kuranova, I. P., E-mail: tostars@mail.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2015-05-15

    Crystals of porcine pancreatic carboxypeptidase B have been grown in microgravity by the capillary counter-diffusion method through a gel layer. The X-ray diffraction study showed that the crystals belong to sp. gr. P4{sub 1}2{sub 1}2 and have the following unit-cell parameters: a = b = 79.58 Å, c = 100.51 Å; α = β = γ = 90.00°. The X-ray diffraction data set suitable for the determination of the three-dimensional structure at atomic resolution was collected from one of the grown crystals at the SPring 8 synchrotron facility to 0.98 Å resolution.

  9. Toward atomic resolution diffractive imaging of isolated molecules with x-ray free-electron lasers

    Stern, Stephan; Holmegaard, Lotte; Filsinger, Frank;

    2014-01-01

    We give a detailed account of the theoretical analysis and the experimental results of an x-ray-diffraction experiment on quantum-state selected and strongly laser-aligned gas-phase ensembles of the prototypical large asymmetric rotor molecule 2,5-diiodobenzonitrile, performed at the Linac Coherent...... Light Source [Phys. Rev. Lett. 112, 083002 (2014)]. This experiment is the first step toward coherent diffractive imaging of structures and structural dynamics of isolated molecules at atomic resolution, i. e., picometers and femtoseconds, using x-ray free-electron lasers....

  10. Toward atomic resolution diffractive imaging of isolated molecules with x-ray free-electron lasers

    Stern, Stephan; Filsinger, Frank; Rouzée, Arnaud; Rudenko, Artem; Johnsson, Per; Martin, Andrew V; Barty, Anton; Bostedt, Christoph; Bozek, John D; Coffee, Ryan N; Epp, Sascha; Erk, Benjamin; Foucar, Lutz; Hartmann, Robert; Kimmel, Nils; Kühnel, Kai-Uwe; Maurer, Jochen; Messerschmidt, Marc; Rudek, Benedikt; Starodub, Dmitri G; Thøgersen, Jan; Weidenspointner, Georg; White, Thomas A; Stapelfeldt, Henrik; Rolles, Daniel; Chapman, Henry N; Küpper, Jochen

    2014-01-01

    We give a detailed account of the theoretical analysis and the experimental results of an x-ray-diffraction experiment on quantum-state selected and strongly laser-aligned gas-phase ensembles of the prototypical large asymmetric rotor molecule 2,5-diiodobenzonitrile, performed at the Linac Coherent Light Source [Phys. Rev. Lett. 112, 083002 (2014)]. This experiment is the first step toward coherent diffractive imaging of structures and structural dynamics of isolated molecules at atomic resolution, i. e., picometers and femtoseconds, using x-ray free-electron lasers.

  11. Simulating Picosecond X-ray Diffraction from shocked crystals by Post-processing Molecular Dynamics Calculations

    Kimminau, G; Nagler, B; Higginbotham, A; Murphy, W; Park, N; Hawreliak, J; Kadau, K; Germann, T C; Bringa, E M; Kalantar, D; Lorenzana, H; Remington, B; Wark, J

    2008-06-19

    Calculations of the x-ray diffraction patterns from shocked crystals derived from the results of Non-Equilibrium-Molecular-Dynamics (NEMD) simulations are presented. The atomic coordinates predicted by the NEMD simulations combined with atomic form factors are used to generate a discrete distribution of electron density. A Fast-Fourier-Transform (FFT) of this distribution provides an image of the crystal in reciprocal space, which can be further processed to produce quantitative simulated data for direct comparison with experiments that employ picosecond x-ray diffraction from laser-irradiated crystalline targets.

  12. Nuclear Bragg diffraction of synchrotron x-rays

    In the last few years several groups have successfully carried out experiments involving the excitation of nuclear resonances using synchrotron radiation. All the experiments so far have used 57Fe as the resonant nucleus. The extremely narrow width of the 14.4 keV resonance in 57Fe makes these experiments very difficult at even the highest-brightness synchrotron beam lines currently available, so much effort is being devoted toward improvements in equipment and techniques. The general aim of this work is to use resonant scattering to produce high-flux beams of extremely monochromatic radiation, which can then be used as source beams for a variety of experiments. This talk, however, will stress the kinds of physics questions that can be answered using broad-band synchrotron radiation to induce resonant nuclear diffraction in perfect crystal samples. Experiments of this type are being carried out today, albeit with difficulty, using present synchrotron sources. They will become technically easy when advanced sources such as the APS become available, and it is expected that nuclear Bragg diffraction will become a standard technique

  13. Characterization of an Yb:LuVO 4 single crystal using X-ray topography, high-resolution X-ray diffraction, and X-ray photoelectron spectroscopy

    Paszkowicz, W.; Romanowski, P.; Bąk-Misiuk, J.; Wierzchowski, W.; Wieteska, K.; Graeff, W.; Iwanowski, R. J.; Heinonen, M. H.; Ermakova, O.; Dąbkowska, H.

    2011-10-01

    Knowledge on the defect and electronic structure allows for improved modeling of material properties. A short literature review has shown that the information on defect structure of rare earth orthovanadate single crystals is limited. In this paper, defect and electronic structure of a needle-shaped Yb:LuVO 4 single crystal grown by the slow cooling method have been studied by means of X-ray diffraction topography employing white synchrotron beam, high-resolution diffraction (HRD) and photoelectron spectroscopy (XPS) techniques. Topographic investigations show that the crystal is composed of two blocks disoriented by about 1.5° and separated by a narrow deformed region. Some contrasts observed within the crystal volume may be attributed to glide bands and sector boundaries. The contrasts appearing in the vicinity of the surface may be interpreted as due to the presence of small inclusions. The HRD study indicates, in particular, that among point defects, the vacancy type defects dominate and that the density of other defects is small in comparison. The XPS measurements enabled, despite highly insulating properties of the studied crystal, an analysis of its bulk electronic structure, including the main core-levels (O 1 s, V 2 p, Lu 4 f) as well as the valence band range.

  14. Precision spectroscopy of Kaonic helium-3 and helium-4 3d-->2p X-rays

    Ishiwatari, T.; Bazzi, M.; Bhang, H.; Beer, G.; Bombelli, L.; Bragadireanu, A. M.; Cargnelli, M.; Choi, S.; Corradi, G.; Curceanu, C.; d'Uffizi, A.; Enomoto, S.; Fiorini, C.; Frizzi, T.; Fujioka, H.; Fujiwara, Y.; Ghio, F.; Girolami, B.; Guaraldo, C.; Hashimoto, T.; Hayano, R. S.; Hiraiwa, T.; Iio, M.; Iliescu, M.; Ishimoto, S.; Itahashi, K.; Iwasaki, M.; Kienle, P.; Kou, H.; Levi Sandri, P.; Longoni, A.; Lucherini, V.; Marton, J.; Matsuda, Y.; Noumi, H.; Ohnishi, H.; Okada, S.; Outa, H.; Pietreanu, D.; Ponta, T.; Rizzo, A.; Romero Vidal, A.; Sakuma, F.; Sato, M.; Scordo, A.; Sekimoto, M.; Shi, H.; Sirghi, D. L.; Sirghi, F.; Suzuki, T.; Tanida, K.; Tatsuno, H.; Tokuda, M.; Tomono, D.; Toyoda, A.; Tsukada, K.; Tudorache, A.; Tudorache, V.; Vazquez Doce, O.; Widmann, E.; Wünschek, B.; Yamazaki, T.; Zmeskal, J.

    2010-08-01

    Recently, the shift of the kaonic helium-4 2p state was precisely determined by the E570 and SIDDHARTA experiments. Prior to the experiment by E570, the average of three earlier experimental results showed -43±8 eV, while most of the theoretical calculations give ˜0 eV. This five-sigma discrepancy between theory and experiment was known as the "kaonic helium puzzle". A recent theoretical model showed a possible resonance-like shift of maximum 10 eV for a certain value of a deep antikaon-nucleon interaction potential, which is different in helium 3 and helium 4. The E570 experiment determined the shift of the kaonic helium-4 2p state as +2±2 (stat)±2 (sys) eV in 2007. The SIDDHARTA experiment determined the shift as 0±6(stat)±2(sys) eV in 2009. The results of these experiments resolved the long-standing puzzle. A new experiment of the kaonic helium-3 X-ray measurement is being prepared by the J-PARC E17 collaborators, and the kaonic helium-3 X-ray data taken very recently by the SIDDHARTA experiment are on the way to be analyzed. The results of the E570, E17 and SIDDHARTA experiments examine the strong interaction for light nuclei with different isospin, and test furthermore recent theoretical predictions.

  15. Differentiation of biological hydroxyapatite compounds by infrared spectroscopy, x-ray diffraction and extended x-ray absorption fine structure

    Chassot, E.; Oudadesse, H.; Irigaray, J.; Curis, E.; Bénazeth, S.; Nicolis, I.

    2001-12-01

    Pure hydroxyapatite (HAP) and HAP doped with 800 ppm of zinc were implanted in cortical bone of femur diaphysis of ovines [J. L. Irigaray et al., Mater. Clin. Appl. 28, 399 (1999)]. We observed that the doped HAP was better resorbed than pure HAP. The first hypothesis is that zinc acts as a stimulator on macrophage cells and improves quantity and quality of osteoblast cells. The second hypothesis is that zinc yields HAP structure that is better resorbed in biological field. For our experiment we used HAP doped with 3000 ppm of zinc in order to have a good sensitivity. In the present work, chemical studies by inductively coupled plasma absorption emission spectrometry, x ray diffraction, and infrared were carried out to determine the composition of major and trace elements in the doped hydroxyapatite, and the crystallographic structure. These studies can indicate possible modifications induced by the insertion of zinc. We used the extended x-ray absorption fine structure experimental station of LURE (Orsay, France) to try to clarify the atomic surroundings of zinc in doped HAP structure and transformations induced in initial lattice. Despite the low zinc concentration, we got good quality fluorescence mode spectra. These spectra showed medium range order of the material that is consistent with its crystalline form. To perform the analysis, we compared the result obtained with another models like β tricalcium phosphate and we created theoretical models of zinc in substitution of calcium in order to reproduce as well as possible the experimental spectrum. After this study, only two models are coherent with experimental spectrum, zinc in substitution of calcium in site I and zinc in the interstice between the two hydroxydes.

  16. X-ray laser–induced electron dynamics observed by femtosecond diffraction from nanocrystals of Buckminsterfullerene

    Abbey, Brian; Dilanian, Ruben A.; Darmanin, Connie; Ryan, Rebecca A.; Putkunz, Corey T.; Martin, Andrew V.; Wood, David; Streltsov, Victor; Jones, Michael W. M.; Gaffney, Naylyn; Hofmann, Felix; Williams, Garth J.; Boutet, Sébastien; Messerschmidt, Marc; Seibert, M. Marvin; Williams, Sophie; Curwood, Evan; Balaur, Eugeniu; Peele, Andrew G.; Nugent, Keith A.; Quiney, Harry M.

    2016-01-01

    X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration.

  17. Volumetric measurement of residual stress using high energy x-ray diffraction

    Whitesell, R.; McKenna, A.; Wendt, S.; Gray, J.

    2016-02-01

    We present results and recent developments from our laboratory, bench-top high energy x-ray diffraction system (HEXRD), between diffraction energies 50 and 150 KeV, to measure internal strain of moderately sized objects. Traditional x-ray strain measurements are limited to a few microns depth due to the use of Cu Kα1 Mo Kα1 radiation. The use of high energy x-rays for volumetric measurements of strain is typically the domain of synchrotron sources. We discuss the use of industrial 320kVp tube sources to generate a brighter x-ray beam along with a method using the intrinsic 43 eV width of the Kα1 characteristic peak of tungsten to measure volumetric strains in a number of industrially relevant materials. We will present volumetric strain measurements from two examples, first, additive manufacturing (AM) parts with various build configurations and, secondly, residual strain depth profiles from shot peened surface treatments. The spatial resolution of these depth profiles is ˜75 microns. The development of a faster method as compared to energy dispersive or θ-2θ scans is based on the intensity variation measurement of the strain using the aforementioned 43 eV characteristic tungsten kα line. We will present recent results on the development of this new tool and on x-ray diffraction measurements at high energy.

  18. X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

    Tsusaka, Y.; Takeda, S.; Takano, H.; Yokoyama, K.; Kagoshima, Y.; Matsui, J.

    2016-02-01

    X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector of each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 105 cm-2.

  19. X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

    Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H. [Graduate School of Material Science, University of Hyogo, 3-2-1, Kouto, Kamigori, Hyogo 678-1297 (Japan); Takeda, S. [SPring-8 Service Co., Ltd., 1-20-5, Kouto, Shingu, Tatsuno, Hyogo 679-5165 (Japan); Yokoyama, K.; Matsui, J. [Synchrotron Radiation Nanotechnology Center, University of Hyogo, 1-490-2, Kouto, Shingu, Tatsuno, Hyogo 679-5165 (Japan); Kagoshima, Y. [Graduate School of Material Science, University of Hyogo, 3-2-1, Kouto, Kamigori, Hyogo 678-1297 (Japan); Synchrotron Radiation Nanotechnology Center, University of Hyogo, 1-490-2, Kouto, Shingu, Tatsuno, Hyogo 679-5165 (Japan)

    2016-02-15

    X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector of each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.

  20. X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

    X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector of each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 105 cm−2

  1. 3D quantitative analysis of graphite morphology in high strength cast iron by high-energy X-ray tomography

    The size and morphology of the graphite particles play a crucial role in determining various mechanical and thermal properties of cast iron. In the present study, we utilized high-energy synchrotron X-ray tomography to perform quantitative 3D-characterization of the distribution of graphite particles in high-strength compacted graphite iron (CGI). The size, shape, and spatial connectivity of graphite were examined. The analysis reveals that the compacted graphite can grow with a coral-tree-like morphology and span several hundred microns in the iron matrix

  2. Magnetic exchange coupling in 3d-4f molecular nanomagnets investigated by X-ray magnetic circular dichroism

    Full text: Single-molecule magnets are exchange-coupled spin clusters showing slow relaxation of magnetization. In recent years, efforts have been intensified to increase the magnetization reversal barrier and thus enhance relaxation times by combining rare earth ions with transition-metal ions. Rare-earth ions exhibit very large magnetic anisotropies due to their strong spin-orbit coupling and their mostly unquenched orbital momentum. In this contribution we use X-ray magnetic circular dichroism to observe element-specific magnetization curves. In conjunction with SQUID magnetization and susceptibility measurements, we are able to obtain information about the magnetic coupling between 3d and 4f ions. (author)

  3. Composite laminate impact damage assessment by high resolution 3D X-ray tomography and laminography

    Bull, D. J.; Sinclair, I.; Spearing, S.M.; Helfen, L.

    2011-01-01

    Improvements to toughening mechanisms in composite materials have hitherto relied on visual inspection techniques that can be rather limited, especially since the inherent damage behaviour is three-dimensional (3D) requiring high resolution to capture micro-cracks and similar damage. To achieve a better understanding of impact damage behaviour, synchrotron radiation computed laminography (SRCL) and computed tomography (SRCT) techniques were used to capture 3D damage mechanisms with voxel size...

  4. MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTITATIVE X-RAY DIFFRACTION PHASE ANALYSIS

    G. Chu; Y.F. Cong; H.J. You

    2003-01-01

    A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

  5. Stress analysis of polycrystalline thin films and surface regions by X-ray diffraction

    The components of the macroscopic mechanical stress tensor of a stressed thin film, coating, multilayer or the region near the surface of a bulk material can in principle be determined by X-ray diffraction. The various analysis methods and measurement strategies, in dependence on specimen and measurement conditions, are summarized and evaluated in this paper. First, different X-ray diffraction geometries (conventional or grazing incidence) are described. Then, the case of macroscopically elastically isotropic, untextured specimens is considered: from the simplest case of a uniaxial state of stress to the most complicated case of a triaxial state of stress. The treatment is organized according to the number of unknowns to be determined (i.e. the state of stress, principal axes known or unknown), the use of one or several values of the rotation angle φ and the tilt angle ψ of the sample, and one or multiple hkl reflections. Next, the focus is on macroscopically elastically anisotropic (e.g. textured) specimens. In this case, the use of diffraction (X-ray) elastic constants is not possible. Instead, diffraction (X-ray) stress factors have to be used. On the basis of examples, it is demonstrated that successful diffraction stress analysis is only possible if an appropriate grain-interaction model is applied

  6. Femtosecond X-ray diffraction from two-dimensional protein crystals

    Matthias Frank

    2014-03-01

    Full Text Available X-ray diffraction patterns from two-dimensional (2-D protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  7. A Numerical Study on X-Ray Diffraction Effects within Objects

    Lehman, S K

    2005-09-29

    X-rays, being waves, always undergo the propagation effects of reflection, refraction, diffraction, geometric attenuation and absorption. In most circumstances the first four effects are considered negligible given the resolution sizes demanded of the measurement systems, x-ray energies involved, and physical properties of the materials under evaluation. We have reached the point, however, in some x-ray non-destructive evaluation (NDE) and imaging where we wish to resolve features of micrometer size in millimeter size objects to less than micrometer resolution. Given this resolution and the sizes of the measurement systems, diffraction effects within the object may become observable. We studied the extent to which diffraction is observable numerically using a two-dimensional paraxial approximation wave propagation code using a multislice method. We modeled realistic parts of interest at worst-case x-ray energies, comparing wave propagation and straight-ray simulated results. In two cases, we compare the numerical results to experimental measurements. The conclusion, based upon the results of the simulation code, is that diffraction effects on the measured data will be insignificant. However, we demonstrate by a single example, that in certain cases diffraction effects may be significant.

  8. Strain tomography of polycrystalline zirconia dental prostheses by synchrotron X-ray diffraction

    Non-destructive, quantitative and precise determination of internal strain distributions within structural materials and components can be accomplished by only a few experimental techniques, amongst which diffraction of penetrating radiation (X-ray and neutron beams) plays a central role. However, due to the various limitations of these methods, the 2-D and 3-D mapping of internal strains within bulk cross-sections at a spatial resolution of 0.1 mm or better has long remained a challenge. The principle of 'strain tomography' proposed by the present authors (an instance of broader 'rich' tomography methodology) makes use of the reconstruction tomography technique widely employed in imaging applications. In the present paper we report successful practical implementation of this principle to the study of bending strains in sintered polycrystalline zirconia used in the fabrication of multi-unit fixed prosthetic dentures. The results demonstrate the power of the technique, and pave the way to wider application of this approach to cross-sectional strain mapping in complex-shaped components under various loading conditions.

  9. New software to model energy dispersive X-ray diffraction in polycrystalline materials

    Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

  10. Quantum-dot-array diffraction grating with single order diffraction property for soft x-ray region

    A gold transmission grating is used routinely to disperse the x-ray spectrum at the Z soft x-ray facility to measure the spectrum and temporal history of the absolute soft x-ray power emitted from z-pinch and hohlraum radiation sources. A quantum-dot-array diffraction grating (QDADG) of 250 lines/mm for soft x-ray is designed and fabricated for the first time according to the principle of binary sinusoidal transmission grating. The diffraction efficiencies of the grating are measured in the 150-300 eV photon energy range on the Beamline 3W1B of Beijing Synchrotron Radiation Facility. This article describes the basic concept and calibration techniques and presents calibration results. It is shown that the 250 lines/mm QDADG can be used to disperse light without higher-order diffractions in soft x-ray range, and the diffraction efficiencies of this grating are nearly constant (about 25%), which is beneficial in the spectrum analysis.

  11. Quantum-dot-array diffraction grating with single order diffraction property for soft x-ray region

    Kuang, Longyu; Wang, Chuanke; Wang, Zhebin; Cao, Leifeng; Zhu, Xiaoli; Xie, Changqing; Liu, Shenye; Ding, Yongkun

    2010-07-01

    A gold transmission grating is used routinely to disperse the x-ray spectrum at the Z soft x-ray facility to measure the spectrum and temporal history of the absolute soft x-ray power emitted from z-pinch and hohlraum radiation sources. A quantum-dot-array diffraction grating (QDADG) of 250 lines/mm for soft x-ray is designed and fabricated for the first time according to the principle of binary sinusoidal transmission grating. The diffraction efficiencies of the grating are measured in the 150-300 eV photon energy range on the Beamline 3W1B of Beijing Synchrotron Radiation Facility. This article describes the basic concept and calibration techniques and presents calibration results. It is shown that the 250 lines/mm QDADG can be used to disperse light without higher-order diffractions in soft x-ray range, and the diffraction efficiencies of this grating are nearly constant (about 25%), which is beneficial in the spectrum analysis.

  12. Two new tensile devices for X-ray diffraction experiments

    Freri, N.; Tintori, A.; Depero, L.E.; Sangaletti, L. [Brescia Univ. (Italy); Cernuschi, F.; Ghia, S. [Ente Nazionale per l`Energia Elettrica, Milan (Italy)

    1995-12-01

    Two tensile devices were designed to be used with parallel beam and parafocusing-geometry diffractometers. In thefirst case the device was designed to be attached to a strainflex diffractometer by Rigaku Inc., dedicated to stress analysis and commonly used in metallurgical industry. Since the sample does not move during the measurement, the tensile device can be kept fixed on the experimental table. The device design takes into account the steric hindrance by moving parts of diffractometer. The maximun load that can be applied to the sample is 60.000 N. An attachement to a Siemens D5000 diffractometer with Eulerian cradle has also benn designed for applying a load up tp 6000 N to a sample in the parafocusing-geometry. The installation does not require a re-alignment of the diffractometer. In both cases strain gages were applied to both sides of the specimen for the simultaneous determination of the macroscopic strains. Experiments based on the use of these devices are planned to determine the crystallographic elastic constants and study the influence of the microstructure on the mechanical behaviour of residual stresses in the zone of almost static stresses as well as the influence of residual stresses on uniaxially loaded samples. In addition, by using these devices, it is possible to measure the unstressed d-0 spacings providing useful information in the neutron diffraction study fo stress fields in steel samples.

  13. Micro X-ray diffraction using X-ray area detector and identifying multiple phases in Zr2TiAl alloy system

    The birth of X-ray diffraction technique and its evolution has catalyzed the development of solid state science and further our understanding of material properties. The first single crystal X-ray diffraction pattern recorded was of Copper Sulphate Hydrate on a photographic film by Laue, and his co-workers Friedrich and Knipping, in 1912, for which he was awarded the Nobel prize. The actual diffraction pattern obtained was pretty awful with vague smudges instead of sharp diffraction spots (1). Development of X-ray detection technology has been playing an important role in advancing the development of new X-ray diffraction and imaging techniques. For instance, developments in electronics in the 1960's to 80's enabled advent of point detectors (eg. Nal scintillation detector) and line detectors (e.g gas filled single wire detector). These led to faster and more sensitive detection of X-rays leading to good XRD patterns. However, important information about microstructural details, defects, etc that are manifest well in the two dimensional map of the reciprocal space could be obtained reliably using area detectors (e.g X-ray films) (2). In the 1990's new developments in 2D X-ray area detectors such as Charge coupled devices (CCD), Imaging Plate Systems (IPS) and Multiwire proportional counters (MPC) led to replacement of the slower and low sensitive X-ray films with extremely sensitive 2D detection technology. This presentation will discuss these 2D detection techniques and their underlying mechanism. Recently the structure of multiple phases in Zr2TiAl alloy system could be identified using micro-XRD and 2D detection technique. Result of this study will be presented. (author)

  14. X-ray diffraction and imaging with a coherent beam: application to X-ray optical elements and to crystals exhibiting phase inhomogeneities

    The exceptional properties of synchrotron light sources have been exploited in very different disciplines, from archaeology to chemistry, from material science to biology, from medicine to physics. Among these properties it is important to mention the high brilliance, continuum spectrum, high degree of polarization, time structure, small source size and divergence of the beam, the last resulting in a high transversal coherence of the produced radiation. This high transversal coherence of the synchrotron sources has permitted the development of new techniques, e.g. phase contrast imaging, X-ray photon correlation spectroscopy and coherent X-ray diffraction imaging (CXDI). This thesis work will consist essentially of three parts. In the first part it will be presented the work done as a member of the X-ray Optics Group of ESRF in the characterization of high quality diamond crystals foreseen as X-ray optical elements. The characterization has been done using different complementary X-ray techniques, such as high resolution diffraction, topography, grazing incidence diffraction, reflectivity and measurements of the coherence preservation using the Talbot effect. In the second part, I will show the result obtained in the study of the temperature behaviours of the domain in periodically poled ferroelectrics crystals. This type of measurements, based on Bragg-Fresnel diffraction, are possible only thanks to the high degree of coherence of the beam. In the third part, I will present the results obtained in the characterization of diamonds foreseen for applications other than X-ray optical elements. (author)

  15. A sample holder for in-house X-ray powder diffraction studies of protein powders

    Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

    2011-01-01

    A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin.......A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximately...

  16. X-ray diffraction patterns of single crystals implanted with high-energy light ions

    X-ray diffraction patterns of silicon and gallium arsenide single crystals implanted with high-energy protons and α-particles were studied. A various models of lattice parameter changes were analysed. The agreement between the simulation and experiment proves that the lattice parameter depth-distribution can be assumed to be proportional to vacancy distribution obtained by Monte-Carlo method and from the Biersack-Ziegler theory. Most of the X-ray experiments were performed using synchrotron source of X-ray radiation in particular in the case of back-reflection and transmission section topographic methods. The new method of direct determination of the implanted ion ranges was proposed using synchrotron radiation back-reflection section topography. A number of new interference phenomena was revealed and explained. These interferences are important in the applications of diffraction theory in studying of the real structure of implanted layers. (author)

  17. X-ray diffraction study of structural stability of giant proteoglycan molecules of mucus

    X-ray diffraction study of various native and modified gastrointestinal mucins was carried out using synchrotron radiation. The mucus X-ray patterns of mammals and invertebrates are very similar and display a large number of sharp diffraction rings at the spacing of about 4.65 nm, which are due to the helical packing of polysaccharide chains covalently connected to the protein core. A comparative analysis of the X-ray patterns obtained earlier by us from various samples of mucus and biological tissues showed that the 4.65(±0.15) nm spacing is a nanoscale structural invariant of giant proteoglycan molecules of both the mucus and the extracellular matrix of tissues. A role of structural dynamics of proteoglycan scaffolding of biological systems in mechanism of modifying adaptation of organisms to significant changes of temperature is discussed.

  18. X-ray diffraction study of structural stability of giant proteoglycan molecules of mucus

    Vazina, A.A. [Institute of Theoretical and Experimental Biophysics, RAS, Institutskaya St. 3, 142290 Pushchino, Moscow Region (Russian Federation); Russian Research Center ' Kurchatov Institute' , 123182 Moscow (Russian Federation)], E-mail: vazina@iteb.ru; Lanina, N.F.; Vasilieva, A.A. [Institute of Theoretical and Experimental Biophysics, RAS, Institutskaya St. 3, 142290 Pushchino, Moscow Region (Russian Federation); Korneev, V.N. [Institute of Cell Biophysics, RAS, 142290 Pushchino (Russian Federation); Zabelin, A.V. [Russian Research Center ' Kurchatov Institute' , 123182 Moscow (Russian Federation); Polyakova, E.P. [Timiryazev Moscow Agricultural Academy, 127550 Moscow (Russian Federation)

    2009-05-11

    X-ray diffraction study of various native and modified gastrointestinal mucins was carried out using synchrotron radiation. The mucus X-ray patterns of mammals and invertebrates are very similar and display a large number of sharp diffraction rings at the spacing of about 4.65 nm, which are due to the helical packing of polysaccharide chains covalently connected to the protein core. A comparative analysis of the X-ray patterns obtained earlier by us from various samples of mucus and biological tissues showed that the 4.65({+-}0.15) nm spacing is a nanoscale structural invariant of giant proteoglycan molecules of both the mucus and the extracellular matrix of tissues. A role of structural dynamics of proteoglycan scaffolding of biological systems in mechanism of modifying adaptation of organisms to significant changes of temperature is discussed.

  19. Structural study on sodium choride by X-ray powder diffraction method

    The procedure for the crystal structure analysis by means of the X-ray powder diffraction method has been shown using the sodium chloride as a sample. The twelve X-ray diffraction intensity peaks for sodium chloride powder were collected rotating 2 THETA sub(hkl). Bragg angle of X-ray diffractometer from 20 to 160 degrees, in which Cu Ksub(α) radition filtered by nickel had been used. For assigning indices of each reflecting plane, the relationship between lattice parameter and interplanar spacing has been used. This result has shown that sodium chloride is face-centered cubic, space group F 4/m 3-2/m with until cell dimension a = 5.36 A and z = 4. The experimental and theoretical integrated intensities of the reflecting planes are in good agreement with each other. (author)

  20. 3D images of human hair using X-ray CT method with age

    Recently interest of the aging effects has been increased in Japanese society but it is still not known much about what happens on the aged hairs. The hair-density measurement revealed that the density of human hair decreases with age, which caused by the follow-out of proteins and peptides from the hairs. According to the results of hair investigation between 20 and 50 years women, effluences of protein and peptide become increasing with the age and the degree of the cosmetic treatment. Further studies based on the X-ray CT show that quantity of voids in hair increases with age, which is thought at the origin of the density decrease. (author)

  1. Mapping electronic ordering in chromium in 3D with x-ray microdiffraction

    Xu, Ruqing

    2015-03-01

    In the antiferromagnetic state of chromium, electrons form spin-density waves and charge-density waves with wave vector along one of the lattice cubic axes; the spontaneous ordering of the electrons breaks the lattice symmetry and creates domains within a single crystal. We report the first 3-dimentional mapping of charge-density wave domains in bulk polycrystalline chromium samples using differential-aperture x-ray microdiffraction at the Advanced Photon Source. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357

  2. Precision spectroscopy of Kaonic Helium 3d {sup {yields}} 2p X-rays

    Okada, S.; Iio, M.; Matsuda, Y.; Ohnishi, H.; Outa, H.; Suzuki, T.; Tomono, D. [Nishina Center for Accelerator-based Science, RIKEN, Wako, 351-0198 (Japan); Beer, G. [Department of Physics and Astronomy, University of Victoria, Victoria (Canada); Bhang, H. [Department of Physics, Seoul National University, Seoul, 151-742 (Korea, Republic of); Cargnelli, M. [Stefan Meyer Institut fuer subatomare Physik, Vienna (Austria); Chiba, J. [Department of Physics, Tokyo University of Science, Noda, 278-8510 (Japan); Choi, S. [Department of Physics, Seoul National University, Seoul, 151-742 (Korea, Republic of); Curceanu, C. [Laboratori Nazionali di Frascati dell' INFN, Frascati (Italy); Fukuda, Y. [Department of Physics, Tokyo Institute of Technology, Meguro, 152-8551 (Japan); Hanaki, T. [Department of Physics, Tokyo University of Science, Noda, 278-8510 (Japan); Hayano, R.S.; Ishikawa, T. [Department of Physics, University of Tokyo, Bunkyo, 113-0033 (Japan); Ishimoto, S. [High Energy Accelerator Research Organization (KEK), Tsukuba, 305-0801 (Japan); Ishiwatari, T.; Juhasz, B.; Kienle, P.; Marton, J. [Stefan Meyer Institut fuer subatomare Physik, Vienna (Austria); Sato, M. [Department of Physics, Tokyo Institute of Technology, Meguro, 152-8551 (Japan); Schmid, P. [Stefan Meyer Institut fuer subatomare Physik, Vienna (Austria); Suzuki, S. [High Energy Accelerator Research Organization (KEK), Tsukuba, 305-0801 (Japan); Tatsuno, H. [Department of Physics, University of Tokyo, Bunkyo, 113-0033 (Japan); Widmann, E. [Stefan Meyer Institut fuer subatomare Physik, Vienna (Austria); Yamazaki, T. [Nishina Center for Accelerator-based Science, RIKEN, Wako, 351-0198 (Japan)]|[Department of Physics, University of Tokyo, Bunkyo, 113-0033 (Japan); Yim, H. [Department of Physics, Seoul National University, Seoul, 151-742 (Korea, Republic of); Zmeskal, J. [High Energy Accelerator Research Organization (KEK), Tsukuba, 305-0801 (Japan)

    2007-06-15

    We have measured the strong-interaction shift of 2p states of kaonic helium-4 atoms with a precision of {approx}2 eV using Silicon Drift Detectors (SDDs) which lead to much improved energy resolution and signal-to-noise ratio compared to the conventional Si(Li) x-ray detector used in the past experiments. The measurement will give an answer to the longstanding 'kaonic helium puzzle' and provide crucial information to understand the basis of the Akaishi-Yamazaki prediction of deeply-bound kaonic nuclei, which is one of the interpretations of the strange multibaryon candidates recently reported at KEK, DA{phi}NE and BNL.

  3. Precision spectroscopy of Kaonic Helium 3d → 2p X-rays

    Okada, S.; Beer, G.; Bhang, H.; Cargnelli, M.; Chiba, J.; Choi, S.; Curceanu, C.; Fukuda, Y.; Hanaki, T.; Hayano, R. S.; Iio, M.; Ishikawa, T.; Ishimoto, S.; Ishiwatari, T.; Itahashi, K.; Iwasaki, M.; Juhász, B.; Kienle, P.; Marton, J.; Matsuda, Y.; Ohnishi, H.; Outa, H.; Sato, M.; Schmid, P.; Suzuki, S.; Suzuki, T.; Tatsuno, H.; Tomono, D.; Widmann, E.; Yamazaki, T.; Yim, H.; Zmeskal, J.

    2007-06-01

    We have measured the strong-interaction shift of 2p states of kaonic helium-4 atoms with a precision of ˜2 eV using Silicon Drift Detectors (SDDs) which lead to much improved energy resolution and signal-to-noise ratio compared to the conventional Si(Li) x-ray detector used in the past experiments. The measurement will give an answer to the longstanding “kaonic helium puzzle” and provide crucial information to understand the basis of the Akaishi-Yamazaki prediction of deeply-bound kaonic nuclei, which is one of the interpretations of the strange multibaryon candidates recently reported at KEK, DAΦNE and BNL.

  4. Multi-wavelength anomalous diffraction at high x-ray intensity

    Son, Sang-Kil; Santra, Robin

    2011-01-01

    The multi-wavelength anomalous diffraction (MAD) method is used to determine phase information in x-ray crystallography by employing dispersion corrections from heavy atoms on coherent x-ray scattering. X-ray free-electron lasers (FELs) show promise for revealing the structure of single molecules or nanocrystals within femtoseconds, but the phase problem remains largely unsolved. Due to the ultrabrightness of x-ray FEL, samples experience severe electronic radiation damage, especially to heavy atoms, which hinders direct implementation of the MAD method with x-ray FELs. We propose a generalized version of the MAD phasing method at high x-ray intensity. We demonstrate the existence of a Karle--Hendrickson-type equation for the MAD method in the high-intensity regime and calculate relevant coefficients with detailed electronic damage dynamics of heavy atoms. Our results show that the bleaching effect on the scattering strength of the heavy atoms can be advantageous to the phasing method. The present method offe...

  5. Structure-function Investigation of Operando Nanostructured Materials Using Coherent X-ray Diffractive Imaging

    Ulvestad, Andrew

    Nanostructured devices promise to help solve grand challenges of our time, including renewable energy generation, storage, and mitigating climate change. Their power lies in the particular influence of the surface on the total free energy when dimensions approach the nanoscale and it is well known that different sizes, shapes, and defects can drastically alter material properties. However, this strength represents a considerable challenge for imaging techniques that can be limited in terms of sample environments, average over large ensembles of particles, and/or lack adequate spatiotemporal resolution for studying the relevant physical processes. The focus of this thesis is the development of in situ coherent X-ray diffractive imaging (CXDI) and its application in imaging strain evolution in battery cathode nanoparticles. Using in situ CXDI, the compressive/tensile strain field in the pristine state is revealed, and found to be linked to a particular concentration of strain inducing Jahn-Teller ions. The evolution of strain during the first charge/discharge cycle shows that the cathode nanoparticle exhibits phase separation. Using the 3D strain field, the strain field energy is calculated and shows interesting hysteresis between charge and discharge. Strain evolution during a disconnection event, in which the cathode nanoparticle is no longer able to exchange electrons and ions with its environment, reveals the formation of a poorly conducting interphase layer. Finally, strain fields were used to study dislocation dynamics in battery nanoparticles. Using the full 3D information, the dislocation line structure is mapped and shown to move in response to charge transfer. The dislocation is used as a way to probe the local material properties and it is discovered that the material enters an ``auxetic", or negative Poisson's ratio, regime.

  6. Magnetic symmetries in neutron and resonant x-ray Bragg diffraction patterns of four iridium oxides

    Lovesey, S. W.; Khalyavin, D. D.; Manuel, P.; Chapon, L. C.; Cao, G.; Qi, T. F.

    2012-12-01

    The magnetic properties of Sr2IrO4, Na2IrO3, Sr3Ir2O7 and CaIrO3 are discussed, principally in the light of experimental data in recent literature for Bragg intensities measured in x-ray diffraction with enhancement at iridium L-absorption edges. The electronic structure factors we report, which incorporate parity-even and acentric entities, serve the immediate purpose of making full use of crystal and magnetic symmetry to refine our knowledge of the magnetic properties of the four iridates from resonant x-ray diffraction data. They also offer a platform on which to interpret future investigations, using dichroic signals, resonant x-ray diffraction and neutron diffraction, for example, as well as ab initio calculations of electronic structure. Unit-cell structure factors, suitable for x-ray Bragg diffraction enhanced by an electric dipole-electric dipole (E1-E1) event, reveal exactly which iridium multipoles are visible, e.g., a magnetic dipole parallel to the crystal c-axis (z-axis) and an electric quadrupole with yz-like symmetry in the specific case of CaIrO3. Magnetic space-groups are assigned to Sr2IrO4, Sr3Ir2O7 and CaIrO3, namely, PIcca, PAban and Cm‧cm‧, respectively, in the Belov-Neronova-Smirnova notation. The assignment for Sr2IrO4 is possible because of our new high-resolution neutron diffraction data, gathered on a powder sample. In addition, the new data are used to show that the ordered magnetic moment of an Ir4+ ion in Sr2IrO4 does not exceed 0.29(4) μB. Na2IrO3 has two candidate magnetic space-groups that are not resolved with currently available resonant x-ray data.

  7. Synchrotron X-ray tomography for 3D chemical diffusion measurement of a flame retardant in polystyrene

    In an on-going tomographic project, material properties of industrial polymer blends are being studied. This project uses 3D chemical analysis techniques to look at a polymer additive problem called blooming, related to the theory of aging and diffusion in glassy materials. The 3D images are acquired with synchrotron X-ray tomography because of its rapidity, good spatial resolution, large field-of-view, and elemental sensitivity. To investigate the chemical process of blooming, new procedures are developed to assess the flame retardant distribution as a function of annealing time in the sample. With the spatial chemical distribution we fit the concentrations to a diffusion equation to each time step in the annealing process. In this preliminary work, we study the dissolutions of a non-blooming flame retardant

  8. Statistical coronary motion models for 2D+t/3D registration of X-ray coronary angiography and CTA

    Baka, N.; Metz, C.T.; Schultz, C.;

    2013-01-01

    Accurate alignment of intra-operative X-ray coronary angiography (XA) and pre-operative cardiac CT angiography (CTA) may improve procedural success rates of minimally invasive coronary interventions for patients with chronic total occlusions. It was previously shown that incorporating patient...... motion models to provide constraints for the 2D+t/3D registration. We propose a methodology for building statistical motion models of the coronary arteries from a training population of 4D CTA datasets. We compare the 2D+t/3D registration performance of the proposed statistical models with other motion...... estimates, including the patient specific motion extracted from 4D CTA, the mean motion of a population, the predicted motion based on the cardiac shape. The coronary motion models, constructed on a training set of 150 patients, had a generalization accuracy of 1mm root mean square point-to-point distance...

  9. 2D-3D shape reconstruction of the distal femur from stereo X-Ray imaging using statistical shape models

    Baka, N.; Kaptein, B.L.; de Bruijne, Marleen; van Walsum, T.; Giphart, J.E.; Niessen, W.J.; Lelieveldt, B.P.F.

    2011-01-01

    as it lowers both the acquisition costs and the radiation dose compared to CT. We propose a method for pose estimation and shape reconstruction of 3D bone surfaces from two (or more) calibrated X-ray images using a statistical shape model (SSM). User interaction is limited to manual initialization of...... the mean shape. The proposed method combines a 3D distance based objective function with automatic edge selection on a Canny edge map. Landmark-edge correspondences are weighted based on the orientation difference of the projected silhouette and the corresponding image edge. The method was evaluated...... segmentations. Rigid registration of the ground truth shape to the biplane fluoroscopy achieved sub-millimeter accuracy (0.68mm) measured as root mean squared (RMS) point-to-surface (P2S) distance. The non-rigid reconstruction from the biplane fluoroscopy using the SSM also showed promising results (1.68mm RMS...

  10. Diffractive optical element for creating visual 3D images.

    Goncharsky, Alexander; Goncharsky, Anton; Durlevich, Svyatoslav

    2016-05-01

    A method is proposed to compute and synthesize the microrelief of a diffractive optical element to produce a new visual security feature - the vertical 3D/3D switch effect. The security feature consists in the alternation of two 3D color images when the diffractive element is tilted up/down. Optical security elements that produce the new security feature are synthesized using electron-beam technology. Sample optical security elements are manufactured that produce 3D to 3D visual switch effect when illuminated by white light. Photos and video records of the vertical 3D/3D switch effect of real optical elements are presented. The optical elements developed can be replicated using standard equipment employed for manufacturing security holograms. The new optical security feature is easy to control visually, safely protected against counterfeit, and designed to protect banknotes, documents, ID cards, etc. PMID:27137530

  11. Non-destructive characterization of recrystallization kinetics using three-dimensional X-ray diffraction microscopy

    Lauridsen, E.M.; Schmidt, Søren; Fæster Nielsen, Søren;

    2006-01-01

    Three-dimensional X-ray diffraction (3DXRD) is used to characterize the nucleation and early growth of individual bulk nuclei in situ during recrystallization of 92% cold-rolled copper. It is found that some cube nuclei, but not all, have a significantly faster initial growth than the average...

  12. Naturally irradiated fluorite as a historic violet pigment: X-ray diffraction and Raman spectroscopic study

    Bezdička, Petr; Čermáková, Zdeňka; Němec, I.; Hradilová, J.; Hradil, David

    Rovinj : ECM29, 2015. s. 529. [European Crystallographic Meeting /29./. 23.08.2015-28.08.2015, Rovinj] Institutional support: RVO:61388980 Keywords : fluorite * X-ray diffraction Subject RIV: CA - Inorganic Chemistry http://ecm29.ecanews.org/wp-content/uploads/Book_of_abstracts_ECM29_final.compressed.pdf

  13. High-pressure x-ray diffraction of icosahedral Zr-Al-Ni-Cu-Ag quasicrystals

    Jiang, Jianzhong; Saksl, Karel; Rasmussen, Helge Kildahl;

    2001-01-01

    The effect of pressure on the structural stability of icosahedral Zr-Al-Ni-Cu-Ag quasicrystals forming from a Zr65Al7.5Ni10Cu7.5Ag10 metallic glass with a supercooled liquid region of 44 K has been investigated by in situ high-pressure angle-dispersive x-ray powder diffraction at ambient temperat...

  14. An X-ray diffraction study of direct-bonded silicon interfaces

    Howes, P.B.; Benamara, M.; Grey, F.;

    1998-01-01

    Semiconductor wafer bonding techniques have been used to create a giant twist grain boundary from two Si(001) wafers. We show, using X-ray diffraction measurements that after annealing the interface forms a highly ordered superstructure with relaxations extending to many layers into the crystals...

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

    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...

  16. Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

    Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

  17. Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

    Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

    2007-01-01

    A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

  18. High-pressure X-ray diffraction study of bulk- and nanocrystalline GaN

    Jorgensen, J.E.; Jakobsen, J.M.; Jiang, Jianzhong;

    2003-01-01

    Bulk- and nanocrystalline GaN have been studied by high-pressure energy-dispersive X-ray diffraction. Pressure-induced structural phase transitions from the wurtzite to the NaCl phase were observed in both materials. The transition pressure was found to be 40 GPa for the bulk-crystalline GaN, while...

  19. X-ray diffraction investigation of self-annealing in nanocrystalline copper electrodeposits

    Pantleon, Karen; Somers, Marcel A. J.

    2006-01-01

    X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multiple...

  20. A three-dimensional X-ray diffraction microscope for deformation studies of polycrystals

    Fæster Nielsen, Søren; Lauridsen, E.M.; Juul Jensen, D.;

    2001-01-01

    -dimensional X-ray diffraction (3DXRD) microscope installed at the European Synchrotron Radiation Facility in Grenoble provides a fast and non-destructive technique for mapping the embedded grains within thick samples in three dimensions. All essential features like the position, volume, orientation, stress...

  1. High-pressure X-ray diffraction of L-ALANINE crystal

    Olsen, J.S.; Gerward, Leif; Souza, A.G.;

    2006-01-01

    L-ALANINE has been studied by X-ray diffraction at ambient temperature and pressure up to 10.3 GPa. The material is found to transform to a tetragonal structure between 2 and 3 GPa. and to a monoclinic structure between 8 and 10 GPa. The experimental bulk modulus is 25(5) GPa for the orthorhombic...

  2. An introduction to three-dimensional X-ray diffraction microscopy

    Poulsen, Henning Friis

    2012-01-01

    Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly...

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

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

    2013-01-01

    In this work the structure of ternary GaxIn1−xP nanowires is investigated with respect to the chemical composition and homogeneity. The nanowires were grown by metal–organic vapor-phase epitaxy. For the investigation of ensemble fluctuations on several lateral length scales, X-ray diffraction...

  4. Modelling the X-ray powder diffraction of nitrogen-expanded austenite using the Debye formula

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

    Stress-free and homogeneous samples of nitrogen-expanded austenite, a defect-rich f.c.c. structure with a high interstitial nitrogen occupancy (between 0.36 and 0.61), have been studied using X-ray powder diffraction and Debye simulations. The simulations confirm the presence of deformation...

  5. On the theory of X-ray diffraction in oscillating piezocrystals

    Certain problems are considered of the X-ray radiation diffraction in oscillating crystals within the framework of the Takagi strict dynamic theory, both, in the case of one-dimensional deformation and in the case of a two-dimensional one. (author)

  6. An X-ray diffraction study of direct-bonded silicon interfaces

    Howes, P.B.; Benamara, M.; Grey, F.;

    1998-01-01

    Semiconductor wafer bonding techniques have been used to create a giant twist grain boundary from two Si(001) wafers. We show, using X-ray diffraction measurements that after annealing the interface forms a highly ordered superstructure with relaxations extending to many layers into the crystals on...

  7. On-line analysis, by x-ray diffraction, of fluorspar-containing slurries

    An on-line instrument developed by the National Institute for Metallugy was used in a feasibility study on the applicability of X-ray diffraction to the analysis of fluorspar-containing slurries. The instrument in shown to have adequate sensitivity and resolution for the purpose, and further testwork is recommended

  8. Stereochemistry Determination by Powder X-ray Diffraction Analysis and NMR Spectroscopy Residual Dipolar Couplings

    Garcia, M.; Pagola, S; Navarro-Vasquez, A; Phillips, D; Gayathri, C; Krakauer, H; Stephens, P; Nicotra, V; Gil, R

    2009-01-01

    A matter of technique: For a new steroidal lactol, jaborosalactol 24 (1), isolated from Jaborosa parviflora, NMR spectroscopy residual dipolar couplings and powder X-ray diffraction analysis independently gave the same stereochemistry at C23-C26. Conventional NMR spectroscopic techniques, such as NOE and {sup 3}J coupling-constant analysis failed to unambiguously determine this stereochemistry.

  9. A-DNA and B-DNA: Comparing Their Historical X-Ray Fiber Diffraction Images

    Lucas, Amand A.

    2008-01-01

    A-DNA and B-DNA are two secondary molecular conformations (among other allomorphs) that double-stranded DNA drawn into a fiber can assume, depending on the relative water content and other chemical parameters of the fiber. They were the first two forms to be observed by X-ray fiber diffraction in the early 1950s, respectively by Wilkins and…

  10. APPLICATION OF SYNCHROTRON RADIATION TO HIGH PRESSURE X-RAY DIFFRACTION

    Hatton, P.

    1984-01-01

    The availability of dedicated, high brightness synchrotron radiation sources is leading to many improvements in x-ray diffraction techniques. In addition to the widely discussed polychromatic energy dispersive techniques, significant advances can be made by the use of monochromatic radiation in either angle- or wavelength-scanning. The application of these techniques, being developed at Daresbury, for high pressure investigations is outlined.

  11. Three-dimensional imaging of dislocations by X-ray diffraction laminography

    Synchrotron radiation laminography with X-ray diffraction contrast enables three-dimensional imaging of dislocations in monocrystalline wafers. We outline the principle of the technique, the required experimental conditions, and the reconstruction procedure. The feasibility and the potential of the method are demonstrated by three-dimensional imaging of dislocation loops in an indent-damaged and annealed silicon wafer.

  12. Three-dimensional imaging of dislocations by X-ray diffraction laminography

    Haenschke, D. [Karlsruhe Institute of Technology (KIT), Laboratory for Applications of Synchrotron Radiation (LAS), 76128 Karlsruhe (Germany); Helfen, L. [Karlsruhe Institute of Technology (KIT), Institute for Photon Science and Synchrotron Radiation (IPS/ANKA), 76344 Eggenstein (Germany); European Synchrotron Radiation Facility (ESRF), BP220, 38043 Grenoble (France); Altapova, V. [Karlsruhe Institute of Technology (KIT), Laboratory for Applications of Synchrotron Radiation (LAS), 76128 Karlsruhe (Germany); National Research Tomsk Polytechnic University, 634050 Tomsk (Russian Federation); Danilewsky, A. [University Freiburg, Kristallographie, Institut fuer Geowissenschaften, 79104 Freiburg (Germany); Baumbach, T. [Karlsruhe Institute of Technology (KIT), Laboratory for Applications of Synchrotron Radiation (LAS), 76128 Karlsruhe (Germany); Karlsruhe Institute of Technology (KIT), Institute for Photon Science and Synchrotron Radiation (IPS/ANKA), 76344 Eggenstein (Germany)

    2012-12-10

    Synchrotron radiation laminography with X-ray diffraction contrast enables three-dimensional imaging of dislocations in monocrystalline wafers. We outline the principle of the technique, the required experimental conditions, and the reconstruction procedure. The feasibility and the potential of the method are demonstrated by three-dimensional imaging of dislocation loops in an indent-damaged and annealed silicon wafer.

  13. Three-dimensional imaging of dislocations by X-ray diffraction laminography

    Hänschke, D.; Helfen, L.; Altapova, V.; Danilewsky, A.; Baumbach, T.

    2012-12-01

    Synchrotron radiation laminography with X-ray diffraction contrast enables three-dimensional imaging of dislocations in monocrystalline wafers. We outline the principle of the technique, the required experimental conditions, and the reconstruction procedure. The feasibility and the potential of the method are demonstrated by three-dimensional imaging of dislocation loops in an indent-damaged and annealed silicon wafer.

  14. Grain orientation measurement of passivated aluminum interconnects by x-ray micro diffraction

    Chang, Chang-Hwan; Valek, B.C.; Padmore, H. A.; MacDowell, A.A.; Celestre, R; Marieb, T.; Bravman, J.C.; Y. M. Koo; Patel, J. R.

    1999-01-01

    The crystallographic orientations of individual grains in a passivated aluminum interconnect line of 0.7-mu m width were investigated by using an incidentwhite x-ray microbeam at the Advanced Light Source, Berkeley National Laboratory. Intergrain orientation mapping was obtained with about 0.05o sensitivity by the micro Laue diffraction technique.

  15. Temperature-dependent vibrational spectroscopic and X-ray diffraction investigation of nanosized nickel chromite

    Matulková, Irena; Holec, Petr; Němec, I.; Kitazawa, H.; Furubayashi, T.; Vejpravová, Jana

    2015-01-01

    Roč. 1090, Jun SI (2015), s. 70-75. ISSN 0022-2860 R&D Projects: GA ČR GAP108/10/1250 Institutional support: RVO:68378271 ; RVO:61388980 Keywords : vibrational spectroscopy * nickel chromite * X- ray diffraction * size effect Subject RIV: BM - Solid Matter Physics ; Magnetism; CA - Inorganic Chemistry (UACH-T) Impact factor: 1.602, year: 2014

  16. X-Ray Diffraction Study of L2005 AG17 (IDPs) by Using SR

    Ohsumi, K. O.; Hagiya, K. H.; Zolensky, M. E.

    2002-01-01

    X-ray diffraction study revealed the existence of magnetite and new type of pyrrhotite with the chemical formula of Fe0.56S in L2005 AG17. Considering the total chemical formula of Fe0.83S, residual iron in amorphous state might exist in this sample. Additional information is contained in the original extended abstract.

  17. Characterization, crystallization and preliminary X-ray diffraction studies of tomato nuclease I

    Koval, Tomáš; Dohnálek, Jan; Lipovová, P.; Podzimek, T.; Matoušek, Jaroslav

    2009-01-01

    Roč. 16, 1a (2009), b33. ISSN 1211-5894. [Discussions in Structural Molecular Biology /7./. 12.03.2009-14.03.2009, Nové Hrady] Institutional research plan: CEZ:AV0Z40500505 Keywords : X-ray diffraction * tomato nuclease Subject RIV: CD - Macromolecular Chemistry

  18. A greedy method for reconstructing polycrystals from three-dimensional X-ray diffraction data

    Kulshreshth, Arun Kumar; Alpers, Andreas; Herman, Gabor T.;

    2009-01-01

    An iterative search method is proposed for obtaining orientation maps inside polycrystals from three-dimensional X-ray diffraction (3DXRD) data. In each step, detector pixel intensities are calculated by a forward model based on the current estimate of the orientation map. The pixel at which the ...

  19. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (Irel). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

  20. Determining grain resolved stresses in polycrystalline materials using three-dimensional X-ray diffraction

    Oddershede, Jette; Schmidt, Søren; Poulsen, Henning Friis; Sørensen, Henning Osholm; Wright, Jonathan; Reimers, Walter

    2010-01-01

    An algorithm is presented for characterization of the grain resolved (type II) stress states in a polycrystalline sample based on monochromatic X-ray diffraction data. The algorithm is a robust 12-parameter-per-grain fit of the centre-of-mass grain positions, orientations and stress tensors...

  1. Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

    Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.; Achilles, C. N.; Downs, R. T.; Farmer, J. D.; Crisp, J. A.; Morookian, J. M.; Des Marais, D. J.; Grotzinger, J. P.; Sarrazin, P.; Yen, A. S.

    2014-01-01

    To obtain detailed mineralogy information, the Mars Science Laboratory rover Curiosity carries CheMin, the first X-ray diffraction (XRD) instrument used on a planet other than Earth. CheMin has provided the first in situ XRD analyses of full phase assemblages on another planet.

  2. Evaluated Plan Stress Of Weld In Pressure Tube Using X Ray Diffraction Technique

    X ray diffraction is a fundamental technique measuring stress, this technique has determined crystal strain in materials, from that determined stress in materials. This paper presents study of evaluating plane stress of weld in pressure tube, using modern XRD apparatus: X Pert Pro. (author)

  3. Simultaneous X-ray diffraction from multiple single crystals of macromolecules

    Paithankar, Karthik S.; Sørensen, Henning Osholm; Wright, Jonathan P.;

    2011-01-01

    The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedure...

  4. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    Barbosa, Caroline M., E-mail: carolmattosb@yahoo.com.br [Instituto de Arqueologia Brasileira (IAB), Belford Roxo, RJ (Brazil); Azeredo, Soraia R.; Lopes, Ricardo T., E-mail: soraia@lin.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/LIN/UFRJ), Rio de Janeiro, RJ (Brazil). Laboratorio de Instrumentacao Nuclear; Souza, Sheila M.F.M de, E-mail: sferraz@ensp.fiocruz.br [Fundacao Oswaldo Cruz (ENSP/FIOCRUZ), Rio de Janeiro, RJ (Brazil). Escola Nacional de Saude Publica Sergio Arouca

    2013-07-01

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (I{sub rel}). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

  5. Quantitative phase analysis of uranium carbide from x-ray diffraction data using the Rietveld method

    Quantitative phase analysis of a uranium carbide sample was carried out from the x-ray diffraction data by Rietveld profile fitting method. The method does not require the addition of any reference material. The percentage of UC, UC2 and UO2 phases in the sample were determined. (author)

  6. Advances in thin film diffraction instrumentation by X-ray optics

    Haase, A. [Rich. Seifert and Co., Analytical X-ray Systems, Ahrensburg (Germany)

    1996-09-01

    The structural characterisation of thin films requires a parallel X-ray beam of high intensity. Parallel beam geometry is commonly used in high resolution and single crystal experiments, but also in the field of X-ray diffraction for polycrystalline material (e.g. in phase, texture and stress analysis). For grazing incidence diffraction (GID), the use of small slits on the primary side and of long soller slits with a flat monochromator on the secondary side is standard. New optical elements have been introduced with polychromatic or monochromatic radiation. By means of different applications the results are compared with those of classical beam optics. X-ray fiber optics utilize total external reflection of X-rays on smooth surfaces. Effects of monochromatization are presented. In many fields of application, fiber optics may replace conventional collimators. The use of primary and secondary channel cut crystals can also produce a high parallel monochromatic X-ray beam. A parabolically bent graded multilayer produces a monochromatic parallel beam of high intensity. Compared with classical Bragg-Brentano (focussing) geometry, excellent results have been obtained, especially for samples with an irregular shape. In combination with a channel cut monochromator there is a substantial gain in intensity leading to an increase of the dynamic intensity range of rocking curves.

  7. X-RAY DIFFRACTION AND X-RAY FLUORESCENCE ANALYSIS OF POTTERY SHARDS FROM NEW ARCHAEOLOGICAL SURVEY IN SOUTH REGION OF SISTAN, IRAN

    Sarhaddi-Dadian, Hossein; Ramli, Zuliskandar; Shuhaimi, Nik Hassan; Rahman, Nik Abdul; Mehrafarin, Reza

    2015-01-01

    The aim of this study is to determine whether pottery shards from new archaeological survey in south region of Sistan are locally made or imported. Many artefacts especially pottery shards have been found during the archaeological survey. These pottery shards are variable in color; from buff, grey, black, and red. The analytical techniques involved X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD), that were applied to determine the major and trace elements and also the mineral content of ...

  8. Efficient feature-based 2D/3D registration of transesophageal echocardiography to x-ray fluoroscopy for cardiac interventions

    Hatt, Charles R.; Speidel, Michael A.; Raval, Amish N.

    2014-03-01

    We present a novel 2D/ 3D registration algorithm for fusion between transesophageal echocardiography (TEE) and X-ray fluoroscopy (XRF). The TEE probe is modeled as a subset of 3D gradient and intensity point features, which facilitates efficient 3D-to-2D perspective projection. A novel cost-function, based on a combination of intensity and edge features, evaluates the registration cost value without the need for time-consuming generation of digitally reconstructed radiographs (DRRs). Validation experiments were performed with simulations and phantom data. For simulations, in silica XRF images of a TEE probe were generated in a number of different pose configurations using a previously acquired CT image. Random misregistrations were applied and our method was used to recover the TEE probe pose and compare the result to the ground truth. Phantom experiments were performed by attaching fiducial markers externally to a TEE probe, imaging the probe with an interventional cardiac angiographic x-ray system, and comparing the pose estimated from the external markers to that estimated from the TEE probe using our algorithm. Simulations found a 3D target registration error of 1.08(1.92) mm for biplane (monoplane) geometries, while the phantom experiment found a 2D target registration error of 0.69mm. For phantom experiments, we demonstrated a monoplane tracking frame-rate of 1.38 fps. The proposed feature-based registration method is computationally efficient, resulting in near real-time, accurate image based registration between TEE and XRF.

  9. A 3D CZT hard x-ray polarimeter for a balloon-borne payload

    Caroli, E.; Alvarez, J. M.; Auricchio, N.;

    2012-01-01

    status of the Crab pulsar, i.e. the polarization level and direction. The detector with 3D spatial resolution is based on a CZT spectrometer in a highly segmented configuration designed to operate as a high performance scattering polarimeter. We discuss different configurations based on recent...

  10. Observation of parametric X-ray radiation in an anomalous diffraction region

    Alexeyev, V. I.; Eliseyev, A. N.; Irribarra, E.; Kishin, I. A.; Kubankin, A. S.; Nazhmudinov, R. M.

    2016-08-01

    A new possibility to expand the energy region of diffraction processes based on the interaction of relativistic charged particles with crystalline structures is presented. Diffracted photons related to parametric X-ray radiation produced by relativistic electrons are detected below the low energy threshold for the X-ray diffraction mechanism in crystalline structures for the first time. The measurements were performed during the interaction of 7 MeV electrons with a textured polycrystalline tungsten foil and a highly oriented pyrolytic graphite crystal. The experiment results are in good agreement with a developed model based on the PXR kinematical theory. The developed experimental approach can be applied to separate the contributions of real and virtual photons to the total diffracted radiation generated during the interaction of relativistic charged particles with crystalline targets.

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

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

    2016-05-01

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

  12. Twisted X-rays: incoming waveforms yielding discrete diffraction patterns for helical structures

    Friesecke, Gero; Jüstel, Dominik

    2015-01-01

    Conventional X-ray methods use incoming plane waves and result in discrete diffraction patterns when scattered at crystals. Here we find, by a systematic method, incoming waveforms which exhibit discrete diffraction patterns when scattered at helical structures. As examples we present simulated diffraction patterns of carbon nanotubes and tobacco mosaic virus. The new incoming waveforms, which we call twisted waves due to their geometric shape, are found theoretically as closed-form solutions to Maxwell's equations. The theory of the ensuing diffraction patterns is developed in detail. A twisted analogue of the Von Laue condition is seen to hold, with the peak locations encoding the symmetry and the helix parameters, and the peak intensities indicating the electronic structure in the unit cell. If suitable twisted X-ray sources can in the future be realized experimentally, it appears from our mathematical results that they will provide a powerful tool for directly determining the detailed atomic structure of ...

  13. Imaging whole Escherichia coli bacteria by using single-particle x-ray diffraction

    Miao, Jianwei; Hodgson, Keith O.; Ishikawa, Tetsuya; Larabell, Carolyn A.; LeGros, Mark A.; Nishino, Yoshinori

    2002-01-01

    We report the first experimental recording, to our knowledge, of the diffraction pattern from intact Escherichia coli bacteria using coherent x-rays with a wavelength of 2 Å. By using the oversampling phasing method, a real space image at a resolution of 30 nm was directly reconstructed from the diffraction pattern. An R factor used for characterizing the quality of the reconstruction was in the range of 5%, which demonstrated the reliability of the reconstruction process. The distribution of...

  14. Video-STM, LEED and X-ray diffraction investigations of PTCDA on graphite

    Ludwig, Christoph; Gompf, Bruno; Glatz, Wolfgang; Petersen, Jörg; Eisenmenger, Wolfgang; Möbus, Manfred; ZIMMERMANN, UWE; Karl, Norbert

    1992-01-01

    Thin films of the organic molecule perylene-3,4,9,10-tetracarboxylic-dianhydride ("PTCDA") on graphite (0001) have been investigated from the mono- to the multilayer regime with low energy electron diffraction (LEED), X-ray-diffraction in Bragg-Brentano geometry, and high resolution scanning tunneling microscopy (STM). These different methods proved epitaxial growth in a coincident superstructure and yielded congruent results concerning details of the crystallographic structure of the epilaye...

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

    K K Pandey; H K Poswal; A K Mishra; Abhilash Dwivedi; R Vasanthi; Nandini Garg; Surinder M Sharma

    2013-04-01

    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 powdered samples. A few recent high-pressure investigations are presented to demonstrate the capabilities of the beamline.

  16. Ultrafast coherent diffractive imaging of nanoparticles using X-ray free-electron laser radiation

    Coherent diffractive imaging with X-ray free-electron lasers (X-FEL) promises high-resolution structure determination of single microscopic particles without the need for crystallization. The diffraction signal of small samples can be very weak, a difficulty that can not be countered by merely increasing the number of photons because the sample would be damaged by a high absorbed radiation dose. Traditional X-ray crystallography avoids this problem by bringing many sample particles into a periodic arrangement, which amplifies the individual signals while distributing the absorbed dose. Depending on the sample, however, crystallization can be very difficult or even impossible. This thesis presents algorithms for a new imaging approach using X-FEL radiation that works with single, non-crystalline sample particles. X-FELs can deliver X-rays with a peak brilliance many orders of magnitude higher than conventional X-ray sources, compensating for their weak interaction cross sections. At the same time, FELs can produce ultra-short pulses down to a few femtoseconds. In this way it is possible to perform ultra-fast imaging, essentially ''freezing'' the atomic positions in time and terminating the imaging process before the sample is destroyed by the absorbed radiation. This thesis primarily focuses on the three-dimensional reconstruction of single (and not necessarily crystalline) particles using coherent diffractive imaging at X-FELs: in order to extract three-dimensional information from scattering data, two-dimensional diffraction patterns from many different viewing angles must be combined. Therefore, the diffraction signal of many identical sample copies in random orientations is measured. The main result of this work is a globally optimal algorithm that can recover the sample orientations solely based on the diffraction signal, enabling three-dimensional imaging for arbitrary samples. The problem of finding three-dimensional orientations is

  17. Phases quantification in titanium oxides by means of X-ray diffraction

    In this work two phases of titanium oxides are quantified which belong to the same crystalline system and by means of a computer program named Quanto created by the first author, contains the information for calculating the absorption coefficients, it can be quantified phases having one of the pure phases and the problem samples. In order to perform this work different mixtures of different titanium oxides were prepared measuring by means of the X-ray diffraction technique in the Siemens X-ray diffractometer of ININ which were processed with the Peakfit package and also they were evaluated by means of the computer program with the necessary information finding acceptable results. (Author)

  18. Scanning acoustic microscopy and X-ray diffraction investigation of near crack tip stresses

    Sathish, S.; Martin, R.W.

    2000-07-01

    Scanning Acoustic Microscopy has been used to measure and map the Rayleigh wave velocity and the Surface Skimming Longitudinal wave velocities near a crack tip in a sample of Ti-6Al-4V. X-ray diffraction measurements have been performed to map the stress in the same region of the sample. The differences in the contrast between the two acoustic velocity images and their sensitivity to stress are examined. Similarities between x-ray stress images and acoustic velocity images are discussed.

  19. Qualitative and quantitative determination of sediments phases in Chillon River by x-ray diffraction

    With this paper, we pretend to contribute with the recovery of Chillon River from a characterization of sediments. The objectives are the identification of pollution places along the bed of the Chillon River, from the Canta Province to Lima Province (Comas) and the determination of the preponderant factors of pollution. The qualitative and semi-quantitative determination of the sediments components have been carried out using the x-ray diffraction and x-ray fluorescence techniques, both of them will allow us to identify the pollute elements, for example the lead level in the Chillon River. (author)

  20. Development of a CZT spectroscopic 3D imager prototype for hard X ray astronomy

    Auricchio, N.; Caroli, E.; Basili, A.;

    2013-01-01

    measurement of the polarization status of the Crab nebula/pulsar between 100 and 500 keV. The prototype is made by packing 8 linear modules, each composed of one basic sensitive unit bonded onto a thin supporting ceramic layer. Each unit is a drift strip detector based on a CZT crystal, irradiated...... for the assembling of the proposed 3D CZT prototype and the result of the first performance tests on the CZT linear modules....

  1. Analysis of renal calculi by X-ray diffraction and electron microprobe: a comparison of two methods

    We analyzed 48 renal calculi by X-ray powder diffraction and electron microprobe techniques. In 35 of these, the presence of a minor constituent, not detected by X-ray diffraction, was revealed--hydroxyapatite was found in 24 stones, struvite in 6, and calcium oxalate in 5. The results of this study, as well as others, show that incomplete assignment of the crystalline constituents of urinary calculi is an inherent risk of the X-ray method and that conclusions concerning total chemical composition should be based on X-ray diffraction analyses coupled with data obtained from other analytical procedures

  2. In situ x-ray diffraction studies of three-dimensional C sub 6 sub 0 polymers

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

    2002-01-01

    In situ investigations into the P/T field of C sub 6 sub 0 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure.

  3. Rapid, low dose X-ray diffractive imaging of the malaria parasite Plasmodium falciparum

    Phase-diverse X-ray coherent diffractive imaging (CDI) provides a route to high sensitivity and spatial resolution with moderate radiation dose. It also provides a robust solution to the well-known phase-problem, making on-line image reconstruction feasible. Here we apply phase-diverse CDI to a cellular sample, obtaining images of an erythrocyte infected by the sexual stage of the malaria parasite, Plasmodium falciparum, with a radiation dose significantly lower than the lowest dose previously reported for cellular imaging using CDI. The high sensitivity and resolution allow key biological features to be identified within intact cells, providing complementary information to optical and electron microscopy. This high throughput method could be used for fast tomographic imaging, or to generate multiple replicates in two-dimensions of hydrated biological systems without freezing or fixing. This work demonstrates that phase-diverse CDI is a valuable complementary imaging method for the biological sciences and ready for immediate application. - Highlights: • Phase-diverse coherent X-ray diffraction microscopy provides high-resolution and high-contrast images of intact biological samples. • Rapid nanoscale resolution imaging is demonstrated at orders of magnitude lower dose than previously possible. • Phase-diverse coherent X-ray diffraction microscopy is a robust technique for rapid, quantitative, and correlative X-ray phase imaging

  4. Rapid, low dose X-ray diffractive imaging of the malaria parasite Plasmodium falciparum

    Jones, Michael W.M., E-mail: michael.jones@latrobe.edu.au [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Dearnley, Megan K. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Biochemistry and Molecular Biology, Bio21 Institute, The University of Melbourne, Victoria 3010 (Australia); Riessen, Grant A. van [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Abbey, Brian [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Melbourne Centre for Nanofabrication, Victoria 3168 (Australia); Putkunz, Corey T. [ARC Centre of Excellence for Coherent X-Ray Science, School of Physics, The University of Melbourne, Victoria 3010 (Australia); Junker, Mark D. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Vine, David J. [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); McNulty, Ian [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); Centre for Nanoscale Materials, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Nugent, Keith A. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Peele, Andrew G. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Australian Synchrotron, 800 Blackburn Road, Clayton 3168 (Australia); Tilley, Leann [ARC Centre of Excellence for Coherent X-Ray Science, Department of Biochemistry and Molecular Biology, Bio21 Institute, The University of Melbourne, Victoria 3010 (Australia)

    2014-08-01

    Phase-diverse X-ray coherent diffractive imaging (CDI) provides a route to high sensitivity and spatial resolution with moderate radiation dose. It also provides a robust solution to the well-known phase-problem, making on-line image reconstruction feasible. Here we apply phase-diverse CDI to a cellular sample, obtaining images of an erythrocyte infected by the sexual stage of the malaria parasite, Plasmodium falciparum, with a radiation dose significantly lower than the lowest dose previously reported for cellular imaging using CDI. The high sensitivity and resolution allow key biological features to be identified within intact cells, providing complementary information to optical and electron microscopy. This high throughput method could be used for fast tomographic imaging, or to generate multiple replicates in two-dimensions of hydrated biological systems without freezing or fixing. This work demonstrates that phase-diverse CDI is a valuable complementary imaging method for the biological sciences and ready for immediate application. - Highlights: • Phase-diverse coherent X-ray diffraction microscopy provides high-resolution and high-contrast images of intact biological samples. • Rapid nanoscale resolution imaging is demonstrated at orders of magnitude lower dose than previously possible. • Phase-diverse coherent X-ray diffraction microscopy is a robust technique for rapid, quantitative, and correlative X-ray phase imaging.

  5. Thermal transport in thin films measured by time-resolved, grazing incidence x-ray diffraction.

    Walko, D. A.; Sheu, Y.-M.; Trigo, M.; Reis, D. A. (X-Ray Science Division); (Univ. of Michigan,); (SLAC National Accelerator Lab.); (Stanford Univ.)

    2011-01-01

    We use depth- and time-resolved x-ray diffraction to study thermal transport across single crystal Bi films grown on sapphire in order to determine the thermal conductivity of the film and the Kapitza conductance of the interface. Ultrafast Ti:sapphire laser pulses were used to heat the films; x-ray diffraction then measured the film's lattice expansion. Use of grazing incidence diffraction geometry provided depth sensitivity, as the x-ray angle of incidence was varied near the critical angle. The shift of the film's Bragg peak position with time was used to determine the film temperature averaged over an x-ray penetration depth that could be selected by choice of the angle of incidence. For films that were thick compared to the laser penetration depth, we observed a large temperature gradient at early times. In this case, measurements with the incident angle near or well above the critical angle were more sensitive to the film conductivity or Kapitza conductance, respectively. For thinner films, however, cooling was dominated by the Kapitza conductance at all accessible time scales.

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

    In this work the structure of ternary GaxIn1−xP nanowires is investigated with respect to the chemical composition and homogeneity. The nanowires were grown by metal–organic vapor-phase epitaxy. For the investigation of ensemble fluctuations on several lateral length scales, X-ray diffraction reciprocal space maps have been analyzed. The data reveal a complicated varying materials composition across the sample and in the nanowires on the order of 20%. The use of modern synchrotron sources, where beam-sizes in the order of several 10 μm are available, enables us to investigate compositional gradients along the sample by recording diffraction patterns at different positions. In addition, compositional variations were found also within single nanowires in X-ray energy dispersive spectroscopy measurements. - Highlights: • GaInP nanowires grown by metal organic vapor phase epitaxy • X-ray diffraction and X-ray energy dispersive spectroscopy investigations • Gradients of the chemical composition found in single nanowires and the ensemble

  7. Composition variations in Cu{sub 2}ZnSnSe{sub 4} thin films analyzed by X-ray diffraction, energy dispersive X-ray spectroscopy, particle induced X-ray emission, photoluminescence, and Raman spectroscopy

    Nam, Dahyun [Department of Physics, Sogang University, Seoul 121-742 (Korea, Republic of); Opanasyuk, A.S.; Koval, P.V.; Ponomarev, A.G. [Department of Electronics and Computer Technology, Sumy State University, Sumy UA-40007 (Ukraine); Jeong, Ah Reum; Kim, Gee Yeong; Jo, William [Department of Physics, Ewha Womans University, Seoul 120-750 (Korea, Republic of); Cheong, Hyeonsik, E-mail: hcheong@sogang.ac.kr [Department of Physics, Sogang University, Seoul 121-742 (Korea, Republic of)

    2014-07-01

    Compositional and structural studies of Cu{sub 2}ZnSnSe{sub 4} (CZTSe) thin films were carried out by X-ray diffraction, energy dispersive X-ray spectroscopy (EDS), particle induced X-ray emission (PIXE), photoluminescence, and Raman spectroscopy. CZTSe thin films with different compositions were deposited on sodalime glass by co-evaporation. The composition of the films measured by two different methods, EDS and PIXE, showed significant differences. Generally, the Zn/Sn ratio measured by EDS is larger than that measured by PIXE. Both the micro-PIXE and the micro-Raman imaging results indicated the compositional and structural inhomogeneity of the sample. - Highlights: • Particle induced X-ray emission was used to analyze the composition of CZTSe films. • Energy dispersive X-ray spectroscopy tends to underestimate the Sn composition. • Local Raman intensity is related with the composition rather than the crystallinity.

  8. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex.

    Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

    2016-01-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

  9. Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

    Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

    2013-01-01

    Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

  10. Study of carbon steel corrosion layer by X-ray diffraction and absorption methods

    Malinovschi, V. [University of Pitesti, Research Center for Advanced Materials, Targul din Vale Street, No.1, 110040 Pitesti, Arges (Romania)]. E-mail: malinov@electra.upit.ro; Ducu, C. [University of Pitesti, Research Center for Advanced Materials, Targul din Vale Street, No.1, 110040 Pitesti, Arges (Romania); Aldea, N. [National Institutes for Research and Development for Isotopic and Molecular Technologies, P.O. Box 700, 3400 Cluj-Napoca (Romania); Fulger, M. [Institutes for Nuclear Research, P.O. Box 0402, 0300 Pitesti (Romania)

    2006-06-30

    To predict the behavior of structural metallic materials into the CANDU nuclear reactor, the oxide films on the surface were growth in a controlled manner using an autoclave simulating the environment specific to the nuclear reactor. In order to establish the structural changes of the oxide films, the X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX) and extended X-ray absorption fine structure spectroscopy (EXAFS) analysis were used. Analysis performed showed differences in morphology of the oxide films from carbon steel samples exposed under different conditions corresponding to primary and secondary circuits in CANDU nuclear reactor. The oxide phases were identified and the thicknesses of the films were calculated. The agreement between results obtained by these methods was discussed according to the microstructure of the samples.

  11. Collagen imaged by Coherent X-ray Diffraction: towards a complementary tool to conventional scanning SAXS

    Third generation x-ray sources offer unique possibilities for exploiting coherence in the study of materials. New insights in the structure and dynamics of soft condensed matter and biological samples can be obtained by coherent x-ray diffraction (CXD). However, the experimental procedures for applying these methods to collagen tissues are still under development. We present here an investigation for the optimal procedure in order to obtain high quality CXD data from collagen tissues. Sample handling and preparation and adequate coherence defining apertures are among the more relevant factors to take into account. The impact of the results is also discussed, in particular in comparison with the information that can be extracted from conventional scanning small angle x-ray scattering (SAXS). Images of collagen tissues obtained by CXD reconstructions will give additional information about the local structure with higher resolution and will complement scanning SAXS images.

  12. Quantitative comparison of imaging performance of x-ray interferometric imaging and diffraction enhanced imaging

    For detailed biomedical observations using the optimum phase-contrast x-ray imaging, quantitative comparisons of imaging performances of two major imaging methods--x-ray interferometric imaging (XII) and diffraction enhanced imaging (DEI)--were performed. Density sensitivity and spatial resolution of each imaging method were evaluated using phantom tomograms obtained by each method with the same x-ray dosage. For practical comparison of the methods, biological samples were also observed under the same conditions. The results show that XII has a higher sensitivity than that of DEI and is thus suitable for observation of soft biological tissues. On the other hand, DEI has a wider dynamic range of density and is thus suitable for observation of samples with large differences in density of different regions.

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

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

  14. Hybrid approach for structural modeling of biological systems from X-ray free electron laser diffraction patterns.

    Tokuhisa, Atsushi; Jonic, Slavica; Tama, Florence; Miyashita, Osamu

    2016-06-01

    We present a new hybrid approach for structural modeling using X-ray free electron laser (XFEL) diffraction patterns from non-crystalline biological samples. Reconstruction of a 3D structure requires a large number of diffraction patterns; however, in the current XFEL experiments with biological systems, the analysis often relies on a small number of 2D diffraction patterns. In this study, we explore the strategies to identify plausible 3D structural models by combining the 2D analysis of such diffraction patterns with computational modeling (normal mode analysis or molecular dynamics simulations). As the first step toward such hybrid modeling, we established a protocol to assess the agreement between the model structure and the target XFEL diffraction pattern and showed that XFEL data can be used to study the conformational transitions of biological molecules. We tested the proposed algorithms using data of three biomolecular complexes of different sizes (elongation factor 2, CCM virus, and ribosome) and examined the experimental conditions that are required to perform such studies, in particular the XFEL beam intensity requirements. The results indicate that the current beam intensity is close to a strength that enables us to study conformational transitions of macromolecules, such as ribosomes. The proposed algorithm can be combined with molecular mechanics approaches, such as molecular dynamics simulations and normal mode analysis, to generate a large number of candidate structures to perform hybrid structural modeling. PMID:26972893

  15. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vekemans, Bart [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Verhaeven, Eddy [Antwerp University, Faculty of Design Sciences, Mutsaardstraat 31, B-2000 Antwerpen (Belgium); Tack, Pieter; De Wolf, Robin; Garrevoet, Jan [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium)

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg–Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials.

  16. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg–Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials

  17. Characterization of nanophase materials by x-ray diffraction and computer simulation

    X-ray diffraction experiments on nanophase Pd have been performed with the primary goal of determining the nature of grain boundary structures in nanophase materials. A kinematical diffraction analysis has been developed to interpret x-ray θ-2θ data by comparing actual scans with scans produced by computer simulation. This simulation program has been used to explore the effects on diffracted intensity of a variety of microstructural and grain boundary structural parameters such as void concentration, grain size, grain boundary width, and changes in interplanar spacing and density in grain boundary regions. It has been found that a reasonable match to experimental data is produced by at least two model structures; in one, the material contains randomly positioned voids or vacancies, while in the other, the interplanar spacings in grain boundary regions are varied with respect to the spacings found in the grain interiors

  18. An X-ray diffraction study on a single rod outer segment from frog retina

    X-ray diffraction was recorded from retinal rod outer segments of frog using a microbeam. X-ray diffraction patterns were recorded from isolated single rod outer segments of frog. The outer segments in Ringer’s solution were exposed to a 6 µm microbeam (15 keV) at the BL40XU beamline, SPring-8. The diffraction pattern demonstrated a remarkable regularity in the stacking and flatness of the disk membranes. The electron density profile calculated from the intensity of up to tenth-order reflections showed a pair of bilayers that comprise a disk membrane. The structure of the disk membrane and the changes in the profile on swelling generally agreed with previous reports. Radiation damage was significant with an irradiation of 5 × 105 Gy which is much lower than the known damaging dose on proteins at the liquid-nitrogen temperature

  19. Automatic detection and high resolution fine structure analysis of conic X-ray diffraction lines

    Bauch, J.; Henschel, F. [TU Dresden, Institut fuer Werkstoffwissenschaft, 01069 Dresden (Germany); Schulze, M. [TU Dresden, Institut fuer Photogrammetrie und Fernerkundung, 01069 Dresden (Germany)

    2011-05-15

    The presented method demonstrates a first step in the development of a high resolution ''Residual stress microscope'' and facilitates through the implementation of largely automated procedures a fast detection of diffraction lines in the form of conic sections. It has been implemented for, but is not exclusively used for the Kossel technique and the ''X-ray Rotation-Tilt Method'' (XRT). The resulting multifaceted evaluable data base of many X-ray diffraction radiographies can be used not only for the systematic analysis of anomalies in diffraction lines (reflection fine structure), but also for direct calculation and output of precision residual stress tensors. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  20. NXDC-neutron and x-ray diffraction code for crystal structures calculations

    A computer program NXDC for the calculations of neutron diffraction and x-ray diffraction intensities is reported. The program is very flexible and allows the intensity of a reflection with a given Miller indices to be calculated if the unit cell and its contents are specified together with the equipement used Neutrons or X-rays-and if necessary introducing temperature and absorption factors corrections. For the refinement of crystal structures provision is made for the comparison of the calculated intensities and the intergrated intensities observed from the diffraction diagrams using the least-squares analysis to obtain the reliability factor R. The program is written in FORTRAN Iv and is very suitable for minicomputers

  1. Preparation of Zn-Ni-Fe-Cr Ferrites and characterisation by X-ray diffraction

    Four samples of the spinel oxide ZnxNi1-xFeCrO4 with x=0.2, 0.4, 0.6 and 0.8 have been prepared using the conventional solid state sintering technique. The stoichiometric mixture of high purity (99.99%) oxides of ZnO, NiO, Fe2O3 and Cr2O3 were taken as starting materials. The samples were pre-sintered at a temperature of 1000oC for 6 hours and then sintered at a temperature of 1250''oC for 8 hours. X-ray diffraction experiments on all the specimens were performed using an X-ray diffractometer (Shimadzu XRD-6000, Japan) with CuK α radiation of wavelength λ =1.540598 A0. For all the samples X-ray diffraction patterns were recorded in the angular range 10o ≤ 2θ ≤ 90o. The diffraction patterns thus obtained showed sharp lines corresponding to the single phase cubic spinel structure. The Bragg diffraction peaks in the pattern could be indexed corresponding to the indexing scheme of the spinel structure. The prepared samples were thus characterized to be spinel structure. The prepared samples were thus characterized to be spinel ferrites. The cell parameters have been calculated from the diffraction patterns which increases with increasing diamagnetic Zn2+ substitution in the system

  2. Dynamical X-ray Diffraction from In x Ga1- x As Heterostructures with Dislocations

    Rago, P. B.; Ayers, J. E.

    2013-08-01

    High-resolution x-ray diffraction is an important nondestructive tool for structural characterization of semiconductor heterostructures, and the diffraction intensity profiles contain information on the depth profiles of strain, composition, and defect densities in device heterostructures. Much of this information remains inaccessible because the lack of phase information prevents direct inversion of the rocking curves. The current practice is to use dynamical simulations in conjunction with a curve-fitting procedure to indirectly extract the profiles of strain and composition, but such dynamical simulations have been based on perfect, dislocation-free laminar crystals, which renders the analysis inapplicable to highly mismatched structures containing dislocation densities greater than about 106 cm-2. In this work we present a dynamical model for Bragg x-ray diffraction in semiconductor device structures with nonuniform composition, strain, and dislocation density, which is based on the Takagi-Taupin equation for distorted crystals and accounts for the diffuse scattering arising from the strain mosaicity and angular mosaicity associated with dislocations. We show theoretically that the x-ray diffraction profiles from In x Ga1- x As/GaAs (001) heterostructures are strongly affected by the depth distribution of the dislocation density as well as the composition and strain, so that in principle all three distributions may be obtained by the analysis of the measured diffraction profiles.

  3. Further optimisation of a simple X-ray diffraction instrument for portable and planetary applications

    This paper extends the work presented in a previous publication (Hansford, 2011 , subsequently referred to as Paper 1) to optimise the performance of a simple reflection-mode X-ray diffraction instrument with respect to the geometrical configuration. Both papers focus on the maximisation or minimisation of quantifiable characteristics of the X-ray beam incident on the sample in order to optimise the peak heights and widths in the resulting diffractogram. The reason for this approach is mathematical tractability, and its success relies on the relationship between the incident beam characteristics and the diffractogram properties. Part of Paper 1 was devoted to the minimisation of the equatorial divergence angle of the X-ray beam, while keeping the total X-ray flux constant, in order to minimise the diffractogram peak widths. While equatorial divergence and peak widths are certainly linked, their relationship is complex and depends quite significantly on other geometric parameters. An alternative optimisation approach is taken in this paper, focusing on the maximisation of the X-ray flux and minimisation of the incident beam axial divergence, while equatorial divergence is kept constant to ensure at least reasonable resolution. The rationale for this approach is that the incident beam flux and the axial divergence angle are more directly linked to diffractogram peak heights and peak asymmetry, respectively. Families of candidate geometric solutions result from this approach which is regarded as advantageous because there is no unique optimised solution and it allows the parameter space to be fully explored.

  4. X-ray Emission Spectroscopy in Magnetic 3d-Transition Metals

    Iota, V; Park, J; Baer, B; Yoo, C; Shen, G

    2003-11-18

    The application of high pressure affects the band structure and magnetic interactions in solids by modifying nearest-neighbor distances and interatomic potentials. While all materials experience electronic changes with increasing pressure, spin polarized, strongly electron correlated materials are expected to undergo the most dramatic transformations. In such materials, (d and f-electron metals and compounds), applied pressure reduces the strength of on-site correlations, leading to increased electron delocalization and, eventually, to loss of its magnetism. In this ongoing project, we study the electronic and magnetic properties of Group VIII, 3d (Fe, Co and Ni) magnetic transition metals and their compounds at high pressures. The high-pressure properties of magnetic 3d-transition metals and compounds have been studied extensively over the years, because of iron being a major constituent of the Earth's core and its relevance to the planetary modeling to understand the chemical composition, internal structure, and geomagnetism. However, the fundamental scientific interest in the high-pressure properties of magnetic 3d-electron systems extends well beyond the geophysical applications to include the electron correlation-driven physics. The role of magnetic interactions in the stabilization of the ''non-standard'' ambient pressure structures of Fe, Co and Ni is still incompletely understood. Theoretical studies have predicted (and high pressure experiments are beginning to show) strong correlations between the electronic structure and phase stability in these materials. The phase diagrams of magnetic 3d systems reflect a delicate balance between spin interactions and structural configuration. At ambient conditions, the crystal structures of {alpha}-Fe(bcc) and {var_epsilon}-Co(hcp) phases depart from the standard sequence (hcp {yields} bcc{yields} hcp {yields} fcc), as observed in all other non-magnetic transition metals with increasing the d

  5. The application of X-ray, γ-ray and neutron diffraction to the characterization of single crystal perfection

    The work is divided into the following three chapters: 1) diffraction by perfect and imperfect crystals, 2) experimental apparatus (describing gamma ray, X-ray and neutron diffractometers), 3) application of diffraction methods to the development of neutron monochromators. (WBU)

  6. Three-dimensional characterization of microstructurally small fatigue-crack evolution using quantitative fractography combined with post-mortem X-ray tomography and high-energy X-ray diffraction microscopy

    An experimental methodology based on post-mortem measurements is proposed to quantify rates of propagation and crack-surface crystallography of a 3-D, naturally nucleated, microstructurally small fatigue crack (MSFC) in a polycrystalline aluminum alloy (Al–Mg–Si). The post-mortem characterization involves: scanning electron microscopy-based fractography to measure crack-front projections (marker bands) at known cycle counts during the load history, X-ray computed tomography to provide high-resolution reconstructions of the 3-D crack-surface morphology, and near-field high-energy X-ray diffraction microscopy to provide 3-D grain geometries and orientations adjacent to fatigue-crack surfaces. Local MSFC-propagation rates are measured by accounting for the 3-D crack-surface morphology and varied by two orders of magnitude in the Al–Mg–Si specimen. Both intergranular and transgranular MSFC evolution were observed, with the latter occurring along a wide range of crystallographic planes. The findings demonstrate: (i) the complexity and variability of 3-D MSFC evolution in the Al–Mg–Si alloy; and (ii) the viability of the post-mortem characterization approach for quantifying 3-D MSFC evolution in polycrystalline alloys

  7. Imaging outside the box: Resolution enhancement in X-ray coherent diffraction imaging by extrapolation of diffraction patterns

    Coherent diffraction imaging is a high-resolution imaging technique whose potential can be greatly enhanced by applying the extrapolation method presented here. We demonstrate the enhancement in resolution of a non-periodical object reconstructed from an experimental X-ray diffraction record which contains about 10% missing information, including the pixels in the center of the diffraction pattern. A diffraction pattern is extrapolated beyond the detector area and as a result, the object is reconstructed at an enhanced resolution and better agreement with experimental amplitudes is achieved. The optimal parameters for the iterative routine and the limits of the extrapolation procedure are discussed

  8. Toward diffraction-limited lightweight x-ray optics for astronomy

    Zhang, William W.; Chan, Kai-Wing; Riveros, Raul E.; Saha, Timo T.

    2015-09-01

    Five characteristics determine the utility of an x-ray optics technology for astronomy: (1) angular resolution, (2) field of view, (3) energy bandwidth, (4) mass per unit photon collecting area, and (5) production cost per unit photon collecting area. These five desired characteristics are always in conflict with each other. As a result, every past, current, and future x-ray telescope represents an astronomically useful compromise of these five characteristics. In this paper, we outline and report the proof of concept of a new approach of using single-crystal silicon to make lightweight x-ray optics. This approach combines the grinding polishing process, which is capable of making diffraction-limited optics of any kind, with the stress-free nature of single-crystal silicon, which enables post-fabrication light-weighting without distortion. As such this technology has the potential of making diffraction-limited lightweight x-ray optics for future astronomical missions, achieving unprecedented performance without incurring prohibitive mass and cost increase.

  9. Coherent convergent-beam time-resolved X-ray diffraction.

    Spence, John C H; Zatsepin, Nadia A; Li, Chufeng

    2014-07-17

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. PMID:24914153

  10. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements

    Barty, Anton; Caleman, Carl; Aquila, Andrew; Timneanu, Nicusor; Lomb, Lukas; White, Thomas A.; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R. M.; Barthelmess, Miriam; Bogan, Michael J.; Bostedt, Christoph; Bozek, John D.; Coffee, Ryan; Coppola, Nicola; Davidsson, Jan; DePonte, Daniel P.; Doak, R. Bruce; Ekeberg, Tomas; Elser, Veit; Epp, Sascha W.; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Fromme, Petra; Graafsma, Heinz; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y.; Hartmann, Robert; Hartmann, Andreas; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Hunter, Mark S.; Johansson, Linda; Kassemeyer, Stephan; Kimmel, Nils; Kirian, Richard A.; Liang, Mengning; Maia, Filipe R. N. C.; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V.; Nass, Karol; Neutze, Richard; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Scott, Howard; Schlichting, Ilme; Schulz, Joachim; Seibert, M. Marvin; Shoeman, Robert L.; Sierra, Raymond G.; Soltau, Heike; Spence, John C. H.; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Ullrich, Joachim; Wang, X.; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia B.; Chapman, Henry N.

    2013-01-01

    X-ray free-electron lasers have enabled new approaches to the structural determination of protein crystals that are too small or radiation-sensitive for conventional analysis1. For sufficiently short pulses, diffraction is collected before significant changes occur to the sample, and it has been predicted that pulses as short as 10 fs may be required to acquire atomic-resolution structural information1–4. Here, we describe a mechanism unique to ultrafast, ultra-intense X-ray experiments that allows structural information to be collected from crystalline samples using high radiation doses without the requirement for the pulse to terminate before the onset of sample damage. Instead, the diffracted X-rays are gated by a rapid loss of crystalline periodicity, producing apparent pulse lengths significantly shorter than the duration of the incident pulse. The shortest apparent pulse lengths occur at the highest resolution, and our measurements indicate that current X-ray free-electron laser technology5 should enable structural determination from submicrometre protein crystals with atomic resolution. PMID:24078834

  11. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    Reischig, Péter; Helfen, Lukas; Wallert, Arie; Baumbach, Tilo; Dik, Joris

    2013-06-01

    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.

  12. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    Reischig, Peter [Karlsruhe Institute of Technology, Institute for Photon Science and Synchrotron Radiation, Eggenstein-Leopoldshafen (Germany); Delft University of Technology, Department of Materials Science and Engineering, Delft (Netherlands); Helfen, Lukas [Karlsruhe Institute of Technology, Institute for Photon Science and Synchrotron Radiation, Eggenstein-Leopoldshafen (Germany); European Synchrotron Radiation Facility, BP 220, Grenoble Cedex (France); Wallert, Arie [Rijksmuseum, Postbus 74888, Amsterdam (Netherlands); Baumbach, Tilo [Karlsruhe Institute of Technology, Institute for Photon Science and Synchrotron Radiation, Eggenstein-Leopoldshafen (Germany); Dik, Joris [Delft University of Technology, Department of Materials Science and Engineering, Delft (Netherlands)

    2013-06-15

    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.)

  13. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    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.)

  14. Digital Pulse Processor for ION Beam Microprobe and Micro X Ray Fluorescence 2-D and 3-D Imaging

    For a long time, the implementation of optimal pulse processing in nuclear spectrometry was only possible with analogue electronic components. Following the development of fast analogue to digital converters, field programmable gate arrays, and digital signal processors, it became feasible to digitize pulses after a preamplifier or phototube and process them in a real time. Therefore, digital electronics, which were limited to data storage and control of the acquisition process, became feasible for signal processing as well. This brought numerous benefits, such as better energy resolution with higher data throughput, reduced size, easier upgrading, the ability to automate adjustment and control of the complete data acquisition process, and self-diagnostic capability. In the same time, evaluation of the Electronic Design Automation tools and Intellectual Property industry enables a System-On-a-Chip paradigm on high density reprogrammable devices and allows new approach for system level design. Such a design provides opportunity for small laboratories to develop a compact 'all digital' customized instrumentation. In this work, we presented a design of FPGA IP core for high resolution, digital X ray, γ ray or particle spectrometry using high level FPGA design tool (Xilinx System Generator and Matlab - Simulink). The IP core has been used to build a simple low cost digital spectrometer (Spartan 3 FPGA based) and advance system for ion beam microprobe and X ray fluorescence 2-D and 3-D imaging. (Virtex 4 FPGA based). (author)

  15. Mobile of 3D-X-Ray tomography for analysis of planar defects in welds by 'TomoCAR'

    Tomographical Computer Aided Radiology (TomoCAR) is based on the mechanical position control of an X-ray tube in front of a welding seam and the application of a planar array detector behind it. Several hundred radiometric projections in small angle steps are acquired. The tomographical reconstruction allows the three-dimensional (3D) representation of the defects. A new radiometric array detector system with a small internal unsharpness and high image contrast is used for the 2- and 3-dimensional visualization and sizing of planar defects with a defect opening of less than 100 μm. This detector is based on a CMOS-flat panel with a direct converting CdTe-single crystal layer. The small design allows the application of the mobile testing equipment for mechanized X-ray inspection in industrial plants. The physical pixel size of the detector amounts to 0,1x0,1 mm2. Nevertheless, this system yields a better spatial resolution than indirect converting detectors (e.g. cameras with fluorescence layers of Gd2O2S). It allows the reliable detection of planar defects with openings far below the detector pixel size by subpixel resolution. 'TomoCAR' is qualified at present in the context with a German pilot study following to the ENIQ guidelines for the employment within the nuclear power industry. (author)

  16. Study of transmission grating diffraction efficiencies for soft X-ray

    1999-01-01

    Tansmission grating spectrometers are extensively used tomeasure absolute X-ray spectra in a photon-energy rangebelow 1000 eV. The transmission grating, as its dispersive element, must be calibrated to obtain its diffraction efficiencies.Calibrations of absolute diffraction efficiencies of the transmissiongrating at photon energy of 844 eV have been carried out onBeijing Synchrotron Radiation Facility. With the aid of gratingmodel, all of the grating structure parameters have been determinedand the absolute diffraction efficiencies in a photon-energy rangebelow 2000 eV have also been calculated and discussed.

  17. Selective imaging of nano-particle contrast agents by a single-shot x-ray diffraction technique

    Stein, Ashley F.; Ilavsky, Jan; Kopace, Rael; Bennett, Eric E.; Wen, Han

    2010-01-01

    Iron oxide nano-particles have very different x-ray diffraction properties from tissue. They can be clearly visualized against suppressed tissue background in a single-shot x-ray diffraction imaging technique. This technique is able to acquire both diffraction and absorption images from a single grating-modulated projection image through analysis in the spatial frequency domain. We describe the use of two orthogonal transmission gratings to selectively retain diffraction signal from iron oxid...

  18. 3D images of paper obtained by phase-contrast X-ray microtomography: image quality and binarisation

    A series of paper samples was investigated using high-resolution phase-contrast microtomography at the beamline ID 22 of the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. It was shown that X-ray microtomography is a non-destructive method suitable for high resolution depicting real 3D-paper structures. The method detects highly localised changes in the refractive index of the sample, such as fibre-pore interfaces. The resulting tomograms represented an outlined image of the fibre structure with an image resolution of 1 μm. Analyses were performed in dry state, but in addition some were done in wet state. The raw data obtained were transformed into 3D images. The reconstructed slices were in general of rather good quality, even if both noise and ring-like artifacts were observed. These required special filtering efforts before a segmented binary volume could be obtained for further use of the data. This approach was made up of semi-automatic routines to convert the structure into a binary format. The resulting binary volumes can be used for further characterisation of the 3D-paper structure

  19. 3D deformation and strain analysis in compacted sugar using x-ray microtomography and digital volume correlation

    Understanding the displacement of granular beds under compaction is important for a range of industrial, geological and civil engineering applications. Such materials exhibit inhomogeneous internal displacements including strain localization, which mean that a method for the in situ evaluation of internal 3D displacement fields at high spatial resolutions would be a major development. This paper presents results from the compaction of a cylindrical bed of sugar, with diameter 7.0 mm and height 8.2 mm, using x-ray microtomography to evaluate the internal structure and digital volume correlation to calculate 3D displacement information from these data. In contrast to previous studies, which generally track a small number of marker particles, the research here uses the natural structure of the sugar to provide a random pattern for 3D image correlation, allowing full-field information to be captured. The results show good agreement when compared with a well-established 2D image correlation technique; moreover, they indicate structural features associated with deformation of granular materials that would not necessarily be observed in a 2D slice

  20. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as may occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period

  1. The Scherrer equation and the dynamical theory of X-ray diffraction.

    Muniz, Francisco Tiago Leitão; Miranda, Marcus Aurélio Ribeiro; Morilla Dos Santos, Cássio; Sasaki, José Marcos

    2016-05-01

    The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6 and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm(-1) the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm. PMID:27126115

  2. Influence of preferred orientation of minerals in the mineralogical identification process by X-ray diffraction

    Silva, Amanda Luzia da; Oliveira, Arno H. de [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear; Fernandes, Maria Lourdes Souza, E-mail: lourdesfernandes@ufmg.b [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Inst. de GeoCiencias. Centro de Pesquisa Professor Manoel Teixeira da Costa

    2011-07-01

    The X-ray diffraction corresponds to one of the main techniques for characterization of microstructures in crystalline materials, widely used in the identification of minerals in samples of geological materials. Some minerals have a property called preferred orientation which corresponds to the orientation tendency of the crystals of ground minerals to orient themselves in certain directions according to a preferred crystallographic plane. This property affects the analysis by X-ray diffraction and this fact can generates erroneous results in the characterization. The purpose of this study is to identify the negative influence of the preferred orientation of a mineral in the generation of diffraction patterns obtained in the X-ray diffraction analysis. For this, a sample of muscovite, a mineral of mica group, was prepared by two different methods: the frontal method and the back loading method. In the analysis using the frontal method there was displacement of the XRD pattern in the abscissa axis, where it was observed changes in interplanar distance and angle 2{theta} values, which are essential information for characterization and identification of a mineral. In the analysis using the back loading method, the generated XRD pattern showed no displacement in the axis of abscissas and showed interplanar distance and angle 2{theta} values closer to the real values for the muscovite. The results showed that one can only make improvements to the process of sample preparation minimizing the effect of preferred orientation in the analysis. There is no need to change conditions of diffractometer measurements. (author)

  3. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals.

    Dao, E Han; Sierra, Raymond G; Laksmono, Hartawan; Lemke, Henrik T; Alonso-Mori, Roberto; Coey, Aaron; Larsen, Kevin; Baxter, Elizabeth L; Cohen, Aina E; Soltis, S Michael; DeMirci, Hasan

    2015-07-01

    In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecond X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser. PMID:26798805

  4. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    E. Han Dao

    2015-07-01

    Full Text Available In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecond X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.

  5. Identification of inversion domains in KTiOPO{sub 4}via resonant X-ray diffraction

    Fabrizi, Federica, E-mail: federica.fabrizi@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, OX11 0DE (United Kingdom); Thomas, Pamela A. [Department of Physics, University of Warwick, Coventry, CV4 7AL (United Kingdom); Nisbet, Gareth; Collins, Stephen P. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, OX11 0DE (United Kingdom)

    2015-05-14

    The identification and high-resolution mapping of the absolute crystallographic structure in multi-domain ferroelectric KTiOPO{sub 4} is achieved through a novel synchrotron X-ray diffraction method. On a single Bragg reflection, the intensity ratio in resonant diffraction below and above the Ti absorption K edge demonstrates a domain contrast up to a factor of ∼270, thus implementing a non-contact, non-destructive imaging technique with micrometre spatial resolution, applicable to samples of arbitrarily large dimensions. A novel method is presented for the identification of the absolute crystallographic structure in multi-domain polar materials such as ferroelectric KTiOPO{sub 4}. Resonant (or ‘anomalous’) X-ray diffraction spectra collected across the absorption K edge of Ti (4.966 keV) on a single Bragg reflection demonstrate a huge intensity ratio above and below the edge, providing a polar domain contrast of ∼270. This allows one to map the spatial domain distribution in a periodically inverted sample, with a resolution of ∼1 µm achieved with a microfocused beam. This non-contact, non-destructive technique is well suited for samples of large dimensions (in contrast with traditional resonant X-ray methods based on diffraction from Friedel pairs), and its potential is particularly relevant in the context of physical phenomena connected with an absence of inversion symmetry, which require characterization of the underlying absolute atomic structure (such as in the case of magnetoelectric coupling and multiferroics)

  6. The structural analysis of zinc borate glass by laboratory EXAFS and X-ray diffraction measurements

    The structure of zinc borate glass has been investigated by laboratory EXAFS and X-ray diffraction measurement as preliminary investigations for the detailed study in SPring-8. The zinc borate glass was prepared in the range from 40 to 65 mol% of zinc oxide content. The X-ray diffraction was measured by horizontal θ-θ goniometer with 60 kV and 300 mA output of Mo target. The EXAFS of zinc borate glass was measured by laboratory EXAFS system with 20 kV, 100 mA output of Mo target for the K absorption edge of zinc atom. From the X-ray diffraction and the EXAFS measurements, it is found that the zinc ion is surrounded by four oxygen atoms and formed a tetrahedral structure whose (Zn-O) distance is about 2 A and that the structure is unchanged with the zinc oxide content. The diffraction data show that the neighboring structure of boron atom transforms from BO4 tetrahedra to BO3 tetragonal planar structure with increasing of the zinc oxide content. (author)

  7. 3D electron density imaging using single scattered x rays with application to breast CT and mammographic screening

    van Uytven, Eric Peter

    Screening mammography is the current standard in detecting breast cancer. However, its fundamental disadvantage is that it projects a 3D object into a 2D image. Small lesions are difficult to detect when superimposed over layers of normal tissue. Commercial Computed Tomography (CT) produces a true 3D image yet has a limited role in mammography due to relatively low resolution and contrast. With the intent of enhancing mammography and breast CT, we have developed an algorithm which can produce 3D electron density images using a single projection. Imaging an object with x rays produces a characteristic scattered photon spectrum at the detector plane. A known incident beam spectrum, beam shape, and arbitrary 3D matrix of electron density values enable a theoretical scattered photon distribution to be calculated. An iterative minimization algorithm is used to make changes to the electron density voxel matrix to reduce regular differences between the theoretical and the experimentally measured distributions. The object is characterized by the converged electron density image. This technique has been validated in simulation using data produced by the EGSnrc Monte Carlo code system. At both mammographic and CT energies, a scanning polychromatic pencil beam was used to image breast tissue phantoms containing lesion-like inhomogeneities. The resulting Monte Carlo data is processed using a Nelder-Mead iterative algorithm (MATLAB) to produce the 3D matrix of electron density values. Resulting images have confirmed the ability of the algorithm to detect various 1x1x2.5 mm3 lesions with calcification content as low as 0.5% (p<0.005) at a dose comparable to mammography.

  8. Classification and quantification of pore shapes in sandstone reservoir rocks with 3-D X-ray micro-computed tomography

    Schmitt, Mayka; Halisch, Matthias; Müller, Cornelia; Peres Fernandes, Celso

    2016-02-01

    Recent years have seen a growing interest in the characterization of the pore morphologies of reservoir rocks and how the spatial organization of pore traits affects the macro behavior of rock-fluid systems. With the availability of 3-D high-resolution imaging, such as x-ray micro-computed tomography (µ-CT), the detailed quantification of particle shapes has been facilitated by progress in computer science. Here, we show how the shapes of irregular rock particles (pores) can be classified and quantified based on binary 3-D images. The methodology requires the measurement of basic 3-D particle descriptors (length, width, and thickness) and a shape classification that involves the similarity of artificial objects, which is based on main pore network detachments and 3-D sample sizes. Two main pore components were identified from the analyzed volumes: pore networks and residual pore ganglia. A watershed algorithm was applied to preserve the pore morphology after separating the main pore networks, which is essential for the pore shape characterization. The results were validated for three sandstones (S1, S2, and S3) from distinct reservoirs, and most of the pore shapes were found to be plate- and cube-like, ranging from 39.49 to 50.94 % and from 58.80 to 45.18 % when the Feret caliper descriptor was investigated in a 10003 voxel volume. Furthermore, this study generalizes a practical way to correlate specific particle shapes, such as rods, blades, cuboids, plates, and cubes to characterize asymmetric particles of any material type with 3-D image analysis.

  9. Critical dimension small angle X-ray scattering measurements of FinFET and 3D memory structures

    Settens, Charles; Bunday, Benjamin; Thiel, Brad; Kline, R. Joseph; Sunday, Daniel; Wang, Chengqing; Wu, Wen-li; Matyi, Richard

    2013-04-01

    We have demonstrated that transmission critical dimension small angle X-ray scattering (CD-SAXS) provides high accuracy and precision CD measurements on advanced 3D microelectronic architectures. The competitive advantage of CD-SAXS over current 3D metrology methods such as optical scatterometry is that CD-SAXS is able to decouple and fit cross-section parameters without any significant parameter cross-correlations. As the industry aggressively scales beyond the 22 nm node, CD-SAXS can be used to quantitatively measure nanoscale deviations in the average crosssections of FinFETs and high-aspect ratio (HAR) memory devices. Fitting the average cross-section of 18:1 isolated HAR contact holes with an effective trapezoid model yielded an average pitch of 796.9 +/- 0.4 nm, top diameter of 70.3 +/- 0.9 nm, height of 1088 +/- 4 nm, and sidewall angle below 0.1°. Simulations of dense 40:1 HAR contact holes and FinFET fin-gate crossbar structures have been analyzed using CD-SAXS to inquire the theoretical precision of the technique to measure important process parameters such as fin CD, height, and sidewall angle; BOX etch recess, thickness of hafnium oxide and titanium nitride layers; gate CD, height, and sidewall angle; and hafnium oxide and titanium nitride etch recess. The simulations of HAR and FinFET structures mimic the characteristics of experimental data collected at a synchrotron x-ray source. Using the CD-SAXS simulator, we estimate the measurement capabilities for smaller similar structures expected at future nodes to predict the applicability of this technique to fulfill important CD metrology needs.

  10. Significant acceleration of 2D-3D registration-based fusion of ultrasound and x-ray images by mesh-based DRR rendering

    Kaiser, Markus; John, Matthias; Borsdorf, Anja; Mountney, Peter; Ionasec, Razvan; Nöttling, Alois; Kiefer, Philipp; Seeburger, Jörg; Neumuth, Thomas

    2013-03-01

    For transcatheter-based minimally invasive procedures in structural heart disease ultrasound and X-ray are the two enabling imaging modalities. A live fusion of both real-time modalities can potentially improve the workflow and the catheter navigation by combining the excellent instrument imaging of X-ray with the high-quality soft tissue imaging of ultrasound. A recently published approach to fuse X-ray fluoroscopy with trans-esophageal echo (TEE) registers the ultrasound probe to X-ray images by a 2D-3D registration method which inherently provides a registration of ultrasound images to X-ray images. In this paper, we significantly accelerate the 2D-3D registration method in this context. The main novelty is to generate the projection images (DRR) of the 3D object not via volume ray-casting but instead via a fast rendering of triangular meshes. This is possible, because in the setting for TEE/X-ray fusion the 3D geometry of the ultrasound probe is known in advance and their main components can be described by triangular meshes. We show that the new approach can achieve a speedup factor up to 65 and does not affect the registration accuracy when used in conjunction with the gradient correlation similarity measure. The improvement is independent of the underlying registration optimizer. Based on the results, a TEE/X-ray fusion could be performed with a higher frame rate and a shorter time lag towards real-time registration performance. The approach could potentially accelerate other applications of 2D-3D registrations, e.g. the registration of implant models with X-ray images.

  11. Crystallization and preliminary X-ray diffraction analysis of maize aldose reductase

    Kiyota, Eduardo [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Sousa, Sylvia Morais de [Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Santos, Marcelo Leite dos; Costa Lima, Aline da [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Menossi, Marcelo [Departamento de Genética e Evolução, Instituto de Biologia, Universidade Estadual de Campinas, Campinas-SP (Brazil); Yunes, José Andrés [Laboratório de Biologia Molecular, Centro Infantil Boldrini, Campinas-SP (Brazil); Aparicio, Ricardo, E-mail: aparicio@iqm.unicamp.br [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil)

    2007-11-01

    Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 Å resolution are reported. Maize aldose reductase (AR) is a member of the aldo-keto reductase superfamily. In contrast to human AR, maize AR seems to prefer the conversion of sorbitol into glucose. The apoenzyme was crystallized in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 47.2, b = 54.5, c = 100.6 Å and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 Å was obtained after data reduction. Phasing was carried out by an automated molecular-replacement procedure and structural refinement is currently in progress. The refined structure is expected to shed light on the functional/enzymatic mechanism and the unusual activities of maize AR.

  12. Microfibril angle variability in Masson Pine (Pinus massoniana Lamb.) using X-ray diffraction

    Zhang Bo; Fei Ben-hua; Yu Yan; Zhao Rong-jun

    2007-01-01

    The microfibril angle of fiber walls is an ultra-microscopic feature affecting the performance of wood products. It is therefore essential to get more definitive information to improve selection and utilization. X-ray diffraction is a rapid method for measuring micro fibril angles. In this paper, the variability of microfibril angle in plantation-grown Masson pine was investigated by peak-fitting method. This method was compared with the traditional hand-drawn method, 40% peak height method and half peak height method. X-ray diffraction measurements indicated that the microfibril angle changed as a function of the position in the tree.The mean micro fibril angle decreased more gradually as the distance increased from the pith and reached the same level in mature wood. The microfibril angle also seemed to decrease clearly from the base upward. Differences of angle-intensity curves between heartwood and sapwood were also examined.

  13. Mössbauer, magnetization and X-ray diffraction characterization methods for iron oxide nanoparticles

    Gabbasov, Raul, E-mail: gabbasov-raul@yandex.ru [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Polikarpov, Michael; Cherepanov, Valery [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Chuev, Michael; Mischenko, Iliya; Lomov, Andrey [Institute of Physics and Technology, Russian Academy of Sciences, Moscow (Russian Federation); Wang, Andrew [Ocean NanoTech. Springdale, AR (United States); Panchenko, Vladislav [National Research Center “Kurchatov Institute”, Moscow (Russian Federation)

    2015-04-15

    Water soluble magnetite iron oxide nanoparticles with oleic polymer coating and average diameters in the range of 5–25 nm, previously determined by TEM, were characterized using Mössbauer, magnetization and X-ray diffraction measurements. Comparative analysis of the results demonstrated a large diversity of magnetic relaxation regimes. Analysis showed the presence of an additional impurity component in the 25 nm nanoparticles, with principally different magnetic nature at the magnetite core. In some cases, X-ray diffraction measurements were unable to estimate the size of the magnetic core and Mössbauer data were necessary for the correct interpretation of the experimental results. - Highlights: • KV parameter, obtained from Mössbauer spectra can be used for nanoparticle size characterization. • Mössbauer spectra of 10–25 nm nanoparticles can be effectively described by ferromagnetic model. • Surface impurities can cause incorrect nanoparticle size determination.

  14. Correlated microradiography, X-ray microbeam diffraction and electron probe microanalysis of calcifications in an odontoma

    Using microradiography, X-ray microbeam diffraction and electron probe microanalysis, a correlated morphologic and crystallographic study was performed on dysplastic enamel in a compound odontoma. The tumor was found in the lateral incisor-canine region of the left mandible of a 36-year-old woman. A conspicuous feature was the presence of hypomineralized areas, which were situated in the proximity of enamel surface and distinctly demarcated from the adjacent enamel. X-ray microbeam diffraction and electron microanalysis showed that these lesions have a lower crystallinity and a higher concentration of magnesium as compared with the adjacent enamel. In addition, the present study revealed the presence of two other types of calcifications: 1) calcified structures within the fissure or on the enamel surface, which include lacunae of varying size and which resemble a form of coronal cementum, and 2) spherical calcifications which may be an epithelial product. (author)

  15. Mössbauer, magnetization and X-ray diffraction characterization methods for iron oxide nanoparticles

    Water soluble magnetite iron oxide nanoparticles with oleic polymer coating and average diameters in the range of 5–25 nm, previously determined by TEM, were characterized using Mössbauer, magnetization and X-ray diffraction measurements. Comparative analysis of the results demonstrated a large diversity of magnetic relaxation regimes. Analysis showed the presence of an additional impurity component in the 25 nm nanoparticles, with principally different magnetic nature at the magnetite core. In some cases, X-ray diffraction measurements were unable to estimate the size of the magnetic core and Mössbauer data were necessary for the correct interpretation of the experimental results. - Highlights: • KV parameter, obtained from Mössbauer spectra can be used for nanoparticle size characterization. • Mössbauer spectra of 10–25 nm nanoparticles can be effectively described by ferromagnetic model. • Surface impurities can cause incorrect nanoparticle size determination

  16. X-ray diffraction analysis of multilayer porous InP(001) structure

    Multilayer structures composed of four porous bilayers have been studied by high-resolution X-ray diffraction using synchrotron radiation, and the photoluminescence of these structures has been investigated at 4 K. The porous structures were formed by anodic oxidation of InP(001) substrates in aqueous HCl solution. The structural parameters of the sublayers were varied by changing the electrochemical etching mode (potentiostatic/galvanostatic). The X-ray scattering intensity maps near the InP 004 reflection are obtained. A model for scattering from such systems is proposed based on the statistical dynamical diffraction theory. Theoretical scattering maps have been fitted to the experimental ones. It is shown that a mathematical analysis of the scattering intensity maps makes it possible to determine the structural parameters of sublayers. The reconstructed parameters (thickness, strain, and porosity of sublayers and the shape and arrangement of pores) are in satisfactory agreement with the scanning electron microscopy data.

  17. Discrimination of liquids by a focal construct X-ray diffraction geometry

    A novel technique for the discrimination of liquids based upon X-ray diffraction and focal construct technology (FCT) is presented. FCT is a new, high efficiency coherent scatter harvesting technique. In this work, the competence of FCT to discriminate liquids was explored. A variety of liquids relevant to security inspection was analysed by FCT for application to liquid security inspection. Discrimination of potential threat liquids was successfully and reliably achieved even for limited data sets. - Highlights: • Description of an X-ray diffraction geometry called focal construct technology (FCT). • Advantages of FCT for aviation security screening posts. • Development of FCT with liquid samples. • Discrimination of threat and non-threat liquids by FCT. • Analysis of miscible and immiscible liquid mixtures by FCT

  18. Crystallization and preliminary X-ray diffraction analysis of alanine racemase from Pseudomonas putida YZ-26

    A recombinant alanine racemase from the Pseudomonas putida YZ-26, has been crystallized by the sitting-drop vapor-diffusion method and X-ray diffraction data were collected to 2.4 Å. A recombinant form of alanine racemase (Alr) from Pseudomonas putida YZ-26 has been crystallized by the sitting-drop vapour diffusion method. X-ray diffraction data were collected to 2.4 Å resolution. The crystals belong to the space group C2221, with unit-cell parameters a = 118.08, b = 141.86, c = 113.83 Å, and contain an Alr dimer in the asymmetric unit. The Matthews coefficient and the solvent content were calculated to be 2.8 Å3 Da−1 and approximately 50%, respectively

  19. Modelling studies of carbon nanotubes-Comparison of simulations and X-ray diffraction data

    Computer simulations of the powder diffraction profiles for multi-wall carbon nanotubes were performed using the Debye equation including a generalized Debye-Waller factor. The X-ray diffraction data were recorded using high-energy synchrotron radiation and an image plate as a detector for the carbon nanotubes produced by a template chemical vapour deposition (CVD) process. The computed and experimental structure factors were converted to real-space via the Fourier transform. The results of computation, obtained in the form of the structure factor and the pair correlation function, are compared with the X-ray experimental data in both reciprocal and real-space. The nanotube model consisting of five layers with the length of 12 A has proved to account very well for the experimental data

  20. In situ X-ray diffraction during MOCVD of III-nitrides

    Simbrunner, C.; Navarro-Quezada, A.; Schmidegg, K.; Bonanni, A.; Sitter, H. [Institute of Semiconductor and Solid State Physics, University Linz (Austria); Kharchenko, A.; Bethke, J. [PANalytical B.V., Almelo (Netherlands); Lischka, K. [Department of Physics, University of Paderborn (Germany)

    2007-08-15

    Nowadays Metal Organic Chemical Vapor Deposition (MOCVD) is the most frequently used fabrication process for growing III-V-nitrides. The missing ultra high vacuum (UHV) conditions narrow the window of possible in situ characterization techniques to only optical methods like spectroscopic ellipsometry (SE) and X-ray diffraction. We are able to observe the growing surface simultaneously with a multi wavelength ellipsometer and a X-ray diffraction (XRD) system mounted on an AIXTRON 200 RF-S reactor. Properties like crystal quality, composition, superlattice periodicity and strain relaxation of hexagonal GaN/AlGaN heterostructures are determined in situ using XRD. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)