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Sample records for x-ray diffraction line

  1. EFFECT OF SATELLITE LINES FROM X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

    EPA Science Inventory

    The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. PA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predict...

  2. X-Ray Diffraction.

    ERIC Educational Resources Information Center

    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)

  3. Grain orientation mapping of passivated aluminum interconnect lines by x-ray micro-diffraction

    SciTech Connect

    Chang, C.H.; MacDowell, A.A.; Padmore, H.A.; Patel, J.R.; Patel, J.R. Thompson, A.C.

    1998-11-01

    A micro x-ray diffraction facility is under development at the Advanced Light Source. Spot sizes are typically about 1-{mu}m size generated by means of grazing incidence Kirkpatrick-Baez focusing mirrors. Photon energy is either white of energy range 6{endash}14 keV or monochromatic generated from a pair of channel cut crystals. Laue diffraction pattern from a single grain in a passivated 2-{mu}m wide bamboo structured Aluminum interconnect line has been recorded. Acquisition times are of the order of seconds. The Laue pattern has allowed the determination of the crystallographic orientation of individual grains along the line length. The experimental and analysis procedure used is described, as is the latest grain orientation result. The impact of x-ray micro-diffraction and its possible future direction are discussed in the context of other developments in the area of electromigration, and other technological problems. {copyright} {ital 1998 American Institute of Physics.}

  4. Grain orientation mapping of passivated aluminum interconnect lines with X-ray micro-diffraction

    SciTech Connect

    Chang, C.H.; Patel, J.R. |; MacDowell, A.A.; Padmore, H.A.; Thompson, A.C.

    1998-09-01

    A micro x-ray diffraction facility is under development at the Advanced Light Source. Spot sizes are typically about 1-{micro}m size generated by means of grazing incidence Kirkpatrick-Baez focusing mirrors. Photon energy is either white of energy range 6--14 keV or monochromatic generated from a pair of channel cut crystals. Laue diffraction pattern from a single grain in a passivated 2-{micro}m wide bamboo structured Aluminum interconnect line has been recorded. Acquisition times are of the order of seconds. The Laue pattern has allowed the determination of the crystallographic orientation of individual grains along the line length. The experimental and analysis procedure used is described, as is the latest grain orientation result. The impact of x-ray micro-diffraction and its possible future direction are discussed in the context of other developments in the area of electromigration, and other technological problems.

  5. Grain orientation mapping of passivated aluminum interconnect lines by x-ray micro-diffraction

    SciTech Connect

    Chang, C. H.; Patel, J. R.; Thompson, A. C.

    1998-11-24

    A micro x-ray diffraction facility is under development at the Advanced Light Source. Spot sizes are typically about 1-{mu}m size generated by means of grazing incidence Kirkpatrick-Baez focusing mirrors. Photon energy is either white of energy range 6-14 keV or monochromatic generated from a pair of channel cut crystals. Laue diffraction pattern from a single grain in a passivated 2-{mu}m wide bamboo structured Aluminum interconnect line has been recorded. Acquisition times are of the order of seconds. The Laue pattern has allowed the determination of the crystallographic orientation of individual grains along the line length. The experimental and analysis procedure used is described, as is the latest grain orientation result. The impact of x-ray micro-diffraction and its possible future direction are discussed in the context of other developments in the area of electromigration, and other technological problems.

  6. Line x-ray source for diffraction enhanced imaging in clinical and industrial applications

    NASA Astrophysics Data System (ADS)

    Wang, Xiaoqin

    Mammography is one type of imaging modalities that uses a low-dose x-ray or other radiation sources for examination of breasts. It plays a central role in early detection of breast cancers. The material similarity of tumor-cell and health cell, breast implants surgery and other factors, make the breast cancers hard to visualize and detect. Diffraction enhanced imaging (DEI), first proposed and investigated by D. Chapman is a new x-ray radiographic imaging modality using monochromatic x-rays from a synchrotron source, which produced images of thick absorbing objects that are almost completely free of scatter. It shows dramatically improved contrast over standard imaging when applied to the same phantom. The contrast is based not only on attenuation but also on the refraction and diffraction properties of the sample. This imaging method may improve image quality of mammography, other medical applications, industrial radiography for non-destructive testing and x-ray computed tomography. However, the size, and cost, of a synchrotron source limits the application of the new modality to be applicable at clinical levels. This research investigates the feasibility of a designed line x-ray source to produce intensity compatible to synchrotron sources. It is composed of a 2-cm in length tungsten filament, installed on a carbon steel filament cup (backing plate), as the cathode and a stationary oxygen-free copper anode with molybdenum coating on the front surface serves as the target. Characteristic properties of the line x-ray source were computationally studied and the prototype was experimentally investigated. SIMIION code was used to computationally study the electron trajectories emanating from the filament towards the molybdenum target. A Faraday cup on the prototype device, proof-of-principle, was used to measure the distribution of electrons on the target, which compares favorably to computational results. The intensities of characteristic x-ray for molybdenum, tungsten and rhodium targets were investigated with different window materials for -30kV to -100kV applied potential. Heat loading and thermal management of the target has been investigated computationally using COMSOL code package, and experimental measurements of target temperature rise was taken via thermocouples attached to the target. Temperature measurements for low voltage, low current regime without active cooling were compared to computational results for code-experiment benchmarking. Two different phantoms were used in the simulation of DEI images, which showed that the designed x-ray source with DEI setup could produce images with significant improved contrast. The computational results, along with experimental measurements on the prototype setup, indicate the possibility of scale up to larger area x-ray source adequate for DEI applications.

  7. THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

    EPA Science Inventory

    The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

  8. In-line holography and coherent diffractive imaging with x-ray waveguides

    NASA Astrophysics Data System (ADS)

    de Caro, L.; Giannini, C.; Pelliccia, D.; Mocuta, C.; Metzger, T. H.; Guagliardi, A.; Cedola, A.; Burkeeva, I.; Lagomarsino, S.

    2008-02-01

    A Fresnel coherent diffraction imaging experiment with hard x rays is here presented, using two planar crossed waveguides as optical elements, leading to a virtual pointlike source. The coherent wave field obtained with this setup is used to illuminate a micrometric single object having the shape of a butterfly. A digital two-dimensional in-line holographic reconstruction of the unknown object at low resolution (200nm) has been obtained directly via fast Fourier transform (FFT) of the raw data. The object and its twin image are well separated because suitable geometrical conditions are satisfied. A good estimate of the incident wave field phase has been extracted directly from the FFT of the raw data. A partial object reconstruction with 50nm spatial resolution was achieved by fast iterative phase retrieval, the major limitation for a full reconstruction being the nonideal structure of the guided beam. The method offers a route for fast and reliable phase retrieval in x-ray coherent diffraction.

  9. In-line holography and coherent diffractive imaging with x-ray waveguides

    SciTech Connect

    De Caro, L.; Giannini, C.; Guagliardi, A.; Mocuta, C.; Metzger, T. H.; Cedola, A.; Burkeeva, I.; Lagomarsino, S.

    2008-02-15

    A Fresnel coherent diffraction imaging experiment with hard x rays is here presented, using two planar crossed waveguides as optical elements, leading to a virtual pointlike source. The coherent wave field obtained with this setup is used to illuminate a micrometric single object having the shape of a butterfly. A digital two-dimensional in-line holographic reconstruction of the unknown object at low resolution (200 nm) has been obtained directly via fast Fourier transform (FFT) of the raw data. The object and its twin image are well separated because suitable geometrical conditions are satisfied. A good estimate of the incident wave field phase has been extracted directly from the FFT of the raw data. A partial object reconstruction with 50 nm spatial resolution was achieved by fast iterative phase retrieval, the major limitation for a full reconstruction being the nonideal structure of the guided beam. The method offers a route for fast and reliable phase retrieval in x-ray coherent diffraction.

  10. X-Ray Diffraction Apparatus

    NASA Technical Reports Server (NTRS)

    Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

    1996-01-01

    An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

  11. Submicron X-ray diffraction

    SciTech Connect

    MacDowell, Alastair; Celestre, Richard; Tamura, Nobumichi; Spolenak, Ralph; Valek, Bryan; Brown, Walter; Bravman, John; Padmore, Howard; Batterman, Boris; Patel, Jamshed

    2000-08-17

    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 instrument is for instance, capable of probing a sub-micron size volume inside micron sized aluminum metal grains buried under a silicon dioxide insulating layer. The resulting Laue pattern is collected on a large area CCD detector and automatically indexed to yield the grain orientation and deviatoric (distortional) strain tensor of this sub-micron volume. A four-crystal monochromator is then inserted into the beam, which allows monochromatic light to illuminate the same part of the sample. Measurement of diffracted photon energy allows for the determination of d spacings. The combination of white and monochromatic beam measurements allow for the determination of the total strain/stress tensor (6 components) inside each sub-micron sized illuminated volume of the sample.

  12. THE CHARACTERIZATION OF A SOLID SORBENT WITH CRYSTALLITE SIZE AND STRAIN DATA FROM X-RAY DIFFRACTION LINE BROADENING

    EPA Science Inventory

    The paper gives results of the characterization of a solid sorbent with crystallite size and strain data from x-ray diffraction line broadening, as part of an EPA investigation of the injection of dry Ca(OH)2 into coal-fired electric power plant burners for the control of SO2 emi...

  13. X-ray diffraction line profile analysis of deformation microstructure in boron modified Ti-6Al-4V alloy

    SciTech Connect

    Sarkar, Apu; Roy, Shibayan; Suwas, Satyam

    2011-01-15

    X-ray diffraction line profile analysis (XRDLPA) techniques have been applied to investigate the deformed microstructure of a recently developed boron modified two-phase titanium alloy Ti-6Al-4V. The alloy was hot compressed at 750 deg. C up to 50% height reduction at two different strain rates (10{sup -3} S{sup -1} and 1 S{sup -1}). Microstructural parameters like average domain size, average microstrain within the domain and dislocation density of the two phases were determined using X-ray diffraction line profile analysis. The results indicate an increase in the microstrain and dislocation density for the {alpha}-phase and decrease for the {beta}-phase in the case of boron modified alloys as compared to the normal material. Microstructural modifications viz. the grain refinement and the presence of hard, brittle TiB particles in the case of boron modified alloy are held responsible for the observed difference in the dislocation density. - Research Highlights: {yields} Microstructural examination of hot compressed Ti64 with and without boron addition by XRDLPA. {yields} Smaller average domain size in alpha-phase compared to the corresponding alpha-phase in all cases. {yields} Higher microstrain and dislocation density for {alpha} phase and lower for {beta} phase in case of Ti64+B. {yields} Decrease in domain size while increase in micro-strain and dislocation density with strain rate. {yields} Strain accumulation around TiB particles responsible for high dislocation density in {alpha} phase.

  14. Diffractive X-Ray Telescopes

    NASA Technical Reports Server (NTRS)

    Skinner, Gerald K.

    2010-01-01

    Diffractive X-ray telescopes, using zone plates, phase Fresnel lenses, or related optical elements have the potential to provide astronomers with true imaging capability with resolution many orders of magnitude better than available in any other waveband. Lenses that would be relatively easy to fabricate could have an angular resolution of the order of micro-arc-seconds or even better, that would allow, for example, imaging of the distorted spacetime in the immediate vicinity of the super-massive black holes in the center of active galaxies. What then is precluding their immediate adoption? Extremely long focal lengths, very limited bandwidth, and difficulty stabilizing the image are the main problems. The history, and status of the development of such lenses is reviewed here and the prospects for managing the challenges that they present are discussed.

  15. An Implementation of the Fundamental Parameters Approach for Analysis of X-ray Powder Diffraction Line Profiles

    PubMed Central

    Mendenhall, Marcus H.; Mullen, Katharine; Cline, James P.

    2015-01-01

    This work presents an open implementation of the Fundamental Parameters Approach (FPA) models for analysis of X-ray powder diffraction line profiles. The original literature describing these models was examined and code was developed to allow for their use within a Python based least squares refinement algorithm. The NIST interest in the FPA method is specific to its ability to account for the optical aberrations of the powder diffraction experiment allowing for an accurate assessment of lattice parameter values. Lattice parameters are one of the primary certified measurands of NIST Standard Reference Materials (SRMs) for powder diffraction. Lattice parameter values obtained from analysis of data from SRMs 640e and 660c using both the NIST FPA Python code and the proprietary, commercial code Topas, that constitutes the only other actively supported, complete implementation of FPA models within a least-squares data analysis environment, agreed to within 2 fm. This level of agreement demonstrates that both the NIST code and Topas constitute an accurate implementation of published FPA models. PMID:26958448

  16. X-Ray Diffractive Optics

    NASA Technical Reports Server (NTRS)

    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. Strength of polycrystalline niobium from high-pressure x-ray diffraction data: A comparison of results from line-width and line-shift analyses

    NASA Astrophysics Data System (ADS)

    Singh, Anil K.; Liermann, Hanns-Peter

    2015-08-01

    High purity polycrystalline niobium was compressed in a diamond anvil cell (DAC) without any pressure transmitting medium and the pressure was increased in steps of ˜5 GPa to the highest pressure of ˜40 GPa. The diffraction pattern was recorded after each pressure increment using angle-dispersive mode with the conventional diffraction geometry, wherein the primary x-ray beam is parallel to the load axis of the DAC. The strength of niobium as function of pressure was determined using the line-width and line-shift analyses. Both e Y and 2 e Y , where Y is the aggregate Young's modulus and e is the strain determined from the line-width analysis, have been used as the measure of strength in earlier studies. In this study, it is e Y that agrees with the strength determined from the line-shift analysis of the radial diffraction data as well as the data from the conventional diffraction geometry. These results have been discussed and compared with a similar observation made earlier on strength of diamond. This study highlights the ambiguity that presently exists in choosing e Y or 2 e Y as a measure of strength while attempting to estimate the strength from the diffraction line width analysis.

  18. Diffraction enhanced x-ray imaging

    SciTech Connect

    Thomlinson, W.; Zhong, Z.; Chapman, D.; Johnston, R.E.; Sayers, D.

    1997-09-01

    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.

  19. Beyond hard x-ray photoelectron spectroscopy: Simultaneous combination with x-ray diffraction

    SciTech Connect

    Rubio-Zuazo, Juan; Castro, German R.

    2013-05-15

    Hard x-ray photoelectron spectroscopy (HAXPES) is a powerful and novel emerging technique for the nondestructive determination of electronic properties and chemical composition of bulk, buried interfaces and surfaces. It benefits from the exceptionally large escape depth of high kinetic energy photoelectrons, increasing the information depth up to several tens of nanometers. Complementing HAXPES with an atomic structure sensitive technique (such as x-ray diffraction) opens a new research field with major applications for materials science. At SpLine, the Spanish CRG beamline at the European Synchrotron Radiation Facility, we have developed a novel experimental set-up that combines HAXPES and x-ray diffraction (x-ray reflectivity, surface x-ray diffraction, grazing incidence x-ray diffraction, and reciprocal space maps). Both techniques can be operated simultaneously on the same sample and using the same excitation source. The set-up includes a robust 2S + 3D diffractometer hosting a ultrahigh vacuum chamber equipped with a unique photoelectron spectrometer (few eV < electron kinetic energy < 15 keV), x-ray tube (Mg/Ti), 15 keV electron gun, and auxiliary standard surface facilities (molecular beam epitaxy evaporator, ion gun, low energy electron diffraction, sample heating/cooling system, leak valves, load-lock sample transfer, etc.). This end-station offers the unique possibility of performing simultaneous HAXPES + x-ray diffraction studies. In the present work, we describe the experimental set-up together with two experimental examples that emphasize its outstanding capabilities: (i) nondestructive characterization of the Si/Ge and HfO{sub 2}/SiO{sub 2} interfaces on Ge-based CMOS devices, and (ii) strain study on La{sub 0.7}Ca{sub 0.3}MnO{sub 3} ultrathin films grown on SrTiO{sub 3}(001) substrate.

  20. La Diffraction X Instantanee Flash X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Jamet, Francis

    1985-02-01

    We present a paper giving a survey about Flash X-Ray Diffraction (FXD) and its progress during the last years. After a brief introduction and a historical survey we determine how to improve flash X-ray systems in order to use them for FXD. A first possibility for increasing the emitted radiation by flash X-ray tubes is to in-crease the voltage. Some authors were successful in applying this method to the recording of powder patterns using 300 kV, 10 ns, pulses. Another possibility for increasing the emitted intensity without increasing the voltage is to use a pulse generator with a very low self-inductance, for example a Blumlein line, which enables attainment of a high discharge current. Finally it should be noted that the intensity of the X-rays falling on the sample can be in-creased by an appropriate shape of the anode in order to keep the focus very small 1,5 mm in diameter). The sensitivity of the detector can be appreciably improved by using highly sensitive films together with fluorescent screens. Another method is to use an image intensifier or a microchannel plate. FXD has been applied to the analysis of the evolution of different kinds of patterns (Laue, Debye-Scherrer,...) of cristals submitted to high deformation rates. We give examples of such rapid changes in the crystalline state due to exploding foils, shock waves or shaped charge effects.

  1. Interlaced X-ray diffraction computed tomography

    PubMed Central

    Vamvakeros, Antonios; Jacques, Simon D. M.; Di Michiel, Marco; Senecal, Pierre; Middelkoop, Vesna; Cernik, Robert J.; Beale, Andrew M.

    2016-01-01

    An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy. PMID:27047305

  2. Single Particle X-ray Diffractive Imaging

    SciTech Connect

    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

    ERIC Educational Resources Information Center

    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. X-Ray Diffraction on NIF

    SciTech Connect

    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.

  5. Quantitative evaluation of the broadening of x-ray diffraction, Raman, and photoluminescence lines by dislocation-induced strain in heteroepitaxial GaN films

    NASA Astrophysics Data System (ADS)

    Kaganer, Vladimir M.; Jenichen, Bernd; Ramsteiner, Manfred; Jahn, Uwe; Hauswald, Christian; Grosse, Frank; Fernández-Garrido, Sergio; Brandt, Oliver

    2015-09-01

    Experimental x-ray diffraction, Raman, and photoluminescence line profiles from GaN films with different densities of threading dislocations are modeled using Monte Carlo calculations of the strain distribution due to these dislocations. We quantitatively analyze and compare the respective line broadenings predicted by these calculations for different dislocation densities. X-ray diffraction and Raman measurements reveal the strain in the whole volume of the film, due to the large penetration depth of the corresponding radiation, while photoluminescence measurements are sensitive to the strain close to the film surface, in a layer limited by the penetration depth of the radiation used for excitation. This difference in information depths becomes especially important for films in which the threading dislocation density is continuously decreasing during growth, as it can be achieved by vapor phase epitaxy methods. An additional narrowing of photoluminescence lines occurs due to two effects: first, the elastic relaxation of the dislocation strain at the free surface, and second, the suppression of luminescence from the most highly strained regions around the dislocation cores which act as centers of nonradiative recombination.

  6. Optical properties of X-rays--dynamical diffraction.

    PubMed

    Authier, André

    2012-01-01

    The first attempts at measuring the optical properties of X-rays such as refraction, reflection and diffraction are described. The main ideas forming the basis of Ewald's thesis in 1912 are then summarized. The first extension of Ewald's thesis to the X-ray case is the introduction of the reciprocal lattice. In the next step, the principles of the three versions of the dynamical theory of diffraction, by Darwin, Ewald and Laue, are given. It is shown how the comparison of the dynamical and geometrical theories of diffraction led Darwin to propose his extinction theory. The main optical properties of X-ray wavefields at the Bragg incidence are then reviewed: Pendellösung, shift of the Bragg peak, fine structure of Kossel lines, standing waves, anomalous absorption, paths of wavefields inside the crystal, Borrmann fan and double refraction. Lastly, some of the modern applications of the dynamical theory are briefly outlined: X-ray topography, location of adsorbed atoms at crystal surfaces, optical devices for synchrotron radiation and X-ray interferometry. PMID:22186282

  7. Iron lines from X-ray binaries

    NASA Technical Reports Server (NTRS)

    Pravdo, S. H.

    1979-01-01

    A summary of the observational evidence of iron lines from satellite X-ray detectors and binary X-ray pulsars is presented. The current theories consider that the continua X-rays from X-ray pulsars originate at or near the surface of neutron stars, and they can then heat or fluoresce iron ions in surrounding physical regions to create the observed emission. Measurements of the line energy, intensity, and width, and the phase dependence of these quantities can help determine the relative importance of contributions of relative sources. The evidence is presented that the iron emission from some sources contains more than one component, and the spectra of other X-ray binaries including transients and cataclysmic variables also contain iron lines. Some implications of the observed line emission are discussed.

  8. Transient x-ray diffraction and its application to materials science and x-ray optics

    SciTech Connect

    Hauer, A.A.; Kopp, R.; Cobble, J.; Kyrala, G.; Springer, R.

    1997-12-01

    Time resolved x-ray diffraction and scattering have been applied to the measurement of a wide variety of physical phenomena from chemical reactions to shock wave physics. Interest in this method has heightened in recent years with the advent of versatile, high power, pulsed x-ray sources utilizing laser plasmas, electron beams and other methods. In this article, we will describe some of the fundamentals involved in time resolved x-ray diffraction, review some of the history of its development, and describe some recent progress in the field. In this article we will emphasize the use of laser-plasmas as the x-ray source for transient diffraction.

  9. Liquids identification with x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Harding, G.; Delfs, J.

    2007-09-01

    A novel identification technique suited to security screening of liquid and amorphous substances with x-ray diffraction (XRD) is presented. The starting point is to fit the high momentum region (independent atom regime) of the XRD profile with a free-atom scatter function corresponding most closely to the effective atomic number of the sample. The Percus-Yevick formulation of the molecular interference function for hard-sphere liquids then enables features to be extracted from liquid/amorphous XRD profiles. These features correspond to such molecular structure parameters as effective particle radius, packing fraction, effective atomic number, particle homogeneity and inter-particle potential. Amorphous substances may thus be classified into functional groups such as oxidisers and fuels. These considerations are illustrated with synchrotron XRD measurements of acetone and hydrogen peroxide, implicated in the London "transatlantic aircraft plot" of 2006 and representative of hazardous liquid fuel and oxidizer combinations.

  10. Preliminary experiment of X-ray diffraction imaging

    NASA Astrophysics Data System (ADS)

    Yamanashi, Masaki; Kometani, Noritsugu; Tsuji, Kouichi

    2015-07-01

    X-ray diffraction (XRD) techniques have been used in various fields, such as, material science, medical science, etc. XRD gives the structure information of materials. An XRD imaging spectrometer equipped with a 2D X-ray detector for obtaining the information of a large observation area was developed in this study. A polycapillary half lens was applied as a 2D collimator to have an X-rays with a large collimated area of 8 mm. The 2D diffracted X-rays were detected by a 2D X-ray detector.

  11. Glass transition in ferroic glass K x (ND4)1-x D2PO4: a complete x-ray diffraction line shape analysis

    NASA Astrophysics Data System (ADS)

    Ranjan Choudhury, Rajul; Chitra, R.; Jayakrishnan, V. B.

    2016-03-01

    Quenching of dynamic disorder in glassy systems is termed as the glass transition. Ferroic glasses belong to the class of paracrystalline materials having crystallographic order in-between that of a perfect crystal and amorphous material, a classic example of ferroic glass is the solid solution of ferroelectric deuterated potassium dihydrogen phosphate and antiferroelectric deuterated ammonium dihydrogen phosphate. Lowering temperature of this ferroic glass can lead to a glass transition to a quenched disordered state. The subtle atomic rearrangement that takes place at such a glass transition can be revealed by careful examination of the temperature induced changes occurring in the x-ray powder diffraction (XRD) patterns of these materials. Hence we report here results of a complete diffraction line shape analysis of the XRD patterns recorded at different temperatures from deuterated mixed crystals DK x A1-x DP with mixing concentration x ranging as 0 < x < 1. Changes observed in diffraction peak shapes have been explained on the basis of structural rearrangements induced by changing O-D-O hydrogen bond dynamics in these paracrystals.

  12. Phase retrieval in x-ray coherent Fresnel projection-geometry diffraction

    SciTech Connect

    De Caro, Liberato; Giannini, Cinzia; Cedola, Alessia; Pelliccia, Daniele; Lagomarsino, Stefano; Jark, Werner

    2007-01-22

    Coherent x-ray diffraction experiments were performed in Fresnel regime, within a line-projection geometry. A planar x-ray waveguide was used to focus coherent cylindrical waves onto a 7.2 {mu}m Kevlar fiber, which acts as a phase object for hard x rays. The phase was retrieved, by using a Fourier-based iterative phasing algorithm, consistent with measured diffraction data and known constraints in real space, with a submicrometer spatial resolution.

  13. X-RAY DIFFRACTION STUDIES ON FROG MUSCLES

    PubMed Central

    Spiegel-Adolf, M.; Henny, G. C.; Ashkenaz, E. W.

    1944-01-01

    1. X-ray diffraction studies of sartorius muscles of Rana pipiens were made in a new x-ray diffraction camera which permits exposures of 3 to 6 minutes. The object-film distance can be varied from 20 to 80 mm; the muscle inside the camera can be electrically stimulated while contracting isotonically or isometrically, and can be observed by a special device. After exposures up to 30 minutes (approximately 40,830 r) muscles are still alive and responsive. 2. Contrary to the x-ray diffraction pattern of powdered dry muscle, which pattern consists of two rings corresponding to spacings of 4.46 Å.u. and 9.66 Å.u., both moist and dried whole sartorius muscle show signs of orientation in both rings, consisting of two equatorial streaks (wet) or points (dry) and meridional sickles. The moist muscle shows in addition a diffuse water ring. The spacings corresponding to the orientation points and elliptical structure show only slight differences in moist and dried samples. Through statistical computations based on two different series consisting of thirteen moist and twenty-eight dried samples, and nine muscles before and after drying, it was shown that only the divergence in the smaller spacing has some real significance, which indicates that most water of the moist muscle is bound intermolecularly. Upon resoaking of dried muscle the x-ray diffraction pattern of the moist muscle is restored. 3. Stretching of muscle by weights below the breaking point produces an additional well defined diffraction line, corresponding to a spacing of 4.32 Å.u. A similar diffraction line can be produced in frog tendon upon stretching. 4. The influence of heat on the x-ray diffraction pattern of muscle depends upon the maximum temperature and the length of action; 5 minutes at 50° C. markedly reduces the orientation of the sample; 5 minutes' immersion in boiling Ringer's solution destroys the orientation and produces a ring corresponding to a spacing of 5.3 to 5.5 Å.u. in the moist and sharpening of the backbone reflection in the dried specimen. 5. Ultraviolet light brings forth changes in the x-ray diffraction pattern varying with the intensity of the irradiation. Ultimately a disappearance of the equatorial points and of the outside sickles is achieved while the elliptical shape of the outside ring and its diffuseness persist. In addition two salt rings characteristic of NaCl indicate that the irradiated muscles have become permeable to the surrounding medium (Ringer's solution). 6. Both faradic and single shock electrical stimulation were tried on muscles. If shortening of the muscle is prevented either by sufficient weight or by tying the muscle in a frame, no changes in the x-ray diffraction pattern occur; if the muscle is allowed to shorten without weights or by using insufficient weights, then the orientation either disappears completely or partially. When the muscle is stretched while contracted by electrical stimulation the orientation of the x-ray diffraction pattern reappears. 7. A number of salts with uni- and bivalent ions in concentrations corresponding osmotically to 0.73 per cent NaCl and 10 per cent NH4Cl were studied in their effects upon the x-ray diffraction of muscles. Of the salts with univalent ions in the lower concentration only KCl causes a marked decrease of orientation and an increase in the permeability of the fiber membranes. Similar effects on the orientation seem to be produced by CaCl2 while MgCl2 causes rather a more pronounced orientation. At hypertonic salt concentrations the orientation disappears completely and the corresponding salt rings become visible. Besides, NaCNS seems to have a specific effect on the outside ring and LiCl produces a ring at 21.3 Å.u. and a splitting of the outside ring. 8. Strong mineral and lactic acids in concentrations up to 0.005 N have little if any influence upon the x-ray diffraction of muscles. A further increase in acidity to 0.01 N and above destroys the orientation completely, causes sharpening of the backbone reflection, and increased membrane permeability. These changes are irreversible upon neutralization. Also the effects of swelling upon the water ring of fresh muscle become manifest. Weak acids at higher concentrations show an effect similar to that of strong acids. 9. Rigor mortis produces a more or less complete loss of orientation. The muscles show signs of increased permeability. 10. Alkalies destroy the orientation of the x-ray diffraction pattern. The effective concentration is higher than the corresponding amount of acid. 11. Formaldehyde produces only minor changes in the x-ray diffraction patterns of muscles. 12. The effects of alcohol depend primarily upon the concentration applied. Low concentrations (5 per cent) seem to have a passing stimulating effect, at concentrations of 15 per cent, the anesthetizing effect becomes manifest in well defined orientation. The diameter of the water ring is reduced. If 95 per cent alcohol is allowed to act upon muscle for more than 12 minutes, then the orientation disappears completely and the backbone spacing becomes as sharp as in boiled muscle. 13. The effects of chloroform depend upon whether the muscle is allowed to contract or not. Only if the muscle is allowed to contract in chloroform-saturated Ringer's solution is the orientation lost and salt rings appear as well as a ring corresponding to a spacing of 22 Å.u,, which has been observed in other changes in muscles. 14. In muscles allowed to shorten in a caffeine-Ringer's solution the orientation disappears, salt rings become visible as well as a decrease in size of the water ring; a new arc corresponding to a spacing of 4.18 Å.u. was observed in one case. PMID:19873411

  14. X-ray diffraction line broadening effects in MBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}(M=Y, Gd) thin films

    SciTech Connect

    Scardi, P.; Matacotta, F.C.; Dediu, V.I.; Correra, L.

    1997-01-01

    X-ray diffraction line profile analysis (LPA) has been carried out on a set of superconducting thin films of MBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} (MBCO, M=Y, Gd), deposited by pulsed and continuous physical vapor deposition (PVD) techniques on different single-crystal substrates. The choice of appropriate deposition conditions, substrates, and buffer layers promoted a high degree of [00{ital l}] preferred orientation, leading to a well-defined columnar grain morphology in the MBCO films. Under such conditions, the LPA of diffraction patterns, collected with the widely spread Bragg{endash}Brentano geometry, gives a detailed information on the distributions of coherent scattering domain (crystallite) size and microstrain along the [00{ital l}] growth direction; considering the particular MBCO film microstructure, the mean crystallite size ({bar M}) can be regarded as the mean distance between extended planar defects parallel to the film surface. The significance of {bar M} goes beyond a merely statistical value. As long as the morphology of the films is similar, {bar M} is found to be strictly connected with the average microstrain by a simple proportionality relation. Moreover, the correlation extends to important superconducting transport parameters, like the transition width {Delta}T{sub c}. These regular behaviors are irrespective of deposition techniques, substrate and film materials, and are a clear indication of some fundamental relation between the defects and the overall properties of the films. {copyright} {ital 1997 Materials Research Society.}

  15. Architectures and algorithms for x-ray diffraction imaging

    NASA Astrophysics Data System (ADS)

    Chen, Ke; Castan, David A.

    2013-03-01

    X-ray imaging is the predominant modality used in luggage inspection systems for explosives detection. Conventional or dual energy X-ray computed tomography imaging reconstructs the X-ray absorption characteristics of luggage contents at the different energies; however, material characterization based on absorption characteristics at these energies is often ambiguous. X-ray diffraction imaging (XDI) measures coherently scattered X-rays to construct diffraction profiles of materials that can provide additional molecular signature information to improve the identification of specific materials. In this paper, we present recent work on developing XDI algorithms for different architectures, which include limited angle tomography and the use of coded aperture masks. We study the potential benefits of fusion of dual energy CT information with X-ray diffraction imaging. We illustrate the performance of different approaches using Monte Carlo propagation simulations through 3-D media.

  16. Femtosecond x-ray diffraction: experiments and limits

    NASA Astrophysics Data System (ADS)

    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.

  17. High-Energy X-Ray Diffraction Analysis Tool

    SciTech Connect

    2011-11-29

    The functionality of heRXD includes the following: distance and angular calibration and viewing flat-panel detector images used for X-ray diffraction; image (polar) rebinning or "caking"; line position fitting in powder diffraction images; image segmentation or "blob finding"; crystal orentation indesing; and lattice vector refinement. These functionalities encompass a critical set analyzing teh data for high-energy diffraction measurements that are currently performed at synchrotron sources such as the Advanced Photon Source (APS). The software design modular and open source under LGPL. The intent is to provide a common framework and graphical user interface that has the ability to utillize internal as well as external subroutines to provide various optins for performing the fuctionalities listed above. The software will initially be deployed at several national user facilities--including APS, ALS, and CHESS--and then made available for download using a hosting service such as sourceforge.

  18. High-Energy X-Ray Diffraction Analysis Tool

    Energy Science and Technology Software Center (ESTSC)

    2011-11-29

    The functionality of heRXD includes the following: distance and angular calibration and viewing flat-panel detector images used for X-ray diffraction; image (polar) rebinning or "caking"; line position fitting in powder diffraction images; image segmentation or "blob finding"; crystal orentation indesing; and lattice vector refinement. These functionalities encompass a critical set analyzing teh data for high-energy diffraction measurements that are currently performed at synchrotron sources such as the Advanced Photon Source (APS). The software design modularmore » and open source under LGPL. The intent is to provide a common framework and graphical user interface that has the ability to utillize internal as well as external subroutines to provide various optins for performing the fuctionalities listed above. The software will initially be deployed at several national user facilities--including APS, ALS, and CHESS--and then made available for download using a hosting service such as sourceforge.« less

  19. Multiwavelength Anomalous Diffraction at High X-Ray Intensity

    NASA Astrophysics Data System (ADS)

    Son, Sang-Kil; Chapman, Henry N.; Santra, Robin

    2011-11-01

    The multiwavelength anomalous diffraction (MAD) method is used to determine phase information in x-ray crystallography by employing anomalous scattering from heavy atoms. X-ray free-electron lasers (FELs) show promise for revealing the structure of single molecules or nanocrystals, but the phase problem remains largely unsolved. Because of the ultrabrightness of x-ray FEL, samples experience severe electronic radiation damage, especially to heavy atoms, which hinders direct implementation of MAD with x-ray FELs. Here, we propose a generalized version of MAD phasing at high x-ray intensity. We demonstrate the existence of a Karle-Hendrickson-type equation in the high-intensity regime and calculate relevant coefficients with detailed electronic damage dynamics of heavy atoms. The present method offers a potential for ab initio structural determination in femtosecond x-ray nanocrystallography.

  20. Laboratory calibration of x-ray transmission diffraction gratings

    NASA Astrophysics Data System (ADS)

    Dewey, Daniel; Humphries, Donald N.; McLean, G. Y.; Moschella, David A.

    1994-09-01

    The 336 individual grating elements making up the High-Energy Transmission Grating (HETG) will be verified and calibrated in laboratory facilities at MIT as they are fabricated. A high instrument resolving power of order E/(Delta) E approximately equals 1000 requires an overall period uniformity of better than 250 ppm. To extract the maximum astrophysical information the diffraction efficiency of the HETG will be calibrated to the 1% level (1(sigma) ). Grating element period variations are measured and mapped in the Laser Reflection facility. Collimated HeCd (3250- angstrom) or HeNe (6328-angstrom) laser light is diffracted by the samples and measured. A per-point measurement noise of below 5 ppm rms and an overall period repeatability of 40 ppm rms have been achieved. X-ray diffraction efficiency in the 0.4 to 10 keV range is calibrated in the X-ray Grating Evaluation Facility (X- GEF). The facility combines a 17 meter vacuum beam line, a multi- anode X-ray source with monitor counter, a piezo-deformed 1D Ir coated focussing optic, a single-pixel solid state detector, and a 2D imaging proportional counter. The facility operation is under computer control and test procedures, instrumentation parameters, and acquired data are managed with a database. The system uses synchrotron-calibrated reference gratings as efficiency transfer standards. Detailed characterization and modeling of the X-GEF components and test/analysis procedures are being carried out to optimize the quality of the HETG calibration.

  1. An X-ray diffraction study of titanium oxidation

    NASA Technical Reports Server (NTRS)

    Wiedemann, K. E.; Unnam, J.

    1984-01-01

    Titanium specimens of commercial purity were exposed at 1100 to 1400 F to laboratory air for times up to 100 hours. The extent of substrate contamination by interstitial oxygen was was determined by a new X-ray diffraction analysis involving transformation of X-ray diffraction intensity bands. The oxygen solid-solubility at the oxide-metal interfaces and its variation with time at temperature were also determined. Diffusion coefficients are deduced from the oxygen depth profiles.

  2. X-ray diffraction study of lead chloride

    NASA Astrophysics Data System (ADS)

    Nitsch, K.; Knížek, K.; Rodová, M.

    1994-08-01

    PbCl 2 was examined by X-ray diffraction in order to test information about polymorphism in this compound. X-ray diffraction patterns of PbCl 2 crystallized from the aqueous solution, as well as of PbCl 2 molten and quenched, are the same. Two modifications in PbCl 2 were not found and polymorphism was not confirmed.

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

    SciTech Connect

    Lorenz, Ulf; Moeller, Klaus B.; Henriksen, Niels E.

    2010-02-15

    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 systems simultaneously illuminated by x rays and a laser beam.

  4. Microbeam X-Ray Standing Wave and High Resolution Diffraction

    SciTech Connect

    Kazimirov, A.; Bilderback, D.H.; Huang, R.; Sirenko, A.

    2004-05-12

    Post-focusing collimating optics are introduced as a tool to condition X-ray microbeams for the use in high-resolution X-ray diffraction and scattering techniques. As an example, a one-bounce imaging capillary and miniature Si(004) channel-cut crystal were used to produce a microbeam with 10 {mu}m size and an ultimate angular resolution of 2.5 arc sec. This beam was used to measure the strain in semiconductor microstructures by using X-ray high resolution diffraction and standing wave techniques to {delta}d/d < 5x10-4.

  5. In-situ mechanical testing during X-ray diffraction

    SciTech Connect

    Van Swygenhoven, Helena Van Petegem, Steven

    2013-04-15

    Deforming metals during recording X-ray diffraction patterns is a useful tool to get a deeper understanding of the coupling between microstructure and mechanical behaviour. With the advances in flux, detector speed and focussing techniques at synchrotron facilities, in-situ mechanical testing is now possible during powder diffraction and Laue diffraction. The basic principle is explained together with illustrative examples.

  6. X-Ray Diffraction Microscopy of Magnetic Structures

    SciTech Connect

    Turner, J.; Lima, E.; Huang, X.; Krupin, O.; Seu, K.; Parks, D.; Kevan, S.; Kisslinger, K.; McNulty, I.; Gambino, R.; Mangin, S.; Roy, S. and Fischer, P.

    2011-07-14

    We report the first proof-of-principle experiment of iterative phase retrieval from magnetic x-ray diffraction. By using the resonant x-ray excitation process and coherent x-ray scattering, we show that linearly polarized soft x rays can be used to image both the amplitude and the phase of magnetic domain structures. We recovered the magnetic structure of an amorphous terbium-cobalt thin film with a spatial resolution of about 75 nm at the Co L{sub 3} edge at 778 eV. In comparison with soft x-ray microscopy images recorded with Fresnel zone plate optics at better than 25 nm spatial resolution, we find qualitative agreement in the observed magnetic structure.

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

    SciTech Connect

    Not Available

    1992-02-01

    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.

  8. Cryogenic X-Ray Diffraction Microscopy for Biological Samples

    SciTech Connect

    Lima, Enju; Wiegart, Lutz; Pernot, Petra; Howells, Malcolm; Timmins, Joanna; Zontone, Federico; Madsen, Anders

    2009-11-06

    X-ray diffraction microscopy (XDM) is well suited for nondestructive, high-resolution biological imaging, especially for thick samples, with the high penetration power of x rays and without limitations imposed by a lens. We developed nonvacuum, cryogenic (cryo-) XDM with hard x rays at 8 keV and report the first frozen-hydrated imaging by XDM. By preserving samples in amorphous ice, the risk of artifacts associated with dehydration or chemical fixation is avoided, ensuring the imaging condition closest to their natural state. The reconstruction shows internal structures of intact D. radiodurans bacteria in their natural contrast.

  9. Experimental investigation of soft x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Xu, Xiangdong; Hong, Yilin; Huo, Tonglin; Jiang, Shipiing; Shan, Xiaobin; Yang, Shaoguang; Fu, Shaojun

    2000-05-01

    The experimental study on soft x-ray diffraction using gold test objects has been carried out with synchrotron radiation at NSRL. Some images, which correspond to 0, 2 and 80 mm away from a specimen, were recorded as relief pattern on photoresist with use of 3.2 nm x-rays from U12A beamline. The experimental result shows that patterns vary with the distance between specimen and photoresist detector, which is in excellent agreement with the theoretical one.

  10. Coherent grating x-ray diffraction (CGXD) and its applications

    SciTech Connect

    Shen, Q.

    1996-09-01

    We show that an x-ray interference phenomenon, coherent grating x-ray diffraction (CGXD), can be used to study lateral nanostructure arrays on crystal surfaces and interfaces. Compared to Fraunhofer grating diffraction of visible light, x-ray grating diffraction contains information not only about geometric profiles of the surface but also about the internal crystalline structures and lattice strain distributions in the grating features. The grating diffraction pattern can also be measured in a white-beam Laue method using highly collimated polychromatic synchrotron radiation, which provides a parallel data collection scheme and may be useful in {ital in} {ital situ} studies on evolution of nanostructure arrays. {copyright} {ital 1996 American Institute of Physics.}

  11. MSL Chemistry and Mineralogy X-ray Diffraction X-ray Fluorescence (CheMin) Instrument

    NASA Astrophysics Data System (ADS)

    Zimmerman, W.; Blake, D.; Harris, W.; Morookian, J. M.; Randall, D.; Reder, L. J.; Sarrazin, P.

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy X-ray 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.

  12. X-ray server : an outline resource for simulations of x-ray diffraction and scattering.

    SciTech Connect

    Stepanov, S.; Biosciences Division

    2004-01-01

    X-ray Server is a public project operational at the APS since 1997 with the goals to explore novel network technologies for providing wide scientific community with access to personal research results, establishing scientific collaborations, and refining scientific software. The Server provides Web-based access to a number of programs developed by the author in the field of X-ray diffraction and scattering. The software code operates directly on the Server available for use without downloading. Currently seven programs are accessible that have been used more than 85,000 times. This report discusses the Server philosophy, provides an overview of the physical models and algorithms beneath the codes and demonstrates some applications of the programs. It is shown with examples and statistics how the Server goals are achieved. The plans for further X-ray Server development are outlined.

  13. X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

    NASA Technical Reports Server (NTRS)

    Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

    2010-01-01

    A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

  14. Ultrafast X-ray Diffraction at the LCLS

    NASA Astrophysics Data System (ADS)

    Weierstall, U.

    2011-10-01

    The recent commissioning of the Linac Coherent Light Source (LCLS), the first hard X-ray femtosecond laser, opens up new and exciting opportunities for biological structure determination. It has been proposed that femtosecond X-ray pulses can be used to outrun damage processes by using single pulses so brief that they terminate before the manifestation of damage to the sample. X-ray crystallography provides so far the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. The high intensity femtosecond X-ray pulses generated at the LCLS allow using nanocrystals or even single particles for biological structure determination. During the first biological imaging beamtimes at the LCLS we have collected millions of snapshot diffraction patterns from membrane protein nanocrystals and single virus particles. New methods for injecting biomolecules/nanocrystals into the X-ray beam as well as new data analysis algorithms had to be developed. I will describe these experiments and their challenges.ootnotetextChapman, H.N., et al., Femtosecond X-ray protein nanocrystallography. Nature, 2011. 470 (7332): p. 73-U81.^,ootnotetextSeibert, M.M., et al., Single mimivirus particles intercepted and imaged with an X-ray laser. Nature, 2011. 470 (7332): p. 78-U86.

  15. Biological imaging by soft x-ray diffraction microscopy

    SciTech Connect

    Shapiro, D.; Thibault, P.; Beetz, T.; Elser, V.; Howells, M.; Jacobsen, C.; Kirz, J.; Lima, E.; Miao, H.; Neiman, A. M.; Sayre, D.

    2005-10-25

    We have used the method of x-ray diffraction microscopy to image the complex-valued exit wave of an intact and unstained yeast cell. The images of the freeze-dried cell, obtained by using 750-eV x-rays from different angular orientations, portray several of the cell's major internal components to 30-nm resolution. The good agreement among the independently recovered structures demonstrates the accuracy of the imaging technique. To obtain the best possible reconstructions, we have implemented procedures for handling noisy and incomplete diffraction data, and we propose a method for determining the reconstructed resolution. This work represents a previously uncharacterized application of x-ray diffraction microscopy to a specimen of this complexity and provides confidence in the feasibility of the ultimate goal of imaging biological specimens at 10-nm resolution in three dimensions.

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

    SciTech Connect

    Dane Morgan, Don Macy, Michael Madlener, Jaiming Morgan

    2007-06-01

    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 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 1 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 studied.

  17. Towards high-resolution ptychographic x-ray diffraction microscopy

    SciTech Connect

    Takahashi, Yukio; Suzuki, Akihiro; Yamauchi, Kazuto; Zettsu, Nobuyuki; Kohmura, Yoshiki; Ishikawa, Tetsuya; Senba, Yasunori; Ohashi, Haruhiko

    2011-06-01

    Ptychographic x-ray diffraction microscopy is a lensless imaging technique with a large field of view and high spatial resolution, which is also useful for characterizing the wavefront of an x-ray probe. The performance of this technique is degraded by positioning errors due to the drift between the sample and illumination optics. We propose an experimental approach for correcting the positioning errors and demonstrate success by two-dimensionally reconstructing both the wavefront of the focused x-ray beam and the complex transmissivity of the weakly scattering objects at the pixel resolution of better than 10 nm in the field of view larger than 5 {mu}m. This method is applicable to not only the observation of organelles inside cells or nano-mesoscale structures buried within bulk materials but also the characterization of probe for single-shot imaging with x-ray free electron lasers.

  18. Modern X-ray Diffraction Methods in Mineralogy and Geosciences

    SciTech Connect

    Lavina, Barbara; Dera, Przemyslaw; Downs, Robert T.

    2014-01-01

    This section is not intended to be comprehensive or detailed, because diffraction is such a vast subject. The principles of diffraction theory, however, are summarized under the assumption that the reader is familiar with basic concepts of the crystalline state. We will briefly review the basics of diffraction techniques, using laboratory and synchrotron X-ray sources and highlight some of their applications in geoscience.

  19. Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

    NASA Technical Reports Server (NTRS)

    Kuriyama, M.; Steiner, B. W.; Dobbyn, R. C.

    1989-01-01

    By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

  20. Multiwavelength anomalous diffraction at high x-ray intensity

    NASA Astrophysics Data System (ADS)

    Santra, Robin

    2013-05-01

    The coherent x-ray scattering pattern of a molecule is connected to the modulus squared of the Fourier transform of the electron density of the molecule. The phase of this Fourier transform is not measured. As a consequence, a reconstruction of the electron density--and thus of the molecular structure--is not immediately possible. In x-ray crystallography at storage-ring-based synchrotron radiation sources, the multiwavelength anomalous diffraction (MAD) method is used to determine phase information by employing anomalous scattering from heavy atoms. X-ray free-electron lasers (FELs) provide the extremely high x-ray intensity required for revealing the structure of single molecules or nanocrystals, but the phase problem remains largely unsolved. A particular challenge is that, at high x-ray intensity, samples experience severe electronic radiation damage, especially to heavy atoms, which hinders direct implementation of MAD with x-ray FELs. In the first part of the talk, I will discuss how MAD phasing can be extended to high x-ray intensity. The proposed technique relies on the existence of a Karle-Hendrickson-type equation in the high-intensity regime and requires the ability to computationally predict the x-ray-induced ionization dynamics of heavy atoms. In the second part of the talk, this ability will be put to the test. I will review x-ray FEL experiments that have been carried out on atomic xenon and will compare the observations to extensive first-principles calculations. At sufficiently high photon energies, there is good agreement between experiment and theory. However, close to inner-shell edges, which play a key role for MAD phasing, specific discrepancies are found. A strategy will be discussed that is expected to allow us to eliminate these discrepancies.

  1. Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

    NASA Technical Reports Server (NTRS)

    Blake, David F.; DeVincenzi, D. (Technical Monitor)

    1999-01-01

    The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

  2. Ultrafast x-ray diffraction of laser-irradiated crystals

    SciTech Connect

    Heimann, P.A.; Larsson, J.; Chang, Z.

    1997-09-01

    An apparatus has been developed for measuring time-dependent x-ray diffraction. X-ray pulses from an Advanced Light Source bend magnet are diffracted by a sagittally-focusing Si(111) crystal and then by a sample crystal, presently InSb(111). Laser pulses with 100 fs duration and a repetition rate of 1 KHz irradiate the sample inducing a phase transition. Two types of detectors are being employed: an x-ray streak camera and an avalanche photodiode. The streak camera is driven by a photoconductive switch and has a 2 ps temporal resolution determined by trigger jitter. The avalanche photodiode has high quantum efficiency and sufficient time resolution to detect single x-ray pulses in ALS two bunch or camshaft operation. A beamline is under construction dedicated for time resolved and micro-diffraction experiments. In the new beamline a toroidal mirror collects 3 mrad horizontally and makes a 1:1 image of the bend magnet source in the x-ray hutch. A laser induced phase transition has been observed in InSb occurring within 70 ps.

  3. Biological imaging by soft x-ray diffraction microscopy

    DOE PAGESBeta

    Shapiro, D.; Thibault, P.; Beetz, T.; Elser, V.; Howells, M.; Jacobsen, C.; Kirz, J.; Lima, E.; Miao, H.; Neiman, A. M.; et al

    2005-10-25

    We have used the method of x-ray diffraction microscopy to image the complex-valued exit wave of an intact and unstained yeast cell. The images of the freeze-dried cell, obtained by using 750-eV x-rays from different angular orientations, portray several of the cell's major internal components to 30-nm resolution. The good agreement among the independently recovered structures demonstrates the accuracy of the imaging technique. To obtain the best possible reconstructions, we have implemented procedures for handling noisy and incomplete diffraction data, and we propose a method for determining the reconstructed resolution. This work represents a previously uncharacterized application of x-ray diffractionmore » microscopy to a specimen of this complexity and provides confidence in the feasibility of the ultimate goal of imaging biological specimens at 10-nm resolution in three dimensions.« less

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

    SciTech Connect

    Dane V. Morgan

    2006-10-01

    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.

  5. Coherent diffraction imaging using focused hard X-rays

    NASA Astrophysics Data System (ADS)

    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.

  6. Assessment of quartz materials crystallinity by x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Korovkin, M.; AnanIeva, L.; Nebera, T.; Antsiferova, A.

    2016-02-01

    The estimated degree of crystallinity of natural and synthetic grown quartz and quartzite by calculating the x-ray diffraction patterns. It is shown that the index of crystallinity of natural quartzite varies widely, reflecting the different degree of their transformation. The highest values of the index of crystallinity are characterized natural and synthetic single crystals of quartz.

  7. A Practical Method of Simulating X-Ray Diffraction

    ERIC Educational Resources Information Center

    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)

  8. X-ray diffraction at Matter in Extreme Conditions endstation

    NASA Astrophysics Data System (ADS)

    Xing, Zhou; Galtier, Eric; Lee, Hae Ja; Nagler, Bob

    2015-11-01

    Understanding dynamic response at the atomic level under extreme conditions is highly sought after goal to science frontiers studying warm dense matter, high pressure, geoscience, astrophysics, and planetary science. Thus it is of importance to determine the high pressure phases or metastable phases of material under shock compression. In situ X-ray diffraction technique using LCLS free electron laser X-ray is a powerful tool to record structural behavior and microstructure evolution in dense matter. Shock-induced compression and phase transitions of material lead to changes of the lattice spacing or evolution of new X-ray diffraction patterns. In this talk, we describe a platform dedicated for the X-ray diffraction studies at Matter in Extreme Conditions (MEC), which can be used to reconstruct a complete diffraction pattern from numerous detectors, optimize detector positioning in a timely manner, extract the lattice spacing profiles and texture features. This platform is available to the user community for real-time analysis. We will also discuss experimental results, using this platform, on the crystalline silicon phase transitions up to 60 GPa.

  9. Coherent X-ray diffraction from collagenous soft tissues

    SciTech Connect

    Berenguer de la Cuesta, Felisa; Wenger, Marco P.E.; Bean, Richard J.; Bozec, Laurent; Horton, Michael A.; Robinson, Ian K.

    2009-09-11

    Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.

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

    ERIC Educational Resources Information Center

    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)

  11. Single photon energy dispersive x-ray diffraction

    SciTech Connect

    Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S.; Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H.; Tang, Henry

    2014-03-15

    With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.

  12. Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

    NASA Technical Reports Server (NTRS)

    Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

    2004-01-01

    High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

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

    SciTech Connect

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; Grant, Thomas D.; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S.; Liang, Mengning; Boutet, Sébastien; Coe, Jesse; Spence, John C. H.; Weierstall, Uwe; Liu, Wei; Fromme, Petra; Cherezov, Vadim; Hogue, Brenda G.

    2015-08-20

    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 a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

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

    DOE PAGESBeta

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; Grant, Thomas D.; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S.; et al

    2015-08-20

    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 diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 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 a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

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

    NASA Technical Reports Server (NTRS)

    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.

  16. Discovery and development of x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Jeong, Yeuncheol; Yin, Ming; Datta, Timir

    2013-03-01

    In 1912 Max Laue at University of Munich reasoned x-rays to be short wavelength electromagnetic waves and figured interference would occur when scattered off crystals. Arnold Sommerfeld, W. Wien, Ewald and others, raised objections to Laue's idea, but soon Walter Friedrich succeeded in recording x-ray interference patterns off copper sulfate crystals. But the Laue-Ewald's 3-dimensional formula predicted excess spots. Fewer spots were observed. William Lawrence Bragg then 22 year old studying at Cambridge University heard the Munich results from father William Henry Brag, physics professor at Univ of Leeds. Lawrence figured the spots are 2-d interference of x-ray wavelets reflecting off successive atomic planes and derived a simple eponymous equation, the Bragg equation d*sin(theta) = n*lamda. 1913 onward the Braggs dominated the crystallography. Max Laue was awarded the physics Nobel in 1914 and the Braggs shared the same in 1915. Starting with Rontgen's first ever prize in 1901, the importance of x-ray techniques is evident from the four out of a total 16 physics Nobels between 1901-1917. We will outline the historical back ground and importance of x-ray diffraction giving rise to techniques that even in 2013, remain work horses in laboratories all over the globe.

  17. Ultrahigh-resolution soft-x-ray microscopy with zone plates in high orders of diffraction.

    PubMed

    Rehbein, S; Heim, S; Guttmann, P; Werner, S; Schneider, G

    2009-09-11

    We present an x-ray optical approach to overcome the current limitations in spatial resolution of x-ray microscopes. Our new BESSY full-field x-ray microscope operates with an energy resolution up to E/DeltaE=10(4). We demonstrate that under these conditions it is possible to employ high orders of diffraction for imaging. Using the third order of diffraction of a zone plate objective with 25 nm outermost zone width, 14 nm lines and spaces of a multilayer test structure were clearly resolved. We believe that high-order imaging paves the way towards sub-10-nm real space x-ray imaging. PMID:19792359

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

    SciTech Connect

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

    2011-09-15

    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.

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

    NASA Astrophysics Data System (ADS)

    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 ) is characteristic of cross-beta sheet structure, consistent with previous results from powder diffraction studies performed on purified, dried tau protein.

  20. Coherent X-ray Diffraction Imaging of Zeolite Microcrystals

    SciTech Connect

    Cha, Wonsuk; Song, Sanghoon; Kim, Hyunjung; Jeong, Nak Cheon; Yoon, Kyung Byung; Harder, Ross; Robinson, Ian K.

    2009-04-19

    We measured coherent x-ray diffraction (CXD), an emerging technique to obtain three-dimensional internal and external images of crystals, on ZSM-5 zeolite microcrystals to get internal density distribution and to map deformation field of strain. The experiments were performed at the beamline 34-ID-C in Advanced Photon Source at Argonne National Laboratory in the US. The CXD patterns of ZSM-5 zeolite microcrystals with sizes of 2 {mu}m by monochromatic coherent x-rays with energy of 9 keV were obtained under continuously surrounding and Bragg conditions as a function of temperature. The oversampled diffraction patterns are inverted to obtain three-dimensional images of the shapes and internal strain fields of zeolite microcrystals using phase retrieval algorithms of error reduction and a hybrid input-output method. The internal density and strain distribution as a function of temperature are discussed.

  1. Liquid detection trial with x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Harding, G.; Fleckenstein, H.; Olesinski, S.; Zienert, G.

    2010-08-01

    SALOME (an acronym for Small Angle Lab Operation Measuring Equipment) is a versatile, energy-dispersive x-ray diffraction imaging (XDi) test-bed facility commissioned and supported by the Transportation Security Laboratory, Atlantic City, USA. In work presented here, the Inverse Fan-beam (IFB) topology has been realized on SALOME and used to investigate the liquids identification capability of x-ray diffraction (XRD). Liquids were investigated from four classes of materials of relevance to security screening of aircraft passenger luggage; namely: dilute aqueous liquids; concentrated aqueous liquids; hydrocarbon fuels; and oxidizers. A set of features associated with the Molecular Interference Function (MIF) were used to classify the liquids. Within the limited scope of this investigation, XRD proved to have excellent capability for discriminating liquids from one another; in particular, for isolating the threat materials without raising false alarms from either household or innocuous substances. Consequences for XRD-based screening of air passenger luggage are summarized.

  2. A new approach to synchrotron energy-dispersive X-ray diffraction computed tomography.

    PubMed

    Lazzari, Olivier; Egan, Christopher K; Jacques, Simon D M; Sochi, Taha; Di Michiel, Marco; Cernik, Robert J; Barnes, Paul

    2012-07-01

    A new data collection strategy for performing synchrotron energy-dispersive X-ray diffraction computed tomography has been devised. This method is analogous to angle-dispersive X-ray diffraction whose diffraction signal originates from a line formed by intersection of the incident X-ray beam and the sample. Energy resolution is preserved by using a collimator which defines a small sampling voxel. This voxel is translated in a series of parallel straight lines covering the whole sample and the operation is repeated at different rotation angles, thus generating one diffraction pattern per translation and rotation step. The method has been tested by imaging a specially designed phantom object, devised to be a demanding validator for X-ray diffraction imaging. The relative strengths and weaknesses of the method have been analysed with respect to the classic angle-dispersive technique. The reconstruction accuracy of the method is good, although an absorption correction is required for lower energy diffraction because of the large path lengths involved. The spatial resolution is only limited to the width of the scanning beam owing to the novel collection strategy. The current temporal resolution is poor, with a scan taking several hours. The method is best suited to studying large objects (e.g. for engineering and materials science applications) because it does not suffer from diffraction peak broadening effects irrespective of the sample size, in contrast to the angle-dispersive case. PMID:22713876

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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

  5. Coherent X-ray diffraction from collagenous soft tissues

    PubMed Central

    Berenguer de la Cuesta, Felisa; Wenger, Marco P. E.; Bean, Richard J.; Bozec, Laurent; Horton, Michael A.; Robinson, Ian K.

    2009-01-01

    Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60–70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the ‘speckled’ nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques. PMID:19706395

  6. X-ray diffraction microscopy on frozen hydrated specimens

    NASA Astrophysics Data System (ADS)

    Nelson, Johanna

    X-rays are excellent for imaging thick samples at high resolution because of their large penetration depth compared to electrons and their short wavelength relative to visible light. To image biological material, the absorption contrast of soft X-rays, especially between the carbon and oxygen K-shell absorption edges, can be utilized to give high contrast, high resolution images without the need for stains or labels. Because of radiation damage and the desire for high resolution tomography, live cell imaging is not feasible. However, cells can be frozen in vitrified ice, which reduces the effect of radiation damage while maintaining their natural hydrated state. X-ray diffraction microscopy (XDM) is an imaging technique which eliminates the limitations imposed by current focusing optics simply by removing them entirely. Far-field coherent diffraction intensity patterns are collected on a pixelated detector allowing every scattered photon to be collected within the limits of the detector's efficiency and physical size. An iterative computer algorithm is then used to invert the diffraction intensity into a real space image with both absorption and phase information. This technique transfers the emphasis away from fabrication and alignment of optics, and towards data processing. We have used this method to image a pair of freeze-dried, immuno-labeled yeast cells to the highest resolution (13 nm) yet obtained for a whole eukaryotic cell. We discuss successes and challenges in working with frozen hydrated specimens and efforts aimed at high resolution imaging of vitrified eukaryotic cells in 3D.

  7. Fabricating Blazed Diffraction Gratings by X-Ray Lithography

    NASA Technical Reports Server (NTRS)

    Mouroulis, Pantazis; Hartley, Frank; Wilson, Daniel

    2004-01-01

    Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

  8. Soft x-ray imaging and vector diffraction theory

    SciTech Connect

    Burge, R.E.; Yuan, X.C.

    1995-12-31

    A comprehensive computational analysis of soft x-ray imaging has been undertaken for both thin transmitting objects and lossy dielectric, potentially binary, objects and some representative results are given here. Both near-field and far-field computations are considered. The theoretical treatment derives from Maxwell`s vector electromagnetic equations rather than scalar diffraction theory. A range of computational approaches is used in the computations ranging from the integral method, to the coupled wave method, and the finite element methods. The relationships between these methods are considered. The results bear upon a range of imaging protocols from contact x-ray images and images taken with high resolution zone plate optics with feature dimensions of a few wavelengths to x-ray masks with sub-micron feature sizes interpreted as lossy waveguides several hundreds of x-ray wavelengths thick. Consideration is also given to the use of vector theory in the investigation of the focal plane intensity profile of a circular Fresnel zone plate when the widths of the outermost zones approach wavelength dimensions.

  9. Coherent x-ray diffraction from quantum dots

    SciTech Connect

    Vartanyants, I.A.; Robinson, I. K.; Onken, J.D.; Pfeifer, M.A.; Williams, G.J.; Pfeiffer, F.; Metzger, H.; Zhong, Z.; Bauer, G.

    2005-06-15

    Coherent x-ray diffraction is a new experimental method for studying perfect and imperfect crystals. Instead of incoherent averaging, a coherent sum of amplitudes produces a coherent diffraction pattern originating from the real space arrangement of the sample. We applied this method for studying quantum dot samples that were specially fabricated GeSi islands of nanometer size and in a regular array embedded into a Si substrate. A coherent beam was focused by special Kirkpatric-Baez optics to a micrometer size. In the experiment it was observed that such a microfocused coherent beam produced coherent diffraction pattern with Bragg spots and broad diffuse maxima. The diffuse peak breaks up into a fine speckle pattern. The grazing incidence diffraction pattern has a typical shape resulting from the periodic array of identical islands. We used this diffraction pattern to reconstruct the average shape of the islands using a model independent approach.

  10. X-ray diffraction computed tomography: a survey and description

    NASA Astrophysics Data System (ADS)

    Kleuker, Ulf

    1997-10-01

    Coherently scattered x-rays are mainly confined to a forward peaked cone, which exhibits, due to their coherence, structural information of the atomic arrangement in the sample. Coherent scattering in amorphous materials, which are of random short range order, therefore results in board diffraction ring patter, whereas crystalline substance show more confined diffraction rings or even Brag spots. X-ray diffraction computed tomography (XRDCT) reconstructs the intensities diffracted from extended objects on a square image grid and thus retrieves the local structure. A short survey is presented about what information can be extracted from diffraction experiments. Hereby a new method is proposed to use the Rietveld refinement for quantitative XRDCT. Also the possible use of XRDCT to reconstruct the spatial distribution of preferred orientation axis is suggested. An imaging system for XRDCT, consisting of a medical image intensifier tube and CCD readout system, is presented, which includes a modified beam stop for recording the intensity of the transmitted beam. Depending on the application this imaging system cam work in first generation or second generation tomography mode. Furthermore a new approach for the reconstruction of the differential coherent cross-section is proposed. It includes an absorption correction based on weighted sinograms. The introduced reconstruction strategy is elucidated by experimental result from a simple phantom. The measured data also validate the simulation program, written to study more complex phantoms under different experimental conditions. Finally possible applications in medical and material science are discussed. A design for a mammography setup using x-ray diffraction is presented.

  11. Synchrotron x-ray powder diffraction studies in pulsed magnetic fields

    SciTech Connect

    Frings, P.; Vanacken, J.; Detlefs, C.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Bras, W.; Rikken, G. L. J. A.

    2006-06-15

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110 kJ to the magnet coil, which was sufficient to generate peak fields of 30 T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8 and 300 K. Powder diffraction patterns of several samples were recorded using 21 keV monochromatic x-rays and an on-line image plate detector. Here we present the first results on the suppression of the Jahn-Teller structural distortion in TbVO{sub 4} by magnetic field. These data clearly demonstrate the feasibility of x-ray powder diffraction experiments under pulsed magnetic fields with relatively inexpensive instrumentation.

  12. Portable energy dispersive X-ray fluorescence and X-ray diffraction and radiography system for archaeometry

    NASA Astrophysics Data System (ADS)

    Mendoza Cuevas, Ariadna; Perez Gravie, Homero

    2011-03-01

    Starting on a laboratory developed portable X-ray fluorescence (PXRF) spectrometer; three different analytical results can be performed: analysis of chemical elements, analysis of major chemical crystalline phase and structural analysis, which represents a contribution to a new, low cost development of portable X-ray analyzer; since these results are respectively obtained with independent equipments for X-ray fluorescence, X-ray diffraction and radiography. Detection limits of PXRF were characterized using standard reference materials for ceramics, glass, bronze and bones, which are the main materials requiring quantitative analysis in art and archeological objects. A setup for simultaneous energy dispersive X-ray fluorescence and diffraction (ED (XRF-XRD)) in the reflection mode has been tested for in situ and non-destructive analysis according to the requirements of art objects inspection. The system uses a single low power X-ray tube and an X-ray energy dispersive detector to measure X-ray diffraction spectrum at a fixed angle. Application to the identification of jadeite-jade mineral in archeological objects by XRD is presented. A local high resolution radiography image obtained with the same low power X-ray tube allows for studies in painting and archeological bones.

  13. X-ray nano-diffraction on cytoskeletal networks

    NASA Astrophysics Data System (ADS)

    Weinhausen, Britta; Nolting, Jens-Friedrich; Olendrowitz, Christian; Langfahl-Klabes, Jannick; Reynolds, Michael; Salditt, Tim; Kster, Sarah

    2012-08-01

    The nano-scale structure of cytoskeletal biopolymers as well as sophisticated superstructures determine the versatile cellular shapes and specific mechanical properties. One example is keratin intermediate filaments in epithelial cells, which form thick bundles that can further organize in a cross-linked network. To study the native structure of keratin bundles in whole cells, high-resolution techniques are required, which do at the same time achieve high penetration depths. We employ scanning x-ray diffraction using a nano-focused x-ray beam to study the structure of keratin in freeze-dried eukaryotic cells. By scanning the sample through the beam we obtain x-ray dark-field images with a resolution of the order of the beam size, which clearly show the keratin network. Each individual diffraction pattern is further analyzed to yield insight into the local sample structure, which allows us to determine the local structure orientation. Due to the small beam size we access the structure in a small sample volume without performing the ensemble average over one complete cell.

  14. Quantum-dot-array diffraction grating with single order diffraction property for soft x-ray region

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed Central

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; Grant, Thomas D.; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S.; Liang, Mengning; Boutet, Sbastien; Coe, Jesse; Spence, John C. H.; Weierstall, Uwe; Liu, Wei; Fromme, Petra; Cherezov, Vadim; Hogue, Brenda G.

    2015-01-01

    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? diameter. Microcrystals delivered in viscous agarose medium diffracted to ?40? 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. PMID:26798819

  16. Synchrotron X-ray Microbeam Diffraction from Abalone Shell

    NASA Astrophysics Data System (ADS)

    Dimasi, Elaine; Sarikaya, Mehmet

    2004-03-01

    Microstructured biomaterials such as mollusk shells receive much attention, due to the promise that advanced materials can be designed and synthesized with biomimetic techniques that take advantage of self-assembly and aqueous, ambient processing conditions. A satisfactory understanding of this process requires characterization of the microstructure at the growth fronts where control over crystal orientation and morphology is enacted. We present synchrotron x-ray microbeam observations near the nacre-prismatic interface of red abalone shell (Haliotis rufescens). The relative orientations of calcite and aragonite grains exhibit differences from the idealizations reported previously. Long calcite grains impinge the boundary at 45^rc angles, suggestive of nucleation on (104) planes followed by c-axis growth. Within 100 μm of the boundary, crystals lose their bulk orientational order. The calcite crystal mosaic measured by x-ray diffraction rocking curves is resolution limited, comparable to geological calcite.

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

    PubMed

    Lawrence, Robert M; Conrad, Chelsie E; Zatsepin, Nadia A; Grant, Thomas D; Liu, Haiguang; James, Daniel; Nelson, Garrett; Subramanian, Ganesh; Aquila, Andrew; Hunter, Mark S; Liang, Mengning; Boutet, Sébastien; Coe, Jesse; Spence, John C H; Weierstall, Uwe; Liu, Wei; Fromme, Petra; Cherezov, Vadim; Hogue, Brenda G

    2015-07-01

    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. PMID:26798819

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

    NASA Astrophysics Data System (ADS)

    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. Diffraction enhanced kinetic depth X-ray imaging

    NASA Astrophysics Data System (ADS)

    Dicken, A.

    An increasing number of fields would benefit from a single analytical probe that can characterise bulk objects that vary in morphology and/or material composition. These fields include security screening, medicine and material science. In this study the X-ray region is shown to be an effective probe for the characterisation of materials. The most prominent analytical techniques that utilise X-radiation are reviewed. The study then focuses on methods of amalgamating the three dimensional power of kinetic depth X-ray (KDFX) imaging with the materials discrimination of angular dispersive X-ray diffraction (ADXRD), thus providing KDEX with a much needed material specific counterpart. A knowledge of the sample position is essential for the correct interpretation of diffraction signatures. Two different sensor geometries (i.e. circumferential and linear) that are able to collect end interpret multiple unknown material diffraction patterns and attribute them to their respective loci within an inspection volume are investigated. The circumferential and linear detector geometries are hypothesised, simulated and then tested in an experimental setting with the later demonstrating a greater ability at discerning between mixed diffraction patterns produced by differing materials. Factors known to confound the linear diffraction method such as sample thickness and radiation energy have been explored and quantified with a possible means of mitigation being identified (i.e. via increasing the sample to detector distance). A series of diffraction patterns (following the linear diffraction approach) were obtained from a single phantom object that was simultaneously interrogated via KDEX imaging. Areas containing diffraction signatures matched from a threat library have been highlighted in the KDEX imagery via colour encoding and match index is inferred by intensity. This union is the first example of its kind and is called diffraction enhanced KDEX imagery. Finally an additional source of information obtained from object disparity is explored as an alternative means of calculating sample loci. This offers a greater level of integration between these two complimentary techniques as object disparity could be used to reinforce the results produced by the linear diffraction geometry.

  20. Diffraction imaging of crystals with focused x-ray beams

    SciTech Connect

    Kazimirov, A.; Kohn, V. G.; Cai, Z.-H.

    2010-06-01

    We describe an imaging technique based on diffraction of a focused x-ray beam in crystals. A focused beam is formed by a zone plate and Bragg diffracted from a crystalline sample positioned between the zone plate and the focus. The intensity pattern is recorded by a high-resolution charge-coupled-device detector placed in the focus. Diffraction images recorded from perfect Si and GaAs crystals for various reflections demonstrate the broadening of the focused beam due to a finite scattering length. The images from semiconductor epitaxial films and heterostructures show additional peaks originating from the interfaces with their spatial position corresponding to the depth from the surface. Diffraction images from isolated defects in Si crystal demonstrate capabilities to study bulk defects. Theoretical simulations for perfect crystals show excellent agreement with experiments. We demonstrate that the new imaging technique is depth sensitive and combines structural sensitivity of traditional x-ray topography methods with spatial in-plane resolution provided by focusing.

  1. Interstellar ultraviolet absorption lines and galactic X-ray sources

    NASA Technical Reports Server (NTRS)

    Mccray, R.; Wright, C.; Hatchett, S.

    1977-01-01

    X-ray photoionization can create zones of highly ionized trace elements in the interstellar gas around a galactic X-ray source. Ultraviolet absorption lines due to the resulting ionic column densities may be observable and may provide information on the environment and age of the X-ray source. The calculated column densities are sensitive to the rates of charge-exchange reactions.

  2. Soft x-ray coherent diffraction imaging on magnetic nanostructures

    NASA Astrophysics Data System (ADS)

    Shi, Xiaowen; Lee, James; Mishra, Shrawan; Parks, Daniel; Tyliszczak, Tolek; Shapiro, David; Roy, Sujoy; Kevan, Steve; Stxm Team At Als Collaboration; Soft X-Ray Microscopy Group At Als Collaboration; Soft X-ray scattering at ALS, LBL Team

    2014-03-01

    Coherent soft X-rays diffraction imaging enable coherent magnetic resonance scattering at transition metal L-edge to be probed so that magnetic domains could be imaged with very high spatial resolution with phase contrast, reaching sub-10nm. One of the overwhelming advantages of using coherent X-rays is the ability to resolve phase contrast images with linearly polarized light with both phase and absorption contrast comparing to real-space imaging, which can only be studied with circularly polarized light with absorption contrast only. Here we report our first results on high-resolution of magnetic domains imaging of CoPd multilayer thin film with coherent soft X-ray ptychography method. We are aiming to resolve and understand magnetic domain wall structures with the highest obtainable resolution here at Advanced Light Source. In principle types of magnetic domain walls could be studied so that Neel or Bloch walls can be distinguished by imaging. This work at LBNL was supported by the Director, Office of Science, Office of Basic Energy Sciences, of the US Department of Energy (contract no. DE-AC02- 05CH11231).

  3. X-ray Mirage Diffraction and Its Interference Fringes

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  5. X-ray diffraction studies of shocked lunar analogs

    NASA Technical Reports Server (NTRS)

    Hanss, R. E.

    1979-01-01

    The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

  6. The three dimensional X-ray diffraction technique

    SciTech Connect

    Jensen, D. Juul; Poulsen, H.F.

    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.

  7. High Pressure X-ray Diffraction Study of Potassium Azide

    SciTech Connect

    C Ji; F Zhang; D Hong; H Zhu; J Wu; M Chyu; V Levitas; Y Ma

    2011-12-31

    Crystal structure and compressibility of potassium azide was investigated by in-situ synchrotron powder X-ray diffraction in a diamond anvil cell at room temperature up to 37.7 GPa. In the body-centered tetragonal (bct) phase, an anisotropic compressibility was observed with greater compressibility in the direction perpendicular to the plane containing N{sub 3}{sup -} ions than directions within that plane. The bulk modulus of the bct phase was determined to be 18.6(7) GPa. A pressure-induced phase transition may occur at 15.5 GPa.

  8. The three dimensional X-ray diffraction technique

    SciTech Connect

    Jensen, D. Juul; Poulsen, H.F.

    2012-10-24

    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.

  9. X-ray diffraction analysis of modulated crystals: Review

    SciTech Connect

    Bolotina, N. B.

    2007-07-15

    The state of the art of X-ray diffraction analysis of modulated crystals is reviewed. The review begins with a brief historical overview followed by the consideration of the main concepts and notations used in this field. Then, methods of structural analysis of modulated crystals are considered with emphasis on recent achievements. The most interesting objects are listed, and the directions of investigation are outlined. Examples of analysis of both individual structures and families of modulated and incommensurate composite structures are given in terms of superspace symmetry.

  10. X-Ray Diffraction Study of Methanol-Water Mixtures

    NASA Astrophysics Data System (ADS)

    Bak, I.; Plinks, G.; Heinzinger, K.

    1994-10-01

    X-ray diffraction patterns o f m ethanol-water mixtures with mole fractions of methanol molecules o f 0.1, 0.25 and 0.9 have been measured. The experimental structure functions of mixtures are compared with those of pure solvents and with recent Molecular Dynamics results. Difference structure functions similar to thermodynamic excess functions are introduced for the analysis of methanol-water interactions. The comparison of the total and the difference structure functions from experiments and simulations shows an overall good agreement.

  11. Ultrafast X-Ray Diffraction of Heterogeneous Solid Hydrogen

    SciTech Connect

    Levitan, Abraham

    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.

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

    SciTech Connect

    Levitan, Abraham

    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.

  13. Anomalous X-ray Diffraction Studies for Photovoltaic Applications

    SciTech Connect

    Not Available

    2011-06-22

    Anomalous X-ray Diffraction (AXRD) has become a useful technique in characterizing bulk and nanomaterials as it provides specific information about the crystal structure of materials. In this project we present the results of AXRD applied to materials for photovoltaic applications: ZnO loaded with Ga and ZnCo{sub 2}O{sub 4} spinel. The X-ray diffraction data collected for various energies were plotted in Origin software. The peaks were fitted using different functions including Pseudo Voigt, Gaussian, and Lorentzian. This fitting provided the integrated intensity data (peaks area values), which when plotted as a function of X-ray energies determined the material structure. For the first analyzed sample, Ga was not incorporated into the ZnO crystal structure. For the ZnCo{sub 2}O{sub 4} spinel Co was found in one or both tetrahedral and octahedral sites. The use of anomalous X-ray diffraction (AXRD) provides element and site specific information for the crystal structure of a material. This technique lets us correlate the structure to the electronic properties of the materials as it allows us to probe precise locations of cations in the spinel structure. What makes it possible is that in AXRD the diffraction pattern is measured at a number of energies near an X-ray absorption edge of an element of interest. The atomic scattering strength of an element varies near its absorption edge and hence the total intensity of the diffraction peak changes by changing the X-ray energy. Thus AXRD provides element specific structural information. This method can be applied to both crystalline and liquid materials. One of the advantages of AXRD in crystallography experiments is its sensitivity to neighboring elements in the periodic tables. This method is also sensitive to specific crystallographic phases and to a specific site in a phase. The main use of AXRD in this study is for transparent conductors (TCs) analysis. TCs are considered to be important materials because of their efficiency and low risk of environmental pollution. These materials are important to solar cells as a result of their remarkable combination of optical and electrical properties, including high electrical conductivity and high optical transparency in the spectrum of visible light. TCs provide a transparent window, which allows sunlight to pass through while also allowing electricity to conduct out of the cell. Spinel materials have the chemical form AB{sub 2}O{sub 4}, and are made of a face-centered cubic (FCC) lattice of oxygen anions and cations in specific interstitial sites. A normal spinel has all A cations on tetrahedral sites and B cations on octahedral sites. In contrast; an inverse spinel has the A and half of the B cations on octahedral sites and the other half of the B cations on tetrahedral sites; a mixed spinel lies between. In the spinel structure, 8 of 64 possible tetrahedral sites and 16 of 32 possible octahedral sites are filled. Normal spinels have particularly high conduction as the linear octahedral chains of B cations likely serve as conduction paths. In this paper we present how the data obtained with AXRD is used to analyze TCs properties as they apply to photovoltaic applications. One of the materials used for this analysis is zinc oxide. It has been loaded with 5% and 10% of Ga, which has an absorption edge of 10367 eV. The peak (100) was measured for the zinc oxide loaded with 10% Ga. In the case of 5% Ga, we measured peaks (100) and (101). With the information provided by the AXRD we can identify if Ga is being incorporated in the ZnO crystal structure. The analysis of 311 plane in the ZnCo{sub 2}O{sub 4} spinel shows if Co is in tetrahedral or octahedral site.

  14. DiffractX: A Simulation Toolbox for Diffractive X-ray Optics

    NASA Astrophysics Data System (ADS)

    Selin, M.; Bertilson, M.; Nilsson, D.; von Hofsten, O.; Hertz, H. M.; Vogt, U.

    2011-09-01

    X-ray wavefront propagation is a powerful technique when simulating the performance of x-ray optical components. Using various numerical methods, interesting parameters such as focusing capability and efficiency can be investigated. Here we present the toolbox DiffractX, implemented in MATLAB. It contains many different wave propagation methods for the simulation of diffractive x-ray optics, including Fresnel propagation, the finite difference method (FDM), the thin object approximation, the rigorous coupled wave theory (RCWT), and the finite element method (FEM). All tools are accessed through a graphical interface, making the design of simulations fast and intuitive, even for users with little or no programming experience. The tools have been utilized to characterize realistic as well as idealized optical components. This will aid further developments of diffractive x-ray optics.

  15. X-ray diffraction of III-nitrides

    NASA Astrophysics Data System (ADS)

    Moram, M A; Vickers, M E

    2009-03-01

    The III-nitrides include the semiconductors AlN, GaN and InN, which have band gaps spanning the entire UV and visible ranges. Thin films of III-nitrides are used to make UV, violet, blue and green light-emitting diodes and lasers, as well as solar cells, high-electron mobility transistors (HEMTs) and other devices. However, the film growth process gives rise to unusually high strain and high defect densities, which can affect the device performance. X-ray diffraction is a popular, non-destructive technique used to characterize films and device structures, allowing improvements in device efficiencies to be made. It provides information on crystalline lattice parameters (from which strain and composition are determined), misorientation (from which defect types and densities may be deduced), crystallite size and microstrain, wafer bowing, residual stress, alloy ordering, phase separation (if present) along with film thicknesses and superlattice (quantum well) thicknesses, compositions and non-uniformities. These topics are reviewed, along with the basic principles of x-ray diffraction of thin films and areas of special current interest, such as analysis of non-polar, semipolar and cubic III-nitrides. A summary of useful values needed in calculations, including elastic constants and lattice parameters, is also given. Such topics are also likely to be relevant to other highly lattice-mismatched wurtzite-structure materials such as heteroepitaxial ZnO and ZnSe.

  16. An image focusing means by using an opaque object to diffract x-rays

    DOEpatents

    Sommargren, Gary E.; Weaver, H. Joseph

    1991-01-01

    The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

  17. Diffractive-refractive optics: X-ray splitter.

    PubMed

    Hrdý, Jaromír

    2010-01-01

    The possibility of splitting a thin (e.g. undulator) X-ray beam based on diffraction-refraction effects is discussed. The beam is diffracted from a crystal whose diffracting surface has the shape of a roof with the ridge lying in the plane of diffraction. The crystal is cut asymmetrically. One half of the beam impinges on the left-hand part of the roof and the other half impinges on the right-hand side of the roof. Owing to refraction the left part of the beam is deviated to the left whereas the right part is deviated to the right. The device proposed consists of two channel-cut crystals with roof-like diffraction surfaces; the crystals are set in a dispersive position. The separation of the beams after splitting is calculated at a distance of 10 m from the crystals for various asymmetry and inclination angles. It is shown that such a splitting may be utilized for long beamlines. Advantages and disadvantages of this method are discussed. PMID:20029121

  18. Synchrotron X-ray Powder Diffraction and Absorption Spectroscopy in Pulsed Magnetic Fields with Milliseconds Duration

    SciTech Connect

    Vanacken, J.; Detlefs, C.; Mathon, O.; Dominguez, M.-C.; Frings, P.; Duc, F.; Nardone, M.; Billette, J.; Zitouni, A.; Rikken, G.; Lorenzo, J. E.; Herczeg, J.; Moshchalkov, V. V.; Bras, W.

    2007-03-30

    X-ray Powder Diffraction and X-ray Absorption Spectroscopy experiments (WAS) and X-ray magnetic circular dichroism (XMCD) experiments were carried out at the ESRF DUBBLE beam line (BM26) and at the energy dispersive beam line (ID24), respectively. A mobile pulse generator, developed at the LNCMP, delivered 110kJ to the load coil, which was sufficient to generate peak fields of 30T with a rise time of about 5 ms. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 4.2K and 300K.Powder diffraction patterns of TbVO4 were recorded in a broad temperature range using 21 keV monochromatic X-rays and using an on-line image plate detector. We observed the suppression of the Jahn-Teller structural distortion in TbVO4 due to the high magnetic pulsed field.XAS spectra could be measured and finite XMCD signals, directly proportional to the magnetic moment on the Gd absorber atom, were measured in thin Gd foils. Thanks to its element and orbital selectivity, XMCD proofs to be very useful in probing the magnetic properties and due to the strong brilliance of the synchrotron beam, the signals can be measured even in the ms range.

  19. X-Ray Properties of Broad-Line Radio Galaxies

    NASA Astrophysics Data System (ADS)

    Eracleous, Michael

    1998-05-01

    With the advant of ASCA and its capability for high-resolution X-ray spectroscopy it has become possible to study the X-ray emission lines from AGNs and their very broad profiles. The Fe Kalpha line is particularly important because it is by far the strongest X-ray line observable in AGN spectra. Its profile carries the kinematic signature of the line-emitting gas and as such is constitutes an extremely useful diagnostic tool. XTE complements ASCA in at least the following obvious ways: (a) since the PCA bandpass can extend in practice up to 15-20 keV (up to 40 keV in principle) it is possible to study the signature of Compton reflection from the same dense gas that emits the Fe Kalpha line observed by ASCA, and (b) its large effective area and flexible scheduling policies allow us to monitor the variability of the X-ray spectrum (flux, shape, EW of Fe Kalpha line, and strength of Compton-reflected X-rays). We have tried to take advantage of the strengths of XTE by observing the hard X-ray spectra and variability broad-line radio galaxies. Accordingly, I will review the properties of the broad-line radio galaxies as observed by ASCA in order to motivate the XTE projects that we have undertaken. I will then present the (preliminary) results of our hard X-ray spectroscopy of Pictor A and 3C 111 and our 2-month monitoring of the X-ray variability of 3C 390.3.

  20. The first X-ray diffraction measurements on Mars.

    PubMed

    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

    2014-11-01

    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. Structured illumination for compressive x-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Greenberg, Joel A.; Brady, David J.

    2013-03-01

    Coherent x-ray scatter (also know as x-ray diffraction) has long been used to non-destructively investigate the molecular structure of materials for industrial, medical, security, and fundamental purposes. Unfortunately, molecular tomography based on coherent scatter typically requires long scan times and/or large incident fluxes, which has limited the practical applicability of such schemes. One can overcome the conventional challenges by employing compressive sensing theory to optimize the information obtained per incident photon. We accomplish this in two primary ways: we use a coded aperture to structure the incident illumination and realize massive measurement parallelization and use photon-counting, energy-sensitive detection to recover maximal information from each detected photon. We motivate and discuss here the general imaging principles, investigate different coding and sampling strategies, and provide results from theoretical studies for our structured illumination scheme. We find that this approach promises real-time molecular tomography of bulk objects without a loss in imaging performance.

  2. The first X-ray diffraction measurements on Mars

    PubMed Central

    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

  3. A versatile X-ray diffraction station at LNLS (Brazil).

    PubMed

    Cusatis, C; Kobayashi Franco, M; Kakuno, E; Giles, C; Morelhão, S; Mello, V; Mazzaro, I

    1998-05-01

    Versatility was a major consideration in the project to provide an X-ray diffraction station at LNLS. At least two techniques are possible at the station: powder diffraction and multiple single-crystal diffraction. A two-crystal monochromator based on monolithic elastic translators, developed at LNLS, with sagittal focusing by the second crystal, allows 10 mrad of a >/=2 keV monochromatic beam to be used on the diffractometer. The station is equipped with a fast scintillation detector, imaging plates, a high-energy-resolution pin-diode detector, an ionization chamber and a high-angular-resolution soller slit. The data collection and control hardware and software were also developed at LNLS. The theta-2theta goniometry for powder diffraction on this 1 m-diameter diffractometer is based on commercial rotation tables. The multiple single-crystal goniometry is realized by an independent elastic axis driven by differential micrometers for both high- and low-resolution angular movements. At least four independent axes can be positioned as necessary on the diffractometer table. Powder diffractograms and double-crystal rocking curves collected with the synchrotron beam show the expected quality. PMID:15263555

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

    NASA Astrophysics Data System (ADS)

    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.

  5. Virtual X-Ray and Electron Diffraction Patterns from Atomistic Simulations on Heterogeneous Computing Platforms

    NASA Astrophysics Data System (ADS)

    Coleman, Shawn; Wang, Yang; Cueva-Parra, Luis; Spearot, Douglas

    2014-03-01

    Electron and X-ray diffraction are well-established experimental methods used to explore the atomic scale structure of materials. In this work, a computational algorithm is developed to produce virtual electron and X-ray diffraction patterns directly from atomistic simulations. In this algorithm, the diffraction intensity is computed via the structure factor equation over a 3-dimensional mesh of {hkl} points in reciprocal space. To construct virtual selected area electron diffraction (SAED) patterns, a thin hemispherical slice of the reciprocal lattice map lying near the surface of the Ewald sphere is isolated and viewed parallel to a specified zone axis. X-ray diffraction 2 θ line profiles are created by virtually rotating the Ewald sphere around the origin of reciprocal space, binning intensities by their associated scattering angle. The diffraction code is parallelized using a heterogeneous mix of MPI and OpenMP. The atom positions are distributed via MPI while the reciprocal space mesh is parallelized using either OpenMP threads launched on regular CPU cores or offloaded to MIC hardware. The complexity of heterogeneous MPI/OpenMP parallelization on mixed hardware will be discussed. This work was supported in part by the NSF under grant 0954505. Simulations were performed on resources supported in part by NSF.

  6. X-Ray Diffraction and Imaging Study of Imperfections of Crystallized Lysozyme with Coherent X-Rays

    NASA Technical Reports Server (NTRS)

    Hu, Zheng-Wei; Chu, Y. S.; Lai, B.; Cai, Z.; Thomas, B. R.; Chernov, A. A.

    2003-01-01

    Phase-sensitive x-ray diffraction imaging and high angular-resolution diffraction combined with phase contrast radiographic imaging are employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in symmetric Laue case. The fill width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal is approximately 16.7 arcseconds, and defects, which include point defects, line defects, and microscopic domains, have been clearly observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front, and they have been found to originate mostly at a central growth area and occasionally at outer growth regions. Individual point defects trapped at a crystal nucleus are resolved in the images of high sensitivity to defects. Slow dehydration has led to the broadening of the 4 4 0 rocking curve by a factor of approximately 2.4. A significant change of the defect structure and configuration with drying has been revealed, which suggests the dehydration induced migration and evolution of dislocations and lattice rearrangements to reduce overall strain energy. The sufficient details of the observed defects shed light upon perfection, nucleation and growth, and properties of protein crystals.

  7. High pressure x-ray diffraction study of tungsten disulfide

    SciTech Connect

    Selvi,E.; Ma, Y.; Aksoy, R.; Ertas, A.; White, A.; Sandhu, J.

    2006-01-01

    Synchrotron X-ray diffraction was used in conjunction with a diamond anvil cell to investigate the properties of tungsten disulfide (WS{sub 2}) to 25.5 GPa at room temperature. No pressure medium was used to generate hydrostatic pressure. No phase transformation was observed in the pressure range studied. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus was determined to be K{sub 0T}=61{+-}1 GPa with its pressure derivative K{prime}{sub 0T}=9.0{+-}0.3. It is also found that the c-direction of the hexagonal structure is much more compressible than the a-direction.

  8. X-ray diffraction study of crystalline barium titanate ceramics

    NASA Astrophysics Data System (ADS)

    Zali, Nurazila Mat; Mahmood, Che Seman; Mohamad, Siti Mariam; Foo, Choo Thye; Murshidi, Julie Adrianny

    2014-02-01

    In this study, BaTiO3 ceramics have been prepared via solid-state reaction method. The powders were calcined for 2 hours at different temperatures ranging from 600C to 1200C. Using X-ray diffraction with a Rietveld analysis, the phase formation and crystal structure of the BaTiO3 powders were studied. Change in crystallite size and tetragonality as a function of calcination temperature were also discussed. It has been found that the formation of pure perovskite phase of BaTiO3 began at calcination condition of 1000 C for 2 hours. The crystal structure of BaTiO3 formed is in the tetragonal structure. The second phases of BaCO3 and TiO2 existed with calcination temperature below 1000 C. Purity, crystallite size and tetragonality of BaTiO3 powders were found to increase with increasing calcination temperature.

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

    USGS Publications Warehouse

    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.

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

    SciTech Connect

    Yastrebov, S. G. Ivanov-Omskii, V. I.

    2007-12-15

    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.

  11. A new theory for X-ray diffraction

    SciTech Connect

    Fewster, Paul F.

    2014-05-01

    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.

  12. X-ray Diffraction Spectra in Cu-Implanted SiO{sub 2} Films on Si(100) Substrates

    SciTech Connect

    Shirokoff, J.; Lewis, J. Courtenay

    2010-10-29

    Cu-implanted SiO{sub 2} films on Si(100) have been studied using x-ray methods and x-ray diffraction pattern processing. The x-ray results indicate the presence of a preferred orientation for Cu {l_brace}111{r_brace} planes parallel to the substrate surface without directional orientation for Cu-implanted SiO{sub 2}/Si(100) and nano-crystalline-Cu/SiO{sub 2}/Si(100)(ie. after implanted and annealed Cu). The x-ray diffraction spectra of the Cu-implanted and nano-crystalline-Cu phases were analyzed (ie. in terms of peak search, profile fit, crystallite size) and compared to data from complimentary techniques (RBS, TEM). Results are discussed with respect to x-ray spectral lines shapes derived from XRD spectra processing and the nanostructure problem.

  13. Development of Coherent X-ray Diffraction Apparatus with Kirkpatrick-Baez Mirror Optics

    SciTech Connect

    Takahashi, Y.; Tsutsumi, R.; Mimura, H.; Matsuyama, S.; Nishino, Y.; Ishikawa, T.; Yamauchi, K.

    2011-09-09

    To realize coherent x-ray diffraction microscopy with higher spatial resolution, it is necessary to increase the density of x-ray photons illuminated onto the sample. In this study, we developed a coherent x-ray diffraction apparatus with Kirkpatrick-Baez mirror optics. By using mirrors fabricated by elastic emission machining, a high-density coherent x-ray beam was produced. In a demonstration experiment using a silver nanocube as a sample, a high-contrast coherent x-ray diffraction pattern was observed over a wide-q range. This proves that both the density and the degree of coherence of the focused beam were high.

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

    SciTech Connect

    Ichiyanagi, Kouhei; Sasaki, Yuji C.; Japan Science and Technology Agency, CREST, CREST, Sasaki-Team, 609 Kiban Building, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8561 ; Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Senba, Yasunori; Ohashi, Haruhiko; Ohta, Noboru; Hoshisashi, Kentaro; Jae-won, Chang; Tokue, Maki; Matsushita, Yufuku; Nishijima, Masaki; Inoue, Yoshihisa; Yagi, Naoto; Japan Synchrotron Radiation Research Institute, SPring-8, 1-1-1 Kouto, Sayo, Hyogo 679-5198

    2013-10-15

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

    NASA Astrophysics Data System (ADS)

    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.

  16. Eta Carinae: X-ray Line Variations during the 2003 X-ray Minimum, and the Orbit Orientation

    NASA Technical Reports Server (NTRS)

    Corcoran, M. F.; Henley, D.; Hamaguchi, K.; Khibashi, K.; Pittard, J. M.; Stevens, I. R.; Gull, T. R.

    2007-01-01

    The future evolution of Eta Carinae will be as a supernova (or hypernova) and black hole. The evolution is highly contingent on mass and angular momentum changes and instabilities. The presence of a companion can serve to trigger instabilities and provide pathways for mass and angular momentum exchange loss. X-rays can be used a a key diagnostic tool: x-ray temperatures trace pre-shock wind velocities, periodic x-ray variability traces the orbit, and x-ray line variations traces the flow and orientation of shocked gas. This brief presentation highlights x-ray line variations from the HETG and presents a model of the colliding wind flow.

  17. A new theory for X-ray diffraction

    PubMed Central

    Fewster, Paul F.

    2014-01-01

    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. PMID:24815975

  18. Nondestructive evaluation of fatigue damage in aluminum 2024 by x-ray diffraction

    NASA Technical Reports Server (NTRS)

    Ferguson, Milton W.

    1994-01-01

    Aluminum alloys are widely used in the automobile and aerospace industries. This is due to their attractive low density-high modulus and low density-high strength characteristics. Unfortunately, cyclic stress-strain deformations alter the microstructure of aluminum alloys when they are placed into service. These structural changes can lead to fatigue damage and ultimately service failure. Since x-ray diffraction analysis is known to be a sensitive nondestructive indicator of structural changes due to deformations, this technique is being used to evaluate changes in the microstructure of cycled aluminum 2024 commercial alloys. Line shapes, widths, and positions in an x-ray diffraction pattern depend on microstructural properties such as grain size, grain orientation, residual stress, microstrain, etc. Changes in the microstructure due to fatigue will appear as changes in the diffraction pattern. One parameter used to characterize a reflection in a diffraction pattern is the full width at half maximum (FWHM). Preliminary x-ray diffraction results on cycled Al 2024 indicate that the (111) and (222) reflections of the matrix phase do not show any variations in the FWHM due to an increase in the fatigue cycles. However, the FWHM of the (200) and (400) reflections of the same phase unexpectedly showed a dramatic decrease. These results can be interpreted as due to the relaxation of some initial nonuniform residual stresses in the matrix phase lattice. Further work is in progress to evaluate the FWHM of the second phase of the cycled alloys.

  19. X-ray line emission from the Tycho supernova remnant

    NASA Technical Reports Server (NTRS)

    Pravdo, S. H.; Smith, B. W.; Charles, P. A.; Tuohy, I. R.

    1979-01-01

    The observation of the X-ray spectrum of the Tycho supernova remnant in the energy range 0.5 to 20 keV is discussed. Four significant line features in the spectrum: The K alpha lines of silicon, sulphur, and iron; and the L lines of iron are examined. Comparisons between the silicon and sulphur equivalent widths and K alpha iron line energies of Tycho and Cas A are discussed. Suggest that the X-ray emitting plasma in Tycho is further from collisional ionization equilibrium than that of Cas A.

  20. X-Ray Absorbed, Broad-Lined, Red AGN and the Cosmic X-Ray Background

    NASA Technical Reports Server (NTRS)

    Mushotzky, Richard (Technical Monitor); Wilkes, Belinda

    2005-01-01

    We have obtained XMM spectra for five red, 2MASS AGN, selected from a sample observed by Chandra to be X-ray bright and to cover a range of hardness ratios. Our results confirm the presence of substantial absorbing material in three sources which have optical classifications ranging from Type 1 to Type 2, with an intrinsically flat (hard) power law continuum indicated in the other two. The presence of both X-ray absorption and broad optical emission lines with the usual strength suggests either a small (nuclear) absorber or a favored viewing angle so as to cover the X-ray source but not the broad emission line region (BELR). A soft excess is detected in all three Type 1 sources. We speculate that this soft X-ray emission may arise in an extended region of ionized gas, perhaps linked with the polarized (scattered) light which is a feature of these sources. The spectral complexity revealed by XMM emphasizes the limitations of the low S/N Chandra data. Overall, the new XMM results strengthen our conclusions (Wilkes et al. 2002) that the observed X-ray continua of red AGN are unusually hard at energies greater than 2 keV. Whether due to substantial line-of-sight absorption or to an intrinsically hard or reflection-dominated spectrum, these 'red' AGN have an observed spectral form consistent with contributing significantly to the missing had absorbed population of the Cosmic X-ray Background (CXRB). When absorption and or reflection is taken into account, all these AGN have power law slopes typical of broad-line (Type 1) AGN (Gamma approximately 1.9). This appears to resolve the spectral paradox which for so long has existed between the CXRB and the AGN thought to be the dominant contributors. It also suggests two scenarios whereby Type 1 AGN/QSOs may be responsible for a significant fraction of the CXRB at energies above 2 keV: 1) X-ray absorbed AGN/QSOs with visible broad emission lines; 2) AGN/QSOs with complex spectra whose hardness greater than 2 keV is not detectable in the typically low S/N data of X-ray surveys. Even if absorption is present in only half of the population, the large number of 'red' AGN suggests a development of unification models, where the continuum source is surrounded, over a substantial solid angle, by the wind or atmosphere of an accretion disk/torus. X-ray observations of such AGN not only provide a check on the presence of absorption, but also a unique probe of the absorbing material. Improved information on their space density, in particular as a function of redshift, will soon be provided by Spitzer-Chandra wide area surveys, allowing better estimates of both the importance of red AGN to the full AGN population and their contribution to the CXRB.

  1. Quantitative biological imaging by ptychographic x-ray diffraction microscopy

    PubMed Central

    Giewekemeyer, Klaus; Thibault, Pierre; Kalbfleisch, Sebastian; Beerlink, André; Kewish, Cameron M.; Dierolf, Martin; Pfeiffer, Franz; Salditt, Tim

    2010-01-01

    Recent advances in coherent x-ray diffractive imaging have paved the way to reliable and quantitative imaging of noncompact specimens at the nanometer scale. Introduced a year ago, an advanced implementation of ptychographic coherent diffractive imaging has removed much of the previous limitations regarding sample preparation and illumination conditions. Here, we apply this recent approach toward structure determination at the nanoscale to biological microscopy. We show that the projected electron density of unstained and unsliced freeze-dried cells of the bacterium Deinococcus radiodurans can be derived from the reconstructed phase in a straightforward and reproducible way, with quantified and small errors. Thus, the approach may contribute in the future to the understanding of the highly disputed nucleoid structure of bacterial cells. In the present study, the estimated resolution for the cells was 85 nm (half-period length), whereas 50-nm resolution was demonstrated for lithographic test structures. With respect to the diameter of the pinhole used to illuminate the samples, a superresolution of about 15 was achieved for the cells and 30 for the test structures, respectively. These values should be assessed in view of the low dose applied on the order of ≃1.3·105 Gy, and were shown to scale with photon fluence. PMID:20018650

  2. Very High Resolution Solar X-ray Imaging Using Diffractive Optics

    NASA Technical Reports Server (NTRS)

    Dennis, B. R.; Skinner, G. K.; Li, M. J.; Shih, A. Y.

    2012-01-01

    This paper describes the development of X-ray diffractive optics for imaging solar flares with better than 0.1 arcsec angular resolution. X-ray images with this resolution of the greater than or equal to 10 MK plasma in solar active regions and solar flares would allow the cross-sectional area of magnetic loops to be resolved and the coronal flare energy release region itself to be probed. The objective of this work is to obtain X-ray images in the iron-line complex at 6.7 keV observed during solar flares with an angular resolution as fine as 0.1 arcsec - over an order of magnitude finer than is now possible. This line emission is from highly ionized iron atoms, primarily Fe xxv, in the hottest flare plasma at temperatures in excess of approximately equal to 10 MK. It provides information on the flare morphology, the iron abundance, and the distribution of the hot plasma. Studying how this plasma is heated to such high temperatures in such short times during solar flares is of critical importance in understanding these powerful transient events, one of the major objectives of solar physics.We describe the design, fabrication, and testing of phase zone plate X-ray lenses with focal lengths of approximately equal to 100 m at these energies that would be capable of achieving these objectives. We show how such lenses could be included on a two-spacecraft formation-flying mission with the lenses on the spacecraft closest to the Sun and an X-ray imaging array on the second spacecraft in the focal plane approximately equal to 100 m away. High resolution X-ray images could be obtained when the two spacecraft are aligned with the region of interest on the Sun. Requirements and constraints for the control of the two spacecraft are discussed together with the overall feasibility of such a formation-flying mission.

  3. X-ray diffraction studies using diamond coated rhenium gasket to megabar pressures

    SciTech Connect

    Akella, J; Catledge, S A; Chesnut, G N; Prokop, H; Vohra, Y K; Weir, S T

    1999-09-30

    X-ray diffraction studies at megabar pressures are limited by the sample thickness between the diamond anvils. High strength gaskets are desirable to improve the quality of x-ray diffraction data. We present a technique which employs a microwave plasma chemical vapor deposited diamond layer on one side of a rhenium gasket. As a test case, we show energy dispersive x-ray diffraction data on rare earth metal neodymium to 153 GPa using a synchrotron source. The increased sample thickness results in an unambiguous crystal structure determination of a monoclinic phase in neodymium above 75 GPa. [chemical vapor deposition, diamond, rhenium gasket, x-ray diffraction, neodymium

  4. X-ray Diffraction Study of Molybdenum to 900 GPa

    NASA Astrophysics Data System (ADS)

    Wang, J.; Coppari, F.; Smith, R.; Eggert, J.; Boehly, T.; Collins, G. W.; Duffy, T. S.

    2013-12-01

    Molybdenum (Mo) is a transition metal that is important as a high-pressure standard. Its equation of state, structure, and melting behavior have been explored extensively in both experimental and theoretical studies. Melting data up to the Mbar pressure region from static compression experiments in the diamond anvil cell [Errandonea et al. 2004] are inconsistent with shock wave sound velocity measurements [Hixson et al., 1989]. There are also conflicting reports as to whether body-centered cubic (BCC) Mo transforms to a face-centered cubic (FCC), hexagonal close packed (HCP) or double hexagonal close packed (DHCP) structure at either high pressure or high pressure and temperature conditions [Belonoshko et al. 2008, Mikhaylushkin et al., 2008 and Cazorla et al., 2008]. Recently, a phase transition from BCC to the DHCP phase at 660 GPa and 0 K was predicted using the particle swam optimization (PSO) method (Wang et al, 2013). Here we report an x-ray diffraction study of dynamically compressed molybdenum. Experiments were conducted using the Omega laser at the Laboratory for Laser Energetics at the University of Rochester. Mo targets were either ramp or shock compressed using a laser drive. In ramp loading, the sample is compressed sufficiently slowly that a shock wave does not form. This results in lower temperatures, keeping the sample in the solid state to higher pressures. X-ray diffraction measurements were performed using quasi-monochromatic x-rays from a highly ionized He-α Cu source and image plate detectors. Upon ramp compression, we found no evidence of phase transition in solid Mo up to 900 GPa. The observed peaks can be assigned to the (110) and (200) or (220) reflections of BCC Mo up to the highest pressure, indicating that Mo does not melt under ramp loading to maximum pressure reached. Under shock loading, we did not observe any evidence for the solid-solid phase transformation around 210 GPa as reported in previous work (Hixson et al, 1989). The BCC phase of Mo remained stable along the Hugoniot up to at least 350 GPa. Our observation of diffraction peaks from shocked Mo shows that Hugoniot does not cross the melting curve until at least this pressure. This indicates that previous diamond cell experiments (Errandonea et al., 2004) have underestimated the Mo melting curve. We acknowledge the Omega staff at LLE for their assistance, and the Target Engineering Team at LLNL for fabrication of the targets used in these experiments. The research was supported by NNSA/DOE through the National Laser Users' Facility Program under contracts DE-NA0000856 and DE-FG52-09NA29037. References: [1] R.S. Hixson, D.A. Boness, and J.W. Shaner, Phys. Rev. Lett., 62, 637 (1989). [2] D. Errandonea, B. Schwager, R. Ditz, C. Gessmann, R. Boehler, and M. Ross, Phys. Rev. B, 63, 132104 (2004). [3] A.B. Belonoshko, L. Burakovsky, S.P. Chen, B. Johansson, A.S. Mikhaylushkin, D.L. Preston, S.I. Simak, and D.C. Swift, Phys. Rev. Lett., 100, 135701 (2008). [4] C. Cazorla, D. Alfè, and M.J. Gillan, Phys. Rev. Lett. 101, 049601 (2008). [5] A.S. Mikhaylushkin, S.I. Simak ,L. Burakovsky, S.P. Chen, B. Johansson, D.L. Preston, D.C. Swift, and A.B. Belonoshko Phys. Rev. Lett., 101, 049602 (2008). [6] B. Wang, G. Zhang, and Y. Wang, J. Alloys Compd., 556, 116-120, (2013).

  5. Measuring the X-ray Resolving Power of Bent Potassium Acid Phthalate Diffraction Crystals

    SciTech Connect

    Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

    2014-11-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories (SNL) in Albuquerque, NM. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a dual goniometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  6. Real-time Studies of Shocked Polycrystalline Materials with Single-Pulse X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Morgan, Dane

    2011-06-01

    Recent advances in pulsed x-ray diffraction (XRD) diagnostic techniques have enabled real-time XRD studies of atomic-scale mechanisms within shocked polycrystalline materials. The direct correlation between solid-state structures and their associated XRD patterns enables direct observation of a material's bulk properties, including phase, grain-size distribution, texture, and micro-strain, during the very short time interval of shock-induced pressure loading. For shock-compressed polycrystalline solids, real time single-pulse XRD probes a macroscopic sample volume, and the measured diffraction pattern is the sum of the responses from the microscopic coherently diffracting domains. These experiments have utilized a Marx-generated, cable-coupled, needle-and-washer diode that emits a 40 ns pulse of line-and-bremsstahlung x-rays. The x-rays are collimated by a circular pinhole, and detected by an image plate or CCD camera coupled to a phosphor. The line emission is selectable to either 0.71 A or 0.56 A, and the hard bremsstahlung direct beam provides a zero-order reference mark in the image. Results from studies of shock-loaded materials including aluminum, tin, and zirconium are shown. Planned experiments and future diagnostic development are discussed.

  7. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystalsa)

    NASA Astrophysics Data System (ADS)

    Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

    2014-11-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  8. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

    SciTech Connect

    Haugh, M. J. Jacoby, K. D.; Wu, M.; Loisel, G. P.

    2014-11-15

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  9. X-ray diffraction study of crystalline barium titanate ceramics

    SciTech Connect

    Zali, Nurazila Mat; Mahmood, Che Seman; Mohamad, Siti Mariam; Foo, Choo Thye; Murshidi, Julie Adrianny

    2014-02-12

    In this study, BaTiO{sub 3} ceramics have been prepared via solid-state reaction method. The powders were calcined for 2 hours at different temperatures ranging from 600°C to 1200°C. Using X-ray diffraction with a Rietveld analysis, the phase formation and crystal structure of the BaTiO{sub 3} powders were studied. Change in crystallite size and tetragonality as a function of calcination temperature were also discussed. It has been found that the formation of pure perovskite phase of BaTiO{sub 3} began at calcination condition of 1000 °C for 2 hours. The crystal structure of BaTiO{sub 3} formed is in the tetragonal structure. The second phases of BaCO{sub 3} and TiO{sub 2} existed with calcination temperature below 1000 °C. Purity, crystallite size and tetragonality of BaTiO{sub 3} powders were found to increase with increasing calcination temperature.

  10. Characterizing Multiferroics: Analyses through X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Wolfe, Evan; Hart, Harley; Blackshire, Sheldon; Polisetty, Srinivas; Chen, Disheng; Zhou, Jinling; Frye, Charles; Holcomb, Mikel

    2011-03-01

    Theory and experiments support that magnetoelectric coupling (electrical control of magnetism and vice versa) can be enhanced by taking advantage of interfacial coupling between magnetic and ferroelectric films. The interface between ferroelectric PZT and ferromagnetic LSMO is a promising candidate for storage and magnetic sensing devices. For example, LSMO, when exposed to a magnetic field, will contract; while PZT when strained will produce a voltage. Combining properties, the PZT/LSMO composite can be utilized to detect magnetic fields, and also be used as an energy scavenging device. In order to maximize the coupling across this interface, proper measurements and characterizations must be taken to detail how the materials interact on the atomic level. X-ray diffraction allows us to determine thickness, composite, and strain of the samples used. By analyzing the peak shift in XRD scans along our samples we can detail the amount of strain placed on the sample, aiding in discovering of the mechanisms responsible for interfacial magnetoelectric coupling. Through analysis, we can ensure the quality of the interface, thus allowing further advances for increases in magnetic sensitivity and higher voltage output.

  11. Dynamical Diffraction Simulation of Transmission X-ray Phase Retarders

    NASA Astrophysics Data System (ADS)

    Macrander, A. T.; Lang, J. C.; Srajer, G.

    1996-03-01

    Circularly polarized photons couple with magnetic moments which makes them a useful probe of the magnetic properties of condensed matter. Circularly polarized photon beams can be created from linearly polarized undulator beams at the Advanced Photon Source using thin single-crystal transmission phase retarders. Tests of such phase retarders have been made and have been compared to dynamical diffraction calculations. (J.C. Lang and G. Srajer, Rev. Sci. Instrumen. 66,1540(1995).) In addition, a phase retarder was successfully used in a circular magnetic x-ray dichroism experiment. (J.C. Lang, G. Srajer, C. Detliefs, A.I. Goldman, H. Konig, X. Wang, B.N. Harmon, and R.W. McCallum, Phys. Rev. Lett. 74,4935(1995).) The focus of this talk is on the calculations that were made using matrix techniques. ( D.W. Berreman and A.T. Macrander, Phys. Rev. B 37,6030(1988).) Such calculations are possible because not only the amplitude but also the phase of the fields are calculated. This work supported by the U.S. Dept. of Energy, BES-Materials Sciences, under contract no. W-31-109-ENG-38.

  12. Federated repositories of X-ray diffraction images.

    PubMed

    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

  13. TYPING SUPERNOVA REMNANTS USING X-RAY LINE EMISSION MORPHOLOGIES

    SciTech Connect

    Lopez, L. A.; Ramirez-Ruiz, E.; Badenes, C.; Huppenkothen, D.; Jeltema, T. E.

    2009-11-20

    We present a new observational method to type the explosions of young supernova remnants (SNRs). By measuring the morphology of the Chandra X-ray line emission in 17 Galactic and Large Magellanic Cloud SNRs with a multipole expansion analysis (using power ratios), we find that the core-collapse SNRs are statistically more asymmetric than the Type Ia SNRs. We show that the two classes of supernovae can be separated naturally using this technique because X-ray line morphologies reflect the distinct explosion mechanisms and structure of the circumstellar material. These findings are consistent with recent spectropolarimetry results showing that core-collapse supernovae explosions are intrinsically more asymmetric.

  14. High intensity line source for x-ray spectrometer calibration

    SciTech Connect

    Thoe, R.S.

    1986-06-01

    A high intensity electron-impact x-ray source using a one-dimensional Pierce lens has been built for the purpose of calibrating a bent crystal x-ray spectrometer. This source focuses up to 100 mA of 20-keV electrons to a line on a liquid-cooled anode. The line (which can serve as a virtual slit for the spectrometer) measures approximately 800 ..mu.. x 2 cm. The source is portable and therefore adaptable to numerous types of spectrometer applications. One particular application, the calibration of a high resolution (r = 10/sup 4/) time-resolved cyrstal spectrometer, will be discussed in detail.

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

    SciTech Connect

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

    2009-11-06

    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 deg. 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 demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

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

    PubMed Central

    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

    2010-01-01

    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 demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics. PMID:20365955

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

    DOE PAGESBeta

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; Lima, Enju; Marchesini, Stefano; Miao, Huijie; Neiman, Aaron M.; Shapiro, David; Steinbrener, Jan; Stewart, Andrew; et al

    2009-11-01

    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 demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

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

    NASA Astrophysics Data System (ADS)

    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

    2009-11-01

    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 demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

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

    SciTech Connect

    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

    2009-11-01

    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 demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

  20. Taking X-ray Diffraction to the Limit: Macromolecular Structures from Femtosecond X-ray Pulses and Diffraction Microscopy of Cells with Synchrotron Radiation

    SciTech Connect

    Chapman, H N; Miao, J; Kirz, J; Sayre, D; Hodgson, K O

    2003-10-01

    The methodology of X-ray crystallography has recently been successfully extended to the structure determination of non-crystalline specimens. The phase problem was solved by using the oversampling method, which takes advantage of ''continuous'' diffraction pattern from non-crystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging non-periodic objects, like cells and cellular structures using coherent and bright X-rays from the 3rd generation synchrotron radiation. In the longer run, the technique may be applied to image single biomolecules by using the anticipated X-ray free electron lasers. Computer simulations have so far demonstrated two important steps: (1) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself, and (2) the phase information can be ab initio retrieved from a set of calculated noisy diffraction patterns of single protein molecules.

  1. Quantitative description of microstructure defects in hexagonal boron nitrides using X-ray diffraction analysis

    SciTech Connect

    Schimpf, C. Motylenko, M.; Rafaja, D.

    2013-12-15

    A routine for simultaneous quantification of turbostratic disorder, amount of puckering and the dislocation and stacking fault density in hexagonal materials was proposed and tested on boron nitride powder samples that were synthesised using different methods. The routine allows the individual microstructure defects to be recognised according to their effect on the anisotropy of the X-ray diffraction line broadening. For quantification of the microstructure defects, the total line broadening is regarded as a linear combination of the contributions from the particular defects. The total line broadening is obtained from the line profile fitting. As testing material, graphitic boron nitride (h-BN) was employed in the form of hot-isostatically pressed h-BN, pyrolytic h-BN or a h-BN, which was chemically vapour deposited at a low temperature. The kind of the dominant microstructure defects determined from the broadening of the X-ray diffraction lines was verified by high resolution transmission electron microscopy. Their amount was attempted to be verified by alternative methods. - Highlights: • Reliable method for quantification of microstructure defects in BN was suggested. • The method is based on the analysis of anisotropic XRD line broadening. • This XRD line broadening is unique and characteristic of the respective defect. • Thus, the quantification of coexistent microstructure defects is possible. • The method was tested on hexagonal BN, which was produced by different techniques.

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

    SciTech Connect

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

    2013-06-15

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

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

    ERIC Educational Resources Information Center

    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

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

    ERIC Educational Resources Information Center

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

    ERIC Educational Resources Information Center

    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)

  6. IDENTIFICATION OF COMPOUNDS IN PARTICULATE POLLUTION BY X-RAY DIFFRACTION

    EPA Science Inventory

    X-ray diffraction is a valuable tool for the identification of crystalline compounds in a multicomponent sample. Two x-ray diffraction techniques (Seeman-Bohlin and Bragg-Brentano) were examined for the identification of small amounts of material deposited on low-mass substrates....

  7. Strain measurement of pure titanium covered with soft tissue using X-ray diffraction.

    PubMed

    Fujisaki, Kazuhiro; Tadano, Shigeru

    2010-03-01

    Measurement of the stress and strain applied to implants and bone tissue in the human body are important for fracture prediction and evaluations of implant adaptation. The strain of titanium (Ti) materials can be measuring by X-ray diffraction techniques. This study applied X-ray diffraction to the skin tissue-covered Ti. Characteristic X-rays of Mo Kalpha were used and the X-rays diffracted from the Ti were detected through the covering skin tissue. The X-ray absorption by skin tissue is large under the diffracted X-rays detected in low angles because the length of penetration depends on the angle of inclination, equal to the Bragg angle. The effects of skin tissue to detect the diffracted X-rays were investigated in the experiments. And the strain measurements were conducted under bending loads applied to the Ti specimen. The effect of skin tissue was absorption of X-rays as well as the X-rays scattered from the physiological saline contained in the tissue. The X-rays scattered by the physiological saline creates a specific background pattern near the peaks from the (002) and (011) lattice planes of Ti in the X-ray diffraction profile. Diffracted X-rays from the Ti were detected after being transmitted through 1 mm thick skin tissue by Mo Kalpha. Individual peaks such as (010), (002), (011), and (110) were clearly established by using a parallel beam arrangement. The strains of (110) lattice planes were measured with or without the tissue cover were very similar. The strain of the (110) lattice planes of Ti could be measured by Mo Kalpha when the Ti specimen was located under the skin tissue. PMID:20459192

  8. Diffraction grating transmission efficiencies for XUV and soft X rays. [for HEAO-B extrasolar astronomy

    NASA Technical Reports Server (NTRS)

    Schnopper, H. W.; Van Speybroeck, L. P.; Delvaille, J. P.; Epstein, A.; Kaellne, E.; Bachrach, R. Z.; Dijkstra, J.; Lantward, L.

    1977-01-01

    The manufacture and properties of a grating intended for extrasolar X-ray studies are described. The manufacturing process uses a split laser beam exposing an interference pattern on the photoresist-coated glass plated with a nickel parting layer. The grating, supporting structure, and mounting frame are electrodeposited on the nickel parting layer, and the final product is lifted from the glass substrate by selective etching of the nickel. A model was derived which relates the number of counts received in a given order m as a function of photon wavenumber. A 4-deg beam line was used to measure the efficiencies of gold transmission gratings for diffraction of X-rays in the range of 45 to 275 eV. The experimental results are in good agreement with model calculations.

  9. Diffraction and imaging study of imperfections of crystallized lysozyme with coherent X-rays

    NASA Technical Reports Server (NTRS)

    Hu, Z. W.; Chu, Y. S.; Lai, B.; Thomas, B. R.; Chernov, A. A.

    2004-01-01

    Phase-contrast X-ray diffraction imaging and high-angular-resolution diffraction combined with phase-contrast radiographic imaging were employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in the symmetric Laue case. The full-width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal was approximately 16.7 arcsec and imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <1 1 0> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Inclusions of impurities or formations of foreign particles in the central growth region are resolved in the images with high sensitivity to defects. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in X-ray diffraction images. The details of the observed defects and the significant change in the revealed microstructures with drying provide insight into the nature of imperfections, nucleation and growth, and the properties of protein crystals.

  10. In Situ High-Pressure X-ray Diffraction Study of H2O Ice VII

    SciTech Connect

    Somayazulu,M.; Shu, J.; Zha, C.; Goncharov, A.; Tschauner, O.; Mao, H.; Hemley, R.

    2008-01-01

    Ice VII was examined over the entire range of its pressure stability by a suite of x-ray diffraction techniques in order to understand a number of unexplained characteristics of its high-pressure behavior. Axial and radial polycrystalline (diamond anvil cell) x-ray diffraction measurements reveal a splitting of diffraction lines accompanied by changes in sample texture and elastic anisotropy. In situ laser heating of polycrystalline samples resulted in the sharpening of diffraction peaks due to release of nonhydrostatic stresses but did not remove the splitting. Radial diffraction measurements indicate changes in strength of the material at this pressure. Taken together, these observations provide evidence for a transition in ice VII near 14 GPa involving changes in the character of the proton order/disorder. The results are consistent with previous reports of changes in phase boundaries and equation of state at this pressure. The transition can be interpreted as ferroelastic with the appearance of spontaneous strain that vanishes at the hydrogen bond symmetrization transition near 60 GPa.

  11. X-ray Emission Line Spectroscopy of Nearby Galaxies

    NASA Astrophysics Data System (ADS)

    Wang, Daniel

    What are the origins of the diffuse soft X-ray emission from non-AGN galaxies? Preliminary analysis of XMM-Newton RGS spectra shows that a substantial fraction of the emission cannot arise from optically-thin thermal plasma, as commonly assumed, and may originate in charge exchange at the interface with neutral gas. We request the support for a comprehensive observing, data analysis, and modeling program to spectroscopically determine the origins of the emission. First, we will use our scheduled XMM-Newton AO-10 368 ks observations of the nearest compact elliptical galaxy M32 to obtain the first spectroscopic calibration of the cumulative soft X-ray emission from the old stellar population and will develop a spectral model for the charge exchange, as well as analysis tools to measure the spatial and kinematic properties of the X-ray line- emitting plasma. Second, we will characterize the truly diffuse emission from the hot plasma and/or its interplay with the neutral gas in a sample of galactic spheroids and active star forming/starburst regions in nearby galaxies observed by XMM-Newton. In particular, we will map out the spatial distributions of key emission lines and measure (or tightly constrain) the kinematics of hot plasma outflows for a few X-ray-emitting regions with high-quality RGS data. For galaxies with insufficient counting statistics in individual emission lines, we will conduct a spectral stacking analysis to constrain the average properties of the X-ray-emitting plasma. We will use the results of these X-ray spectroscopic analyses, together with complementary X-ray CCD imaging/spectral data and observations in other wavelength bands, to test the models of the emission. In addition to the charge exchange, alternative scenarios such as resonance scattering and relic AGN photo-ionization will also be examined for suitable regions. These studies are important to the understanding of the relationship between the diffuse soft X-ray emission and various high-energy feedback processes of the galaxies.

  12. Capability of X-ray diffraction for the study of microstructure of metastable thin films

    PubMed Central

    Rafaja, David; Wüstefeld, Christina; Dopita, Milan; Motylenko, Mykhaylo; Baehtz, Carsten

    2014-01-01

    Metastable phases are often used to design materials with outstanding properties, which cannot be achieved with thermodynamically stable compounds. In many cases, the metastable phases are employed as precursors for controlled formation of nanocomposites. This contribution shows how the microstructure of crystalline metastable phases and the formation of nanocomposites can be concluded from X-ray diffraction experiments by taking advantage of the high sensitivity of X-ray diffraction to macroscopic and microscopic lattice deformations and to the dependence of the lattice deformations on the crystallographic direction. The lattice deformations were determined from the positions and from the widths of the diffraction lines, the dependence of the lattice deformations on the crystallographic direction from the anisotropy of the line shift and the line broadening. As an example of the metastable system, the supersaturated solid solution of titanium nitride and aluminium nitride was investigated, which was prepared in the form of thin films by using cathodic arc evaporation of titanium and aluminium in a nitrogen atmosphere. The microstructure of the (Ti,Al)N samples under study was tailored by modifying the [Al]/[Ti] ratio in the thin films and the surface mobility of the deposited species. PMID:25485125

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

    PubMed

    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

  14. Coherent X-Ray Diffraction Imaging of Chloroplasts from Cyanidioschyzon merolae by Using X-Ray Free Electron Laser.

    PubMed

    Takayama, Yuki; Inui, Yayoi; Sekiguchi, Yuki; Kobayashi, Amane; Oroguchi, Tomotaka; Yamamoto, Masaki; Matsunaga, Sachihiro; Nakasako, Masayoshi

    2015-07-01

    Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles. PMID:25745031

  15. A method for implementing the diffraction of a widely divergent X-ray beam

    SciTech Connect

    Avetyan, K. T.; Arakelyan, M. M.

    2008-11-15

    A method for implementing the diffraction of a widely divergent characteristic X-ray beam from a standard X-ray tube with a linear focal spot was improved. X rays, passing through a diaphragm 30 {mu}m in diameter, diffract from a crystal adjacent to the diaphragm. The crystal, together with a photographic plate, rotates around the axis perpendicular to the plate. It is shown that the diffraction image is a set of hyperbolas in this case. The equations of the hyperbolas are obtained and investigated. A method for interpreting the diffraction images in the case of small crystal asymmetry is proposed.

  16. Real-time X-ray Diffraction Measurements of Shocked Polycrystalline Tin and Aluminum

    SciTech Connect

    Dane V. Morgan, Don Macy, Gerald Stevens

    2008-11-22

    A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35-ns pulse. The characteristic Kα lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic Kβ line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3-mm by 6-mm spot and 1° full-width-half-maximum (FWHM) angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5°. A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device (CCD) camera through a coherent fiberoptic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1-mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic (fcc) aluminum lattice with no phase transformation.

  17. X-ray diffraction and Raman scattering studies of proton-induced, modified polyethylene terephthalate microfiber

    NASA Astrophysics Data System (ADS)

    Mallick, B.; Behera, R. C.; Tiwari, T. N.; Panigrahi, S.; Samal, S. K.

    Polyethylene terephthalate (PET) microfiber of 1.5 denier per filament (dpf) has been irradiated with 3-MeV proton at two different fluences: 1 × 1013 and 1 × 1015p/cm2. Molecular deformation because of in-air proton irradiation straining of PET filaments has been investigated. Study of the effects of irradiation by using X-ray diffraction (XRD), Raman spectroscopy and Instron technique shows microstress and crosslinks on the surface of fiber (as revealed from XRD line shift and Raman shift). However, the Young's modulus is found to be larger at an irradiation dose of 1 × 1013p/cm2.

  18. Structural Depth Profiling by Glancing Angle X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    York, B. R.; Austin, A. B.

    1986-08-01

    Presented here is a technique to structurally depth profile multilayer films using a Seemann-Bohlin triple axis x-ray diffractometer and a 12 kW rotation anode x-ray source. This paper discusses the Seemann-Bohlin geometry and aberrations related to depth profiling and refraction. The technique was successfully applied to multilayer metallic-thin films a few hundred angstroms thick and demonstrated to have an excellent sensitivity to ultra thin-metallic films less than 25 angstroms thick.

  19. Coherent X-ray diffraction imaging of zinc oxide crystals

    NASA Astrophysics Data System (ADS)

    Leake, S. J.

    Zinc Oxide (ZnO) exhibits a plethora of physical properties potentially advantageous in many roles and is why it one of the most studied semiconductor compounds. When doped or in its intrinsic state ZnO demonstrates a multitude of electronic, optical and magnetic properties in a large variety of manufacturable morphologies. Thus it is inherently important to understand why these properties arise and the impact potentially invasive sample preparation methods have for both the function and durability of the material and its devices. Coherent X-ray Diffraction Imaging (CXDI) is a recently established non-destructive technique which can probe the whole three dimensional structure of small crystalline materials and has the potential for sub angstrom strain resolution. The iterative methods employed to overcome the `phase problem' are described fully. CXDI studies of wurtzite ZnO crystals in the rod morphology with high aspect ratio are presented. ZnO rods synthesised via Chemical Vapour Transport Deposition were studied in post growth state and during in-situ modification via metal evaporation processing and annealing. Small variations in post growth state were observed, the physical origin of which remains unidentified. The doping of a ZnO crystal with Iron, Nickel and Cobalt by thermal evaporation and subsequent annealing was studied. The evolution of diffusing ions into the crystal lattice from was not observed, decomposition was found to be the dominant process. Improvements in experimental technique allowed multiple Bragg reflections from a single ZnO crystal to be measured for the first time. Large aspect ratio ZnO rods were used to probe the coherence properties of the incident beam. The longitudinal coherence function of the illuminating radiation was mapped using the visibility of the interference pattern at each bragg reflection and an accurate estimate of the longitudinal coherence length obtained, xi(L) = 0.66pm 0.02 mu m. The consequences for data analysis are discussed. The combination of multiple Bragg reflections to realise three dimensional displacement fields was also approached.

  20. Observing soft X-ray line emission from the interstellar medium with X-ray calorimeter on a sounding rocket

    NASA Technical Reports Server (NTRS)

    Zhang, J.; Edwards, B.; Juda, M.; Mccammon, D.; Skinner, M.; Kelley, R.; Moseley, H.; Schoelkopf, R.; Szymkowiak, A.

    1990-01-01

    For an X-ray calorimeter working at 0.1 K, the energy resolution ideally can be as good as one eV for a practical detector. A detector with a resolution of 17 eV FWHM at 6 keV has been constructed. It is expected that this can be improved by a factor of two or more. With X-ray calorimeters flown on a sounding rocket, it should be possible to observe soft X-ray line emission from the interstellar medium over the energy range 0.07 to 1 keV. Here, a preliminary design for an X-ray calorimeter rocket experiment and the spectrum which might be observed from an equilibrium plasma are presented. For later X-ray calorimeter sounding rocket experiments, it is planned to add an aluminum foil mirror with collecting area of about 400 sq cm to observe line features from bright supernova remnants.

  1. K alpha line emission during solar X-ray bursts

    NASA Technical Reports Server (NTRS)

    Phillips, K. J. H.; Neupert, W. M.

    1973-01-01

    The expected flux of K alpha line emission from sulfur, argon, calcium, and iron is calculated during both thermal and nonthermal solar X-ray events. Such emission is shown to be weak during the course of most of the nonthermal hard X-ray bursts that Kane and Anderson (1970) have observed. If Compton backscattering is significant at high energies, the flux is reduced still further for disk flares, but it is noted that the strong, near-limb burst of June 26 would have produced about 100 photons /sq cm/sec of sulfur and iron K alpha emission. The impulsive hard X-ray bursts may in general be too short-lived for much K alpha emission. It may be noted that sulfur K alpha emission in particular depends sensitively on the lower-energy limit of the nonthermal electron spectrum, assuming such a sharply defined boundary exists. During soft X-ray bursts, when temperatures of a few 10 to the 7th power K are obtained, K alpha emission from certain iron ions, specifically Fe XVIII-XXIII, may be important.

  2. X-ray Diffraction Crystal Calibration and Characterization

    SciTech Connect

    Michael J. Haugh; Richard Stewart; Nathan Kugland

    2009-06-05

    National Security Technologies’ X-ray Laboratory is comprised of a multi-anode Manson type source and a Henke type source that incorporates a dual goniometer and XYZ translation stage. The first goniometer is used to isolate a particular spectral band. The Manson operates up to 10 kV and the Henke up to 20 kV. The Henke rotation stages and translation stages are automated. Procedures have been developed to characterize and calibrate various NIF diagnostics and their components. The diagnostics include X-ray cameras, gated imagers, streak cameras, and other X-ray imaging systems. Components that have been analyzed include filters, filter arrays, grazing incidence mirrors, and various crystals, both flat and curved. Recent efforts on the Henke system are aimed at characterizing and calibrating imaging crystals and curved crystals used as the major component of an X-ray spectrometer. The presentation will concentrate on these results. The work has been done at energies ranging from 3 keV to 16 keV. The major goal was to evaluate the performance quality of the crystal for its intended application. For the imaging crystals we measured the laser beam reflection offset from the X-ray beam and the reflectivity curves. For the curved spectrometer crystal, which was a natural crystal, resolving power was critical. It was first necessary to find sources of crystals that had sufficiently narrow reflectivity curves. It was then necessary to determine which crystals retained their resolving power after being thinned and glued to a curved substrate.

  3. High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

    NASA Technical Reports Server (NTRS)

    Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

    2000-01-01

    We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

  4. Anti-contamination device for cryogenic soft X-ray diffraction microscopy

    DOE PAGESBeta

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

    2011-05-01

    Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

  5. X-Ray Diffraction Studies on Material Corrosions in Renewable Energy Storage Electrolyzers

    NASA Astrophysics Data System (ADS)

    Mo, J.; Steen, S. M., Iii; Zhang, F.-Y.

    2014-11-01

    As a core component of the proton exchange water electrolyzer system, membrane electrode assemblies degrade due to the corrosion of the material. This creates a loss of interfacial contact necessary for the electron transports and electrochemical reactions, thus decreasing the performance. X-ray diffraction has been demonstrated to be an effective method that readily provides quantitative information about the phase-composition of solid materials. In this study, a group of materials have been selected and tested in the standard conditions for investigating the corrosion mechanisms with X-ray diffraction. The material lattice parameter and the crystal size were examined by X-ray diffraction spectrum.

  6. Grain orientation mapping of passivated aluminum interconnect wires with X-ray micro-diffraction

    SciTech Connect

    MacDowell, A.A.; Padmore, H.A.; Thompson, A.C.; Chang, C.H.; Patel, J.R. |

    1998-06-01

    A micro x-ray diffraction facility is under development at the Advanced Light source. Spot sizes are typically about 1-{micro}m size generated by means of grazing incidence Kirkpatrick-Baez focusing mirrors. Photon energy is either white of energy range 6--14 keV or monochromatic generated from a pair of channel cut crystals. A Laue diffraction pattern from a single grain in passivated 2-{micro}m wide bamboo structured Aluminum interconnect line has been recorded. Acquisition times are of the order of a few seconds. The Laue pattern has allowed the determination of the crystallographic orientation of individual grains along the line length. The experimental and analysis procedures used are described, as is a grain orientation result. The future direction of this program is discussed in the context of strain measurements in the area of electromigration.

  7. X-RAY DIFFRACTION PHASE ANALYSIS OF PROCESS AND POLLUTION CONTROL DEVICE SAMPLES

    EPA Science Inventory

    The paper describes the application of x-ray diffraction (XRD) analysis to several samples which show the information available from the technique. X-ray fluorescence (XRF) spectrometry was used for the elemental analysis because it provides very complete information with minimal...

  8. Temperature-controlled vacuum chamber for x-ray diffraction studies

    NASA Astrophysics Data System (ADS)

    Mudd, Courtney P.; Tipton, Harold; Parsegian, Adrian V.; Rau, Don

    1987-11-01

    In order to apply the osmotic stress method for direct measurement of forces between membranes or between macromolecules, we have designed and built an x-ray camera which can control the sample temperature from 0 C to 70 C while confining the path of diffracted x rays to an evacuated space between the sample and film. The system uses a linear feedback sensor which provides 0.1 C accuracy and a base-line stability of 0.02 C over the entire operating range. The controller uses solid-state thermoelectric modules to regulate the temperature of the sample and is capable of automatically shifting from the heating to cooling mode of operation to regulate at temperatures near room temperature. The sample solutions are mounted between two Mylar windows in a removable cell which can be cleaned and loaded outside the instrument. The film plate is mounted on a slide which can be positioned between 4 and 22 in. from the sample. A beam stop is also mounted on the film plate holder and can be adjusted 1 in. both vertically and laterally. The x-ray entry port also has lateral and vertical adjustments for easy alignment with the collimator. The sample cell and film plate mechanism are located within an aluminum and polycarbonate chamber for operation at pressures as low as 0.001 atm.

  9. Compressive single-pixel snapshot x-ray diffraction imaging.

    PubMed

    Greenberg, Joel; Krishnamurthy, Kalyani; Brady, David

    2014-01-01

    We present a method for realizing snapshot, depth-resolved material identification using only a single, energy-sensitive pixel. To achieve this result, we employ a coded aperture with subpixel features to modulate the energy spectrum of coherently scattered photons and recover the object properties using an iterative inversion algorithm based on compressed sensing theory. We demonstrate high-fidelity object estimation at x-ray wavelengths for a variety of compression ratios exceeding unity. PMID:24365835

  10. Relative intensity of the K ?5 X-ray line

    NASA Astrophysics Data System (ADS)

    Trk, I.; Papp, T.; Plinks, J.; Budnar, M.; Mhleisen, A.; Kawai, J.; Campbell, J. L.

    1996-06-01

    The relative intensity of the K ?5 (K-M IV,V) X-ray line as a function of the atomic number of the emitting elements is very strongly enhanced around Z = 24 (chromium) relative to predictions of the single-particle model for this electric dipole (E1) forbidden transition. The enhancement is attributed to solid state or chemical effects. The K ?5 transition can be E1-allowed because in chemical compounds the outermost 3d level forms the valence shells, while in metals it becomes a broad band. The intensity of this line can therefore vary with the chemical state. We have determined the {K? 5}/{K? 1} intensity ratio that results from proton impact on Ca, Ti and Cr, and we have collected the experimental data available in the literature. The influence of the sharp increase in the K ?5 intensity on the {K? }/{K? } intensity ratio and on X-ray analytical methods (e.g. proton induced X-ray emission, electron probe microanalysis, etc.) is discussed.

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

    SciTech Connect

    Andreeva, N. S.

    2006-12-15

    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.

  12. K alpha line emission during solar X-ray bursts

    NASA Technical Reports Server (NTRS)

    Phillips, K. J. H.; Neupert, W. M.

    1973-01-01

    Calculations of K alpha line emission from S, Ar, Ca and Fe are presented. It is reported that on the basis of data for hard X-ray bursts, the flux during most impulsive, non-thermal events is likely to be weak, though for a few strong bursts, a flux of approximately 100 photons/cm/s may be expected. The amount of S K alpha emission particularly is sensitively dependent on the value of the lower energy bound of the non-thermal electron distribution, offering a possible means of determining this. Thermal K alpha emission is only significant for Fe ions. The calculated thermal K alpha radiation is much less than that observed during an intense soft X-ray burst. It is concluded that a detailed temperature structure for the emission source is required in order to explain the discrepancy.

  13. Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

    DOEpatents

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

  14. Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

    DOEpatents

    Berman, R.M.; Cohen, I.

    1988-04-26

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

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

    SciTech Connect

    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.

  16. X-ray Diffraction and Polarized X-ray Absorption Study of Single Crystal LiFePO4

    NASA Astrophysics Data System (ADS)

    Liang, Gan; Benson, Ron; Li, Jiying; Vaknin, David; Croft, Mark

    2006-10-01

    Large size LiFePO4 single crystals have been grown by standard flux growth technique with the LiCl as the flux. Single crystal x-ray diffraction (XRD) and synchrotron polarized x-ray absorption spectroscopy (XAS) measurements have been performed on the crystals. The XRD measurements were performed at T = 293 K using Mo K? radiation (? = 0.7107) to a resolution corresponding to sin?/? = 0.6486 -1, with 2?max = 54.9 . A total number of 1330 reflections were processed with 350 unique data. The obtained crystal structure data were the following: lithium iron (II) phosphate, LiFePO4, orthorhombic, space group Pnma, lattice constants: a = 10.3172 (11) , b = 6.0096(8) , c = 4.6775 (4) , Z = 4, formula weight: 157.76, density: 3.613, ? = 55.562 cm-1. The bond lengths between Fe and O and between P and O were obtained. The polarized XAS was performed at the Fe K-edge with the x-ray E-vector along the a-, b-, and c-axis. The XAS results show that the Fe ions in the LiFePO4 single crystals are divalent. We also observed a big shift in both the energies of the pre-edge 1s -> 3d transition feature and the main edge when the polarization direction of the E-vector changes from along a-axis to along c-axis.

  17. Plasticity and X-ray Line Profile Analysis of the semicrystalline polymer poly(3-hydroxybutyrate)

    NASA Astrophysics Data System (ADS)

    Spieckermann, F.; Wilhelm, H.; Schafler, E.; Kerber, M.; Bernstorff, S.; Zehetbauer, M. J.

    2010-07-01

    The evolution of the microstructure during compressive deformation of the biodegradable polymer poly(3-hydroxybutyrate) (P3HB) was investigated in-situ via X-ray diffraction using synchrotron radiation. Flow curves were measured in-situ together with X-ray profiles for several degrees of deformation. The profiles were analysed using Multi-Reflection X-ray Line Profile Analysis (MXPA) adapted by the authors for semicrystalline polymers providing lamella thickness, crystallinity, and the presence and density of dislocations as a function of the deformation. In contrast to previous investigations in α crystallised isotactic polypropylene (α-iPP), P3HB does not exhibit a deformation induced increase of the dislocation density which suggests mechanisms other than dislocations to be involved in plastic deformation of P3HB.

  18. Three-Dimensional Visualization of a Human Chromosome Using Coherent X-Ray Diffraction

    SciTech Connect

    Nishino, Yoshinori; Ishikawa, Tetsuya; Takahashi, Yukio; Imamoto, Naoko; Maeshima, Kazuhiro

    2009-01-09

    Coherent x-ray diffraction microscopy is a lensless phase-contrast imaging technique with high image contrast. Although electron tomography allows intensive study of the three-dimensional structure of cellular organelles, it has inherent difficulty with thick objects. X rays have the unique benefit of allowing noninvasive analysis of thicker objects and high spatial resolution. We observed an unstained human chromosome using coherent x-ray diffraction. The reconstructed images in two or three dimensions show an axial structure, which has not been observed under unstained conditions.

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

    NASA Astrophysics Data System (ADS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

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

  20. Structure-induced negatively skewed X-ray diffraction pattern of carbon onions

    NASA Astrophysics Data System (ADS)

    Siklitskaya, Alexandra; Yastrebov, Sergey; Smith, Roger

    2013-10-01

    The idea is discussed that a gradual change of intershell separation in carbon onions may introduce a negative skewness into the most intense X-ray diffraction band. As an example, the experimental X-ray diffraction pattern of carbon onions is analysed using a weighted Lorentzian X-ray profile broadening model for each intershell separation contributing to the profile. The dependence of the mean radius for carbon onion shells on the intershell spacing between the adjacent shells is derived from the model analysis. Comparison with the internal distribution of atomic density in carbon onions measured with high resolution transmission electron microscopy is discussed.

  1. An atomic layer deposition chamber for in situ x-ray diffraction and scattering analysis

    NASA Astrophysics Data System (ADS)

    Geyer, Scott M.; Methaapanon, Rungthiwa; Johnson, Richard W.; Kim, Woo-Hee; Van Campen, Douglas G.; Metha, Apurva; Bent, Stacey F.

    2014-05-01

    The crystal structure of thin films grown by atomic layer deposition (ALD) will determine important performance properties such as conductivity, breakdown voltage, and catalytic activity. We report the design of an atomic layer deposition chamber for in situ x-ray analysis that can be used to monitor changes to the crystal structural during ALD. The application of the chamber is demonstrated for Pt ALD on amorphous SiO2 and SrTiO3 (001) using synchrotron-based high resolution x-ray diffraction, grazing incidence x-ray diffraction, and grazing incidence small angle scattering.

  2. An atomic layer deposition chamber for in situ x-ray diffraction and scattering analysis.

    PubMed

    Geyer, Scott M; Methaapanon, Rungthiwa; Johnson, Richard W; Kim, Woo-Hee; Van Campen, Douglas G; Metha, Apurva; Bent, Stacey F

    2014-05-01

    The crystal structure of thin films grown by atomic layer deposition (ALD) will determine important performance properties such as conductivity, breakdown voltage, and catalytic activity. We report the design of an atomic layer deposition chamber for in situ x-ray analysis that can be used to monitor changes to the crystal structural during ALD. The application of the chamber is demonstrated for Pt ALD on amorphous SiO2 and SrTiO3 (001) using synchrotron-based high resolution x-ray diffraction, grazing incidence x-ray diffraction, and grazing incidence small angle scattering. PMID:24880424

  3. An atomic layer deposition chamber for in situ x-ray diffraction and scattering analysis

    SciTech Connect

    Geyer, Scott M.; Methaapanon, Rungthiwa; Kim, Woo-Hee; Bent, Stacey F.; Johnson, Richard W.; Van Campen, Douglas G.; Metha, Apurva

    2014-05-15

    The crystal structure of thin films grown by atomic layer deposition (ALD) will determine important performance properties such as conductivity, breakdown voltage, and catalytic activity. We report the design of an atomic layer deposition chamber for in situ x-ray analysis that can be used to monitor changes to the crystal structural during ALD. The application of the chamber is demonstrated for Pt ALD on amorphous SiO{sub 2} and SrTiO{sub 3} (001) using synchrotron-based high resolution x-ray diffraction, grazing incidence x-ray diffraction, and grazing incidence small angle scattering.

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

    NASA Astrophysics Data System (ADS)

    Kasai, Hidetaka; Nishibori, Eiji

    2016-04-01

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

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

    DOEpatents

    Gibson, David M. (Voorheesville, NY); Gibson, Walter M. (Voorheesville, NY); Huang, Huapeng (Latham, NY)

    2007-06-26

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

  6. High resolution x-ray scattering and diffraction

    SciTech Connect

    Moncton, D.

    1983-01-01

    In the general class of high resolution x-ray scattering studies experiments one analyzes the distribution of photon energies and wave vectors resulting from illumination of a sample with collimated monochromatic radiation. Applications abound in the field of structural physics, which may be described as the study of structures for their intrinsic physical interest. This includes studies of novel states of matter, phase transitions, and dynamics. As both the wave vector and the energy of scattered photons are of interest, one may conceptually divide high resolution experimental setups for this work into two classes: those with high Q-resolution (momemtum transfer analysis) and those with high E-resolution (energy transfer analysis). The former class is exemplified by the existing experimental station on SSRL wiggler experimental station VII-2 and the proposed high Q-resolution wiggler station for NSLS Phase II. The latter class is dependent on extremely high flux, as discussed more fully below, and the possibility of constructing a high E-resolution scattering station fed by an x-ray undulator is one of the exciting opportunities presented by the proposed construction of a 6 GeV storage ring.

  7. Application of Laser Plasma X-rays to Time-resolved Debye-Sherrer Diffraction

    SciTech Connect

    Kanegae, Y.; Kinoshita, K.; Hosokai, T.; Ohkubo, T.; Yoshii, K.; Ueda, T.; Watanabe, T.; Zhidkov, A.; Uesaka, M.

    2003-08-26

    We have studied Laser Plasma X-ray(LPX) in order to apply to time-resolved protein crystallography. We consider that our works will contribute for application of X-ray pulse and breed short pulse handling techniques. LPX pulse duration is femto{approx}pico-second. So, we expect that the laser plasma X-ray system has the potential to satisfy the requirement of time-scale to resolve the early period of protein's structural change. We need about more than 1012photns/shot X-ray to get a diffraction image of organics. We have reinforced our LPX system to get a diffraction image. Now, we try laser pre-pulse effect by experiments and calculations. As the first step of our aim, we will obtain the Debey-Sherrer diffraction image of a biological sample.

  8. High-resolution ab initio three-dimensional x-ray diffraction microscopy

    SciTech Connect

    Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; Noy, Aleksandr; Hau-Riege, Stefan P.; Cui, Congwu; Howells, Malcolm R.; Rosen, Rachel; He, Haifeng; Spence, John C. H.; Weierstall, Uwe; Beetz, Tobias; Jacobsen, Chris; Shapiro, David

    2006-01-01

    Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and 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 three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatial resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.

  9. Stoichiometry optimization of homoepitaxial oxide thin films using x-ray diffraction

    SciTech Connect

    LeBeau, James M.; Engel-Herbert, Roman; Jalan, Bharat; Cagnon, Joeel; Moetakef, Pouya; Stemmer, Susanne; Stephenson, G. Brian

    2009-10-05

    Homoepitaxial SrTiO{sub 3} thin films grown by molecular beam epitaxy are analyzed using high-resolution x-ray diffraction and transmission electron microscopy. Measured 00L x-ray scans from stoichiometric and nonstoichiometric films are compared with calculations that account for the effects of film thickness, lattice parameter, fractional site occupancy, and an offset between film and substrate at the interface. It is found that thickness fringes, commonly observed around Bragg reflections even in stoichiometric homoepitaxial SrTiO{sub 3} films, arise from a film/substrate interface offset. Transmission electron microscopy studies confirm the presence of strain at those homoepitaxial interfaces that show an offset in x-ray diffraction. The consequences for stoichiometry optimization of homoepitaxial films using high-resolution x-ray diffraction and the quality of regrown oxide interfaces are discussed.

  10. Evaluation of In-Vacuum Imaging Plate Detector for X-Ray Diffraction Microscopy

    SciTech Connect

    Nishino, Yoshinori; Takahashi, Yukio; Yamamoto, Masaki; Ishikawa, Tetsuya

    2007-01-19

    We performed evaluation tests of a newly developed in-vacuum imaging plate (IP) detector for x-ray diffraction microscopy. IP detectors have advantages over direct x-ray detection charge-coupled device (CCD) detectors, which have been commonly used in x-ray diffraction microscopy experiments, in the capabilities for a high photon count and for a wide area. The detector system contains two IPs to make measurement efficient by recording data with the one while reading or erasing the other. We compared speckled diffraction patterns of single particles taken with the IP and a direct x-ray detection CCD. The IP was inferior to the CCD in spatial resolution and in signal-to-noise ratio at a low photon count.

  11. X-ray diffraction and scanning electron microscopy of galvannealed coatings on steel.

    PubMed

    Schmid, P; Uran, K; Macherey, F; Ebert, M; Ullrich, H-J; Sommer, D; Friedel, F

    2009-04-01

    The formation of Fe-Zn intermetallic compounds, as relevant in the commercial product galvannealed steel sheet, was investigated by scanning electron microscopy and different methods of X-ray diffraction. A scanning electron microscope with high resolution was applied to investigate the layers of the galvannealed coating and its topography. Grazing incidence X-ray diffraction (GID) was preferred over conventional Bragg-Brentano geometry for analysing thin crystalline layers because of its lower incidence angle alpha and its lower depth of information. Furthermore, in situ experiments at an environmental scanning electron microscope (ESEM) with an internal heating plate and at an X-ray diffractometer equipped with a high-temperature chamber were carried out. Thus, it was possible to investigate the phase evolution during heat treatment by X-ray diffraction and to display the growth of the zeta crystals in the ESEM. PMID:19153722

  12. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    DOE PAGESBeta

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stephano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

  13. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    SciTech Connect

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stephano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.

  14. High-resolution ab initio three-dimensional x-ray diffraction microscopy

    DOE PAGESBeta

    Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; Noy, Aleksandr; Hau-Riege, Stefan P.; Cui, Congwu; Howells, Malcolm R.; Rosen, Rachel; He, Haifeng; Spence, John C. H.; et al

    2006-01-01

    Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and 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 three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

  15. Direct measurement of the x-ray refractive index by Fresnel diffraction at a transparent edge.

    PubMed

    Gayer, C W; Hemmers, D; Stelzmann, C; Pretzler, G

    2013-05-01

    We demonstrate the feasibility of measuring x-ray refractive indices by transparent edge diffraction without recourse to the Kramers-Kronig relations. The method requires a coherent x-ray source, a transparent sample with a straight edge, and a high resolution x-ray detector. Here, we use the aluminum Kα radiation originating from a laser-produced plasma to coherently illuminate the edge of thin aluminum and beryllium foils. The resulting diffraction patterns are recorded with an x-ray CCD camera. From least-squares fits of Fresnel diffraction modeling to the measured data we determine the refractive index of Al and Be at the wavelength of the Al Kα radiation (0.834 nm, 1.49 keV). PMID:23632552

  16. High pressure synchrotron X-ray diffraction studies of biological molecules using the diamond anvil technique

    NASA Astrophysics Data System (ADS)

    Czeslik, C.; Malessa, R.; Winter, R.; Rapp, G.

    1996-02-01

    A system for high pressure synchrotron X-ray diffraction studies of biological samples in a diamond anvil cell (DAC) is described. It is capable of operating in the whole temperature and pressure range of interest for studies of biological molecules, i.e., in the temperature range from -40 to 100C at pressures between 1 bar and 50 kbar. The pressure is calibrated by measuring the pressure dependence of the ruby fluorescence line at 694 nm. Two linear detectors connected in series are used to measure simultaneously the small- and wide-angle X-ray scattering. The advantage of the experimental technique is threefold: Firstly, the amount of sample can be kept to a minimum (ca. 30 nl) using the high intensity of synchrotron radiation. Secondly, only the diamond anvil technique allows to reach extreme pressures. Thirdly, the use of the dual detector system allows recording of diffraction data both in the small- and wide-angle region at the same time. Examples of hitherto unknown phases of aqueous lipid and protein samples illustrate the potential of the system.

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

    NASA Technical Reports Server (NTRS)

    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.

  18. Dynamical x-ray diffraction from an icosahedral Al-Pd-Mn quasicrystal

    SciTech Connect

    Kycia, S.

    1996-04-23

    Primary extinction effects in diffraction from single grains of Al-Pd- Mn, and presumably many other FCI alloys, may be significant and should be corrected for prior to use of diffraction data in structural determinations. Probes based on dynamical diffraction effects, such as x-ray standing wave fluorescence, multiple beam interference, and x-ray transmission topographs, may now be used to study the bulk and surface structure of some quasicrystals. The observation of dynamical diffraction from icosahedral Al-Pd-Mn is a striking confirmation of the fact that quasicrystals can present a degree of structural perfection comparable to that found in the best periodic intermetallic crystals.

  19. In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

    1996-01-01

    Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a pinhole camera (transmission geometry, flat two-dimensional detector perpendicular to the direct beam), the instrument (which we call CHEMIN, for Chemistry and Mineralogy) uses an X-ray sensitive CCD detector which will allow concurrent positional and energy-dispersive analysis of collected photons. Thus XRF (energy) and XRD (geometry) analysis of transmitted X-rays will be performed at the same time. Tests performed with single minerals and simple mixtures give promising results. Refinements of the prototype promise interpretable results on complex samples.

  20. High temperature x-ray diffraction in transmission under controlled environment

    SciTech Connect

    Margulies, L.; Kramer, M.J.; Williams, J.J.; Deters, E.M.; McCallum, R.W.; Goldman, A.I.; Haeffner, D.R.; Lang, J.C.; Kycia, S.

    1998-12-31

    A compact tube furnace has been developed for high temperature X-ray diffraction studies using high energy synchrotron radiation. The furnace design has a low absorption path in transmission yet allows for a high degree of control of the sample atmosphere and a minimal temperature gradient across the sample. The design allows for a maximum temperature of 1,500 C with a variety of atmospheres including inert, reducing, and oxidizing. Preliminary results obtained at the SRI-CAT 1-ID undulator line (60 keV) at the APS facility and the A2 24 pole wiggler line (45 keV) at CHESS on the Ti{sub 5}Si{sub 3}Z{sub .5} (Z = C, N, O) system will be presented to demonstrate the feasibility of this approach.

  1. PROINSULIN: CRYSTALLIZATION AND PRELIMINARY X-RAY DIFFRACTION STUDIES*

    PubMed Central

    Fullerton, W. Wardle; Potter, Reginald; Low, Barbara W.

    1970-01-01

    Bovine proinsulin has been crystallized under a variety of conditions at both neutral and acid pH. Microtechniques were employed with sample weights of about 200 ?g and volumes of 5-20 ?l. The crystalline preparations all differ from each other morphologically. X-ray photographs of one form, tetragonal bipyramids grown at pH 3 with added ammonium sulphate solution, established the space group P41212 (or its enantiomorph P43212). The cell dimensions are a = 50.8 0.2 , c = 148.0 0.4 . The asymmetric unit in this form is a dimer of proinsulin which is also the dominant species in solution at this pH. Images PMID:5273450

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

    SciTech Connect

    Frank, Matthias; Carlson, David B.; Hunter, Mark; Williams, Garth J.; Messerschmidt, Marc; Zatsepin, Nadia A.; Barty, Anton; Benner, Henry; Chu, Kaiqin; Graf, Alexander; Hau-Riege, Stefan; Kirian, Rick; Padeste, Celestino; Pardini, Tommaso; Pedrini, Bill; Segelke, Brent; Seibert, M. M.; Spence, John C.; Tsai, Ching-Ju; Lane, Steve M.; Li, Xiao-Dan; Schertler, Gebhard; Boutet, Sebastien; Coleman, Matthew A.; Evans, James E.

    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.

  3. Exploring X-ray lines as scotogenic signals

    NASA Astrophysics Data System (ADS)

    Faisel, Gaber; Ho, Shu-Yu; Tandean, Jusak

    2014-11-01

    We consider some implications of X-ray lines from certain astronomical objects as potential effects of dark matter decay in the context of the scotogenic model, where neutrinos acquire mass radiatively via one-loop interactions with dark matter. As an example, we focus on the 3.5 keV line recently detected in the X-ray spectra of galaxy clusters, assuming that it stands future scrutiny. We explore the scenario in which the line originates from the slow decay of fermionic dark matter in the model. After obtaining a number of benchmark points representing the parameter space consistent with the new data and various other constraints, we make predictions on several observables in leptonic processes. They include the effective Majorana mass in neutrinoless double-beta decay, the sum of neutrino masses, and the rate of flavor-changing decay μ → eγ, as well as the cross sections of e+e- collisions into final states containing nonstandard particles in the model. These are testable in ongoing or future experiments and thus offer means to probe the scotogenic scenario studied.

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

    NASA Astrophysics Data System (ADS)

    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.

  5. Real-time observation of coherent acoustic phonons generated by an acoustically mismatched optoacoustic transducer using x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Persson, A. I. H.; Enquist, H.; Jurgilaitis, A.; Andreasson, B. P.; Larsson, J.

    2015-11-01

    The spectrum of laser-generated acoustic phonons in indium antimonide coated with a thin nickel film has been studied using time-resolved x-ray diffraction. Strain pulses that can be considered to be built up from coherent phonons were generated in the nickel film by absorption of short laser pulses. Acoustic reflections at the Ni-InSb interface leads to interference that strongly modifies the resulting phonon spectrum. The study was performed with high momentum transfer resolution together with high time resolution. This was achieved by using a third-generation synchrotron radiation source that provided a high-brightness beam and an ultrafast x-ray streak camera to obtain a temporal resolution of 10 ps. We also carried out simulations, using commercial finite element software packages and on-line dynamic diffraction tools. Using these tools, it is possible to calculate the time-resolved x-ray reflectivity from these complicated strain shapes. The acoustic pulses have a peak strain amplitude close to 1%, and we investigated the possibility to use this device as an x-ray switch. At a bright source optimized for hard x-ray generation, the low reflectivity may be an acceptable trade-off to obtain a pulse duration that is more than an order of magnitude shorter.

  6. Apparatus for use in examining the lattice of a semiconductor wafer by X-ray diffraction

    NASA Technical Reports Server (NTRS)

    Parker, D. L.; Porter, W. A. (Inventor)

    1978-01-01

    An improved apparatus for examining the crystal lattice of a semiconductor wafer utilizing X-ray diffraction techniques was presented. The apparatus is employed in a method which includes the step of recording the image of a wafer supported in a bent configuration conforming to a compound curve, produced through the use of a vacuum chuck provided for an X-ray camera. The entire surface thereof is illuminated simultaneously by a beam of incident X-rays which are projected from a distant point-source and satisfy conditions of the Bragg Law for all points on the surface of the water.

  7. Quality experimental and calculated powder x-ray diffraction

    SciTech Connect

    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).

  8. Quantitative determination of mineral composition by powder x-ray diffraction

    DOEpatents

    Pawloski, G.A.

    1984-08-10

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  9. Quantitative determination of mineral composition by powder X-ray diffraction

    DOEpatents

    Pawloski, Gayle A.

    1986-01-01

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

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

    NASA Astrophysics Data System (ADS)

    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.

  11. Phase sensitive x-ray diffraction imaging of defects in biological macromolecular crystals

    NASA Technical Reports Server (NTRS)

    Hu, Z. W.; Lai, B.; Chu, Y. S.; Cai, Z.; Mancini, D. C.; Thomas, B. R.; Chernov, A. A.

    2001-01-01

    Conventional x-ray diffraction topography is currently used to map defects in the bulk of protein crystals, but the lack of sufficient contrast is frequently a limiting factor. We experimentally demonstrate that this barrier can be circumvented using a method that combines phase sensitive and diffraction imaging principles. Details of defects revealed in tetragonal lysozyme and cubic ferritin crystals are presented and discussed. The approach enabling the detection of the phase changes of diffracted x rays should prove to be useful in the study of defect structures in a broad range of biological macromolecular crystals.

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

    ERIC Educational Resources Information Center

    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

  13. Monitoring model drug microencapsulation in PLGA scaffolds using X-ray powder diffraction

    PubMed Central

    Aina, Adeyinka; Gupta, Manish; Boukari, Yamina; Morris, Andrew; Billa, Nashiru; Doughty, Stephen

    2015-01-01

    The microencapsulation of three model drugs; metronidazole, paracetamol and sulphapyridine into Poly (dl-Lactide-Co-Glycolide) (PLGA) scaffolds were probed using X-ray Powder Diffraction (XRPD). Changes in the diffraction patterns of the PLGA scaffolds after encapsulation was suggestive of a chemical interaction between the pure drugs and the scaffolds and not a physical intermixture. PMID:27013917

  14. Study of titanate nanotubes by X-ray and electron diffraction and electron microscopy

    SciTech Connect

    Brunatova, Tereza; Popelkova, Daniela; Wan, Wei; Oleynikov, Peter; Danis, Stanislav; Zou, Xiaodong; Kuzel, Radomir

    2014-01-15

    The structure of titanate nanotubes (Ti-NTs) was studied by a combination of powder X-ray diffraction (PXRD), electron diffraction and high resolution transmission electron microscopy (HRTEM). Ti-NTs are prepared by hydrothermal treatment of TiO{sub 2} powder. The structure is identified by powder X-ray diffraction as the one based on the structure of H{sub 2}Ti{sub 2}O{sub 5}·H{sub 2}O phase. The same structure is obtained by projected potential from HRTEM through-focus image series. The structure is verified by simulated PXRD pattern with the aid of the Debye formula. The validity of the model is tested by computing Fourier transformation of a single nanotube which is proportional to measured electron diffraction intensities. A good agreement of this calculation with measured precession electron diffraction data is achieved. - Highlights: • Titanate nanotubes were prepared by hydrothermal method. • X-ray powder diffraction indicated their structure based on that of H{sub 2}Ti{sub 2}O{sub 5}·H{sub 2}O. • Structural model was created with the aid of high-resolution electron microscopy. • The model was verified with electron diffraction data. • X-ray powder diffraction pattern was calculated with the aid of the Debye formula.

  15. Monitoring model drug microencapsulation in PLGA scaffolds using X-ray powder diffraction.

    PubMed

    Aina, Adeyinka; Gupta, Manish; Boukari, Yamina; Morris, Andrew; Billa, Nashiru; Doughty, Stephen

    2016-03-01

    The microencapsulation of three model drugs; metronidazole, paracetamol and sulphapyridine into Poly (dl-Lactide-Co-Glycolide) (PLGA) scaffolds were probed using X-ray Powder Diffraction (XRPD). Changes in the diffraction patterns of the PLGA scaffolds after encapsulation was suggestive of a chemical interaction between the pure drugs and the scaffolds and not a physical intermixture. PMID:27013917

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

    ERIC Educational Resources Information Center

    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…

  17. X-Ray Diffraction Study on the Strain Anisotropy and Dislocation Structure of Deformed Lath Martensite

    NASA Astrophysics Data System (ADS)

    Hossein Nedjad, S.; Hosseini Nasab, F.; Movaghar Garabagh, M. R.; Damadi, S. R.; Nili Ahmadabadi, M.

    2011-08-01

    18Ni (300) maraging steel possessing lath martensite structure was deformed by four passes of equal-channel angular pressing (ECAP) at ambient temperature. Line profile analysis (LPA) of X-ray diffraction (XRD) patterns identified strong strain anisotropy and remarkable increases in the relative fraction of screw dislocations after ECAP. The strain anisotropy was reasonably accounted for by the anisotropy of elastic constants. Domination of screw dislocations in the deformed structure was attributed to the preferred annihilation of edge dislocations in the early stages of deformation along with the difficulties for annihilation of screw dislocations by cross slipping. Cobalt addition was mainly assumed to make cross slipping difficult by reducing stacking-fault energy and favoring short-range ordering.

  18. High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

    NASA Technical Reports Server (NTRS)

    Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

    2004-01-01

    Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

  19. A high-resolution x-ray diagnostic technique using simultaneous diffraction from several planes of acid phthalate crystals

    NASA Astrophysics Data System (ADS)

    Burkhalter, P. G.; Brown, D. B.; Gersten, M.

    1981-07-01

    An x-ray diagnostic tool was developed for acquiring and interpreting high-resolution spectra for hot-plasma emission from selected elements. A convex, curved potassium acid phthalate (KAP) crystal was used to collect spectral data from an exploded-A1-wire plasma over a wide exposure latitude with the 001, 002, and the 013 planes simultaneously diffracting. The curved-crystal diffraction efficiencies were calculated for these three planes in KAP and evaluated with x-ray line intensities derived from the experimental A1 data. The crystal efficiencies were also computed for two other commonly used acid phthalate crystals rubidium acid phthalate (RAP) and thallium acid phthalate (TAP), to compare with KAP crystals. The calculated efficiencies for the first-order diffraction in KAP, RAP, and TAP agreed with available experimental data.

  20. In situ X-ray diffraction investigation of nanocrystallization of amorphous Co-Fe-Zr-B alloys

    NASA Astrophysics Data System (ADS)

    Bednarčík, J.; Nicula, R.; Stir, M.; Burkel, E.

    2007-09-01

    Cobalt-rich soft-magnetic alloys were recently developed as amorphous materials with promising engineering properties, e.g. high mechanical strength, excellent magnetic properties and high corrosion resistance. The crystallization of the as-prepared amorphous alloys plays a crucial role in most technological applications of these advanced soft-magnetic nanomaterials. Amorphous ribbons with nominal composition Co 56Fe 16Zr 8B 20 (at%) were here obtained by single-roller melt spinning. The nucleation and growth of nanoscale phases during constant-rate heating of as-quenched and of high-energy ball-milled Co-rich amorphous soft-magnetic alloys were investigated by differential scanning calorimetry and by in situ high-temperature powder X-ray diffraction using synchrotron radiation. The temperature/time evolution of the crystallite size and of average microstrain was obtained from the X-ray diffraction line-profile analysis (LPA) of the powder diffraction patterns.

  1. Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

    NASA Technical Reports Server (NTRS)

    2008-01-01

    We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

  2. X-Ray Weak Broad-Line Quasars: Absorption or Intrinsic X-Ray Weakness

    NASA Technical Reports Server (NTRS)

    Risaliti, Guido; Mushotzky, Richard F. (Technical Monitor)

    2004-01-01

    XMM observations of X-ray weak quasars have been performed during 2003. The data for all but the last observation are now available (there has been a delay of several months on the initial schedule, due to high background flares which contaminated the observations: as a consequence, most of them had to be rescheduled). We have reduced and analyzed these data, and obtained interesting preliminary scientific results. Out of the eight sources, 4 are confirmed to be extrimely X-ray weak, in agreement with the results of previous Chandra observations. 3 sources are confirmed to be highly variable both in flux (by factors 20-50) and in spectral properties (dramatic changes in spectral index). For both these groups of objects, an article is in preparation. Preliminary results have been presented at an international workshop on AGN surveys in December 2003, in Cozumel (Mexico). In order to further understand the nature of these X-ray weak quasars, we submitted proposals for spectroscopy at optical and infrared telescopes. We obtained time at the TNG 4 meter telescope for near-IR observations, and at the Hobby-Eberly Telescope for optical high-resolution spectroscopy. These observations will be performed in early 2004, and will complement the XMM data, in order to understand whether the X-ray weakness of these sources is an intrinsic property or is due to absorption by circumnuclear material.

  3. High Pressure X-Ray Diffraction Studies on Nanocrystalline Materials

    NASA Technical Reports Server (NTRS)

    Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Pielaszek, R.; Bismayer, U.; Werner, S.; Palosz, W.

    2003-01-01

    Application of in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2 to 30 nrn diameter in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (< 30 nm) are discussed. It is shown that due to the complex structure, constituting a two-phase, core/surface shell system, no unique lattice parameter value and, consequently, no unique compressibility coefficient can satisfactorily describe the behavior of nanocrystalline powders under pressure. We offer a tentative interpretation of the distribution of macro- and micro-strains in nanoparticles of different grain size.

  4. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers.

    SciTech Connect

    Parrot, I. M.; Urban, Volker S; Gardner, K. H.; Forsyth, V. T.

    2005-04-01

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar{reg_sign} or Twaron{reg_sign}.

  5. Quantification of minor phases in growth kinetics experiments with powder x-ray diffraction.

    SciTech Connect

    Hanchar, J. M.; Nagy, K. L.; Fenter, P.; Finch, R. J.; Beno, D. J.; Sturchio, N. C.; Environmental Research; Sandia National Lab.

    2000-01-01

    Minor amounts of clay minerals precipitated from aqueous solution can be rapidly identified and quantified in a mineral mixture with powder X-ray diffraction using a rotating-anode source and a position-sensitive detector. For the case of gibbsite precipitated on a kaolinite powder substrate we demonstrate a simple method having a minimum detection limit of 0.1 wt%, using pure gibbsite as the intensity reference in mechanical mixtures of gibbsite and kaolinite. The amount of gibbsite precipitated onto kaolinite at 80 C, pH 3 is higher when determined from solution chemistry than from the X-ray method, and the difference in amounts increases with increasing Al concentration in solution. This discrepancy can be explained by assuming that a fraction of the precipitated material is effectively invisible to the X-ray diffraction technique, either due to a small diffracting domain size along the gibbsite [001] direction or formation of an Al-phase that is amorphous to X-rays. This method should be generally useful for a range of mineral mixtures where at least one intense reflection for the phase of interest is not obscured. The ability to identify, characterize, and quantify trace phases by X-ray diffraction, especially when combined with surface analysis by electron or atomic force imaging, is an important complement to the conventional approach of monitoring solution composition in growth kinetics experiments.

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

    DOE PAGESBeta

    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 numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

  7. X-ray diffraction study of some fossil and modern resins.

    PubMed

    Frondel, J W

    1967-03-17

    Samples of both fossil and modern resins have been investigated by x-ray diffraction techniques. Most fossil resins (ambers) yield only diffuse x-ray diffraction patterns, though some (settlingite, Highgate copalite, and guayaquillite) have relatively sharp patterns. Many modern resins, including those from species of Pinus and other conifers such as Picea and Abies, and many of those from Protium and Bursera, and Styrax benzoin, give sharp and distinctive patterns. Some crystalline constituents of the resins which yield the x-ray diffraction patterns have been identified. The similarity between the Protium and Bursera patterns and those of Highgate copalite and guayaquillite may indicate a possible genetic relationship between these modern and fossil resins. PMID:17839614

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

    SciTech Connect

    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 numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.

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

    PubMed Central

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

    2010-01-01

    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 numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. This can be an important advantage for studying radiation-sensitive biological and soft matter specimens. PMID:19654762

  10. Model studies of chromatin structure based on X-ray diffraction data.

    PubMed Central

    Subirana, J A; Martnez, A B

    1976-01-01

    Model calculations are presented in order to interpret the X-ray diffraction diagrams given by chromatin gels. It is shown that by taking into account the hydration of chromatin subunits, the problem of calculating the interference function in concentrated gels is greatly simplified. In this way it is spossible to fully interpret the influence of concentration on the position and intensity of the various rings present in the X-ray diffraction patterns. The possibilities and limitations of models based on spherical symmetry are also discussed. It is concluded that each chromatin subunit most likely contains three turns of DNA in each 200 base pairs segment surrounding a central protein core. With the method presented here it is possible to test if other models of chromatin based on different kinds of evidence are compatible with the X-ray diffraction data. PMID:1005111

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

    SciTech Connect

    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.

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

    SciTech Connect

    Sun, Cheng-Jun Brewe, Dale L.; Heald, Steve M.; Zhang, Bangmin; Department of Materials Science and Engineering, National University of Singapore, 117575 Singapore; NUSNNI-Nanocore, National University of Singapore, 117411 Singapore ; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.; Department of Physics, National University of Singapore, 117542 Singapore; Department of Electrical and Computer Engineering, National University of Singapore, 117575 Singapore

    2014-04-15

    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 Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} 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.

  13. Pump-probe X-ray Diffraction Technique for Irreversible Phase Change Materials

    SciTech Connect

    Fukuyama, Yoshimitsu; Yasuda, Nobuhiro; Kimura, Shigeru; Osawa, Hitoshi; Kim, Jungeun; Tanaka, Yoshihito; Takata, Masaki; Murayama, Haruno; Moritomo, Yutaka; Toriumi, Koshiro; Tanaka, Hitoshi

    2010-06-23

    We have developed a pump-probe X-ray diffraction measurement system for a sample with irreversible reaction at BL40XU in the SPring-8. The system mainly consists of a time-resolved measurement system, a sample disk rotation system, and an X-ray microbeam system. The time-resolved measurement system gives time resolution of 50 ps in laser-pump and X-ray probe method. A sample disk rotation system for repetitive measurements was made to give a virgin sample for every measurement. The number of repetitions for one sample disk was increased by using the X-ray microbeam technique. To keep the overlap of the X-ray microbeam and the laser beam on the sample surface during the disk rotation, the sample disk rotation system was constructed by a low-eccentric spindle motor. By using this system, the pump-probe X-ray diffraction measurement was demonstrated for a crystallization process of a DVD material.

  14. In-plate protein crystallization, in situ ligand soaking and X-ray diffraction.

    PubMed

    le Maire, Albane; Gelin, Muriel; Pochet, Sylvie; Hoh, François; Pirocchi, Michel; Guichou, Jean François; Ferrer, Jean Luc; Labesse, Gilles

    2011-09-01

    X-ray crystallography is now a recognized technique for ligand screening, especially for fragment-based drug design. However, protein crystal handling is still tedious and limits further automation. An alternative method for the solution of crystal structures of proteins in complex with small ligands is proposed. Crystallization drops are directly exposed to an X-ray beam after cocrystallization or soaking with the desired ligands. The use of dedicated plates in connection with an optimal parametrization of the G-rob robot allows efficient data collection. Three proteins currently under study in our laboratory for ligand screening by X-ray crystallography were used as validation test cases. The protein crystals belonged to different space groups, including a challenging monoclinic case. The resulting diffraction data can lead to clear ligand recognition, including indication of alternating conformations. These results demonstrate a possible method for automation of ligand screening by X-ray crystallography. PMID:21904027

  15. Coherent x-ray diffraction imaging of paint pigmentparticles by scanning a phase plate modulator

    SciTech Connect

    Chu Y. S.; Chen B.; Zhang F.; Berenguer F.; Bean R.; Kewish C.; Vila-Comamala J.; Rodenburg J.; Robinson I.

    2011-10-19

    We have implemented a coherent x-ray diffraction imaging technique that scans a phase plate to modulate wave-fronts of the x-ray beam transmitted by samples. The method was applied to measure a decorative alkyd paint containing iron oxide red pigment particles. By employing an iterative algorithm for wave-front modulation phase retrieval, we obtained an image of the paint sample that shows the distribution of the pigment particles and is consistent with the result obtained from a transmission x-ray microscope. The technique has been experimentally proven to be a feasible coherent x-ray imaging method with about 120 nm spatial resolution and was shown to work well with industrially relevant specimens.

  16. Diffraction crystal for sagittally focusing x-rays

    DOEpatents

    Ice, Gene E.; Sparks, Jr., Cullie J.

    1984-01-01

    The invention is a new type of diffraction crystal designed for sagittally focusing photons of various energies. The invention is based on the discovery that such focusing is not obtainable with conventional crystals because of distortion resulting from anticlastic curvature. The new crystal comprises a monocrystalline base having a front face contoured for sagittally focusing photons and a back face provided with rigid, upstanding, stiffening ribs restricting anticlastic curvature. When mounted in a suitable bending device, the reflecting face of the crystal can be adjusted to focus photons having any one of a range of energies.

  17. An X-ray diffractometer using mirage diffraction

    PubMed Central

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

    2014-01-01

    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

  18. An X-ray diffractometer using mirage diffraction.

    PubMed

    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

  19. Diffraction crystals for sagittally focusing x-rays

    DOEpatents

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

    1982-06-07

    The invention is a new type of diffraction crystal designed for sagittally focusing photons of various energies. The invention is based on the discovery that such focusing is not obtainable with conventional crystals because of distortion resulting from anticlastic curvature. The new crystal comprises a monocrystalline base having a front face contoured for sagittally focusing photons and a back face provided with rigid, upstanding, stiffening ribs restricting anticlastic curvature. When mounted in a suitable bending device, the reflecting face of the crystal can be adjusted to focus photons having any one of a range of energies.

  20. Bone structure studies with HNDT and x-ray diffraction methods

    NASA Astrophysics Data System (ADS)

    Silvennoinen, Raimo V. J.; Nygren, Kaarlo; Rouvinen, Juha; Petrova, Valentina V.

    1993-09-01

    Changes in molecular texture and structure of isolated radioulnar bones of subadult European moose collected in various environmental pollution areas of Finland were investigated by using HNDT and x-ray diffraction methods. By using small caudo-cranial bending forces, the bones were tested by using HNDT. For bone molecular texture and structure studies by using x-ray diffraction methods, samples were taken from the ulnar metaphyse (Olecranon). Results show that the bones obtained from the Harjavalta area and one from North Karelia showed changes in molecular texture and structure compared with samples from apparently normal animals.

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

    SciTech Connect

    Akparov, V. Kh.; Timofeev, V. I. Kuranova, I. P.

    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.

  2. Nanoscale Imaging of Mineral Crystals inside Biological Composite Materials Using X-Ray Diffraction Microscopy

    NASA Astrophysics Data System (ADS)

    Jiang, Huaidong; Ramunno-Johnson, Damien; Song, Changyong; Amirbekian, Bagrat; Kohmura, Yoshiki; Nishino, Yoshinori; Takahashi, Yukio; Ishikawa, Tetsuya; Miao, Jianwei

    2008-01-01

    We for the first time applied x-ray diffraction microscopy to the imaging of mineral crystals inside biological composite materials—intramuscular fish bone—at the nanometer scale resolution. We identified mineral crystals in collagen fibrils at different stages of mineralization. Based on the experimental results and biomineralization analyses, we suggested a dynamic model to account for the nucleation and growth of mineral crystals in the collagen matrix. The results obtained from this study not only further our understanding of the complex structure of bone, but also demonstrate that x-ray diffraction microscopy will become an important tool to study biological materials.

  3. X-ray and neutron diffraction determination of residual stresses in a pressed and welded component

    NASA Astrophysics Data System (ADS)

    Albertini, G.; Bruno, G.; Fiori, F.; Girardin, E.; Giuliani, A.; Quadrini, E.

    2000-03-01

    X-ray and neutron diffraction experiments have been carried out, in order to determine the residual stress (RS) field in a pressed and welded mock-up of an engine support for motor-bike technology. Such investigation is suggested by the need to know the stress state of the component after forming and welding. This allows to assess the quality of the first machining and further to theoretically simulate its performances under operation. Results are presented below, showing a good agreement between X-ray and neutron diffraction experiments.

  4. Antibiotic amphotericin B-DPPC lipid complex: X-ray diffraction and FTIR studies

    NASA Astrophysics Data System (ADS)

    Kamiński, Daniel M.; Arczewska, Marta; Pociecha, Damian; Górecka, Ewa; Stępniewski, Andrzej; Gagoś, Mariusz

    2015-01-01

    In this work, we studied the formation of a complex between the polyene antibiotic amphotericin B (AmB) and dipalmitoylphosphatidylcholine (DPPC) lipid multibilayers by means of X-ray diffraction and FTIR spectroscopy. The complex formation can be detected in multibilayers by characteristic reflection around 2.2 Å-1. The FTIR spectra indicate that in this case AmB lowers the main phase transition of DPPC. Additionally, with an increase in temperature, a shift of AmB towards the hydrophilic part of the DPPC bilayer is observed. For the first time, such complex formation has been observed by X-ray diffraction and discussed.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    SciTech Connect

    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.

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

    PubMed

    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

  8. Elastic properties of supported polycrystalline thin films and multilayers: An X-ray diffraction study

    SciTech Connect

    Goudeau, P.; Villain, P.; Tamura, N.; Renault, P.-O.; Badawi, K.F.; Padmore, H.A.

    2003-08-13

    Numerous experimental and theoretical studies have shown that thin film elastic behavior may be different from the bulk one due to size effects related to grain boundaries, free surfaces and interfaces. In addition, thin films often present high compressive residual stresses which may be responsible of thin film buckling. These two features will be discussed in this communication through recent x-ray diffraction experiments: in situ tensile testing for elastic constant analysis and scanning x-ray micro diffraction for stress relaxation measurements associated with film buckling.

  9. Magnetic x-ray circular dichroism in spin-polarized photoelectron diffraction

    SciTech Connect

    Waddill, G.D.; Tobin, J.G.; Guo, X.; Tong, S.Y.

    1994-07-12

    The first structural determination with spin-polarized, energy-dependent photoelectron diffraction using circularly-polarized x-rays is reported for Fe films on Cu(001). Circularly-polarized x-rays produced spin-polarized photoelectrons from the Fe 2p doublet, and intensity asymmetries in the 2p{sub 3/2} level are observed. Fully spin-specific multiple scattering calculations reproduced the experimentally-determined energy and angular dependences. A new analytical procedure which focuses upon intensity variations due to spin-dependent diffraction is introduced. A sensitivity to local geometric and magnetic structure is demonstrated.

  10. X-Ray Line Spectroscopy of Massive X-Ray Binaries

    NASA Technical Reports Server (NTRS)

    Liedahl, D. A.; Sako, M.; Wojdowski, P. S.; Paerels, F.; Kahn, S. M.

    2000-01-01

    Spectra from ASCA have provided the most, detailed view to date of the X-ray spectral properties of stellar winds in massive X-ray binaries. Using detailed atomic models that account for recombination cascade kinetics, we have reexamined archival data from Vela X-1 and Cen X-3 in the context of simple models of their wind geometries and velocity distributions. Our approach emphasizes apparent differential emission measure (DEM) distributions, and their dependence on orbital phase and wind parameters. A grid of theoretical DEM distributions is used to generate model spectra, which are compared to the data. We obtain good fits, and derive constraints oil the stellar wind parameters. We provide a summary of the method, and show that, even though the companion stars in Vela X-1 and Cen X-3 have comparable mass-loss rates, the winds in these two systems are dramatically different, in character.

  11. Real-time direct and diffraction X-ray imaging of irregular silicon wafer breakage.

    PubMed

    Rack, Alexander; Scheel, Mario; Danilewsky, Andreas N

    2016-03-01

    Fracture and breakage of single crystals, particularly of silicon wafers, are multi-scale problems: the crack tip starts propagating on an atomic scale with the breaking of chemical bonds, forms crack fronts through the crystal on the micrometre scale and ends macroscopically in catastrophic wafer shattering. Total wafer breakage is a severe problem for the semiconductor industry, not only during handling but also during temperature treatments, leading to million-dollar costs per annum in a device production line. Knowledge of the relevant dynamics governing perfect cleavage along the {111} or {110} faces, and of the deflection into higher indexed {hkl} faces of higher energy, is scarce due to the high velocity of the process. Imaging techniques are commonly limited to depicting only the state of a wafer before the crack and in the final state. This paper presents, for the first time, in situ high-speed crack propagation under thermal stress, imaged simultaneously in direct transmission and diffraction X-ray imaging. It shows how the propagating crack tip and the related strain field can be tracked in the phase-contrast and diffracted images, respectively. Movies with a time resolution of microseconds per frame reveal that the strain and crack tip do not propagate continuously or at a constant speed. Jumps in the crack tip position indicate pinning of the crack tip for about 1-2 ms followed by jumps faster than 2-6 m s(-1), leading to a macroscopically observed average velocity of 0.028-0.055 m s(-1). The presented results also give a proof of concept that the described X-ray technique is compatible with studying ultra-fast cracks up to the speed of sound. PMID:27006774

  12. Real-time direct and diffraction X-ray imaging of irregular silicon wafer breakage

    PubMed Central

    Rack, Alexander; Scheel, Mario; Danilewsky, Andreas N.

    2016-01-01

    Fracture and breakage of single crystals, particularly of silicon wafers, are multi-scale problems: the crack tip starts propagating on an atomic scale with the breaking of chemical bonds, forms crack fronts through the crystal on the micrometre scale and ends macroscopically in catastrophic wafer shattering. Total wafer breakage is a severe problem for the semiconductor industry, not only during handling but also during temperature treatments, leading to million-dollar costs per annum in a device production line. Knowledge of the relevant dynamics governing perfect cleavage along the {111} or {110} faces, and of the deflection into higher indexed {hkl} faces of higher energy, is scarce due to the high velocity of the process. Imaging techniques are commonly limited to depicting only the state of a wafer before the crack and in the final state. This paper presents, for the first time, in situ high-speed crack propagation under thermal stress, imaged simultaneously in direct transmission and diffraction X-ray imaging. It shows how the propagating crack tip and the related strain field can be tracked in the phase-contrast and diffracted images, respectively. Movies with a time resolution of microseconds per frame reveal that the strain and crack tip do not propagate continuously or at a constant speed. Jumps in the crack tip position indicate pinning of the crack tip for about 1–2 ms followed by jumps faster than 2–6 m s−1, leading to a macroscopically observed average velocity of 0.028–0.055 m s−1. The presented results also give a proof of concept that the described X-ray technique is compatible with studying ultra-fast cracks up to the speed of sound. PMID:27006774

  13. Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

    DOE PAGESBeta

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; Payzant, E. A.; Salvador, J. R.; Thompson, A. J.; Sharp, J.; Brown, D.; Miller, D.

    2016-02-17

    N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

  14. Neutron and X-ray Powder Diffraction Study of Skutterudite Thermoelectrics

    SciTech Connect

    Wang, Hsin; Kirkham, Melanie J; Watkins, Thomas R; Payzant, E Andrew; Salvador, James R.; Thompson, A. J.; Sharp, Jeff; Brown, David; Miller, David J.

    2016-01-01

    N-type and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray powder diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba-Yb-Co-Sb and the p-type material consists of Di-Fe-Ni-Sb or Di-Fe-Co-Sb (Di = Didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors (GM) and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubic symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. This knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.

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

    NASA Astrophysics Data System (ADS)

    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. Phase tomography from x-ray coherent diffractive imaging projections.

    PubMed

    Guizar-Sicairos, Manuel; Diaz, Ana; Holler, Mirko; Lucas, Miriam S; Menzel, Andreas; Wepf, Roger A; Bunk, Oliver

    2011-10-24

    Coherent diffractive imaging provides accurate phase projections that can be tomographically combined to yield detailed quantitative 3D reconstructions with a resolution that is not limited by imaging optics. We present robust algorithms for post-processing and alignment of these tomographic phase projections. A simple method to remove undesired constant and linear phase terms on the reconstructions is given. Also, we provide an algorithm for automatic alignment of projections that has good performance even for samples with no fiducial markers. Currently applied to phase projections, this alignment algorithm has proven to be robust and should also be useful for lens-based tomography techniques that pursue nanoscale 3D imaging. Lastly, we provide a method for tomographic reconstruction that works on phase projections that are known modulo 2π, such that the phase unwrapping step is avoided. We demonstrate the performance of these algorithms by 3D imaging of bacteria population in legume root-nodule cells. PMID:22108985

  17. Soft X-Ray Microscopy at HZB: Zone Plate Development and Imaging Using the Third Order of Diffraction

    SciTech Connect

    Rehbein, S.; Guttmann, P.; Werner, S.; Schneider, G.

    2011-09-09

    The Helmholtz-Zentrum Berlin (HZB) operates a transmission x-ray microscope (TXM) in the soft x-ray photon energy range with an energy resolution up to E/{Delta}E = 10{sup 4}. An approach to achieve ultrahigh spatial resolution with conventional, standard zone plate optics is to employ higher orders of diffraction of the zone plate objective. In this paper, we demonstrate that 11-nm lines and spaces of a multilayer test structure are clearly resolved by the x-ray microscope using the third order of diffraction of a zone plate objective with 20-nm outermost zone width. The disadvantage of high-order imaging is an about one order of magnitude lower diffraction efficiency of the used zone plates employed in the third order compared to the first order of diffraction. In addition, the measured background signal in the TXM images is no longer negligible. Therefore, we worked on the fabrication of zone plates with sub-20-nm outermost zone width to increase the spatial resolution in the first order of diffraction. A new high-resolution 100-keV e-beam lithography system from VISTEC, which was recently installed at the Helmholtz-Zentrum Berlin, makes these developments possible. Initial results on zone plates with an outermost zone width down to 15 nm exposed with the new e-beam system are presented. Furthermore, the contrast transfer function of the transmission x-ray microscope operating in partial coherence mode is measured by using the first and third diffraction order of the zone plate objective.

  18. X-ray bumps, iron K-alpha lines, and X-ray suppression by obscuring tori in Seyfert galaxies

    NASA Technical Reports Server (NTRS)

    Krolik, Julian H.; Madau, Piero; Zycki, Piotr T.

    1994-01-01

    We investigate the X-ray spectral properties of unobscured type 1 and obscured type 2 Seyferts as predicted by the unified Seyfert scheme. We consider the reprocessing of X-ray photons by photoelectric absorption, iron fluorescence, and Compton downscattering in the obscuring tori surrounding these active nuclei, and compute by Monte Carlo methods the reprocessed spectra as a function of the viewing angle. Depending on the optical depth and shape of the torus, and on the viewing angle, the X-ray flux can be suppressed by substantial factors when our line of sight is obscured. We show that an immediate consequence of the existence of an obscuring thick torus is the production in the spectra of type 1 Seyfert galaxies of a bump in the continuum above 10-20 keV and an Fe K-alpha line with significant equivalent width. In those type 2 Seyferts for which the hard X-ray spectrum has been substantially suppressed, the equivalent width of the Fe K-alpha line in the transmitted spectrum can be very large.

  19. Femtosecond X-ray diffraction from two-dimensional protein crystals

    PubMed Central

    Frank, Matthias; Carlson, David B.; Hunter, Mark S.; Williams, Garth J.; Messerschmidt, Marc; Zatsepin, Nadia A.; Barty, Anton; Benner, W. Henry; Chu, Kaiqin; Graf, Alexander T.; Hau-Riege, Stefan P.; Kirian, Richard A.; Padeste, Celestino; Pardini, Tommaso; Pedrini, Bill; Segelke, Brent; Seibert, M. Marvin; Spence, John C. H.; Tsai, Ching-Ju; Lane, Stephen M.; Li, Xiao-Dan; Schertler, Gebhard; Boutet, Sebastien; Coleman, Matthew; Evans, James E.

    2014-01-01

    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. PMID:25075325

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

    SciTech Connect

    Bogan, M.J.; Boutet, S.; Barty, A.; Benner, W.H.; Frank, M.; Lomb, L.; Shoeman, R.; Starodub, D.; Seibert, M.M.; Hau-Riege, S.P.; Woods, B.; Decorwin-Martin, P.; Bajt, S.; Schulz, J.; Rohner, U.; Iwan, B.; Timneanu, N.; Marchesini, S.; Schlichting, I.; Hajdu, J.; Chapman, H.N.; /DESY /Hamburg U., Inst. Theor. Phys. II

    2012-04-18

    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.

  1. Weak hard X-ray emission from broad absorption line quasars: evidence for intrinsic X-ray weakness

    SciTech Connect

    Luo, B.; Brandt, W. N.; Scott, A. E.; Alexander, D. M.; Gandhi, P.; Stern, D.; Teng, S. H.; Arévalo, P.; Bauer, F. E.; Boggs, S. E.; Craig, W. W.; Christensen, F. E.; Comastri, A.; Farrah, D.; Hailey, C. J.; Harrison, F. A.; Koss, M.; Ogle, P.; Puccetti, S.; Saez, C.; and others

    2014-10-10

    We report NuSTAR observations of a sample of six X-ray weak broad absorption line (BAL) quasars. These targets, at z = 0.148-1.223, are among the optically brightest and most luminous BAL quasars known at z < 1.3. However, their rest-frame ≈2 keV luminosities are 14 to >330 times weaker than expected for typical quasars. Our results from a pilot NuSTAR study of two low-redshift BAL quasars, a Chandra stacking analysis of a sample of high-redshift BAL quasars, and a NuSTAR spectral analysis of the local BAL quasar Mrk 231 have already suggested the existence of intrinsically X-ray weak BAL quasars, i.e., quasars not emitting X-rays at the level expected from their optical/UV emission. The aim of the current program is to extend the search for such extraordinary objects. Three of the six new targets are weakly detected by NuSTAR with ≲ 45 counts in the 3-24 keV band, and the other three are not detected. The hard X-ray (8-24 keV) weakness observed by NuSTAR requires Compton-thick absorption if these objects have nominal underlying X-ray emission. However, a soft stacked effective photon index (Γ{sub eff} ≈ 1.8) for this sample disfavors Compton-thick absorption in general. The uniform hard X-ray weakness observed by NuSTAR for this and the pilot samples selected with <10 keV weakness also suggests that the X-ray weakness is intrinsic in at least some of the targets. We conclude that the NuSTAR observations have likely discovered a significant population (≳ 33%) of intrinsically X-ray weak objects among the BAL quasars with significantly weak <10 keV emission. We suggest that intrinsically X-ray weak quasars might be preferentially observed as BAL quasars.

  2. Weak Hard X-Ray Emission from Broad Absorption Line Quasars: Evidence for Intrinsic X-Ray Weakness

    NASA Astrophysics Data System (ADS)

    Luo, B.; Brandt, W. N.; Alexander, D. M.; Stern, D.; Teng, S. H.; Arévalo, P.; Bauer, F. E.; Boggs, S. E.; Christensen, F. E.; Comastri, A.; Craig, W. W.; Farrah, D.; Gandhi, P.; Hailey, C. J.; Harrison, F. A.; Koss, M.; Ogle, P.; Puccetti, S.; Saez, C.; Scott, A. E.; Walton, D. J.; Zhang, W. W.

    2014-10-01

    We report NuSTAR observations of a sample of six X-ray weak broad absorption line (BAL) quasars. These targets, at z = 0.148-1.223, are among the optically brightest and most luminous BAL quasars known at z < 1.3. However, their rest-frame ≈2 keV luminosities are 14 to >330 times weaker than expected for typical quasars. Our results from a pilot NuSTAR study of two low-redshift BAL quasars, a Chandra stacking analysis of a sample of high-redshift BAL quasars, and a NuSTAR spectral analysis of the local BAL quasar Mrk 231 have already suggested the existence of intrinsically X-ray weak BAL quasars, i.e., quasars not emitting X-rays at the level expected from their optical/UV emission. The aim of the current program is to extend the search for such extraordinary objects. Three of the six new targets are weakly detected by NuSTAR with <~ 45 counts in the 3-24 keV band, and the other three are not detected. The hard X-ray (8-24 keV) weakness observed by NuSTAR requires Compton-thick absorption if these objects have nominal underlying X-ray emission. However, a soft stacked effective photon index (Γeff ≈ 1.8) for this sample disfavors Compton-thick absorption in general. The uniform hard X-ray weakness observed by NuSTAR for this and the pilot samples selected with <10 keV weakness also suggests that the X-ray weakness is intrinsic in at least some of the targets. We conclude that the NuSTAR observations have likely discovered a significant population (gsim 33%) of intrinsically X-ray weak objects among the BAL quasars with significantly weak <10 keV emission. We suggest that intrinsically X-ray weak quasars might be preferentially observed as BAL quasars.

  3. New software to model energy dispersive X-ray diffraction in polycrystalline materials

    NASA Astrophysics Data System (ADS)

    Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

    2012-02-01

    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.

  4. Perspective: Structural dynamics in condensed matter mapped by femtosecond x-ray diffraction

    SciTech Connect

    Elsaesser, T.; Woerner, M.

    2014-01-14

    Ultrashort soft and hard x-ray pulses are sensitive probes of structural dynamics on the picometer length and femtosecond time scales of electronic and atomic motions. Recent progress in generating such pulses has initiated new directions of condensed matter research, exploiting a variety of x-ray absorption, scattering, and diffraction methods to probe photoinduced structural dynamics. Atomic motion, changes of local structure and long-range order, as well as correlated electron motion and charge transfer have been resolved in space and time, providing a most direct access to the physical mechanisms and interactions driving reversible and irreversible changes of structure. This perspective combines an overview of recent advances in femtosecond x-ray diffraction with a discussion on ongoing and future developments.

  5. X-ray diffraction studies of CdTe grown on InSb

    NASA Astrophysics Data System (ADS)

    Bhat, Ishwara B.; Patel, Kshyamasil; Taskar, Nikhil R.; Ayers, John E.; Ghandhi, Sorab K.

    1988-04-01

    Cadmium telluride layers, grown on InSb substrates which were (100) 2° oriented towards (110), were examined using double crystal X-ray diffraction in conjunction with secondary ion mass spectrometry and photoluminescence. The layers were grown by organometallic vapor phase epitaxy at atmospheric pressure. The crystal quality of the CdTe is shown to be related to the substrate temperature and the nature of the surface prior to growth. Growth on diethyltelluride stabilized InSb substrates resulted in epitaxial layers with a misorientation of about 235 arc sec with respect to the substrates. On the other hand, layers followed the orientation of the substrates, when dimethylcadmium stabilized InSb was used. Growth at 350° C resulted in the smallest X-ray rocking curve (DCRC), with a full width at half maximum (FWHM) of about 20 arc sec Secondary ion mass spectrometry and photoluminescence data complement the results of this X-ray diffraction study.

  6. X-ray diffraction of indirect flight muscle from Drosohila in vivo

    SciTech Connect

    Irving, T.

    2007-02-09

    The indirect flight muscle (IFM) of the fruit fly, Drosophila, represents a powerful model system for integrated structure and function studies because of the ease of genetically manipulating this organism. Recent advances in synchrotron technology have allowed collection of high quality two dimensional x-ray fiber diffraction patterns from the IFM of living fruit flies both at rest and during tethered flight. Based on many decades of x-ray and electron microscopic studies of vertebrate muscle and IFM from the waterbug, Lethocerus, there now exists a framework for interpreting changes in the x-ray diffraction patterns in terms of structural changes at the myofilament level. These developments allow testing of hypotheses concerning muscle function in a truly in vivo system.

  7. Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation.

    PubMed

    Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M; Pernot, Petra

    2014-10-01

    We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ∼10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering. PMID:25375529

  8. Spectrometer for hard X-ray free-electron laser based on diffraction focusing.

    PubMed

    Kohn, V G; Gorobtsov, O Y; Vartanyants, I A

    2013-03-01

    X-ray free-electron lasers (XFELs) generate sequences of ultra-short spatially coherent pulses of X-ray radiation. A diffraction focusing spectrometer (DFS), which is able to measure the whole energy spectrum of the radiation of a single XFEL pulse with an energy resolution of ΔE/E 2 × 10(-6), is proposed. This is much better than for most modern X-ray spectrometers. Such resolution allows one to resolve the fine spectral structure of the XFEL pulse. The effect of diffraction focusing occurs in a single-crystal plate due to dynamical scattering, and is similar to focusing in a Pendry lens made from a metamaterial with a negative refraction index. Such a spectrometer is easier to operate than those based on bent crystals. It is shown that the DFS can be used in a wide energy range from 5 keV to 20 keV. PMID:23412482

  9. Determination of multiwavelength anomalous diffraction coefficients at high x-ray intensity

    NASA Astrophysics Data System (ADS)

    Son, Sang-Kil; Chapman, Henry N.; Santra, Robin

    2013-08-01

    The high-intensity version of multiwavelength anomalous diffraction (MAD) has a potential for solving the phase problem in femtosecond crystallography with x-ray free-electron lasers (XFELs). For MAD phasing, it is required to calculate or measure the MAD coefficients involved in the key equation, which depend on XFEL pulse parameters. In this work, we revisit the generalized Karle-Hendrickson equation to clarify the importance of configurational fluctuations of heavy atoms induced by intense x-ray pulses, and investigate the high-intensity cases of transmission and fluorescence measurements of samples containing heavy atoms. Based on transmission/fluorescence and diffraction experiments with crystalline samples of known structures, we propose an experimental procedure to determine all MAD coefficients at high x-ray intensity, which can be used in ab initio phasing for unknown structures.

  10. Data management and visualization of x-ray diffraction spectra from thin film ternary composition spreads

    SciTech Connect

    Takeuchi, I.; Long, C.J.; Famodu, O.O.; Murakami, M.; Hattrick-Simpers, J.; Rubloff, G.W.; Stukowski, M.; Rajan, K.

    2005-06-15

    We discuss techniques for managing and visualizing x-ray diffraction spectrum data for thin film composition spreads which map large fractions of ternary compositional phase diagrams. An in-house x-ray microdiffractometer is used to obtain spectra from over 500 different compositions on an individual spread. The MATLAB software is used to quickly organize the data and create various plots from which one can quickly grasp different information regarding structural and phase changes across the composition spreads. Such exercises are valuable in rapidly assessing the 'overall' picture of the structural evolution across phase diagrams before focusing in on specific composition regions for detailed structural analysis. We have also shown that simple linear correlation analysis of the x-ray diffraction peak information (position, intensity and full width at half maximum) and physical properties such as magnetization can be used to obtain insight about the physical properties.

  11. Hydrogen atoms in protein structures: high-resolution X-ray diffraction structure of the DFPase

    PubMed Central

    2013-01-01

    Background Hydrogen atoms represent about half of the total number of atoms in proteins and are often involved in substrate recognition and catalysis. Unfortunately, X-ray protein crystallography at usual resolution fails to access directly their positioning, mainly because light atoms display weak contributions to diffraction. However, sub-Ångstrom diffraction data, careful modeling and a proper refinement strategy can allow the positioning of a significant part of hydrogen atoms. Results A comprehensive study on the X-ray structure of the diisopropyl-fluorophosphatase (DFPase) was performed, and the hydrogen atoms were modeled, including those of solvent molecules. This model was compared to the available neutron structure of DFPase, and differences in the protein and the active site solvation were noticed. Conclusions A further examination of the DFPase X-ray structure provides substantial evidence about the presence of an activated water molecule that may constitute an interesting piece of information as regard to the enzymatic hydrolysis mechanism. PMID:23915572

  12. Coherent X-Ray Diffraction Imaging of Morphology and Strain in Nanomaterials

    NASA Astrophysics Data System (ADS)

    Harder, Ross; Robinson, Ian K.

    2013-09-01

    The last decade has seen a remarkable surge in x-ray characterization methods (Willmott, An Introduction to Synchrotron Radiation, John Wiley & Sons, Inc., New York, 2011). Imaging with x-rays has evolved from simple radiography, to image internal structure and diagnose injury, to a full-fledged tool for nanoscale characterization (Holt et al., Annu Rev Mater Res 43:1, 2013). Central to this development has been the advent of high-brilliance synchrotron and free electron laser sources of x-rays. The high degree of spacial coherence of the resulting beams has enabled novel imaging methods. Of these, coherent diffraction imaging has proven highly successful at imaging the structure in nano materials (Miao et al., Nature 400:342, 1999). In addition, this imaging method can be combined with Bragg diffraction to image strain with high sensitivity (Pfeifer et al., Nature 442:63, 2006; Robinson and Harder, Nat Mater 8:291, 2009).

  13. Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation

    NASA Astrophysics Data System (ADS)

    Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M.; Pernot, Petra

    2014-10-01

    We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ˜10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering.

  14. X-ray diffraction study of structural stability of giant proteoglycan molecules of mucus

    NASA Astrophysics Data System (ADS)

    Vazina, A. A.; Lanina, N. F.; Vasilieva, A. A.; Korneev, V. N.; Zabelin, A. V.; Polyakova, E. P.

    2009-05-01

    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.

  15. Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

    PubMed

    Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

    2009-09-01

    Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures. PMID:19713643

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

    SciTech Connect

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  17. Explosion dynamics of sucrose nanospheres monitored by time of flight spectrometry and coherent diffractive imaging at the split-and-delay beam line of the FLASH soft X-ray laser.

    PubMed

    Rath, Asawari D; Timneanu, Nicusor; Maia, Filipe R N C; Bielecki, Johan; Fleckenstein, Holger; Iwan, Bianca; Svenda, Martin; Hasse, Dirk; Carlsson, Gunilla; Westphal, Daniel; Mühlig, Kerstin; Hantke, Max; Ekeberg, Tomas; Seibert, M Marvin; Zani, Alessandro; Liang, Mengning; Stellato, Francesco; Kirian, Richard; Bean, Richard; Barty, Anton; Galli, Lorenzo; Nass, Karol; Barthelmess, Miriam; Aquila, Andrew; Toleikis, Sven; Treusch, Rolf; Roling, Sebastian; Wöstmann, Michael; Zacharias, Helmut; Chapman, Henry N; Bajt, Saša; DePonte, Daniel; Hajdu, Janos; Andreasson, Jakob

    2014-11-17

    We use a Mach-Zehnder type autocorrelator to split and delay XUV pulses from the FLASH soft X-ray laser for triggering and subsequently probing the explosion of aerosolised sugar balls. FLASH was running at 182 eV photon energy with pulses of 70 fs duration. The delay between the pump-probe pulses was varied between zero and 5 ps, and the pulses were focused to reach peak intensities above 10¹⁶W/cm² with an off-axis parabola. The direct pulse triggered the explosion of single aerosolised sucrose nano-particles, while the delayed pulse probed the exploding structure. The ejected ions were measured by ion time of flight spectrometry, and the particle sizes were measured by coherent diffractive imaging. The results show that sucrose particles of 560-1000 nm diameter retain their size for about 500 fs following the first exposure. Significant sample expansion happens between 500 fs and 1 ps. We present simulations to support these observations. PMID:25402130

  18. Ultrafast Structural Dynamics by X-Ray Diffraction and Structural Spectroscopy

    NASA Astrophysics Data System (ADS)

    Weber, Peter M.

    2015-05-01

    The ability to observe molecular reactions in real time is expected to aid the exploration of new reaction mechanisms, the development of catalysts, the understanding of biomolecular processes and the control of chemical reactions and material properties on a molecular level. To reach this goal, we have developed a gas-phase x-ray diffraction experiment that uses the ultrashort x-ray pulses from the Linac Coherent Light Source (LCLS) to capture atomic motions within molecules in a dilute gas (< 5 Torr). The delay time dependence of the gas x-ray diffraction pattern is measured in a pump-probe scheme with 267 nm excitation laser and 8.3 keV X-ray probe pulses. Optical excitation prepares 1,3-cyclohexadiene on the excited 1B surface, from where it accelerates past a conical intersection down the 2A potential energy surfaces before opening the ring structure on a 140 fs time scale. A ``molecular movie'' of the observed dynamics is constructed by comparing ab initio quantum molecular dynamics simulations with the experimental diffraction signal to derive weighted trajectories that provide a good representation of the structural dynamics, with the weighted ensemble of trajectories corresponding to the nuclear flux during the chemical reaction. The x-ray structural data thus provide reaction pathways for which ionization energies can be calculated at each step. We use ultrafast time-resolved multiphoton - ionization photoelectron spectroscopy to measure the travel time required for the molecule to reach certain resonance windows to Rydberg states. By so combining the results from the ultrafast x-ray diffraction with observations from ultrafast (structural) spectroscopy, it appears that we can make significant progress towards the ultimate goal: a comprehensive understanding of the spatially resolved photochemical reaction dynamics.

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

    NASA Astrophysics Data System (ADS)

    Guo, Xin; Jiang, Zhou-Ya; Chen, Long; Chen, Li-Ming; Xin, Jian-Guo; Peter, M. Rentzepis; Chen, Jie

    2015-10-01

    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. Project supported by the National Natural Science Foundation of China (Grant Nos. 61222509 and 11421064) and the W. M. Keck Foundation.

  20. Mapping Strain in Nanocrystalline Nitinol: an X-ray Diffraction Method (SULI paper)

    SciTech Connect

    Bibee, Mathew; /SLAC, SSRL

    2006-01-04

    Understanding the mechanical properties of biomedical devices is critical in predicting and preventing their failure in the body. Such knowledge is essential, for example, in the design of biomedical stents, which must undergo repeated strain over their ten year lifetimes without breaking. Computational models are used to predict mechanical response of a device, but these models are not complete; there are significant deviations from the predictions, especially when devices are subjected to repeated multi-axial loads. Improving these models requires comparisons with actual measurements of strained nitinol. Local measurements of the full strain tensor can be made using X-ray diffraction techniques, but they are currently limited to materials whose grain size is larger than the X-ray beam size or require several diffraction patterns produced by rotation of the sample. Nitinol stents are nanocrystalline, with grains smaller than any available X-ray beam. We present a method for measuring the local strain in a nanocrystalline material from a single X-ray diffraction pattern by extending current powder diffraction techniques. The components of the strain tensor are mapped onto a displacement ellipsoid, which is then reconstructed from diffraction data through Bragg's law and least-squares fitting. Using simulated diffraction data, we performed sensitivity tests to examine how the accuracy of the method depends on how much of the diffraction pattern is measured. We found that strain can be accurately calculated from measurements of at least three diffraction arcs of at least 20{sup o} in length. Thus we believe that our method is a viable approach to calculating strain provided a sufficient amount of diffraction pattern is recorded.

  1. Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

    ERIC Educational Resources Information Center

    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

  2. A-DNA and B-DNA: Comparing Their Historical X-Ray Fiber Diffraction Images

    ERIC Educational Resources Information Center

    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

  3. A-DNA and B-DNA: Comparing Their Historical X-Ray Fiber Diffraction Images

    ERIC Educational Resources Information Center

    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…

  4. X-Ray Diffraction Study of L2005 AG17 (IDPs) by Using SR

    NASA Technical Reports Server (NTRS)

    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.

  5. Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

    NASA Technical Reports Server (NTRS)

    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.

  6. Parametric X-ray Radiation and Diffraction Bremsstrahlung from Moderately Relativistic Electrons in Pyrolytic Graphite Crystal

    SciTech Connect

    Vagner, A. R.; Potylitsyn, A. P.; Kuznecov, S. I.; Uglov, S. R.; Zabaev, V. N.; Razin, S. V.

    2007-11-26

    Spectral maxima of parametric X-ray radiation (PXR) and diffraction bremsstrahlung (DBS) from moderately relativistic electrons and bremsstrahlung interacting with crystal have been observed. The maxima position of PXR and DBS depends on the crystal orientation angle and corresponds to theoretical calculations.

  7. Synchrotron X-ray diffraction characterization of healthy and fluorotic human dental enamel

    NASA Astrophysics Data System (ADS)

    Colaço, M. V.; Barroso, R. C.; Porto, I. M.; Gerlach, R. F.; Costa, F. N.; Braz, D.; Droppa, R.; de Sousa, F. B.

    2012-10-01

    With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basic physical-chemistry reactions of demineralization and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using Synchrotron X-ray diffraction. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the Brazilian Synchrotron Light Laboratory—LNLS, Campinas, Brazil. X-ray diffraction experiments were performed both in powder samples and polished surfaces. The powder samples were analyzed to obtain the characterization of a typical healthy enamel pattern. The polished surfaces were analyzed in specific areas that have been identified as fluorotic ones. X-ray diffraction data were obtained for all samples and these data were compared with the control samples and also with the literature data.

  8. Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

    ERIC Educational Resources Information Center

    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…

  9. Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

    SciTech Connect

    Veluraja, K.; Vennila, K.N.; Umamakeshvari, K.; Jasmine, A.; Velmurugan, D.

    2011-03-25

    Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of the homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.

  10. Three-dimensional imaging of dislocations by X-ray diffraction laminography

    SciTech Connect

    Haenschke, D.; Helfen, L.; Altapova, V.; Danilewsky, A.; Baumbach, T.

    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.

  11. Synchrotron X-ray Powder Diffraction Studies in Pulsed Magnetic Fields

    SciTech Connect

    Detlefs, C.; Frings, P.; Duc, F.; Nardone, M.; Billette, J.; Zitouni, A.; Rikken, G. L. J. A.; Vanacken, J.; Lorenzo, J. E.; Bras, W.

    2007-01-19

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110kJ to the magnet coil, which was sufficient to generate peak fields of 30T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8K and 300K.

  12. Synchrotron radiation (hard) X-ray diffraction microscopy of carbon fibre reinforced plastic (CFRP)

    NASA Astrophysics Data System (ADS)

    Stephenson, J. D.; Hentschel, M. P.; Lange, A.

    1994-05-01

    A simple "straight through" (hard) synchrotron radiation (SR) X-ray diffraction microscope of spatial resolution ≈ 25 μm (for photon energies ≈ 8 keV) is described for the bulk examination of an advanced material, carbon fibre reinforced plastic (CFRP).

  13. Stereochemistry Determination by Powder X-ray Diffraction Analysis and NMR Spectroscopy Residual Dipolar Couplings

    SciTech Connect

    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.

  14. An Inquiry Based Exercise Using X-ray Diffraction Data to Incite Student Learning

    NASA Astrophysics Data System (ADS)

    Rogow, D. L.; McDonald, W.; Bresler, M. R.

    2010-12-01

    An inquiry based learning exercise was designed for an upper division advanced inorganic laboratory course that meets one of the requirements for the Bachelor of Science degree in Chemistry and Biochemistry at the University of California, Santa Cruz. The content goals of this exercise were evaluation of whether a given solid state structure was previously known by using powder X-ray diffraction data, and understanding how the diffraction pattern relates to the crystal structure of the compound in question. The scientific process goals included searching a database to match the patterns and preparing data for oral presentations. The goals of the exercise were addressed via an activity allowing students to utilize real X-ray powder diffraction data to search and match with known structures in a database (International Crystal Structure Database) and to give an oral presentation. After students found their structures in the database, they prepared oral presentations justifying their choice for the match and their reasoning through structural analysis of the X-ray data. Students learned about X-ray diffraction theory in an inquiry type environment and gained valuable experience and confidence in presenting their findings using strong reasoning and communication skills. Assessment was implemented during active facilitation throughout the activity and during the final oral presentations.

  15. X-RAY POWDER DIFFRACTION SYSTEM FOR CHEMICAL SPECIATION OF PARTICULATE AEROSOL SAMPLES

    EPA Science Inventory

    An x-ray powder diffraction system has been developed for the automated measurement and analysis of particulate aerosol samples. The system is optimized to process samples with particle loadings of about 100 micrograms/sq cm which are acquired with dichotomous air samplers. A pos...

  16. Residual stress evaluation and fatigue life prediction in the welded joint by x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Yoo, Keun Bong; Hwang, Kwon Tae; Chang, Jung Chel; Kim, Jae Hoon

    2009-07-01

    In the fossil power plant, the reliability of the components which consist of the many welded parts depends on the quality of welding. The residual stress is occurred by the heat flux of high temperature during weld process. This decreases the mechanical properties as the strength of fatigue and fracture. The residual stress of the welded part in the recently constructed power plants has been the cause of a variety of accidents. The objective of this study is measurement of the residual stress and the full width at half maximum intensity (FWHM) by X-ray diffraction method and to estimate the feasibility of this application for fatigue life assessment of the high-temperature pipeline. The materials used for the study is P92 steel for the use of high temperature pipe on super critical condition. The test results were analyzed by the distributed characteristics of residual stresses and FWHM in x-ray diffraction intensity curve. Also, X-ray diffraction tests using specimens simulated low cycle fatigue damage were performed in order to analyze fatigue properties when fatigue damage conditions become various stages. As a result of X-ray diffraction tests for specimens simulated fatigue damages, we conformed that the ratio of the FWHM due to fatigue damage has linear relationship with fatigue life ratio algebraically. From this relationship, it was suggested that direct expectation of the life consumption rate was feasible.

  17. High spatial resolution X-ray and gamma ray imaging system using diffraction crystals

    DOEpatents

    Smither, Robert K.

    2011-05-17

    A method and a device for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation are provided. The device comprises a plurality of arrays, with each array comprising a plurality of elements comprising a first collimator, a diffracting crystal, a second collimator, and a detector.

  18. Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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 ...

  19. Development of an x-ray diffraction camera used in magnetic fields up to 10 T

    SciTech Connect

    Mitsui, Yoshifuru; Takahashi, Kohki; Watanabe, Kazuo; Koyama, Keiichi

    2011-12-15

    A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials.

  20. Development of an x-ray diffraction camera used in magnetic fields up to 10 T

    NASA Astrophysics Data System (ADS)

    Mitsui, Yoshifuru; Koyama, Keiichi; Takahashi, Kohki; Watanabe, Kazuo

    2011-12-01

    A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials.

  1. Development of an x-ray diffraction camera used in magnetic fields up to 10 T.

    PubMed

    Mitsui, Yoshifuru; Koyama, Keiichi; Takahashi, Kohki; Watanabe, Kazuo

    2011-12-01

    A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials. PMID:22225246

  2. X-ray imaging and diffraction from surface phonons on GaAs

    NASA Astrophysics Data System (ADS)

    Sauer, W.; Streibl, M.; Metzger, T. H.; Haubrich, A. G. C.; Manus, S.; Wixforth, A.; Peisl, J.; Mazuelas, A.; Härtwig, J.; Baruchel, J.

    1999-09-01

    Surface acoustic waves (SAWs) are excited on the GaAs (001) surface by using interdigital transducers, designed for frequencies of up to 900 MHz. The emitted phonons with wavelengths down to 3.5 μm are visualized and characterized by combined x-ray diffraction techniques. Using stroboscopic topography, the SAW emission of a parallel and a focusing transducer geometry are imaged. High-resolution x-ray diffraction profiles show up to 12 phonon-induced satellite reflections besides the GaAs (004) reflection, with a width of 9 arcsec each. The diffraction pattern is simulated numerically, applying the kinematical scattering theory to a model crystal. From fits to measured diffraction profiles at different excitation voltages, the SAW amplitudes were calculated and found to be in the sub-nm range.

  3. Design and performance of an imaging plate system for X-ray diffraction study

    NASA Astrophysics Data System (ADS)

    Amemiya, Yoshiyuki; Matsushita, Tadashi; Nakagawa, Atsushi; Satow, Yoshinori; Miyahara, Junji; Chikawa, Jun-ichi

    1988-04-01

    A new readout system for a BaFBr: Eu 2+ photostimulable phosphor screen (imaging plate) was constructed by modifying a drum scanner, with a design optimized for X-ray diffraction and scattering applications. An effort was made to achieve a high detective quantum efficiency below 20 keV, a small pixel size (25 μm × 25 μm), a low quantization noise (0.22%) using 12-bit A/D converters, and the capability to cover an inherent dynamic range (1:10 5) of the photostimulated luminescence by using two photomultiplier tubes. This system is being used in several synchrotron radiation experiments: Laue diffraction of protein crystals, small angle diffraction from a single muscle fiber, powder diffraction from crystals in a diamond anvil cell, and time-resolved small-angle X-ray scattering from a synthetic polymer during stretching.

  4. Application of a pnCCD in X-ray diffraction: a three-dimensional X-ray detector.

    PubMed

    Leitenberger, Wolfram; Hartmann, Robert; Pietsch, Ullrich; Andritschke, Robert; Starke, Ines; Strüder, Lothar

    2008-09-01

    The first application of a pnCCD detector for X-ray scattering experiments using white synchrotron radiation at BESSY II is presented. A Cd arachidate multilayer was investigated in reflection geometry within the energy range 7 keV < E < 35 keV. At fixed angle of incidence the two-dimensional diffraction pattern containing several multilayer Bragg peaks and respective diffuse-resonant Bragg sheets were observed. Since every pixel of the detector is able to determine the energy of every incoming photon with a resolution DeltaE/E approximately 10(-2), a three-dimensional dataset is finally obtained. In order to achieve this energy resolution the detector was operated in the so-called single-photon-counting mode. A full dataset was evaluated taking into account all photons recorded within 10(5) detector frames at a readout rate of 200 Hz. By representing the data in reciprocal-space coordinates, it becomes obvious that this experiment with the pnCCD detector provides the same information as that obtained by combining a large number of monochromatic scattering experiments using conventional area detectors. PMID:18728315

  5. Specific features of two diffraction schemes for a widely divergent X-ray beam

    NASA Astrophysics Data System (ADS)

    Avetyan, K. T.; Levonyan, L. V.; Semerjian, H. S.; Arakelyan, M. M.; Badalyan, O. M.

    2015-03-01

    We investigated the specific features of two diffraction schemes for a widely divergent X-ray beam that use a circular diaphragm 30-50 ?m in diameter as a point source of characteristic radiation. In one of the schemes, the diaphragm was set in front of the crystal (the diaphragm-crystal ( d-c) scheme); in the other, it was installed behind the crystal (the crystal-diaphragm ( c-d) scheme). It was established that the diffraction image in the c-d scheme is a topographic map of the investigated crystal area. In the d-c scheme at L = 2 l ( l and L are the distances between the crystal and the diaphragm and between the photographic plate and the diaphragm, respectively), the branches of hyperbolas formed in this family of planes ( hkl) by the characteristic K ? and K ? radiations, including higher order reflections, converge into one straight line. It is experimentally demonstrated that this convergence is very sensitive to structural inhomogeneities in the crystal under study.

  6. Hydration kinetics of oriented lipid membranes investigated by energy dispersive x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Caracciolo, Giulio; Sadun, Claudia; Caminiti, Ruggero

    2004-08-01

    Energy dispersive x-ray diffraction was applied to investigate the hydration kinetics of highly aligned 1,2-dioleoyl-3-trimethylammonium-propane membrane system. First, the adsorption of water into the lipid film results in a continous gain of interbilayer spatial coherence until a maximum is reached. Further, adsorbed water molecules behave as bulk water promoting loss of spatial coherence and leading to a progressive lowering and broadening of diffraction peaks. The possible molecular origin of this phenomenon is discussed.

  7. Photoelectron diffraction from laser-aligned molecules with X-ray free-electron laser pulses

    PubMed Central

    Nakajima, Kyo; Teramoto, Takahiro; Akagi, Hiroshi; Fujikawa, Takashi; Majima, Takuya; Minemoto, Shinichirou; Ogawa, Kanade; Sakai, Hirofumi; Togashi, Tadashi; Tono, Kensuke; Tsuru, Shota; Wada, Ken; Yabashi, Makina; Yagishita, Akira

    2015-01-01

    We report on the measurement of deep inner-shell 2p X-ray photoelectron diffraction (XPD) patterns from laser-aligned I2 molecules using X-ray free-electron laser (XFEL) pulses. The XPD patterns of the I2 molecules, aligned parallel to the polarization vector of the XFEL, were well matched with our theoretical calculations. Further, we propose a criterion for applying our molecular-structure-determination methodology to the experimental XPD data. In turn, we have demonstrated that this approach is a significant step toward the time-resolved imaging of molecular structures. PMID:26369428

  8. Diffractive imaging of nonperiodic materials with future coherent X-ray sources.

    PubMed

    Shen, Qun; Bazarov, Ivan; Thibault, Pierre

    2004-09-01

    Coherent diffractive imaging using a coherent X-ray source promises to be a useful microscopic method for imaging noncrystalline objects at high spatial resolution. In this article a simple method to estimate the coherently scattered signal as a function of resolution is presented, and it is shown that the required X-ray flux or dose scales as the inverse third power of resolution for a specimen of constant volume and density. A simulated case study using the proposed energy-recovery linac source is also presented, which confirms the estimated flux requirement. PMID:15310961

  9. Interaction between Lipid Monolayers and Poloxamer 188: An X-Ray Reflectivity and Diffraction Study

    PubMed Central

    Wu, Guohui; Majewski, Jaroslaw; Ege, Canay; Kjaer, Kristian; Weygand, Markus Jan; Lee, Ka Yee C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase separating from the lipids, forces the lipid molecules to pack tightly and restore the barrier function of the membrane. Upon compression to bilayer equivalent pressure, P188 is squeezed out from the lipid monolayer, allowing a graceful exit of P188 when the membrane integrity is restored. PMID:16100276

  10. MBE apparatus for in situ grazing incidence x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Akimoto, K.; Mizuki, J.; Hirosawa, I.; Matsui, J.

    1989-07-01

    A molecular beam epitaxy (MBE) apparatus furnished with two E-gun evaporators, two Knudsen cells and RHEED, was built for in situ grazing incidence x-ray diffraction studies. By adopting horizontal sample setting geometry, the entire ultrahigh vacuum chamber was rotated simply with the aid of a spring, and a large sample area was irradiated by the x-rays. Using this apparatus, we observed the 7×7 superstructure on a Si(111) surface and at a SiO2/Si(111) interface.

  11. High-pressure structural studies of dysprosium using angle-dispersive x-ray diffraction

    SciTech Connect

    Shen Yongrong; Kumar, Ravhi S.; Cornelius, Andrew L.; Nicol, Malcolm F.

    2007-02-01

    We present structural results under pressure for elemental dysprosium (Dy) up to 87 GPa using in situ angle-dispersive x-ray diffraction measurements with synchrotron x rays and a diamond-anvil cell. Dy exhibits the structural transition sequence, hP2{yields}hR9{yields}hP4{yields}distorted cF4, from Rietveld full-profile refinements. Clear evidence is documented for the high-pressure distorted cF4 phase observed above 45 GPa to be an orthorhombic oS8 (Cmmm) structure for Dy in the lanthanide phase diagram.

  12. X-ray powder diffraction study of poly/carbon monofluoride/, CF/1.12/

    NASA Technical Reports Server (NTRS)

    Mahajan, V. K.; Badachhape, R. B.; Margrave, J. L.

    1974-01-01

    Data from X-ray diffraction studies of the poly(carbon monofluoride) with empirical formula CF(1.09-1.15) are reported, and possible intercalation arrangements for the substance are discussed. The data do not conform to true hexagonal symmetry, indicating that the carbon atoms are not coplanar. Each bond angle of carbon is 118.8 deg, and the carbon-carbon distance is 1.47 A. The interlayer distance is 5.76 A. A total absence of (hkl) reflections in the X-ray pattern shows that the separate CF layers are not regularly arranged with respect to one another.

  13. Emission lines from X-ray-heated accretion disks in low-mass X-ray binaries

    NASA Technical Reports Server (NTRS)

    Ko, Yuan-Kuen; Kallman, Timothy R.

    1994-01-01

    We investigate the structure of accretion disks illuminated by X-rays from a central compact object in a binary system. X-rays can photoionize the upper atmosphere of the disk and form an accretion disk corona (ADC) where emission lines can form. We construct a model to calculate the vertical structure and the emission spectrum of the ADC with parameters appropriate to low-mass X-ray binaries. These models are made by nonlocal thermodynamic equilibrium calculations of ion and level populations and include a large number of atomic processes for 10 cosmically abundant elements. Transfer of radiation is treated by using the escape probability formalism. The vertical temperature profile of the ADC consists of a Compton-heated region and a mid-T zone where the temperature is approximately 10(exp 6) K. A thermal instability occurs close to the disk photosphere and causes the temperature of the ADC to drop abruptly from 10(exp 6) K to several times 10(exp 4) K. The emission spectrum in the optical, ultraviolet, extreme ultraviolet, and X-ray range is discussed and compared with the observations.

  14. X-ray diffraction pattern of a Gulyaev-Bleustein surface acoustic wave in grazing geometry

    SciTech Connect

    Levonyan, L. V. Khachaturyan, G. K.

    2006-12-15

    The X ray diffraction pattern of a Gulyaev-Bleustein surface acoustic wave (SAW) under grazing angles of incidence in noncoplanar symmetric Laue geometry has been considered. It is supposed that the propagation direction of an SAW makes a small angle with the diffraction vector. It is shown that small deviations from the Bragg angle ({approx}0.01'' induced by the SAW and do not affect the reflection coefficient lead to the formation of diffraction satellites both in the cases of standing and traveling SAWs. It has been established that the recorded diffraction pattern, which is a time-averaged intensity distribution, has characteristic profiles for odd and even satellites.

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

    PubMed

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

    2009-09-01

    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 A 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. PMID:19690369

  16. Protein crystallography: From X-ray diffraction spots to a three dimensional image

    SciTech Connect

    Terwilliger, T.C.; Berendzen, J.

    1998-02-25

    Proteins are remarkable molecular machines that are essential for life. They can do many things ranging from the precise control of blood clotting to synthesizing complex organic compounds. Pictures of protein molecules are in high demand in biotechnology because they are important for applications such as drug discovery and for engineering enzymes for commercial use. X-ray crystallography is the most common method for determining the three-dimensional structures of protein molecules. When a crystal of a protein is placed in an X-ray beam, scattering of X-rays off the ordered molecules produces a diffraction pattern that can be measured on a position-sensitive CCD or image-plate detector. Protein crystals typically contain thousands of atoms and the diffraction data are generally measured to relatively low resolution. Consequently the direct methods approaches generally cannot be applied. Instead, if the crystal is modified by adding metal atoms at specific sites or by tuning the wavelength of the X-rays to cross an absorption edge of a metal atom in the crystal, then the information from these additional measurements is sufficient to first identify the /locations of the metal atoms. This information is then used along with the diffraction data to make a three-dimensional picture of electron densities. This picture can be used to determine the position of most or all of the atoms in the protein.

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

    PubMed

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

    2011-01-17

    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 window of photon energies where the high scattering contrast between carbon and oxygen is well-suited to image biological samples. In particular, we have reconstructed the complex sample transmission function of a fossil diatom at a photon energy of 517 eV. In imaging a lithographically fabricated test sample a resolution on the order of 50 nm (half-period length) has been achieved. Along with this proof-of-principle for PCDI at soft x-ray wavelengths, we discuss the experimental and technical challenges which can occur especially for soft x-ray PCDI. PMID:21263642

  18. Ultra-high aspect ratio high-resolution nanofabrication for hard X-ray diffractive optics.

    PubMed

    Chang, Chieh; Sakdinawat, Anne

    2014-01-01

    Although diffractive optics have played a major role in nanoscale soft X-ray imaging, high-resolution and high-efficiency diffractive optics have largely been unavailable for hard X-rays where many scientific, technological and biomedical applications exist. This is owing to the long-standing challenge of fabricating ultra-high aspect ratio high-resolution dense nanostructures. Here we report significant progress in ultra-high aspect ratio nanofabrication of high-resolution, dense silicon nanostructures using vertical directionality controlled metal-assisted chemical etching. The resulting structures have very smooth sidewalls and can be used to pattern arbitrary features, not limited to linear or circular. We focus on the application of X-ray zone plate fabrication for high-efficiency, high-resolution diffractive optics, and demonstrate the process with linear, circular, and spiral zone plates. X-ray measurements demonstrate high efficiency in the critical outer layers. This method has broad applications including patterning for thermoelectric materials, battery anodes and sensors among others. PMID:24970569

  19. Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

    NASA Astrophysics Data System (ADS)

    Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

    2015-10-01

    The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

  20. X-ray lines and self-interacting dark matter

    NASA Astrophysics Data System (ADS)

    Mambrini, Yann; Toma, Takashi

    2015-12-01

    We study the correlation between a monochromatic signal from annihilating dark matter and its self-interacting cross section. We apply our argument to a complex scalar dark sector, where the pseudo-scalar plays the role of a warm dark matter candidate while the scalar mediates its interaction with the Standard Model. We combine the recent observation of the cluster Abell 3827 for self-interacting dark matter and the constraints on the annihilation cross section for monochromatic X-ray lines. We also confront our model to a set of recent experimental analyses and find that such an extension can naturally produce a monochromatic keV signal corresponding to recent observations of Perseus or Andromeda, while in the meantime it predicts a self-interacting cross section of the order of σ /m ˜eq 0.1{-}1 {cm^2/g}, as recently claimed in the observation of the cluster Abell 3827. We also propose a way to distinguish such models by future direct detection techniques.

  1. X-Ray Continua of Broad Absorption Line Quasars

    NASA Technical Reports Server (NTRS)

    Mathur, S.

    1999-01-01

    The targets for this program, PG1416-129 and LBQS 2212-1759 were known to be Broad Absorption Line Quasars (BALQSOs). BALQSOs are highly absorbed in soft X-rays. Good high energy response of Rossi-XTE made them ideal targets for observation. We observed LBQS 2212-1759 with PCA. We have now analyzed the data and found that the source was not detected. Since our target was expected to be faint, reliable estimate of background was very important. With the release of new FTOOLS (version 4.1) we were able to do so. We also analyzed a well known bright object and verified our results with the published data. This gave us confidence in the non-detection of our target LBQS 2212-1759. We are currently investigating the implications of this non-detection. Due to some scheduling problems, our second target PG1416-129 was not observed in A01. It was observed on 06/26/98. This target was detected with RXTE. We are now working on the spectral analysis with XSPEC.

  2. Simultaneous femtosecond X-ray spectroscopy and diffraction of photosystem II at room temperature.

    PubMed

    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

    2013-04-26

    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

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

    SciTech Connect

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

    2007-01-19

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

  4. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex.

    PubMed

    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

  5. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

    PubMed Central

    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

  6. Texture analysis of zirconium samples deformed by uniaxial tension using neutron and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Kucerakova, M.; Vratislav, S.; Kalvoda, L.; Trojanova, Z.

    2015-04-01

    Seven zirconium samples were studied by neutron and X-ray diffraction after deformation on uniaxial tensile machine INSTRON 5882 from strain 5% to strain 30% (strain step was 5%). Preferred orientation parameters were determined by using pole figures and inverse pole figures. The X-ray measurements were performed at theta/theta X'Pert PRO diffractometer with Cr X-ray tube. Observed data were processed by software packages GSAS and X'Pert Texture. Our results can be summarized as follows: (i) Samples prefer orientation of planes (100) and (110) perpendicular to rolling direction. (ii) The position of the basal poles is tilted by 30° from the normal direction toward the transverse direction. (iii) Samples prefer orientation of planes (102) and (103) perpendicular to normal direction. (iv) Level of resulting texture increases with deformation. The obtained results are characteristic for zirconium.

  7. Direct Modeling of X-Ray Diffraction Pattern from Contracting Skeletal Muscle

    PubMed Central

    Koubassova, Natalia A.; Bershitsky, Sergey Y.; Ferenczi, Michael A.; Tsaturyan, Andrey K.

    2008-01-01

    A direct modeling approach was used to quantitatively interpret the two-dimensional x-ray diffraction patterns obtained from contracting mammalian skeletal muscle. The dependence of the calculated layer line intensities on the number of myosin heads bound to the thin filaments, on the conformation of these heads and on their mode of attachment to actin, was studied systematically. Results of modeling are compared to experimental data collected from permeabilized fibers from rabbit skeletal muscle contracting at 5°C and 30°C and developing low and high isometric tension, respectively. The results of the modeling show that: i), the intensity of the first actin layer line is independent of the tilt of the light chain domains of myosin heads and can be used as a measure of the fraction of myosin heads stereospecifically attached to actin; ii), during isometric contraction at near physiological temperature, the fraction of these heads is ∼40% and the light chain domains of the majority of them are more perpendicular to the filament axis than in rigor; and iii), at low temperature, when isometric tension is low, a majority of the attached myosin heads are bound to actin nonstereospecifically whereas at high temperature and tension they are bound stereospecifically. PMID:18539638

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

    SciTech Connect

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

    2009-09-01

    A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts.

  9. X-ray spectral line coincidences between fluorine VIII (and IX) and transition metal lines

    SciTech Connect

    Charatis, G.; Rockett, P.D.; Burkhalter, P.G.

    1983-01-01

    X-ray spectroscopy was performed in the 12 to 15 A region, recording L-shell lines from selected laser-irradiated transition metals. Line coincidences and near coincidences were identified between Fe, Cr, Mn, and Ni L-spectra, and F VIII and F IX K-shell lines. Wavelengths were determined to accuracies of 1 to 3 mA and will be utilized in selecting potential pumping candidates in future x-ray lasing schemes. High-resolution x-ray spectra were collected under controlled illumination and target conditions using 1.05 ..mu..m and 0.527 ..mu..m laser excitation with the KMS CHROMA laser.

  10. A geometry for sub-nanosecond X-ray diffraction from laser-shocked polycrystalline foils

    SciTech Connect

    Wark, Justin; Higginbotham, Andrew; Kimminau, Giles; Murphy, William; Nagler, Bob; Whitcher, Thomas; Hawreliak, James; Kalantar, Dan; Butterfield, Martin; El-Dasher, Bassem; McNaney, James; Milathianaki, Despina; Lorenzana, Hector; Remington, Bruce; Davies, Huw; Thornton, Lee; Park, Nigel; Lukezic, Stan

    2007-12-12

    In situ picosecond X-ray diffraction has proved to be a useful tool in furthering our understanding of the response of shocked crystals at the lattice level. To date the vast majority of this work has used single crystals as the shocked samples, owing to their diffraction efficiency, although the study of the response of polycrystalline samples is clearly of interest for many applications. We present here the results of experiments to develop sub-nanosecond powder/polycrystalline diffraction using a cylindrical pinhole camera. By allowing the incident X-ray beam to impinge on the sample at non-normal angles, the response of grains making a variety of angles to the shock propagation direction can potentially be interrogated.

  11. Apparatus for X-ray diffraction microscopy and tomography of cryo specimens

    DOE PAGESBeta

    Beetz, T.; Howells, M. R.; Jacobsen, C.; Kao, C. -C.; Kirz, J.; Lima, E.; Mentes, T. O.; Miao, H.; Sanchez-Hanke, C.; Sayre, D.; et al

    2005-03-14

    An apparatus for diffraction microscopy of biological and materials science specimens is described. In this system, a coherent soft X-ray beam is selected with a pinhole, and the illuminated specimen is followed by an adjustable beamstop and CCD camera to record diffraction data from non-crystalline specimens. In addition, a Fresnel zone plate can be inserted to allow for direct imaging. The system makes use of a cryogenic specimen holder with cryotransfer capabilities to allow frozen hydrated specimens to be loaded. The specimen can be tilted over a range of ± 80 ° degrees for three-dimensional imaging; this is done bymore » computer-controlled motors, enabling automated alignment of the specimen through a tilt series. The system is now in use for experiments in soft X-ray diffraction microscopy.« less

  12. Transient x-ray diffraction with simultaneous imaging under high strain-rate loading

    NASA Astrophysics Data System (ADS)

    Fan, Duan; Luo, Sheng-Nian; The Peac Institute of Multiscale Sciences Team

    2015-06-01

    Real time, in situ, multiframe, diffraction, and imaging measurements on bulk samples under high and ultrahigh strain-rate loading are highly desirable for micro- and mesoscale sciences. We present an experimental demonstration of multiframe transient x-ray diffraction (TXD) along with simultaneous imaging under high strain-rate loading at the Advanced Photon Source beamline 32ID. The feasibility study utilizes high strain-rate Hopkinson bar loading on a Mg alloy. The exposure time in TXD is 2-3 μs, and the frame interval is 26.7-62.5 μs. Various dynamic deformation mechanisms are revealed by TXD, including lattice expansion or compression, crystal plasticity, grain or lattice rotation, and likely grain refinement, as well as considerable anisotropy in deformation. Dynamic strain fields are mapped via x-ray digital image correlation, and are consistent with the diffraction measurements and loading histories.

  13. Transient x-ray diffraction with simultaneous imaging under high strain-rate loading

    SciTech Connect

    Fan, D.; E, J. C.; Zhao, F.; Luo, S. N.; Lu, L.; Li, B.; Qi, M. L.; Sun, T.; Fezzaa, K.; Chen, W.

    2014-11-15

    Real time, in situ, multiframe, diffraction, and imaging measurements on bulk samples under high and ultrahigh strain-rate loading are highly desirable for micro- and mesoscale sciences. We present an experimental demonstration of multiframe transient x-ray diffraction (TXD) along with simultaneous imaging under high strain-rate loading at the Advanced Photon Source beamline 32ID. The feasibility study utilizes high strain-rate Hopkinson bar loading on a Mg alloy. The exposure time in TXD is 2–3 μs, and the frame interval is 26.7–62.5 μs. Various dynamic deformation mechanisms are revealed by TXD, including lattice expansion or compression, crystal plasticity, grain or lattice rotation, and likely grain refinement, as well as considerable anisotropy in deformation. Dynamic strain fields are mapped via x-ray digital image correlation, and are consistent with the diffraction measurements and loading histories.

  14. Single-particle structure determination by correlations of snapshot X-ray diffraction patterns.

    PubMed

    Starodub, D; Aquila, A; Bajt, S; Barthelmess, M; Barty, A; Bostedt, C; Bozek, J D; Coppola, N; Doak, R B; Epp, S W; Erk, B; Foucar, L; Gumprecht, L; Hampton, C Y; Hartmann, A; Hartmann, R; Holl, P; Kassemeyer, S; Kimmel, N; Laksmono, H; Liang, M; Loh, N D; Lomb, L; Martin, A V; Nass, K; Reich, C; Rolles, D; Rudek, B; Rudenko, A; Schulz, J; Shoeman, R L; Sierra, R G; Soltau, H; Steinbrener, J; Stellato, F; Stern, S; Weidenspointner, G; Frank, M; Ullrich, J; Strüder, L; Schlichting, I; Chapman, H N; Spence, J C H; Bogan, M J

    2012-01-01

    Diffractive imaging with free-electron lasers allows structure determination from ensembles of weakly scattering identical nanoparticles. The ultra-short, ultra-bright X-ray pulses provide snapshots of the randomly oriented particles frozen in time, and terminate before the onset of structural damage. As signal strength diminishes for small particles, the synthesis of a three-dimensional diffraction volume requires simultaneous involvement of all data. Here we report the first application of a three-dimensional spatial frequency correlation analysis to carry out this synthesis from noisy single-particle femtosecond X-ray diffraction patterns of nearly identical samples in random and unknown orientations, collected at the Linac Coherent Light Source. Our demonstration uses unsupported test particles created via aerosol self-assembly, and composed of two polystyrene spheres of equal diameter. The correlation analysis avoids the need for orientation determination entirely. This method may be applied to the structural determination of biological macromolecules in solution. PMID:23232406

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

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

  16. Apparatus for X-ray diffraction microscopy and tomography of cryo specimens

    SciTech Connect

    Beetz, T.; Howells, M. R.; Jacobsen, C.; Kao, C. -C.; Kirz, J.; Lima, E.; Mentes, T. O.; Miao, H.; Sanchez-Hanke, C.; Sayre, D.; Shapiro, D.

    2005-03-14

    An apparatus for diffraction microscopy of biological and materials science specimens is described. In this system, a coherent soft X-ray beam is selected with a pinhole, and the illuminated specimen is followed by an adjustable beamstop and CCD camera to record diffraction data from non-crystalline specimens. In addition, a Fresnel zone plate can be inserted to allow for direct imaging. The system makes use of a cryogenic specimen holder with cryotransfer capabilities to allow frozen hydrated specimens to be loaded. The specimen can be tilted over a range of ± 80 ° degrees for three-dimensional imaging; this is done by computer-controlled motors, enabling automated alignment of the specimen through a tilt series. The system is now in use for experiments in soft X-ray diffraction microscopy.

  17. Transient x-ray diffraction with simultaneous imaging under high strain-rate loading

    PubMed Central

    Fan, D.; Lu, L.; Li, B.; Qi, M. L.; E, J. C.; Zhao, F.; Sun, T.; Fezzaa, K.; Chen, W.; Luo, S. N.

    2014-01-01

    Real time, in situ, multiframe, diffraction, and imaging measurements on bulk samples under high and ultrahigh strain-rate loading are highly desirable for micro- and mesoscale sciences. We present an experimental demonstration of multiframe transient x-ray diffraction (TXD) along with simultaneous imaging under high strain-rate loading at the Advanced Photon Source beamline 32ID. The feasibility study utilizes high strain-rate Hopkinson bar loading on a Mg alloy. The exposure time in TXD is 2–3 μs, and the frame interval is 26.7–62.5 μs. Various dynamic deformation mechanisms are revealed by TXD, including lattice expansion or compression, crystal plasticity, grain or lattice rotation, and likely grain refinement, as well as considerable anisotropy in deformation. Dynamic strain fields are mapped via x-ray digital image correlation, and are consistent with the diffraction measurements and loading histories. PMID:25430119

  18. High-pressure X-ray diffraction studies of potassium chlorate

    SciTech Connect

    Pravica, Michael; Bai, Ligang; Bhattacharya, Neelanjan

    2012-03-15

    Two static high-pressure X-ray diffraction (XRD) studies of potassium chlorate have been performed at pressures of up to {approx}14.3 GPa in a diamond anvil cell at ambient temperature using the 16 ID-B undulator beamline at the Advanced Photon Source for the X-ray source. The first experiment was conducted to ascertain decomposition rates of potassium chlorate as a function of pressure. Below 2 GPa, the sample was observed to decompose rapidly in the presence of the X-ray beam and release oxygen. Above 2 GPa (near the phase I phase II transition), the decomposition rate dramatically slowed so that good quality XRD patterns could be acquired. This suggests a phase-dependent decomposition rate. In the second study, X-ray diffraction spectra were collected at pressures from 2 to 14.3 GPa by aligning virgin portions of the sample into the focused X-ray beam at each pressure. The results suggest the co-existence of mixed monoclinic (I) and rhombohedral (II) phases of potassium chlorate near 2 GPa. At pressures beyond 4 GPa, the XRD patterns show a very good fit to KClO{sub 3} in the rhombohedral phase with space group R3m, in agreement with earlier studies. No further phase transitions were observed with pressure. Decompression of the sample to ambient pressure indicated mixed phases I and II coupled with a small amount of synchrotron X-ray-induced decomposition product. The equation of state within this pressure regime has been determined.

  19. Limit of Detection in X-ray Diffraction Measurements of Tissue Equivalent Samples

    NASA Astrophysics Data System (ADS)

    Zheng, Y.; Vassiljev, N.; Konstantinidis, A.; Griffiths, J.; Speller, R.

    2015-09-01

    There is a suggestion of a new approach to mammography whereby following a conventional mammogram, the radiologist could interrogate suspicious regions using X-ray diffraction whilst the patient is still present and to establish the true extent of disease. A starting point for this work is to quantify the minimum detectable amount of breast cancer within a realistic thickness phantom. Perspex has a similar diffraction pattern to healthy breast tissue whilst water is similar to breast tumour, hence these two materials are used as tissue equivalent test objects for X-ray diffraction measurements. The preliminary results show linear agreement between the ratio of Perspex to water and the ratio of the diffraction peak intensities at 0.7 nm-1 and 1.5 nm-1. The minimum detectable limit for a component of the two ‘tissue’ mix was found to be 4.1%. This suggests that X-ray diffraction can be used to quantify tissue like mixtures down to the 4.1% / 95.9% mix level and hence has a strong potential for delineating the extent of infiltration disease.

  20. Dynamical X-ray Diffraction from In x Ga1- x As Heterostructures with Dislocations

    NASA Astrophysics Data System (ADS)

    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.

  1. Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

    NASA Astrophysics Data System (ADS)

    Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

    2013-12-01

    Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed.

  2. Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

    NASA Astrophysics Data System (ADS)

    Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

    2014-09-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

  3. Study of X-ray diffraction from a surface acoustic wave in the grazing geometry with allowance for the curvature of the unperturbed crystal surface

    SciTech Connect

    Mkrtchyan, A. R. Kocharyan, V. R.; Levonyan, L. V.; Khachaturyan, G. K.

    2006-12-15

    Fresnel X-ray diffraction from a concave crystal surface in the presence of a surface acoustic wave (SAW) has been considered for grazing angles of incidence in noncoplanar symmetric Laue geometry. It is shown that the main peak and diffraction satellites are focused at different distances from a crystal. The effect of deviation from the Bragg angle, the spectral line width, and the SAW amplitude on the X-ray diffraction pattern has been analyzed. It is established that the contrast of an X-ray diffraction pattern of an SAW in Bragg-Laue grazing geometry is related to the character of irregularities of the crystal surface, and the pattern details depend on the measurement mode. The sensitivity of the method is about a nanometer. The focal image of the SAW serves as a scale landmark for determining the crystal surface characteristics.

  4. Synchrotron-based ultrafast x-ray diffraction at high repetition rates.

    PubMed

    Navirian, H; Shayduk, R; Leitenberger, W; Goldshteyn, J; Gaal, P; Bargheer, M

    2012-06-01

    We present a setup for ultrafast x-ray diffraction (UXRD) based at the storage ring BESSY II, in particular, a pump laser that excites the sample using 250 fs laser-pulses at repetition rates ranging from 208 kHz to 1.25 MHz. We discuss issues connected to the high heat-load and spatio-temporal alignment strategies in the context of a UXRD experiment at high repetition rates. The spatial overlap between laser pump and x-ray probe pulse is obtained with 10 μm precision and transient lattice changes can be recorded with an accuracy of δa/a(0) = 10(-6). We also compare time-resolved x-ray diffraction signals from a laser excited LSMO/STO superlattice with phonon dynamics simulations. From the analysis we determine the x-ray pulse duration to 120 ps in standard operation mode and below 10 ps in low-α mode. PMID:22755618

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

    PubMed

    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

  6. Toward diffraction-limited lightweight x-ray optics for astronomy

    NASA Astrophysics Data System (ADS)

    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.

  7. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements.

    PubMed

    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

    2012-01-01

    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 analysis(1). 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 information(1-4). 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 technology(5) should enable structural determination from submicrometre protein crystals with atomic resolution. PMID:24078834

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

    PubMed Central

    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 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

  9. Small-angle X-ray diffraction investigation of twinned opal-like structures

    NASA Astrophysics Data System (ADS)

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

    2012-10-01

    Small-angle X-ray diffraction from synthetic opal films has been investigated as a function of the orientation of the sample. All the observed ( hkl) diffraction reflections have been interpreted. The reconstruction of the reciprocal lattice of the studied opal films has been carried out. The diffraction patterns and scattering intensity profiles along chains of reciprocal lattice points have been calculated. It has been shown that, in the reconstructed reciprocal lattice of the opal films, the appearance of chains of partially overlapping nodes that are oriented along the direction Γ → L is caused by two factors: the small thickness of the film and the existence of stacking faults in it.

  10. Dynamic crystal rotation resolved by high-speed synchrotron X-ray Laue diffraction.

    PubMed

    Huang, J W; E, J C; Huang, J Y; Sun, T; Fezzaa, K; Luo, S N

    2016-05-01

    Dynamic compression experiments are performed on single-crystal Si under split Hopkinson pressure bar loading, together with simultaneous high-speed (250-350 ns resolution) synchrotron X-ray Laue diffraction and phase-contrast imaging. A methodology is presented which determines crystal rotation parameters, i.e. instantaneous rotation axes and angles, from two unindexed Laue diffraction spots. Two-dimensional translation is obtained from dynamic imaging by a single camera. High-speed motion of crystals, including translation and rotation, can be tracked in real time via simultaneous imaging and diffraction. PMID:27140150

  11. X-ray diffraction analysis of titanium tritide film during 1600 days

    NASA Astrophysics Data System (ADS)

    Xiaosong, Zhou; Xinggui, Long; Lin, Zhang; Shuming, Peng; Shunzhong, Luo

    2010-01-01

    The generation and accumulation of 3He by tritium decay modified the physical and chemical properties of tritides. Here the evolution of lattice defects in long-aged titanium tritide films is investigated by X-ray diffraction and changes in the positions, intensities and line shapes of diffraction peaks have been determined over a period of about 1600 days (>4 years). Texture effects are also observed by biased intensities in standard θ-2θ scans. The results show that the TiT1.5 film keeps an fcc structure during 1600 days and reveals an hkl-dependent unit-cell expansion and line width broadening which are interpreted in terms of isolated tetrahedral interstitial 3He atoms and isolated bubble growth models by dislocation loop-punching or dislocation dipole expansion combined with Krivoglaz theory. In the first 12 days of aging, isolated tetrahedral interstitial 3He atoms or 3He clusters are formed, then interstitial 3He atoms diffuse into (1 1 1) planes and precipitate into clusters. The spontaneous formation of Frenkel pairs, the self-interstitial atoms produced are built into dislocations resulting in formation platelet bubbles and dislocation dipoles between 12 and 27 days. Above 27 days, multiple stages of 3He bubbles growth appear: (1) between 27 and 85 days platelet helium bubbles growth by dislocation dipoles expansion, (2) between 85 and 231 days the transition from platelet bubbles to sphere bubbles by loop emission, (3) after 231 days sphere bubbles growth by dislocation loop-punching and probably formation of sub-grain boundaries by dislocation rearrangement.

  12. Quantitative Imaging of Single Unstained Magnetotactic Bacteria by Coherent X-ray Diffraction Microscopy.

    PubMed

    Fan, Jiadong; Sun, Zhibin; Zhang, Jian; Huang, Qingjie; Yao, Shengkun; Zong, Yunbing; Kohmura, Yoshiki; Ishikawa, Tetsuya; Liu, Hong; Jiang, Huaidong

    2015-06-16

    Novel coherent diffraction microscopy provides a powerful lensless imaging method to obtain a better understanding of the microorganism at the nanoscale. Here we demonstrated quantitative imaging of intact unstained magnetotactic bacteria using coherent X-ray diffraction microscopy combined with an iterative phase retrieval algorithm. Although the signal-to-noise ratio of the X-ray diffraction pattern from single magnetotactic bacterium is weak due to low-scattering ability of biomaterials, an 18.6 nm half-period resolution of reconstructed image was achieved by using a hybrid input-output phase retrieval algorithm. On the basis of the quantitative reconstructed images, the morphology and some intracellular structures, such as nucleoid, polyβ-hydroxybutyrate granules, and magnetosomes, were identified, which were also confirmed by scanning electron microscopy and energy dispersive spectroscopy. With the benefit from the quantifiability of coherent diffraction imaging, for the first time to our knowledge, an average density of magnetotactic bacteria was calculated to be ∼1.19 g/cm(3). This technique has a wide range of applications, especially in quantitative imaging of low-scattering biomaterials and multicomponent materials at nanoscale resolution. Combined with the cryogenic technique or X-ray free electron lasers, the method could image cells in a hydrated condition, which helps to maintain their natural structure. PMID:26006162

  13. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    SciTech Connect

    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

    2015-04-30

    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.

  14. The Scherrer equation and the dynamical theory of X-ray diffraction.

    PubMed

    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

  15. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    DOE PAGESBeta

    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; et al

    2015-04-30

    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, femtosecondmore » 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.« less

  16. Identification of inversion domains in KTiOPO{sub 4}via resonant X-ray diffraction

    SciTech Connect

    Fabrizi, Federica; Thomas, Pamela A.; Nisbet, Gareth; Collins, Stephen P.

    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)

  17. X-ray Diffraction Studies of the Thick Filament in Permeabilized Myocardium from Rabbit

    SciTech Connect

    Xu,S.; Martyn, D.; Zaman, J.; Yu, L.

    2007-01-01

    Low angle x-ray diffraction patterns from relaxed permeabilized rabbit cardiac trabeculae and psoas muscle fibers were compared. Temperature was varied from 25{sup o}C to 5{sup o}C at 200 mM and 50 mM ionic strengths ({mu}), respectively. Effects of temperature and {mu} on the intensities of the myosin layer lines (MLL), the equatorial intensity ratio I{sub 1,1}/I{sub 1,0}, and the spacing of the filament lattice are similar in both muscles. At 25{sup o}C, particularly at {mu} = 50 mM, the x-ray patterns exhibited up to six orders of MLL and sharp meridional reflections, signifying that myosin heads (cross-bridges) are distributed in a well-ordered helical array. Decreasing temperature reduced MLL intensities but increased I{sub 1,1}/I{sub 1,0}. Decreases in the MLL intensities indicate increasing disorder in the distribution of cross-bridges on the thick filaments surface. In the skeletal muscle, order/disorder is directly correlated with the hydrolysis equilibrium of ATP by myosin, [M.ADP.P{sub i}]/[M.ATP]. Similar effects of temperature on MLL and similar biochemical ATP hydrolysis pathway found in both types of muscles suggest that the order/disorder states of cardiac cross-bridges may well be correlated with the same biochemical and structural states. This implies that in relaxed cardiac muscle under physiological conditions, the unattached cross-bridges are largely in the M.ADP.P{sub i} state and with the lowering of the temperature, the equilibrium is increasingly in favor of [M.ATP] and [A.M.ATP]. There appear to be some differences in the diffraction patterns from the two muscles, however. Mainly, in the cardiac muscle, the MLL are weaker, the I{sub 1,1}/I{sub 1,0} ratio tends to be higher, and the lattice spacing D{sub 10}, larger. These differences are consistent with the idea that under a wide range of conditions, a greater fraction of cross-bridges is weakly bound to actin in the myocardium.

  18. X-ray Diffraction Studies of the Thick Filament in Permeabilized Myocardium from Rabbit

    SciTech Connect

    Xu,S.; Martyn, D.; Zaman, J.; Yu, L.

    2006-01-01

    Low angle x-ray diffraction patterns from relaxed permeabilized rabbit cardiac trabeculae and psoas muscle fibers were compared. Temperature was varied from 25{sup o}C to 5{sup o}C at 200 mM and 50 mM ionic strengths ({mu}), respectively. Effects of temperature and {mu} on the intensities of the myosin layer lines (MLL), the equatorial intensity ratio I{sub 1,1}/I{sub 1,0}, and the spacing of the filament lattice are similar in both muscles. At 25{sup o}C, particularly at {mu} = 50 mM, the x-ray patterns exhibited up to six orders of MLL and sharp meridional reflections, signifying that myosin heads (cross-bridges) are distributed in a well-ordered helical array. Decreasing temperature reduced MLL intensities but increased I{sub 1,1}/I{sub 1,0}. Decreases in the MLL intensities indicate increasing disorder in the distribution of cross-bridges on the thick filaments surface. In the skeletal muscle, order/disorder is directly correlated with the hydrolysis equilibrium of ATP by myosin, [M.ADP.P{sub i}]/[M.ATP]. Similar effects of temperature on MLL and similar biochemical ATP hydrolysis pathway found in both types of muscles suggest that the order/disorder states of cardiac cross-bridges may well be correlated with the same biochemical and structural states. This implies that in relaxed cardiac muscle under physiological conditions, the unattached cross-bridges are largely in the M.ADP.P{sub i} state and with the lowering of the temperature, the equilibrium is increasingly in favor of [M.ATP] and [A.M.ATP]. There appear to be some differences in the diffraction patterns from the two muscles, however. Mainly, in the cardiac muscle, the MLL are weaker, the I{sub 1,1}/I{sub 1,0} ratio tends to be higher, and the lattice spacing D{sub 10}, larger. These differences are consistent with the idea that under a wide range of conditions, a greater fraction of cross-bridges is weakly bound to actin in the myocardium.

  19. Bayesian orientation estimate and structure information from sparse single-molecule x-ray diffraction images.

    PubMed

    Walczak, Michał; Grubmüller, Helmut

    2014-08-01

    We developed a Bayesian method to extract macromolecular structure information from sparse single-molecule x-ray free-electron laser diffraction images. The method addresses two possible scenarios. First, using a "seed" structural model, the molecular orientation is determined for each of the provided diffraction images, which are then averaged in three-dimensional reciprocal space. Subsequently, the real space electron density is determined using a relaxed averaged alternating reflections algorithm. In the second approach, the probability that the "seed" model fits to the given set of diffraction images as a whole is determined and used to distinguish between proposed structures. We show that for a given x-ray intensity, unexpectedly, the achievable resolution increases with molecular mass such that structure determination should be more challenging for small molecules than for larger ones. For a sufficiently large number of recorded photons (>200) per diffraction image an M^{1/6} scaling is seen. Using synthetic diffraction data for a small glutathione molecule as a challenging test case, successful determination of electron density was demonstrated for 20000 diffraction patterns with random orientations and an average of 82 elastically scattered and recorded photons per image, also in the presence of up to 50% background noise. The second scenario is exemplified and assessed for three biomolecules of different sizes. In all cases, determining the probability of a structure given set of diffraction patterns allowed successful discrimination between different conformations of the test molecules. A structure model of the glutathione tripeptide was refined in a Monte Carlo simulation from a random starting conformation. Further, effective distinguishing between three differently arranged immunoglobulin domains of a titin molecule and also different states of a ribosome in a tRNA translocation process was demonstrated. These results show that the proposed method is robust and enables structure determination from sparse and noisy x-ray diffraction images of single molecules spanning a wide range of molecular masses. PMID:25215765

  20. Grain orientation measurement of passivated aluminum interconnectsby x-ray micro diffraction

    SciTech Connect

    Chang, Chang-Hwan; Valek, B.C.; Padmore,H.A.; MacDowell, A.A.; Celestre, R.; Marieb, T.; Bravman, J.C.; Koo, Y.M.; Patel, J.R.

    1999-07-01

    The crystallographic orientations of individual grains in apassivated aluminum interconnect line of 0.7-mu m width were investigatedby using an incidentwhite x-ray microbeam at the Advanced Light Source,Berkeley National Laboratory. Intergrain orientation mapping was obtainedwith about 0.05o sensitivity by the micro Laue diffractiontechnique.

  1. X-ray diffraction imaging of metal–oxide epitaxial tunnel junctions made by optical lithography: use of focused and unfocused X-ray beams

    PubMed Central

    Mocuta, Cristian; Barbier, Antoine; Stanescu, Stefan; Matzen, Sylvia; Moussy, Jean-Baptiste; Ziegler, Eric

    2013-01-01

    X-ray diffraction techniques are used in imaging mode in order to characterize micrometre-sized objects. The samples used as models are metal–oxide tunnel junctions made by optical lithography, with lateral sizes ranging from 150 µm down to 10 µm and various shapes: discs, squares and rectangles. Two approaches are described and compared, both using diffraction contrast: full-field imaging (topography) and raster imaging (scanning probe) using a micrometre-sized focused X-ray beam. It is shown that the full-field image gives access to macroscopic distortions (e.g. sample bending), while the local distortions, at the micrometre scale (e.g. tilts of the crystalline planes in the vicinity of the junction edges), can be accurately characterized only using focused X-ray beams. These local defects are dependent on the junction shape and larger by one order of magnitude than the macroscopic curvature of the sample. PMID:23412494

  2. High temperature X-ray diffraction, Raman spectroscopy and dielectric studies on yttrium orthochromites

    NASA Astrophysics Data System (ADS)

    Mall, Ashish Kumar; Garg, Ashish; Gupta, Rajeev

    2016-05-01

    The structural, thermal and dielectric properties of YCrO3 ceramic prepared by solid state reaction method have been investigated by a combination of XRD, Raman spectroscopy and permittivity measurement. The X-ray diffraction spectra shows single phase orthorhombically distorted perovskite structure with Pnma symmetry over a wide range of temperature 300K to 1100K. Impedance spectroscopy study on the sample showed that the dielectric constant, tangent loss and ac conductivity with frequency increases on increasing the temperature. Dielectric measurement shows a relaxor like transition at about 460K. Non-Debye type relaxation is observed with activation energy of 0.25 eV extracted from ac conductivity at 11 kHz frequency. We believe that the oxygen ion vacancies play an important role in conduction processes in addition to polaron hopping at higher temperatures. Raman scattering measurements were performed over a wide temperature range from 300K to 600 K. The line width of the modes due to CrO6 bending and in-plane O2 stretching broadens with increasing temperature.

  3. Spectroscopic and X-ray Diffraction Study of Structural Disorder in Cryomilled and Amorphous Griseofulvin

    SciTech Connect

    A Zarow; B Zhou; X Wang; R Pinal; Z Iqbal

    2011-12-31

    Structural disorder induced by cryogenic milling and by heating to the amorphous phase in the active pharmaceutical ingredient Griseofulvin has been studied using Raman spectroscopy, X-ray powder diffraction (XRPD), and fluorescence spectroscopy. A broad, exciting-frequency-independent scattering background in the Raman spectra and changes in intensities and splitting of some of the Raman lines due to lattice and molecular modes have been observed. In the cryomilled samples this strong background is deconvoluted into two components: one due to lattice disorder induced by cryomilling and the other due to Mie scattering from nanosized crystallites. A single-component background scattering attributed to lattice disorder is seen in the Raman spectrum of the amorphous sample. Fluorescence measurements showed an intrinsic fluorescence signal in as-received Griseofulvin that does not correspond to the inelastic background in the Raman spectra and, moreover, decreases in intensity upon cryomilling, thus excluding an assignment of the Raman background intensity to impurity- or molecular-defect-induced fluorescence. Wide-angle XRPD measurements on cryomilled Griseofulvin shows a broad two-component background consistent with the background-scattering component in the Raman data associated with lattice disorder, but at longer correlation lengths. Persistence of this disorder to even longer lengths is evident in small-angle synchrotron XRPD data on micronized Griseofulvin taken as a function of temperature from the crystalline to the amorphous phase.

  4. Theoretical study of the properties of X-ray diffraction moiré fringes. I

    SciTech Connect

    Yoshimura, Jun-ichi

    2015-05-14

    A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory, where the effect of the Pendellösung intensity oscillation on the moiré pattern is explained in detail. A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general.

  5. Real-time Studies of Shocked Polycrystalline Materials with Single-Pulse X-ray Diffraction

    SciTech Connect

    Dane V. Morgan

    2011-05-25

    Characteristic K-α x-rays used for single-pulse XRD are conventionally produced by a 37-stage high-voltage Marx pulse generator coupled to a vacuum needle-and-washer x-ray diode via coaxial transmission line. A large field-of-view x-ray image plate detection system typically enables observation of several Debye-Scherrer rings. Recently, we have developed a fiber-optic reducer, coupled to a CCD camera, to obtain low-noise, large field-of-view images. The direct beam spot is produced by bremsstrahlung radiation attenuated by a twomillimeter tungsten beam stop. Determination of the direct beam position is necessary to perform the ring integration.

  6. Ultrafast lattice response of photoexcited thin films studied by X-ray diffraction

    PubMed Central

    Herzog, Marc; Bojahr, André; Leitenberger, Wolfram; Hertwig, Andreas; Bargheer, Matias

    2014-01-01

    Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates. PMID:26798784

  7. High-pressure x-ray diffraction and Raman spectra study of indium oxide

    SciTech Connect

    Liu, D.; Lei, W.W.; Zou, B.; Yu, S.D.; Hao, J.; Wang, K.; Liu, B.B.; Cui, Q.L.; Zou, G.T.

    2009-06-30

    High-pressure synchrotron radiation x-ray diffraction and Raman spectroscopy measurements of indium oxide (In{sub 2}O{sub 3}) were carried out at room temperature up to 27.8 and 26.2 GPa, respectively. A pressure-induced phase transition from cubic-phase (Ia{bar 3}) was observed at a pressure above 12.8-15.3 GPa, which disagrees with earlier theoretical prediction (3.8 GPa). According to the x-ray diffraction experimental data, the high-pressure phase is isostructural with hexagonal corundum-type structure (R{bar 3}c symmetry). However, broad peaks observed in Raman spectra suggest that the high-pressure structure is disordered. The volume change from cubic phase to corundum phase is about 4% and the axial ratio c/a in the corundum phase decreases with increasing pressure.

  8. TOPICAL REVIEW Quantitative strain analysis of surfaces and interfaces using extremely asymmetric x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Akimoto, Koichi; Emoto, Takashi

    2010-12-01

    Strain can reduce carrier mobility and the reliability of electronic devices and affect the growth mode of thin films and the stability of nanometer-scale crystals. To control lattice strain, a technique for measuring the minute lattice strain at surfaces and interfaces is needed. Recently, an extremely asymmetric x-ray diffraction method has been developed for this purpose. By employing Darwin's dynamical x-ray diffraction theory, quantitative evaluation of strain at surfaces and interfaces becomes possible. In this paper, we review our quantitative strain analysis studies on native SiO2/Si interfaces, reconstructed Si surfaces, Ni/Si(111)-H interfaces, sputtered III-V compound semiconductor surfaces, high-k/Si interfaces, and Au ion-implanted Si.

  9. Experimental Approaches for Solution X-Ray Scattering And Fiber Diffraction

    SciTech Connect

    Tsuruta, H.; Irving, T.C.

    2009-05-26

    X-ray scattering and diffraction from non-crystalline systems have gained renewed interest in recent years, as focus shifts from the structural chemistry information gained by high-resolution studies to the context of structural physiology at larger length scales. Such techniques permit the study of isolated macromolecules as well as highly organized macromolecular assemblies as a whole under near-physiological conditions. Time-resolved approaches, made possible by advanced synchrotron instrumentation, add a crucial dimension to many of these investigations. This article reviews experimental approaches in non-crystalline X-ray scattering and diffraction that may be used to illuminate important scientific questions such as protein/nucleic acid folding and structure-function relationships in large macromolecular assemblies.

  10. Resonant X-ray diffraction in incommensurately modulated crystals. Symmetry consideration of anisotropic anomalous scattering.

    PubMed

    Ovchinnikova; Dmitrienko

    1999-01-01

    Symmetry restrictions on the intensities and polarization properties of main reflections and their satellites are found for incommensurately modulated crystals in the case of anisotropic anomalous X-ray diffraction near absorption edges. It is shown that the modulation becomes a source of additional anisotropy for each resonant scatterer and induces a modulated behaviour of the susceptibility tensor. The four-dimensional approach is used to calculate the set of possible reflections. It is found that additional ('forbidden') reflections may appear both in the system of main reflections and in the system of satellites. The anisotropy also results in complex azimuthal and polarization properties of each reflection. The displacive modulation is discussed in detail. The ATS reflections corresponding to the resonant X-ray diffraction near the K-edge of iron in pyrrhotite-5.5C are considered. PMID:10927227

  11. X-ray diffraction analysis of multilayer porous InP(001) structure

    SciTech Connect

    Lomov, A. A.; Punegov, V. I.; Vasil'ev, A. L.; Nohavica, D.; Gladkov, P.; Kartsev, A. A.; Novikov, D. V.

    2010-03-15

    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.

  12. Crystallization and preliminary X-ray diffraction analysis of maize aldose reductase

    SciTech Connect

    Kiyota, Eduardo; Sousa, Sylvia Morais de; Santos, Marcelo Leite dos; Costa Lima, Aline da; Menossi, Marcelo; Yunes, José Andrés; Aparicio, Ricardo

    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.

  13. X-ray and neutron diffraction study of nanocrystalline Ti-Ru-Fe-O compounds

    SciTech Connect

    Blouin, M.; Guay, D.; Huot, J.; Schulz, R.; Swainson, I.P.

    1998-11-01

    The effect of adding oxygen on the structure of nanocrystalline Ti-Ru-Fe compounds obtained by high-energy ball-milling has been studied by X-ray and neutron diffraction using a Rietveld refinement analysis. It is shown that oxygen atoms readily oxidize Ti to form various types of titanium oxides depending on the oxygen content. In each case, a simple cubic structure (cP2-CsCl) is also formed during milling but with a concentration higher than expected on the basis of various reaction schemes. Through a detailed analysis of the neutron and X-ray diffraction peaks, it is shown that the 1a site of the CsCl-type unit cell is depleted from Ti atoms by preferential substitution with Fe. At high oxygen concentration, the alloy is a multiphase material containing Ti{sub 2{minus}x}Ru{sub 1+y}Fe{sub 1+z}, Ti oxides, Ru, and Fe.

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

    PubMed Central

    Kriegner, D.; Persson, J.M.; Etzelstorfer, T.; Jacobsson, D.; Wallentin, J.; Wagner, J.B.; Deppert, K.; Borgström, M.T.; Stangl, J.

    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 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. PMID:24089580

  15. Method for characterizing mask defects using image reconstruction from X-ray diffraction patterns

    DOEpatents

    Hau-Riege, Stefan Peter

    2007-05-01

    The invention applies techniques for image reconstruction from X-ray diffraction patterns on the three-dimensional imaging of defects in EUVL multilayer films. The reconstructed image gives information about the out-of-plane position and the diffraction strength of the defect. The positional information can be used to select the correct defect repair technique. This invention enables the fabrication of defect-free (since repaired) X-ray Mo--Si multilayer mirrors. Repairing Mo--Si multilayer-film defects on mask blanks is a key for the commercial success of EUVL. It is known that particles are added to the Mo--Si multilayer film during the fabrication process. There is a large effort to reduce this contamination, but results are not sufficient, and defects continue to be a major mask yield limiter. All suggested repair strategies need to know the out-of-plane position of the defects in the multilayer.

  16. Time Resolved X-Ray Diffraction of Reactive Solids Under Dynamic Loadings

    NASA Astrophysics Data System (ADS)

    Yoo, Choong-Shik

    2015-06-01

    We present novel time-resolved (TR) x-ray diffraction and TR Raman spectroscopy capable of probing structural and chemical evolutions of solids undergoing chemical and phase transformations. These methods are applicable to a wide range of dynamic experiments to study both single event phenomena of solids under thermal, electric or mechanical impact conditions and non-single event phenomena under dynamic-diamond anvil cell (d-DAC) and high frequency pulse (or ramp) laser-heated DAC. In this talk, relevant technology developments are described with several examples of our recent studies on reactive metals and dense molecular systems, which are synergistic to many proposed activities to develop dynamic synchrotron x-ray diffraction capabilities centered at advanced third and fourth generation light sources.

  17. X-ray micro-diffraction studies of heterogeneous interfaces between cementitious materials and geological formations

    NASA Astrophysics Data System (ADS)

    Dähn, R.; Popov, D.; Schaub, Ph.; Pattison, P.; Grolimund, D.; Mäder, U.; Jenni, A.; Wieland, E.

    In the present study the challenge of analyzing complex micro X-ray diffraction (microXRD) patterns from cement-clay interfaces has been addressed. In order to extract the maximum information concerning both the spatial distribution and the crystal structure type associated with each of the many diffracting grains in heterogeneous, polycrystalline samples, an approach has been developed in which microXRD was applied to thin sections which were rotated in the X-ray beam. The data analysis, performed on microXRD patterns collected from a filled vein of a cement-clay interface from the natural analogue in Maqarin (Jordan), and a sample from a two-year-old altered interface between cement and argillaceous rock, demonstrate the potential of this method.

  18. X-ray diffraction studies of phase transformations in heavy-metal fluoride glasses

    NASA Technical Reports Server (NTRS)

    Bansal, N. P.; Doremus, R. H.

    1985-01-01

    Powder X-ray diffraction and differential scanning calorimetry studies of the crystallization properties of five ZrF4-based glass compositions have indicated that the crystalline phase in Zr-Ba-La-Pb fluoride glass is beta-BaZrF6; no such identification of crystal phases was obtainable, however, for the other glasses. Reversible polymorphic phase transformations occur in Zr-Ba-La-Li and Zr-Ba-La-Na fluoride glasses, upon heating to higher temperatures.

  19. Crystallization and preliminary X-ray diffraction studies of aspartic proteinase from Irpex lacteus.

    PubMed

    Kobayashi, H; Kasamo, K; Mizuno, H; Kim, H; Kusakabe, I; Murakami, K

    1992-08-20

    Crystals of ILAP (Irpex lacteus aspartic proteinase) have been obtained by the hanging drop method using ammonium sulfate as a precipitant. The crystals are monoclinic, space group P2(1) with cell dimensions a = 54.5 A, b = 79.6 A, c = 37.5 A, beta = 96.8 degrees. The crystals are quite stable to X-rays and diffract beyond 1.9 A resolution. There is one molecule in the asymmetric unit. PMID:1518059

  20. X-Ray Diffraction Study of Elemental Erbium to 65 GPa

    SciTech Connect

    Pravica, M.G.; Lipinska-Kalita, K.; Quine, Z.; Romano, E.; Nicol, M.F.

    2006-02-02

    We have investigated phase transitions in elemental erbium in a diamond anvil cell up to 65 GPa using x-ray powder diffraction methods. We present preliminary evidence of a series of phase transitions that appear to follow the expected hcp {yields} Sm-type {yields} dhcp {yields} distorted fcc sequence. In particular, we believe that we have evidence for the predicted dhcp {yields} distorted fcc transition between 43 GPa and 65 GPa.

  1. Planar techniques for fabricating X-ray diffraction gratings and zone plates

    NASA Technical Reports Server (NTRS)

    Smith, H. I.; Anderson, E. H.; Hawryluk, A. M.; Schattenburg, M. L.

    1984-01-01

    The state of current planar techniques in the fabrication of Fresnel zone plates and diffraction gratings is reviewed. Among the fabrication techniques described are multilayer resist techniques; scanning electron beam lithography; and holographic lithography. Consideration is also given to: X-ray lithography; ion beam lithography; and electroplating. SEM photographs of the undercut profiles obtained in a type AZ 135OB photoresistor by holographic lithography are provided.

  2. Structure of nanosized materials by high-energy x-ray diffraction : study of titanate nanotubes.

    SciTech Connect

    Gateshki, M.; Chen, Q.; Peng, L.-M.; Chupas, P.; Petkov, V.; Central Michigan Univ.; Peking Univ.

    2007-01-01

    High-energy X-ray diffraction and atomic Pair Distribution Function analysis are employed to determine the atomic-scale structure of titanate nanotubes. It is found that the nanotube walls are built of layers of Ti-O{sub 6} octahedra simular to those observed in crystalline layered titanates. In the nanotubes, however, the layers are bent and not stacked in perfect registry as in the crystal.

  3. A Deeper View of Materials: Coupling electrostatic levitation and high energy x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Goldman, Alan

    2006-03-01

    The ability to measure changes in the atomic scale structure, associated with novel thermophysical properties, will lead to tremendous advances in our understanding of the underlying physics of materials. This talk will focus on the integration of electrostatic levitation (ESL) techniques and high energy x-ray diffraction. The use of high energy x-rays (E > 100 keV) offers several distinct advantages over conventional x-ray methods. First and foremost, high energy x-rays are required for full penetration of the levitated samples, which are typically 2-3 millimeters in diameter. This ensures that the bulk, rather than near-surface, structures are sampled in the measurement. A second important benefit of high energy x-rays lies in the fact that diffraction patterns can be collected over a relatively wide momentum transfer range for a small range of angles. The relatively small range of scattering angles required for most measurements allows the use of area detectors for fast data acquisition while the sample is either held at a constant temperature or during continuous heating/cooling cycles. The latter method is particularly suitable for continuous studies of phase transformations as the sample is heated from room temperature to the liquidus temperature and above, or cooled from high temperatures. This is, perhaps, best illustrated by recent work on the atomic scale structure of deeply undercooled liquid metals and semiconductors, such as silicon, where time resolved (100ms/frame) data have shown that, in contrast to previous structural measurements and several theoretical treatments, there is no evidence for a liquid-liquid phase transition in the undercooled regime.

  4. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

    SciTech Connect

    Lambert, P. K.; Hustedt, C. J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C.; Vecchio, K. S.; Huskins, E. L.; Casem, D. T.; Gruner, S. M.; Tate, M. W.; Philipp, H. T.; Purohit, P.; Weiss, J. T.; Woll, A. R.; Kannan, V.; Ramesh, K. T.; Kenesei, P.; Okasinski, J. S.; Almer, J.

    2014-09-15

    We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼10{sup 3}–10{sup 4} s{sup −1} in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10–20 keV) and is well suited to weakly absorbing materials such as magnesium alloys. The second technique is useful for more strongly absorbing materials, and uses high-energy x-rays (86 keV) and a fast shutter synchronized with the Kolsky bar to produce short (∼40 μs) pulses timed with the arrival of the strain pulse at the specimen, recording the diffraction pattern on a large-format amorphous silicon detector. For both techniques we present sample data demonstrating the ability of these techniques to characterize elastic strains and polycrystalline texture as a function of time during high-rate deformation.

  5. Residual stress characterization of welds and post-weld processes using x-ray diffraction techniques

    NASA Astrophysics Data System (ADS)

    Brauss, Michael E.; Pineault, James A.; Eckersley, John S.

    1998-03-01

    This paper illustrates the importance of residual stress characterization in welds and post weld processes. The failure to characterize residual stresses created during welding and/or post weld processes can lead to unexpected occurrences of stress corrosion cracking, distortion, fatigue cracking as well as instances of over design or over processing. The development of automated residual stress mapping and the availability of portable and fast equipment have now made the characterization of residual stresses using x-ray diffraction practical for process control and optimization. The paper presents examples where x-ray diffraction residual stress characterization techniques were applied on various kinds of welds including arc welds, TIG welds, resistance welds, laser welds and electron beam welds. The nondestructive nature of the x-ray diffraction technique has made the residual stress characterization of welds a useful tool for process optimization and failure analysis, particularly since components can be measured before and after welding and post welding processes. Some examples presented show the residual stresses before and after the application of post weld processes such as shot peening, grinding and heat treatment.

  6. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

    PubMed Central

    Lambert, P. K.; Hustedt, C. J.; Vecchio, K. S.; Huskins, E. L.; Casem, D. T.; Gruner, S. M.; Tate, M. W.; Philipp, H. T.; Woll, A. R.; Purohit, P.; Weiss, J. T.; Kannan, V.; Ramesh, K. T.; Kenesei, P.; Okasinski, J. S.; Almer, J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C.

    2014-01-01

    We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼103–104 s−1 in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10–20 keV) and is well suited to weakly absorbing materials such as magnesium alloys. The second technique is useful for more strongly absorbing materials, and uses high-energy x-rays (86 keV) and a fast shutter synchronized with the Kolsky bar to produce short (∼40 μs) pulses timed with the arrival of the strain pulse at the specimen, recording the diffraction pattern on a large-format amorphous silicon detector. For both techniques we present sample data demonstrating the ability of these techniques to characterize elastic strains and polycrystalline texture as a function of time during high-rate deformation. PMID:25273733

  7. X-Ray Diffraction Analysis of NLO Crystals: Traditional Applications and More New Opportunities

    NASA Technical Reports Server (NTRS)

    Antipin, Mikhail Yu.; Clark, Ronald D.; Nesterov, Vladimir N.

    1998-01-01

    Single crystal X-ray diffraction analysis is one of the more important methods for the molecular and crystal structure determination of matter and therefore it has a great importance in material science including design and engineering of different compounds with non-linear optical (NLO) properties. It was shown in our previous publications that this method provides unique information about molecular structure of NLO compounds, their crystal symmetry and crystal packing arrays, molecular conformation and geometries and many other structural and electronic characteristics that are important for understanding the nature of NLO properties of solids. A very new application of the X-ray diffraction method is related to analysis of the electron density distribution p(r) in crystals and some of its characteristics (atomic and group charges, dipole and higher multipole moments, etc.), that may be obtained directly form the diffraction measurements. In the present work, we will discuss our preliminary low temperature high-resolution X-ray data for the m-nitroaniline (mNA) single crystal (VI). This is one of the "classical" organic NLO materials and electron density distribution analysis in this simple compound has a great scientific interest.

  8. Quantitative energy-dispersive x-ray diffraction for identification of counterfeit medicines: a preliminary study

    NASA Astrophysics Data System (ADS)

    Crews, Chiaki C. E.; O'Flynn, Daniel; Sidebottom, Aiden; Speller, Robert D.

    2015-06-01

    The prevalence of counterfeit and substandard medicines has been growing rapidly over the past decade, and fast, nondestructive techniques for their detection are urgently needed to counter this trend. In this study, energy-dispersive X-ray diffraction (EDXRD) combined with chemometrics was assessed for its effectiveness in quantitative analysis of compressed powder mixtures. Although EDXRD produces lower-resolution diffraction patterns than angular-dispersive X-ray diffraction (ADXRD), it is of interest for this application as it carries the advantage of allowing the analysis of tablets within their packaging, due to the higher energy X-rays used. A series of caffeine, paracetamol and microcrystalline cellulose mixtures were prepared with compositions between 0 - 100 weight% in 20 weight% steps (22 samples in total, including a centroid mixture), and were pressed into tablets. EDXRD spectra were collected in triplicate, and a principal component analysis (PCA) separated these into their correct positions in the ternary mixture design. A partial least-squares (PLS) regression model calibrated using this training set was validated using both segmented cross-validation, and with a test set of six samples (mixtures in 8:1:1 and 5⅓:2⅓:2⅓ ratios) - the latter giving a root-mean square error of prediction (RMSEP) of 1.30, 2.25 and 2.03 weight% for caffeine, paracetamol and cellulose respectively. These initial results are promising, with RMSEP values on a par with those reported in the ADXRD literature.

  9. Femtosecond Diffractive Imaging with a Soft-X-Ray Free-Electron Laser

    SciTech Connect

    Chapman, Henry N.; Barty, Anton: AUTHOR = Bogan, Michael J.; Boutet, Sebastian; Frank, Matthias; Hau-Riege, Stefan P.; Marchesini, Stefano; Woods, Bruce W.; Bajt, Sasa; Benner, W.Henry; London, Richard A.; Plonjes, Elke; Kuhlmann, Marion; Treusch, Rolf; Dusterer, Stefan; Tschentscher, Thomas; Schneider, Jochen R.; Spiller, Eberhard; Moller, Thomas; Bostedt, Christoph; Hoener, Matthias; Shapiro, David A.; /UC, Davis /SLAC /Uppsala U. /LLNL, Livermore /Uppsala U. /Uppsala U. /SLAC /Uppsala U.

    2010-10-07

    Theory predicts that with an ultrashort and extremely bright coherent X-ray pulse, a single diffraction pattern may be recorded from a large macromolecule, a virus, or a cell before the sample explodes and turns into a plasma. Here we report the first experimental demonstration of this principle using the FLASH soft X-ray free-electron laser. An intense 25 fs, 4 x 10{sup 13} W/cm{sup 2} pulse, containing 10{sup 12} photons at 32 nm wavelength, produced a coherent diffraction pattern from a nano-structured non-periodic object, before destroying it at 60,000 K. A novel X-ray camera assured single photon detection sensitivity by filtering out parasitic scattering and plasma radiation. The reconstructed image, obtained directly from the coherent pattern by phase retrieval through oversampling, shows no measurable damage, and extends to diffraction-limited resolution. A three-dimensional data set may be assembled from such images when copies of a reproducible sample are exposed to the beam one by one.

  10. Prediction of Elastic Modulus + Anisotropy Using X-Ray and Electron Backscattered Diffraction Texture Quantification and Ultrasonic (Electromagnetic Acoustic Transducer) Measurements in Aluminum Sheets

    NASA Astrophysics Data System (ADS)

    Davis, C. L.; Strangwood, M.; Potter, M.; Dixon, S.; Morris, P. F.

    2008-03-01

    Crystallographic texture is generally measured using X-ray diffraction, performed off-line using small samples determining near-surface texture only; electron backscattered diffraction (EBSD) can also be used, but only samples relatively small areas. Ultrasonic methods determine elastic property anisotropy and texture, via orientation distribution coefficients (ODCs), and while there is substantial literature comparing ultrasonically determined properties with X-ray or neutron diffraction texture, there is little discussion about texture inhomogeneity (place to place in a sheet or through thickness) and sampling volume effects (X-ray compared to EBSD) on the accuracy of the correlations. In this article, the crystallographic texture of nominally pure aluminum and commercial aluminum alloy sheets has been determined by X-ray diffraction and EBSD and used to calculate the elastic anisotropy, which is then compared to ultrasonic electromagnetic acoustic transducer (EMAT) velocity anisotropy taking into account through-thickness texture variations. Significant and consistent spatial variability in texture occurs in the aluminum sheet samples (sheet edge to center and through thickness). Predictions of elastic anisotropy based on surface texture determination, as characterized by X-ray diffraction or surface EBSD, gave poor correlations with EMAT velocity anisotropy when the sample contained significant through thickness texture variations; however, accounting for this using multiple EBSD scans through thickness gave good correlations.

  11. X-ray diffraction studies of the contractile mechanism in single muscle fibres.

    PubMed

    Lombardi, Vincenzo; Piazzesi, Gabriella; Reconditi, Massimo; Linari, Marco; Lucii, Leonardo; Stewart, Alex; Sun, Yin-Biao; Boesecke, Peter; Narayanan, Theyencheri; Irving, Tom; Irving, Malcolm

    2004-12-29

    The molecular mechanism of muscle contraction was investigated in intact muscle fibres by X-ray diffraction. Changes in the intensities of the axial X-ray reflections produced by imposing rapid changes in fibre length establish the average conformation of the myosin heads during active isometric contraction, and show that the heads tilt during the elastic response to a change in fibre length and during the elementary force generating process: the working stroke. X-ray interference between the two arrays of myosin heads in each filament allows the axial motions of the heads following a sudden drop in force from the isometric level to be measured in situ with unprecedented precision. At low load, the average working stroke is 12 nm, which is consistent with crystallographic studies. The working stroke is smaller and slower at a higher load. The compliance of the actin and myosin filaments was also determined from the change in the axial spacings of the X-ray reflections following a force step, and shown to be responsible for most of the sarcomere compliance. The mechanical properties of the sarcomere depend on both the motor actions of the myosin heads and the compliance of the myosin and actin filaments. PMID:15647164

  12. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques. PMID:21615981

  13. X-ray and neutron diffraction measurements of dislocation density and subgrain size in a friction stir welded aluminum alloy

    SciTech Connect

    Claussen, Bjorn; Woo, Wanchuck; Zhili, Feng; Edward, Kenik; Ungar, Tamas

    2009-01-01

    The dislocation density and subgrain size were determined in the base material and friction-stir welds of 6061-T6 aluminum alloy. High-resolution X-ray diffraction measurement was performed in the base material. The result of the line profile analysis of the X-ray diffraction peak shows that the dislocation density is about 4.5 x 10{sup 14} m{sup 02} and the subgrain size is about 200 nm. Meanwhile, neutron diffraction measurements have been performed to observe the diffraction peaks during friction-stir welding (FSW). The deep penetration capability of the neutron enables us to measure the peaks from the midplane of the Al plate underneath the tool shoulder of the friction-stir welds. The peak broadening analysis result using the Williamson-Hall method shows the dislocation density of about 3.2 x 10{sup 15} m{sup -2} and subgrain size of about 160 nm. The significant increase of the dislocation density is likely due to the severe plastic deformation during FSW. This study provides an insight into understanding the transient behavior of the microstructure under severe thermomechanical deformation.

  14. Multilayer graphene stacks grown by different methods-thickness measurements by X-ray diffraction, Raman spectroscopy and optical transmission

    SciTech Connect

    Tokarczyk, M. Kowalski, G.; Kępa, H.; Grodecki, K.; Drabińska, A.; Strupiński, W.

    2013-12-15

    X-ray diffraction, Raman spectroscopy and Optical absorption estimates of the thickness of graphene multi layer stacks (number of graphene layers) are presented for three different growth techniques. The objective of this work was focused on comparison and reconciliation of the two already widely used methods for thickness estimates (Raman and Absorption) with the calibration of the X-ray method as far as Scherer constant K is concerned and X-ray based Wagner-Aqua extrapolation method.

  15. The effect of specimen surface curvature on x-ray diffraction peak profiles

    NASA Astrophysics Data System (ADS)

    Zhigachev, Andrey O.

    2013-09-01

    The effect of specimen surface curvature on profiles of asymmetric X-ray diffraction peaks obtained using the Bragg-Brentano geometry with a position sensitive detector (PSD) was studied. Asymmetric diffraction peaks were experimentally obtained from cylindrical surfaces with controlled curvature. Peaks were collected for a set of curvature radii, diffraction angles, and materials. A mathematical approach and a computer model for calculations of peak profiles were developed: a general method for computation of peak profiles is consideration of diffraction cones intersection with the PSD surface. Effects of axial and radial divergence, finite sample size, and local surface tilt were included in the model. Calculated peak profiles agree with reflections obtained experimentally at a wide range of curvature radii and diffraction angle values. Computation of important characteristics such as the peak centroid and change in position of the maximum and full-width-half-maximum is provided.

  16. The effect of specimen surface curvature on x-ray diffraction peak profiles.

    PubMed

    Zhigachev, Andrey O

    2013-09-01

    The effect of specimen surface curvature on profiles of asymmetric X-ray diffraction peaks obtained using the Bragg-Brentano geometry with a position sensitive detector (PSD) was studied. Asymmetric diffraction peaks were experimentally obtained from cylindrical surfaces with controlled curvature. Peaks were collected for a set of curvature radii, diffraction angles, and materials. A mathematical approach and a computer model for calculations of peak profiles were developed: a general method for computation of peak profiles is consideration of diffraction cones intersection with the PSD surface. Effects of axial and radial divergence, finite sample size, and local surface tilt were included in the model. Calculated peak profiles agree with reflections obtained experimentally at a wide range of curvature radii and diffraction angle values. Computation of important characteristics such as the peak centroid and change in position of the maximum and full-width-half-maximum is provided. PMID:24089864

  17. Grazing-incidence X-ray diffraction from a crystal with subsurface defects

    SciTech Connect

    Gaevskii, A. Yu. Golentus, I. E.

    2015-03-15

    The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaks are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.

  18. PREFACE: XTOP 2004 -- 7th Biennial Conference on High Resolution X-Ray Diffraction and Imaging

    NASA Astrophysics Data System (ADS)

    Holý, Vaclav

    2005-05-01

    The 7th Biennial Conference on High Resolution X-Ray Diffraction and Imaging (XTOP 2004) was held in the Prague suburb of Pruhonice, Czech Republic, during 7-10 September 2004. It was organized by the Czech and Slovak Crystallographic Association in cooperation with the Institute of Physics, Academy of Sciences of the Czech Republic, Prague, Masaryk University, Brno, and Charles University, Prague. XTOP 2004 took place just after EPDIC IX (European Powder Diffraction Conference) organised in Prague by the same Association during 2-5 September 2004. The Organizing Committee was supported by an International Programme Committee including about 20 prominent scientists from several European and overseas countries, whose helpful suggestions for speakers are acknowledged. The conference was sponsored by the International Union of Crystallography and by several industrial sponsors; this sponsorship allowed us to support about 20 students and young scientists. In total, 147 official delegates and 8 accompanying persons from 16 countries of three continents attended our conference. The scientific programme of the conference was divided into 11 half-day sessions and 2 poster sessions. The participants presented 147 accepted contributions; of these 9 were 45-minute long invited talks, 34 were 20-minute oral presentations and 104 were posters. All posters were displayed for the whole meeting to ensure maximum exposure and interaction between delegates. We followed the very good experience from the previous conference, XTOP 2002, and also organized pre-conference tutorial lectures presented by experts in the field: `Imaging with hard synchrotron radiation' (J Härtwig, Grenoble), `High-resolution x-ray diffractometry: determination of strain and composition' (J Stangl, Linz), `X-ray grazing-incidence scattering from surfaces and nanostructures' (U Pietsch, Potsdam) and `Hard x-ray optics' (J Hrdý, Prague). According to the recommendation of the International Program Committee, the invited lectures covered a broader field than the original conference subject, namely coherent speckle diffraction (I Robinson, Urbana), scattering from soft-matter films (W de Jeu, Amsterdam), femtosecond diffraction (J Wark, Oxford), magnetic soft x-ray microscopy (P Fischer, Stuttgart), x-ray standing-wave imaging (J Zegenhagen, Grenoble), new trends in hard x-ray imaging (J Baruchel, Grenoble), anomalous x-ray scattering from nanostructures, (T Schülli, Grenoble), in-situ x-ray scattering (G Renaud, Grenoble) and x-ray waveguides (W Jark, Trieste). The topics of the oral presentations and posters can be divided into two large groups, namely x-ray imaging and x-ray diffraction. In the first group, the contributions concentrated on new developments in methods and instrumentation, including in-situ imaging, phase-contrast imaging and three-dimensional imaging. In the second group, attention was paid to anomalous scattering methods and scattering from thin films and nanostructures. The full list of all contributions together with their abstracts are available at the website http://www.xray.cz/xtop. During one session, Professor Andrew Lang, one of the pioneers of x-ray topography who gave his name to the popular topographic technique, and honorary guest of XTOP 2004, celebrated his 80th birthday. In a celebration address Professor A Authier reviewed Professor Lang's career and his invaluable contribution to the development of our field. We continue the tradition of previous XTOPs and publish a selection of original contributions from the conference in this special issue of Journal of Physics D: Applied Physics. The papers have been subject to peer review according to the normal practice of the journal. Generally, we observed that a new generation of young and very talented scientists has appeared, who are publishing very interesting and important papers. Therefore, the future prospects of x-ray imaging and high-resolution diffraction are bright and we all look forward to the next XTOP conference, organized by Tilo Baumbach and his group, which will take place in Karlsruhe, Germany, in 2006.

  19. Time-Domain X-ray Diffraction in the Pulsed Laser Heated Diamond Anvil Cell

    NASA Astrophysics Data System (ADS)

    Prakapenka, V.; Goncharov, A. F.; Struzhkin, V.; Kantor, I.; Rivers, M. L.; Dalton, D. A.

    2011-12-01

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell (DAC) at pressure up to 100 GPa and 3500 K. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 microseconds pulse width synchronized with a gated x-ray detector (Pilatus) and time resolved radiometric temperature measurements. For the special APS hybrid mode, the measurements were also synchronized with a 500 ns long bunch carrying 88% of the ring current. This setup enables time domain measurements as a function of temperature in a micrometers time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration samples 4 micrometers thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformity as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. We will show examples of studies of the melting, thermal equation of state, and chemical reactivity. We acknowledge support from NSF EAR-0842057, DOE/ NNSA (CDAC), and EFree, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Award No. DESC0001057. X-ray diffraction measurements were performed at GSECARS (APS) supported by DOE Contract No.W-31-109- Eng-38.

  20. Diffractive imaging at large Fresnel number: Challenge of dynamic mesoscale imaging with hard x rays

    NASA Astrophysics Data System (ADS)

    Barber, John L.; Barnes, Cris W.; Sandberg, Richard L.; Sheffield, Richard L.

    2014-05-01

    Real materials have structure at both the atomic or crystalline scale as well as at interfaces and defects at the larger scale of grains. There is a need for the study of materials at the "mesoscale," the scale at which subgranular physical processes and intergranular organization couple to determine microstructure, crucially impacting constitutive response at the engineering macroscale. Diffractive imaging using photons that can penetrate multiple grains of material would be a transformative technique for the study of the performance of materials in dynamic extremes. Thicker samples imply higher energy photons of shorter wavelength, and imaging of multiple grains implies bigger spot sizes. Such imaging requires the use of future planned and proposed hard x-ray free electron lasers (such as the European XFEL) to provide both the spatial coherence transverse to the large spots and the peak brilliance to provide the short illumination times. The result is that the Fresnel number of the system becomes large and is no longer in the Fraunhofer far-field limit. The interrelated issues of diffractive imaging at large Fresnel number are analyzed, including proof that diffractive imaging is possible in this limit and estimates of the signal-to-noise possible. In addition, derivation of the heating rates for brilliant pulses of x rays are presented. The potential and limitations on multiple dynamic images are derived. This paper will present a study of x-ray interactions with materials in this new regime of spatially coherent but relatively large mesoscale spots at very hard energies. It should provide the theory and design background for the experiments and facilities required to control materials in extreme environments, in particular for the next generation of very-hard-x-ray free electron lasers.

  1. X-ray third-order nonlinear dynamical diffraction in a crystal

    SciTech Connect

    Balyan, M. K.

    2015-12-15

    The dynamic diffraction of an X-ray wave in a crystal with a third-order nonlinear response to external field strength has been theoretically investigated. General equations for the wave propagation in crystal and nonlinear Takagi equations for both ideal and deformed crystals are derived. Integrals of motion are determined for the nonlinear problem of dynamic diffraction. The results of the numerical calculations of reflectivity in the symmetric Laue geometry for an incident plane wave and the intensity distributions on the output crystal surface for a point source are reported as an example.

  2. X-ray third-order nonlinear dynamical diffraction in a crystal

    NASA Astrophysics Data System (ADS)

    Balyan, M. K.

    2015-12-01

    The dynamic diffraction of an X-ray wave in a crystal with a third-order nonlinear response to external field strength has been theoretically investigated. General equations for the wave propagation in crystal and nonlinear Takagi equations for both ideal and deformed crystals are derived. Integrals of motion are determined for the nonlinear problem of dynamic diffraction. The results of the numerical calculations of reflectivity in the symmetric Laue geometry for an incident plane wave and the intensity distributions on the output crystal surface for a point source are reported as an example.

  3. X-ray diffraction from high pressure Ge using synchrotron radiation

    NASA Technical Reports Server (NTRS)

    Baublitz, M., Jr.; Ruoff, A. L.

    1982-01-01

    The high pressure structural phase transition in Ge has been studied using the energy dispersive X-ray diffraction technique and a synchrotron radiation source. Ge was observed to transform to the beta-Sn tetragonal structure in agreement with the earlier results of Jamieson, but the phase transition began at 80 + or - 5 kilobars, a somewhat lower value than generally reported. These experimental diffraction results are compared with the recent self-consistent pseudopotential calculations of Yin and Cohen (1981) and with the observed transition pressure for shock wave loaded Ge.

  4. High resolution X-ray diffraction imaging of lead tin telluride

    NASA Technical Reports Server (NTRS)

    Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Spal, Richard; Simchick, Richard; Fripp, Archibald

    1991-01-01

    High resolution X-ray diffraction images of two directly comparable crystals of lead tin telluride, one Bridgman-grown on Space Shuttle STS 61A and the other terrestrially Bridgman-grown under similar conditions from identical material, present different subgrain structure. In the terrestrial, sample 1 the appearance of an elaborate array of subgrains is closely associated with the intrusion of regions that are out of diffraction in all of the various images. The formation of this elaborate subgrain structure is inhibited by growth in microgravity.

  5. Streaked speckle in Cu{sub 3}Au coherent x-ray diffraction

    SciTech Connect

    Pitney, J. A.; Robinson, I. K.; Vartaniants, I. A.; Appleton, R.; Flynn, C. P.

    2000-11-15

    Coherent x-ray diffraction from the binary alloy Cu{sub 3}Au has speckled superstructure Bragg reflections due to its antiphase domain structure. For nonspecular superstructure reflections, it is possible to vary the diffraction geometry through a range of incidence and exit angles. Under grazing-exit conditions on a prepared Cu{sub 3}Au(111) thin-film sample, the superstructure speckles are found to become highly elongated and rotated on the detector. A detailed geometrical explanation of this behavior is developed to explain the effect.

  6. Time-resolved coherent X-ray diffraction imaging of surface acoustic waves

    PubMed Central

    Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J. R.; Krenner, Hubert J.; Wixforth, Achim; Salditt, Tim

    2014-01-01

    Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length). PMID:25294979

  7. New Approach to Improve X-Ray Diffraction Pattern of Protein Crystal Using UV-Laser Ablative Processing

    NASA Astrophysics Data System (ADS)

    Kitano, Hiroshi; Adachi, Hiroaki; Murakami, Atsutoshi; Matsumura, Hiroyoshi; Takano, Kazufumi; Inoue, Tsuyoshi; Mori, Yusuke; Owa, Soichi; Sasaki, Takatomo

    2004-02-01

    A newly proposed processing technique for protein crystals, Pulsed UV Laser Soft Ablation (PULSA), is found to be practically useful for X-ray diffraction analysis. We experimentally confirmed that a diffraction pattern from a cracked protein crystal was considerably improved by eliminating the damaged section with the PULSA processing. This technique will enable us to easily process protein crystals mounted on X-ray diffraction equipments without any extra mechanical handling of the crystals.

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

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

  9. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    SciTech Connect

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-15

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  10. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    NASA Astrophysics Data System (ADS)

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-01

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  11. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility.

    PubMed

    Gupta, Y M; Turneaure, Stefan J; Perkins, K; Zimmerman, K; Arganbright, N; Shen, G; Chow, P

    2012-12-01

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization∕x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS. PMID:23278003

  12. Analysis of field of view limited by a multi-line X-ray source and its improvement for grating interferometry.

    PubMed

    Du, Yang; Huang, Jianheng; Lin, Danying; Niu, Hanben

    2012-08-01

    X-ray phase-contrast imaging based on grating interferometry is a technique with the potential to provide absorption, differential phase contrast, and dark-field signals simultaneously. The multi-line X-ray source used recently in grating interferometry has the advantage of high-energy X-rays for imaging of thick samples for most clinical and industrial investigations. However, it has a drawback of limited field of view (FOV), because of the axial extension of the X-ray emission area. In this paper, we analyze the effects of axial extension of the multi-line X-ray source on the FOV and its improvement in terms of Fresnel diffraction theory. Computer simulation results show that the FOV limitation can be overcome by use of an alternative X-ray tube with a specially designed multi-step anode. The FOV of this newly designed X-ray source can be approximately four times larger than that of the multi-line X-ray source in the same emission area. This might be beneficial for the applications of X-ray phase contrast imaging in materials science, biology, medicine, and industry. PMID:22729354

  13. A-DNA and B-DNA: Comparing Their Historical X-ray Fiber Diffraction Images

    NASA Astrophysics Data System (ADS)

    Lucas, Amand A.

    2008-05-01

    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 Gosling and by Franklin and Gosling. Their corresponding historical diffraction diagrams played an equally crucial role in the discovery of the primary double-helical structure of the DNA molecule by Watson and Crick in 1953. This paper provides a comparative explanation of the structural content of the two diagrams treated on the same footing. The analysis of the diagrams is supported by the optical transform method with which both A-DNA and B-DNA X-ray images can be simulated optically. The simulations use a simple laser pointer and a dozen optical diffraction gratings, all held on a single diffraction slide. The gratings have been specially designed to pinpoint just which of the structural elements of the molecule is responsible for each of the revealing features of the fiber diffraction images.

  14. A study of X-ray multiple diffraction by means of section topography.

    PubMed

    Kohn, V G; Smirnova, I A

    2015-09-01

    The results of theoretical and experimental study are presented for the question of how the X-ray multiple diffraction in a silicon single crystal influences the interference fringes of section topography for the 400 reflection in the Laue case. Two different cases of multiple diffraction are discovered for zero and very small values of the azimuthal angle for the sample in the form of a plate with the surface normal to the 001 direction. The cases are seen on the same topogram without rotation of the crystal. Accurate computer simulations of the section topogram for the case of X-ray multiple diffraction are performed for the first time. It is shown that the structure of interference fringes on the section topogram in the region of multiple diffraction becomes more complicated. It has a very sharp dependence on the azimuthal angle. The experiment is carried out using a laboratory source under conditions of low resolution over the azimuthal angle. Nevertheless, the characteristic inclination of the interference fringes on the tails of the multiple diffraction region is easily seen. This phenomenon corresponds completely to the computer simulations. PMID:26317194

  15. Nondestructive evaluation of residual stress in short-fiber reinforced plastics by x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Tanaka, Keisuke; Tokoro, Syouhei; Akiniwa, Yoshiaki; Egami, Noboru

    2014-06-01

    The X-ray diffraction method is used to measure the residual stress in injection-molded plates of short-fiber reinforced plastics (SFRP) made of crystalline thermoplastics, polyphenylene sulphide (PPS), reinforced by carbon fibers with 30 mass%. Based on the orientation of carbon fibers, injection molded plates can be modeled as three-layered lamella where the core layer is sandwiched by skin layers. The stress in the matrix in the skin layer was measured using Cr-Kα radiation with the sin2Ψ method. Since the X-ray penetration depth is shallow, the state of stresses measured by X-rays in FRP can be assumed to be plane stress. The X-ray measurement of stress in carbon fibers was not possible because of high texture. A new method was proposed to evaluate the macrostress in SFRP from the measurement of the matrix stress. According to micromechanics analysis of SFRP, the matrix stresses in the fiber direction, σ1m, and perpendicular to the fiber direction, σ2m, and shear stress τ12m can be expressed as the functions of the applied (macro-) stresses, σ1A, σ2A , τ12A as follows: σ1m = α11σ1A +α12σ2A, σ2m = α21σ1A + α22σ2A, τ12m = α66τ12A, where α11 ,α12, α21, α22, α66 are stress-partitioning coefficients. Using skin-layer strips cut parallel, perpendicular and 45° to the molding direction, the stress in the matrix was measured under the uniaxial applied stress and the stress-partitioning coefficients of the above equations were determined. Once these relations are established, the macrostress in SFRP can be determined from the measurements of the matrix stresses by X-rays.

  16. Mineral identification in Colombian coals using Mössbauer spectroscopy and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Fajardo, M.; Mojica, J.; Barraza, J.; Pérez Alcázar, G. A.; Tabares, J. A.

    1999-11-01

    Minerals were identified in three Colombian coal samples from the Southwest of the country using Mössbauer spectroscopy and X-ray diffraction. Original and sink separated coal fractions of specific gravity 1.40 and 1.60 with particle size less than 600 µm were used in the study. Using Mössbauer spectroscopy, the minerals identified in the original coal samples were pyrite jarosite, ankerite, illite and ferrous sulfate, whereas by means of X-ray diffraction, minerals identified were kaolinite, quartz, pyrite, and jarosite. Differences in mineral composition were found in the original and sink separated fractions using both techniques. Mössbauer spectra show that the mineral phases in low concentrations such as illite, ankerite and ferrous sulfate do not always appear in the spectra of sink coals, despite of those minerals occurring in the original coal, due to the fact that they are associated with the organic matter and not liberated in the grinding process. X-ray results show that the peak intensity grows as the specific gravity is increased indicating that the density separation method could be an effective process to clean coal.

  17. X-ray diffraction in the pulsed laser heated diamond anvil cell

    SciTech Connect

    Goncharov, Alexander F.; Prakapenka, Vitali B.; Struzhkin, Viktor V.; Kantor, Innokenty; Rivers, Mark L.; Dalton, D. Allen

    2010-11-03

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2–10 kHz repetition rate, 1064–1075 nm fiber laser with 1–100 μs pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 μm thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.

  18. X-ray diffraction in the pulsed laser heated diamond anvil cell

    SciTech Connect

    Goncharov, Alexander F.; Prakapenka, Vitali B.; Struzhkin, Viktor V.; Kantor, Innokenty; Rivers, Mark L.; Dalton, D. Allen

    2010-11-19

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 {micro}s pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 {micro}m thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.

  19. X-ray diffraction in the pulsed laser heated diamond anvil cell

    SciTech Connect

    Goncharov, Alexander F.; Struzhkin, Viktor V.; Dalton, D. Allen; Prakapenka, Vitali B.; Kantor, Innokenty; Rivers, Mark L.

    2010-11-15

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 {mu}s pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10 000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 {mu}m thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.

  20. Imaging live cell in micro-liquid enclosure by X-ray laser diffraction

    PubMed Central

    Kimura, Takashi; Joti, Yasumasa; Shibuya, Akemi; Song, Changyong; Kim, Sangsoo; Tono, Kensuke; Yabashi, Makina; Tamakoshi, Masatada; Moriya, Toshiyuki; Oshima, Tairo; Ishikawa, Tetsuya; Bessho, Yoshitaka; Nishino, Yoshinori

    2014-01-01

    Emerging X-ray free-electron lasers with femtosecond pulse duration enable single-shot snapshot imaging almost free from sample damage by outrunning major radiation damage processes. In bioimaging, it is essential to keep the sample close to its natural state. Conventional high-resolution imaging, however, suffers from severe radiation damage that hinders live cell imaging. Here we present a method for capturing snapshots of live cells kept in a micro-liquid enclosure array by X-ray laser diffraction. We place living Microbacterium lacticum cells in an enclosure array and successively expose each enclosure to a single X-ray laser pulse from the SPring-8 Angstrom Compact Free-Electron Laser. The enclosure itself works as a guard slit and allows us to record a coherent diffraction pattern from a weakly-scattering submicrometre-sized cell with a clear fringe extending up to a 28-nm full-period resolution. The reconstructed image reveals living whole-cell structures without any staining, which helps advance understanding of intracellular phenomena. PMID:24394916

  1. Structural Study of Trehalose Dihydrate by Neutron and X-ray Diffraction Experiments

    NASA Astrophysics Data System (ADS)

    Miwako Takahashi,; Takuro Kawasaki,; Kunimitsu Kataoka,; Masashi Watanabe,; Yukio Noda,; Ken-ichi Ohshima,

    2010-07-01

    The structure of α,α-trehalose dihydrate was studied by neutron and X-ray diffraction experiments to understand the relation between its superior biological protective function and the role of the hydrogen bond connecting the trehalose molecules. By direct observation of hydrogen using the neutron diffraction method, the nuclear positions and anisotropic thermal parameters of hydrogen atoms are determined accurately. The nuclear positions show clear discrepancies from the centers of the electron cloud of hydrogen determined from the X-ray data. The result is interpreted in terms of a local electric dipole moment in the hydrogen atoms. The magnitude of the dipole moment is markedly large for the hydrogen atoms participating in the hydrogen bond. The detailed electron density distribution has been determined by using X-ray data obtained at 150 K. It clearly shows the electron cloud of hydrogen spreading over the chain of hydrogen bonds. It was found that there is a part where the electron density is very low on the hydrogen bond between water and trehalose molecules, implying a loose connection between them. The mechanism of the biological protective function is discussed from the viewpoint of crystal deformation process through the loose connection.

  2. Microelemental and mineral compositions of pathogenic biomineral concrements: SRXFA, X-ray powder diffraction and vibrational spectroscopy data

    NASA Astrophysics Data System (ADS)

    Moroz, T. N.; Palchik, N. A.; Dar'in, A. V.

    2009-05-01

    X-ray fluorescence analysis using synchrotron radiation (SRXRF), X-ray powder diffraction, infrared and Raman spectroscopy had been applied for determination of microelemental and mineral composition of the kidney stones, gallstones and salivalities from natives of Novosibirsk and Novosibirsk region, Russia. The relationship between mineral, organic and microelemental composition of pathogenic calcilus was shown.

  3. Time-, frequency-, and wavevector-resolved x-ray diffraction from single molecules

    PubMed Central

    Bennett, Kochise; Biggs, Jason D.; Zhang, Yu; Dorfman, Konstantin E.; Mukamel, Shaul

    2014-01-01

    Using a quantum electrodynamic framework, we calculate the off-resonant scattering of a broadband X-ray pulse from a sample initially prepared in an arbitrary superposition of electronic states. The signal consists of single-particle (incoherent) and two-particle (coherent) contributions that carry different particle form factors that involve different material transitions. Single-molecule experiments involving incoherent scattering are more influenced by inelastic processes compared to bulk measurements. The conditions under which the technique directly measures charge densities (and can be considered as diffraction) as opposed to correlation functions of the charge-density are specified. The results are illustrated with time- and wavevector-resolved signals from a single amino acid molecule (cysteine) following an impulsive excitation by a stimulated X-ray Raman process resonant with the sulfur K-edge. Our theory and simulations can guide future experimental studies on the structures of nano-particles and proteins. PMID:24880284

  4. Structure determination of thin CoFe films by anomalous x-ray diffraction

    SciTech Connect

    Gloskovskii, Andrei; Stryganyuk, Gregory; Ouardi, Siham; Fecher, Gerhard H.; Felser, Claudia; Hamrle, Jaroslav; Pistora, Jaromir; Bosu, Subrojati; Saito, Kesami; Sakuraba, Yuya; Takanashi, Koki

    2012-10-01

    This work reports on the investigation of structure-property relationships in thin CoFe films grown on MgO. Because of the very similar scattering factors of Fe and Co, it is not possible to distinguish the random A2 (W-type) structure from the ordered B2 (CsCl-type) structure with commonly used x-ray sources. Synchrotron radiation based anomalous x-ray diffraction overcomes this problem. It is shown that as grown thin films and 300 K post annealed films exhibit the A2 structure with a random distribution of Co and Fe. In contrast, films annealed at 400 K adopt the ordered B2 structure.

  5. Pathway of a damaging mechanism - Analyzing chloride attack by synchrotron based X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Schlegel, M. C.; Stroh, J.; Malaga, K.; Meng, B.; Panne, U.; Emmerling, F.

    2015-06-01

    Typically, the changes of the phase compositions due to the chemical attack are studied in-situ only by chemical analysis or microscopy. In this study, the chloride transport and binding in the cement matrix in different cementitious materials was analyzed by synchrotron based X-ray diffraction (SyXRD) and energy dispersive X-ray spectroscopy (EDX). Sample materials consisting of cement paste were embedded in high concentrated sodium chloride solution over different time spans. Afterwards, the phase and chemical compositions were determined. The high spatial resolution and the information about the chloride distribution offer a detailed view of chloride binding in the cement matrix and allow the conclusions about the degradation mechanisms. The results are discussed related to the influence of different supplementary cementitious materials on the damaging mechanism.

  6. Time-, frequency-, and wavevector-resolved x-ray diffraction from single molecules

    SciTech Connect

    Bennett, Kochise Biggs, Jason D.; Zhang, Yu; Dorfman, Konstantin E.; Mukamel, Shaul

    2014-05-28

    Using a quantum electrodynamic framework, we calculate the off-resonant scattering of a broadband X-ray pulse from a sample initially prepared in an arbitrary superposition of electronic states. The signal consists of single-particle (incoherent) and two-particle (coherent) contributions that carry different particle form factors that involve different material transitions. Single-molecule experiments involving incoherent scattering are more influenced by inelastic processes compared to bulk measurements. The conditions under which the technique directly measures charge densities (and can be considered as diffraction) as opposed to correlation functions of the charge-density are specified. The results are illustrated with time- and wavevector-resolved signals from a single amino acid molecule (cysteine) following an impulsive excitation by a stimulated X-ray Raman process resonant with the sulfur K-edge. Our theory and simulations can guide future experimental studies on the structures of nano-particles and proteins.

  7. Pseudomonoenergetic x-ray diffraction measurements using balanced filters for coherent-scatter computed tomography

    SciTech Connect

    Beath, S. R.; Cunningham, I. A.

    2009-05-15

    Coherent-scatter computed tomography (CSCT) is a method of ''composition'' imaging based on measurements of diffraction patterns from tissues. Use of an x-ray tube degrades scatter pattern angular resolution due to the x-ray spectral width, making it difficult to uniquely identify some materials. The use of two transmission filters with similar atomic numbers (balanced ''Ross filters'') to generate pseudomonoenergetic scatter patterns is described as it applies to CSCT. An analysis of angular-blur mechanisms reveals that focal spot size and beam width are the most important factors determining Bragg-peak width when Er-Tm filters are used. A relative RMS spectral width of 1% can be achieved in the difference spectrum and a Bragg-peak RMS angular width of approximately 0.14 deg. (relative width of 3% at 5 deg. scatter angle) can be achieved with an effective energy of 58 keV.

  8. High-Angular-Resolution Microbeam X-Ray Diffraction with CCD Detector

    SciTech Connect

    Imai, Yasuhiko; Kimura, Shigeru; Sakaia, Akira; Sakata, Osami

    2010-04-06

    We have introduced a CCD-type two-dimensional X-ray detector for a microbeam X-ray diffraction system using synchrotron radiation, so that we can measure local reciprocal space maps (RSM) of samples rapidly. A local RSM of a strain-relaxed SiGe 004 grown on a Si (001) substrate was measured in higher-angular-resolution and faster than a conventional way. The measurement was achieved in 1 h 40 min. with the 2theta resolution of 80 murad and the spatial resolution of 1.4(h)x0.5(v) {mu}m{sup 2}. The introduction of the CCD enabled us to measure RSMs at many points in a sample, that is, the distribution of strain fields and lattice tilts can be revealed in high-angular- and high-spatial-resolution.

  9. Automated high pressure cell for pressure jump x-ray diffraction

    SciTech Connect

    Brooks, Nicholas J.; Gauthe, Beatrice L. L. E.; Templer, Richard H.; Ces, Oscar; Seddon, John M.; Terrill, Nick J.; Rogers, Sarah E.

    2010-06-15

    A high pressure cell for small and wide-angle x-ray diffraction measurements of soft condensed matter samples has been developed, incorporating a fully automated pressure generating network. The system allows both static and pressure jump measurements in the range of 0.1-500 MPa. Pressure jumps can be performed as quickly as 5 ms, both with increasing and decreasing pressures. Pressure is generated by a motorized high pressure pump, and the system is controlled remotely via a graphical user interface to allow operation by a broad user base, many of whom may have little previous experience of high pressure technology. Samples are loaded through a dedicated port allowing the x-ray windows to remain in place throughout an experiment; this facilitates accurate subtraction of background scattering. The system has been designed specifically for use at beamline I22 at the Diamond Light Source, United Kingdom, and has been fully integrated with the I22 beamline control systems.

  10. X-ray diffraction results from Mars Science Laboratory: mineralogy of Rocknest at Gale crater.

    PubMed

    Bish, D L; Blake, D F; Vaniman, D T; Chipera, S J; Morris, R V; Ming, D W; Treiman, A H; Sarrazin, P; Morrison, S M; Downs, R T; Achilles, C N; Yen, A S; Bristow, T F; Crisp, J A; Morookian, J M; Farmer, J D; Rampe, E B; Stolper, E M; Spanovich, N

    2013-09-27

    The Mars Science Laboratory rover Curiosity scooped samples of soil from the Rocknest aeolian bedform in Gale crater. Analysis of the soil with the Chemistry and Mineralogy (CheMin) x-ray diffraction (XRD) instrument revealed plagioclase (~An57), forsteritic olivine (~Fo62), augite, and pigeonite, with minor K-feldspar, magnetite, quartz, anhydrite, hematite, and ilmenite. The minor phases are present at, or near, detection limits. The soil also contains 27 ± 14 weight percent x-ray amorphous material, likely containing multiple Fe(3+)- and volatile-bearing phases, including possibly a substance resembling hisingerite. The crystalline component is similar to the normative mineralogy of certain basaltic rocks from Gusev crater on Mars and of martian basaltic meteorites. The amorphous component is similar to that found on Earth in places such as soils on the Mauna Kea volcano, Hawaii. PMID:24072925

  11. RASOR: an advanced instrument for soft x-ray reflectivity and diffraction.

    PubMed

    Beale, T A W; Hase, T P A; Iida, T; Endo, K; Steadman, P; Marshall, A R; Dhesi, S S; van der Laan, G; Hatton, P D

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (theta, 2theta, and chi) diffractometer with an additional removable rotation (phi) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument. PMID:20687739

  12. X-ray diffraction determination of stress in magnetron-sputtered Permalloy films

    NASA Astrophysics Data System (ADS)

    England, C. D.; Falco, C. M.; Aboaf, J. A.

    1988-04-01

    The stresses in magnetron-sputtered films depend on the deposition parameters. Magnetron-sputtered Permalloy (Ni 81%, Fe 19%) films were deposited onto fused quartz substrates using varying deposition parameters, including argon pressure, substrate bias, deposition rate, and film thickness. A Bragg-Brentano diffractometer was used to find the average stress in the films. A Seemann-Bohlin diffractometer was used to measure the strain either parallel or perpendicular to the magnetic easy axis in the Permalloy film. Kroner x-ray elastic constants were used to calculate the stresses from the strains determined by x-ray diffraction techniques. The average stress in the magnetron-sputtered Permalloy films was highly tensile but could be reduced by the appropriate combination of deposition parameters. The strain difference could also be modified by changing the deposition parameters.

  13. RASOR: An advanced instrument for soft x-ray reflectivity and diffraction

    NASA Astrophysics Data System (ADS)

    Beale, T. A. W.; Hase, T. P. A.; Iida, T.; Endo, K.; Steadman, P.; Marshall, A. R.; Dhesi, S. S.; van der Laan, G.; Hatton, P. D.

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (θ, 2θ, and χ) diffractometer with an additional removable rotation (ϕ) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.

  14. Pseudomonoenergetic x-ray diffraction measurements using balanced filters for coherent-scatter computed tomography.

    PubMed

    Beath, S R; Cunningham, I A

    2009-05-01

    Coherent-scatter computed tomography (CSCT) is a method of "composition" imaging based on measurements of diffraction patterns from tissues. Use of an x-ray tube degrades scatter pattern angular resolution due to the x-ray spectral width, making it difficult to uniquely identify some materials. The use of two transmission filters with similar atomic numbers (balanced "Ross filters") to generate pseudomonoenergetic scatter patterns is described as it applies to CSCT. An analysis of angular-blur mechanisms reveals that focal spot size and beam width are the most important factors determining Bragg-peak width when Er-Tm filters are used. A relative RMS spectral width of 1% can be achieved in the difference spectrum and a Bragg-peak RMS angular width of approximately 0.14 degree (relative width of 3% at 5 degrees scatter angle) can be achieved with an effective energy of 58 keV. PMID:19544803

  15. Linear polarization of the characteristic x-ray lines following inner-shell photoionization of tungsten

    NASA Astrophysics Data System (ADS)

    Kämpfer, T.; Uschmann, I.; Wu, Z. W.; Surzhykov, A.; Fritzsche, S.; Förster, E.; Paulus, G. G.

    2016-03-01

    The linear polarization of the characteristic lines L α1 (3 d5 /2→2 p3 /2 ) and L α2 (3 d3 /2→2 p3 /2) , following inner-shell photoionization of neutral tungsten, is analyzed both experimentally and theoretically. In the experiment, a tungsten target is photoionized by the primary emission of an x-ray tube with incident photon energies in the range of 10.2-30 keV. The σ and π components of the emitted fluorescence are measured by using a spectropolarimeter, based on x-ray diffraction at Bragg angles close to 45∘. The degree of linear polarization of the L α1 and L α2 lines is determined to be +(1.6 ±0.5 )% and -(7 ±2 )% , respectively. In addition, this degree of polarization is calculated within the framework of the density-matrix theory as a function of the incident photon energy. These calculations are in good agreement with the experimental results and show only a weak dependence of the degree of polarization on the energy of the incident photoionizing photon.

  16. Data preparation and evaluation techniques for x-ray diffraction microscopy

    SciTech Connect

    Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; Marchesini, Stefano; Shapiro, David; Turner, Joshua J.; Jacobsen, Chris

    2010-01-01

    The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. In addition, we show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffraction patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.

  17. A novel wafer-scale CMOS APS X-ray detector for breast cancer diagnosis using X-ray diffraction studies

    NASA Astrophysics Data System (ADS)

    Konstantinidis, A.; Zheng, Y.; Philip, D.; Vinnicombe, S.; Speller, R.

    2012-12-01

    The current study uses a novel large area (12.8 cm × 13.1 cm) complementary metal-oxide-semiconductor (CMOS) active pixel sensor (APS) X-ray detector, named Dynamic range Adjustable for Medical Imaging Technology (DynAMITe), for breast cancer diagnosis. The detector consists of two geometrically superimposed grids: a) 2560 × 2624 fine-pitch grid of pixels (50 μm pitch), named Sub-Pixels (SP camera), for low intrinsic noise and high spatial resolution and b) 1280 × 1312 large-pitch grid of pixels (100 μm pitch), named Pixels (P camera), for high dynamic range. X-ray performance characterization measurements show that the detective quantum efficiency (DQE) of the SP camera is in the range 0.7-0.75 at low spatial frequencies using a tungsten (W) anode X-ray source at 28 kV. Hence, the detector is suitable for mammography. Furthermore, we used the SP camera to combine mammograms with angle dispersive X-ray diffraction (ADXRD) measurements in order to apply the X-ray biopsy concept in one examination. The results show that ADXRD technique indicates the presence of cancer in suspicious areas on the mammogram. Hence, it could be used to determine the region affected by cancer and assist in planning surgery. This study is the proof of concept that mammography and ADXRD can be combined in one examination.

  18. Diffraction-Based Techniques For High Contrast X-ray Imaging

    NASA Astrophysics Data System (ADS)

    Peerzada, Lubna Naseem

    Two X-ray diffraction based techniques for high contrast were explored to improve contrast in radiology: diffraction enhanced imaging (DEI) and coherent scatter imaging. DEI produces contrast in images based upon the difference in the X-ray refractive indices of materials or tissues. Two DEI systems were devised. Both were comprised of a conventional polychromatic copper X-ray source, polycapillary collimating optics and two silicon crystals.Lucite step phantoms and nylon tubing were imaged. No fringe effects were observed. The lack of observable edge enhancement may have been due to the optic structure which obscured refraction effects. Better results might have been achieved if a higher resolution detector or phantom of larger step size or larger diameter thin walled tubing had been used. The second technique was coherent scatter X-ray imaging. The purpose of this work was to differentiate between healthy and diseased human breast tissues. For instance, breast carcinoma is known to have a peak coherent scattering angle at 12.2° for Mo Ka radiation at 17.5 keV, whereas fatty tissue peaks around 9°. A system which would be compatible with screening mammography was developed. The system was expanded to include sample scanning to allow for a larger image area. The modulation transfer function was computed for static and scanned images of a resolution phantom. These showed good agreement, indicating that the scanning was properly aligned and timed. Static and scanned images of phantoms were taken and the contrast was calculated for a series of experimental parameters including, grid tilt angle. A complex phantom was also then imaged. It was possible to distinguish tissue-equivalent phantom types. Good contrast resolution scanned images were obtained which is promising for a diagnostic system.

  19. Discovery of an X-ray Violently Variable Broad Absorption Line Quasar

    NASA Technical Reports Server (NTRS)

    Ghosh, Kajal K.; Gutierrez, Carlos M.; Punsly, Brian; Chevallier, Loic; Goncalves, Anabela C.

    2006-01-01

    In this letter, we report on a quasar that is violently variable in the X-rays, XVV. It is also a broad absorption line quasar (BALQSO) that exhibits both high ionization and low ionization UV absorption lines (LoBALQSO). It is very luminous in the X-rays (approximately 10(exp 46) ergs s(sup -l) over the entire X-ray band). Surprisingly, this does not over ionize the LoBAL outflow. The X-rays vary by a factor of two within minutes in the quasar rest frame, which is shorter than 1/30 of the light travel time across a scale length equal to the black hole radius. We concluded that the X-rays are produced in a relativistic jet beamed toward earth in which variations in the Doppler enhancement produce the XVV behavior.

  20. Theory of radial X-ray Diffraction from a Polycrystalline Sample Undergoing Plastic Deformation

    SciTech Connect

    S Karato

    2011-12-31

    Theory of lattice strain in a polycrystalline aggregate under deviatoric stress is extended to include the influence of ongoing plastic deformation. When deviatoric stress is applied to a polycrystalline material at high temperatures (or above the yield stress), applied macroscopic stress is redistributed to individual grains by plastic deformation according to their orientations with respect to the macroscopic stress and plastic anisotropy of a given crystal. This microstress causes elastic deformation of individual grains that can be measured by x-ray diffraction. Consequently, the observed lattice strain depends on two material properties, viscosity (plasticity) and elastic compliance as well as the applied macroscopic stress and the stress-strain distribution among various grains. The influence of plastic deformation on lattice strain is analyzed using an anisotropic and nonlinear power-law constitutive relationship. In this model, the dependence of inferred macroscopic stress on the crystallographic orientation of diffraction plane (hkl) comes from elastic and plastic anisotropy of a crystal. In many materials, plastic anisotropy dominates over elastic anisotropy. This explains the observed large dependence of inferred stress on the diffraction plane and means that the determination of elastic anisotropy is difficult when plastic deformation occurs with anisotropic plasticity. When elastic anisotropy is known, plastic anisotropy of single crystal and/or stress-strain distribution in a deformed polycrystal can be determined from radial x-ray diffraction using the present model. Some examples are presented using the data on MgO.

  1. X-ray diffraction effect from surface acoustic waves traveling on a deposited multilayer

    SciTech Connect

    Dong Jun; Qi Jianxia; Miao Runcai

    2010-04-10

    We investigate the x-ray diffraction effects from surface acoustic waves (SAW) traveling along a multilayer. The diffraction intensity distribution depends on the incidence angle and the multilayer SAW (MLSAW) amplitude. Particularly, a small departure deviating from the Bragg incidence angle at a certain amplitude will produce a larger variation of the intensity distribution. This shows that the diffraction intensity from MLSAW has an extremely high sensitivity to the Bragg incidence angle, which is different from a SAW traveling along a solid surface without deposited layers. By carefully analyzing the relationship between the intensity distribution I and the incidence angle {theta}, the corresponding analytic expression of the intensity distribution is theoretically derived. Our theoretical prediction is in great agreement with the experimental results previously obtained. A theoretical model that can be applied to study the x-ray diffraction effect from MLSAW is developed. The extremely high sensitivity to the Bragg angle will help us in acousto-optic instrument research with MLSAW.

  2. Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction

    PubMed Central

    Hughes, Ronny C.; Coates, Leighton; Blakeley, Matthew P.; Tomanicek, Steve J.; Langan, Paul; Kovalevsky, Andrey Y.; García-Ruiz, Juan M.; Ng, Joseph D.

    2012-01-01

    Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a = 106.11, b = 95.46, c = 113.68 Å, α = γ = 90.0, β = 98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure–function and mechanism studies of IPPase. PMID:23192028

  3. X-ray diffraction study of short-period AlN/GaN superlattices

    SciTech Connect

    Kyutt, R. N. Shcheglov, M. P.; Ratnikov, V. V.; Yagovkina, M. A.; Davydov, V. Yu.; Smirnov, A. N.; Rozhavskaya, M. M.; Zavarin, E. E.; Lundin, V. V.

    2013-12-15

    The structure of short-period hexagonal GaN/AlN superlattices (SLs) has been investigated by X-ray diffraction. The samples have been grown by metalorganic vapor-phase epitaxy (MOVPE) in a horizontal reactor at a temperature of 1050°C on (0001)Al{sub 2}O{sub 3} substrates using GaN and AlN buffer layers. The SL period changes from 2 to 6 nm, and the thickness of the structure varies in a range from 0.3 to 1 μm. The complex of X-ray diffraction techniques includes a measurement of θ-2θ rocking curves of symmetric Bragg reflection, the construction of intensity maps for asymmetric reflections, a measurement and analysis of peak broadenings in different diffraction geometries, a precise measurement of lattice parameters, and the determination of radii of curvature. The thickness and strain of separate SL layers are determined by measuring the θ-2θ rocking curves subsequent simulation. It is shown that most SL samples are completely relaxed as a whole. At the same time, relaxation is absent between sublayers, which is why strains in the AlN and GaN sublayers (on the order of 1.2 × 10{sup −2}) have different signs. An analysis of diffraction peak half-widths allows us to determine the densities of individual sets of dislocations and observe their change from buffer layers to SLs.

  4. A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

    SciTech Connect

    Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

    2015-09-26

    A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.

  5. Structure-function Investigation of Operando Nanostructured Materials Using Coherent X-ray Diffractive Imaging

    NASA Astrophysics Data System (ADS)

    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. Analysis of energy dispersive x-ray diffraction profiles for material identification, imaging and system control

    NASA Astrophysics Data System (ADS)

    Cook, Emily Jane

    2008-12-01

    This thesis presents the analysis of low angle X-ray scatter measurements taken with an energy dispersive system for substance identification, imaging and system control. Diffraction measurements were made on illicit drugs, which have pseudo- crystalline structures and thus produce diffraction patterns comprising a se ries of sharp peaks. Though the diffraction profiles of each drug are visually characteristic, automated detection systems require a substance identification algorithm, and multivariate analysis was selected as suitable. The software was trained with measured diffraction data from 60 samples covering 7 illicit drugs and 5 common cutting agents, collected with a range of statistical qual ities and used to predict the content of 7 unknown samples. In all cases the constituents were identified correctly and the contents predicted to within 15%. Soft tissues exhibit broad peaks in their diffraction patterns. Diffraction data were collected from formalin fixed breast tissue samples and used to gen erate images. Maximum contrast between healthy and suspicious regions was achieved using momentum transfer windows 1.04-1.10 and 1.84-1.90 nm_1. The resulting images had an average contrast of 24.6% and 38.9% compared to the corresponding transmission X-ray images (18.3%). The data was used to simulate the feedback for an adaptive imaging system and the ratio of the aforementioned momentum transfer regions found to be an excellent pa rameter. Investigation into the effects of formalin fixation on human breast tissue and animal tissue equivalents indicated that fixation in standard 10% buffered formalin does not alter the diffraction profiles of tissue in the mo mentum transfer regions examined, though 100% unbuffered formalin affects the profile of porcine muscle tissue (a substitute for glandular and tumourous tissue), though fat is unaffected.

  7. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

    2011-12-01

    The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I., Baliva, A., Stevoli, A., Ambrosi, R., Critani, F., Delhez, R., Scandelli, L., Holland, A., Nelms, N. & the Mars-XRD Team, Proceedings of the 38th Lunar and Planetary Science Conference, 12 - 16 March 2007, League City, Texas, USA. [2] L. Marinangeli, I. B. Hutchinson, A. Stevoli, G. Adami, R. Ambrosi, R. Amils, V. Assis Fernandes, A. Baliva, A. T. Basilevsky, G. Benedix, P. Bland, A. J. Böttger, J. Bridges, G. Caprarelli, G. Cressey, F. Critani, N. d'Alessandro, R. Delhez, C. Domeneghetti, D. Fernandez-Remolar, R. Filippone, A. M. Fioretti, J. M. Garcia Ruiz, M. Gilmore, G. M. Hansford, G. Iezzi, R. Ingley, M. Ivanov, G. Marseguerra, L. Moroz, C. Pelliciari, P. Petrinca, E. Piluso, L. Pompilio, J. Sykes, F. Westall and the MARS-XRD Team, EPSC-DPS Joint Meeting 2011, 3 - 7 October 2011, La Cité Internationale des Congrès Nantes Métropole, Nantes, France.

  8. Determination of line profiles on photomasks using DUV, EUV, and x-ray scattering

    NASA Astrophysics Data System (ADS)

    Scholze, F.; Bodermann, B.; Burger, S.; Endres, J.; Haase, A.; Krumrey, M.; Laubis, C.; Soltwisch, V.; Ullrich, A.; Wernecke, J.

    2014-10-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. GISAXS provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range which allow for much steeper angles of incidence but preserve the large range of momentum transfer that can be observed. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, a finite element method (FEM) Maxwell solver and least-squares optimization yielded consistent results for EUV and deep ultraviolet (DUV) scatterometry. For EUV photomasks, the actinic wavelength EUV scatterometry yields particular advantages. A significant polarization dependence of the diffraction intensities for 0th and +1st orders in the geometry with the grating lines perpendicular to the plane of reflection is observed and the 0th order intensity shows sufficient sensitivity to the line width such that a CD-resolution below 0.1 nm is within reach. In this contribution we present scatterometry data for line gratings using GISAXS, and EUV and DUV scatterometry and consistent reconstruction results of the line geometry for EUV and DUV scatterometry.

  9. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

    DOE PAGESBeta

    Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; et al

    2016-04-12

    Here, 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 solvedmore » 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.« less

  10. Thermal, structural and diffraction analyses of a gallium-cooled x- ray monochromator

    SciTech Connect

    Rogers, C.S.; Macrander, A.T.; Mills, D.M.

    1992-06-01

    The next generation of synchrotron radiation sources will produce very high power and power density x-ray beams. For example, the Advanced Photon Source (APS) under construction at Argonne National Laboratory will produce beams containing up to 5 kill of power and peak normal power densities in excess of 150 W/mm{sup 2}. Normally, the first optical component to intercept the x-ray beam is a crystal monochromator. This device typically uses a single crystal of silicon or germanium as a band-pass filter according to Braggs` law of diffraction. Under the severe heat loading of modem synchrotron beams, the performance of the monochromator is degraded by reducing the photon throughput and increasing the beam divergence. This paper describes the methods used to calculate the thermally induced deformations in standardly configured monochromator crystals using finite element analysis. The results of these analyses are compared to recent experiments conducted at the Cornell High Energy Synchrotron Source (CHESS) using a high-performance, gallium-cooled crystal. Computer simulations can be used to evaluate the performance of high-heat-load x-ray optics for future synchrotron sources.

  11. Thermal, structural and diffraction analyses of a gallium-cooled x- ray monochromator

    SciTech Connect

    Rogers, C.S.; Macrander, A.T.; Mills, D.M.

    1992-06-01

    The next generation of synchrotron radiation sources will produce very high power and power density x-ray beams. For example, the Advanced Photon Source (APS) under construction at Argonne National Laboratory will produce beams containing up to 5 kill of power and peak normal power densities in excess of 150 W/mm{sup 2}. Normally, the first optical component to intercept the x-ray beam is a crystal monochromator. This device typically uses a single crystal of silicon or germanium as a band-pass filter according to Braggs' law of diffraction. Under the severe heat loading of modem synchrotron beams, the performance of the monochromator is degraded by reducing the photon throughput and increasing the beam divergence. This paper describes the methods used to calculate the thermally induced deformations in standardly configured monochromator crystals using finite element analysis. The results of these analyses are compared to recent experiments conducted at the Cornell High Energy Synchrotron Source (CHESS) using a high-performance, gallium-cooled crystal. Computer simulations can be used to evaluate the performance of high-heat-load x-ray optics for future synchrotron sources.

  12. Structure of ZnO Nanorods using X-ray Diffraction

    SciTech Connect

    Howdyshell, Marci; /Albion Coll. /SLAC

    2007-11-07

    Many properties of zinc oxide, including wide bandgap semiconductivity, photoconductivity, and chemical sensing, make it a very promising material for areas such as optoelectronics and sensors. This research involves analysis of the formation, or nucleation, of zinc oxide by electrochemical deposition in order to gain a better understanding of the effect of different controlled parameters on the subsequently formed nanostructures. Electrochemical deposition involves the application of a potential to an electrolytic solution containing the species of interest, which causes the ions within to precipitate on one of the electrodes. While there are other ways of forming zinc oxide, this particular process is done at relatively low temperatures, and with the high amount of x-ray flux available at SSRL it is possible to observe such nucleation in situ. Additionally, several parameters can be controlled using the x-ray synchrotron; the concentration of Zn{sup 2+} and the potential applied were controlled during this project. The research involved both gathering the X-ray diffraction data on SSRL beamline 11-3, and analyzing it using fit2d, Origin 6.0 and Microsoft Excel. A time series showed that both the in-plane and out-of-plane components of the ZnO nanorods grew steadily at approximately the same rate throughout deposition. Additionally, analysis of post-scans showed that as potential goes from less negative to more negative, the resulting nanostructures become more oriented.

  13. A Pipelining Implementation for Parsing X-ray Diffraction Source Data and Removing the Background Noise

    NASA Astrophysics Data System (ADS)

    Bauer, Michael A.; Biem, Alain; McIntyre, Stewart; Xie, Yuzhen

    2010-11-01

    Synchrotrons can be used to generate X-rays in order to probe materials at the atomic level. One approach is to use X-ray diffraction (XRD) to do this. The data from an XRD experiment consists of a sequence of digital image files which for a single scan could consist of hundreds or even thousands of digital images. Existing analysis software processes these images individually sequentially and is usually used after the experiment is completed. The results from an XRD detector can be thought of as a sequence of images, generated during the scan by the X-ray beam. If these images could be analyzed in near real-time, the results could be sent to the researcher running the experiment and used to improve the overall experimental process and results. In this paper, we report on a stream processing application to remove background from XRD images using a pipelining implementation. We describe our implementation techniques of using IBM Infosphere Streams for parsing XRD source data and removing the background. We present experimental results showing the super-linear speedup attained over a purely sequential version of the algorithm on a quad-core machine. These results demonstrate the potential of making good use of multi-cores for high-performance stream processing of XRD images.

  14. Elastic strains in antler trabecular bone determined by synchrotron x-ray diffraction.

    SciTech Connect

    Akhtar, R.; Daymond, M.; Almer, J.; Mummery, P.; X-Ray Science Division; Univ. of Manchester; Queen's Univ.

    2008-01-01

    The microstructure and associated mechanical properties of antler trabecular bone have been studied using a variety of techniques. The local trabeculae properties, as well as the three-dimensional architecture were characterized using nanoindentation and X-ray microtomography, respectively. An elastic modulus of 10.9+/-1.1 GPa is reported for dry bone, compared with 5.4+/-0.9 GPa for fully hydrated bone. Trabeculae thickness and separation were found to be comparable to those of bovine trabecular bone. Uniaxial compression conducted in situ during X-ray microtomography showed that antler can undergo significant architectural rearrangement, dominated by trabeculae bending and buckling, due to its low mineral content. High-energy synchrotron X-ray diffraction was used to measure elastic strains in the apatite crystals of the trabeculae, also under in situ uniaxial compression. During elastic loading, strain was found to be accommodated largely by trabeculae aligned parallel to the loading direction. Prior to the macroscopic yield point, internal strains increased as trabeculae deformed by bending, and load was also found to be redistributed to trabeculae aligned non-parallel to the loading direction. Significant bending of trabecular walls resulted in tensile strains developing in trabeculae aligned along the loading direction

  15. Energy dispersive x-ray diffraction of charge density waves via chemical filtering

    SciTech Connect

    Feng Yejun; Somayazulu, M. S.; Jaramillo, R.; Rosenbaum, T.F.; Isaacs, E.D.; Hu Jingzhu; Mao Hokwang

    2005-06-15

    Pressure tuning of phase transitions is a powerful tool in condensed matter physics, permitting high-resolution studies while preserving fundamental symmetries. At the highest pressures, energy dispersive x-ray diffraction (EDXD) has been a critical method for geometrically confined diamond anvil cell experiments. We develop a chemical filter technique complementary to EDXD that permits the study of satellite peaks as weak as 10{sup -4} of the crystal Bragg diffraction. In particular, we map out the temperature dependence of the incommensurate charge density wave diffraction from single-crystal, elemental chromium. This technique provides the potential for future GPa pressure studies of many-body effects in a broad range of solid state systems.

  16. Performance characteristics needed for protein crystal diffraction x-ray detectors.

    SciTech Connect

    Westbrook, E. M.

    1999-09-21

    During the 1990's, macromolecular crystallography became progressively more dependent on synchrotrons X-ray sources for diffraction data collection. Detectors of this diffraction data at synchrotrons beamlines have evolved over the decade, from film to image phosphor plates, and then to CCD systems. These changes have been driven by the data quality and quantity improvements each newer detector technology provided. The improvements have been significant. It is likely that newer detector technologies will be adopted at synchrotron beamlines for crystallographic diffraction data collection in the future, but these technologies will have to compete with existing CCD detector systems which are already excellent and are getting incrementally better in terms of size, speed, efficiency, and resolving power. Detector development for this application at synchrotrons must concentrate on making systems which are bigger and faster than CCDs and which can capture weak data more efficiently. And there is a need for excellent detectors which are less expensive than CCD systems.

  17. Modeling kinematical x-ray diffraction excited by a coherent nanobeam.

    SciTech Connect

    Ying, A.; Osting, B.; Noyan, I. C.; Murray, C. E.; Holt, H. V.; Maser, J.

    2010-01-01

    A rigorous model of a diffraction experiment utilizing a coherent, monochromatic, X-ray beam, focused by a Fresnel zone plate onto a thin, perfect, single-crystal layer is presented. In this model, first the coherent wave emanating from an ideal zone plate equipped with a direct-beam stop and order-sorting aperture is computed. Then, diffraction of the focused wavefront by a thin silicon film positioned at the primary focal spot is calculated. This diffracted wavefront is propagated to the detector position, and the intensity distribution at the detector plane is extracted. The predictions of this model agree quite well with experimental data measured at the Center for Nanoscale Materials nanoprobe instrument at Sector 26 of the Advanced Photon Source.

  18. Spectral X-Ray Diffraction using a 6 Megapixel Photon Counting Array Detector

    PubMed Central

    Muir, Ryan D.; Pogranichniy, Nicholas R.; Muir, J. Lewis; Sullivan, Shane Z.; Battaile, Kevin P.; Mulichak, Anne M.; Toth, Scott J.; Keefe, Lisa J.; Simpson, Garth J.

    2016-01-01

    Pixel-array array detectors allow single-photon counting to be performed on a massively parallel scale, with several million counting circuits and detectors in the array. Because the number of photoelectrons produced at the detector surface depends on the photon energy, these detectors offer the possibility of spectral imaging. In this work, a statistical model of the instrument response is used to calibrate the detector on a per-pixel basis. In turn, the calibrated sensor was used to perform separation of dual-energy diffraction measurements into two monochromatic images. Targeting applications include multi-wavelength diffraction to aid in protein structure determination and X-ray diffraction imaging. PMID:27041789

  19. Data preparation and evaluation techniques for x-ray diffraction microscopy

    DOE PAGESBeta

    Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; Marchesini, Stefano; Shapiro, David; Turner, Joshua J.; Jacobsen, Chris

    2010-01-01

    The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. In addition, we show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffractionmore » patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.« less

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

    NASA Astrophysics Data System (ADS)

    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.

  1. Laboratory manual: mineral X-ray diffraction data retrieval/plot computer program

    USGS Publications Warehouse

    Hauff, Phoebe L.; VanTrump, George

    1976-01-01

    The Mineral X-Ray Diffraction Data Retrieval/Plot Computer Program--XRDPLT (VanTrump and Hauff, 1976a) is used to retrieve and plot mineral X-ray diffraction data. The program operates on a file of mineral powder diffraction data (VanTrump and Hauff, 1976b) which contains two-theta or 'd' values, and intensities, chemical formula, mineral name, identification number, and mineral group code. XRDPLT is a machine-independent Fortran program which operates in time-sharing mode on a DEC System i0 computer and the Gerber plotter (Evenden, 1974). The program prompts the user to respond from a time-sharing terminal in a conversational format with the required input information. The program offers two major options: retrieval only; retrieval and plot. The first option retrieves mineral names, formulas, and groups from the file by identification number, by the mineral group code (a classification by chemistry or structure), or by searches based on the formula components. For example, it enables the user to search for minerals by major groups (i.e., feldspars, micas, amphiboles, oxides, phosphates, carbonates) by elemental composition (i.e., Fe, Cu, AI, Zn), or by a combination of these (i.e., all copper-bearing arsenates). The second option retrieves as the first, but also plots the retrieved 2-theta and intensity values as diagrammatic X-ray powder patterns on mylar sheets or overlays. These plots can be made using scale combinations compatible with chart recorder diffractograms and 114.59 mm powder camera films. The overlays are then used to separate or sieve out unrelated minerals until unknowns are matched and identified.

  2. Purification, crystallization and preliminary X-ray diffraction analysis of royal palm tree (Roystonea regia) peroxidase

    SciTech Connect

    Watanabe, Leandra; Nascimento, Alessandro S.; Zamorano, Laura S.; Shnyrov, Valery L.; Polikarpov, Igor

    2007-09-01

    The purification, crystallization, X-ray diffraction data acquisition and molecular-replacement results of royal palm tree (R. regia) peroxidase are described. Royal palm tree peroxidase (RPTP), which was isolated from Roystonea regia leaves, has an unusually high stability that makes it a promising candidate for diverse applications in industry and analytical chemistry [Caramyshev et al. (2005 ▶), Biomacromolecules, 6, 1360–1366]. Here, the purification and crystallization of this plant peroxidase and its X-ray diffraction data collection are described. RPTP crystals were obtained by the hanging-drop vapour-diffusion method and diffraction data were collected to a resolution of 2.8 Å. The crystals belong to the trigonal space group P3{sub 1}21, with unit-cell parameters a = b = 116.83, c = 92.24 Å, and contain one protein molecule per asymmetric unit. The V{sub M} value and solvent content are 4.07 Å{sup 3} Da{sup −1} and 69.8%, respectively.

  3. Effect of grain size on stability of X-ray diffraction patterns used for threat detection

    NASA Astrophysics Data System (ADS)

    Ghammraoui, B.; Rebuffel, V.; Tabary, J.; Paulus, C.; Verger, L.; Duvauchelle, Ph.

    2012-08-01

    Energy Dispersive X-ray Diffraction (EDXRD) is well-suited to detecting narcotics and a wide range of explosives. The integrated intensity of an X-ray diffraction peak is proportional to the number of grains in the inspected object which are oriented such that they satisfy Bragg's condition. Several parameters have a significant influence on this number. Among them, we can list grain size and the fill rate for polycrystalline materials that both may significantly vary for a same material according to its way of production. Consequently, peak intensity may change significantly from one measurement to another one, thus increasing the risk of losing peaks. This instability is one of the many causes of false alarms. To help avoid these, we have developed a model to quantify the stability of the diffraction patterns measured. Two methods (extension of the detector in a direction perpendicular to the diffractometer plane and slow rotation of both source and detector) can be used to decrease the coefficient of variation, leading to a more stable spectral measurement.

  4. Quantitative analysis of carbonate sediments using powder X-ray diffraction and the Rietveld method

    SciTech Connect

    Post, J.E. . Dept. of Mineral Sciences)

    1992-01-01

    Critical to most studies of carbonate sediments is information about the relative abundances of different carbonate minerals and the Mg mole-percent of the calcite phases. Traditional powder X-ray diffraction methods for extracting these data rely upon measurement of the integrated area and d-spacing of the 104 calcite peak. This approach, however, is difficult for diffraction patterns with severely overlapping peaks and is prone to a range of systematic errors. The Rietveld analysis method makes use of the entire powder X-ray diffraction pattern and can quickly yield accurate quantitative phase analysis (without the need for standards) and unit-cell parameters for even complex mixtures. Furthermore, corrections for certain systematic errors (e.g. sample displacement) are also refined, eliminating the need to add internal standards to the samples. The d-spacings, a, and c values from the refinement can be used with standard determinative curves for Mg mole-percent. Also, in many cases, the Rietveld refinement can yield directly the Mg composition of each calcite phase. Results from several prepared two and three phase carbonate mixtures will be shown to demonstrate the accuracy of the technique. Applications to natural samples of mollusk shells, coralline algae, echinoderm spines, and carbonate muds will also be discussed.

  5. Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

    DOEpatents

    Green, L.A.; Heck, J.L. Jr.

    1985-04-23

    A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

  6. Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

    DOEpatents

    Green, Lanny A.; Heck, Jr., Joaquim L.

    1987-01-01

    A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

  7. Load transfer in bovine plexiform bone determined by synchrotron x-ray diffraction.

    SciTech Connect

    Akhtar, R.; Daymond, M.; Almer, J.; Mummery, P.; The Univ. of Manchester; Queen's Univ.

    2008-02-01

    High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.

  8. Atomic motion of resonantly vibrating quartz crystal visualized by time-resolved X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Aoyagi, Shinobu; Osawa, Hitoshi; Sugimoto, Kunihisa; Fujiwara, Akihiko; Takeda, Shoichi; Moriyoshi, Chikako; Kuroiwa, Yoshihiro

    2015-11-01

    Transient atomic displacements during a resonant thickness-shear vibration of AT-cut α-quartz are revealed by time-resolved X-ray diffraction under an alternating electric field. The lattice strain resonantly amplified by the alternating electric field is ˜104 times larger than that induced by a static electric field. The resonantly amplified lattice strain is achieved by fast displacements of oxygen anions and collateral resilient deformation of Si-O-Si angles bridging rigid SiO4 tetrahedra, which efficiently transduce electric energy into elastic energy.

  9. Surface, morphology and X-ray diffraction studies of Co (II) complexes of pyrazole ligands

    NASA Astrophysics Data System (ADS)

    Mishra, A.; Jain, Garima; Ninama, S.

    2014-09-01

    Pyrazole based complexes of the cobalt (II) Bis-(diethyl 4-amino-1-(P-nitrophenyl) 1H-pyrazole-3,5dicarboxylate) [Co (D4A1(P-N)1HP35D)] and cobalt (II) Bis-(diethyl 4- amino-1-(3-chlorophenyl) 1H-pyrazole-3,5dicarboxylate) [Co (D4A1(3-Cl)1HP35D)] were synthesized by chemical root method and characterized by different method viz. X-ray diffraction, Fourier transform infrared spectroscopy and Transmission electron microscopy studies. All these studies were in good agreement with the synthesized complexes.

  10. In situ X-ray diffraction investigation of nitride coatings at high-temperature oxidation

    NASA Astrophysics Data System (ADS)

    Krysina, O. V.; Koval, N. N.; Shmakov, A. N.; Vinokurov, Z. S.

    2016-01-01

    Structural and phase researches of the multicomponent nanocrystalline coatings synthesized by plasma-assisted vacuum arc method at high-temperature influence by method of X-ray diffraction with the use of synchrotron radiation in situ have been carried out. The main features of these coatings are the superhardness (39 - 45 GPa) and nanocrystalline structure (5 - 20 nm). The analysis of results of structural and phase researches, physical and mechanical characteristics after oxidation of multicomponent nitride coatings at high-temperature heating in open air is presented.

  11. X-ray diffraction peaks from correlated dislocations:Monte Carlo study of dislocation screening.

    PubMed

    Kaganer, Vladimir M; Sabelfeld, Karl K

    2010-11-01

    X-ray diffraction peak profiles are calculated by the Monte Carlo method for arbitrarily correlated dislocations without making any approximations or simplifications. The arrangement of dislocations in pairs with opposite Burgers vectors provides screening of the long-range strains. Moreover, any screening can be modeled by appropriate distribution of the dislocation pairs. Analytical description of the peak profiles is compared with the Monte Carlo results. Symmetric peaks due to screw dislocations and asymmetric peaks due to edge dislocations are simulated and analyzed. PMID:20962380

  12. Synchrotron X-ray diffraction analysis of a cast nickel alloy after barothermal action

    NASA Astrophysics Data System (ADS)

    Padalko, A. G.; Yur'ev, G. S.; Zubarev, G. I.; Tsarev, V. I.; Talanova, G. V.

    2011-11-01

    Synchrotron X-ray diffraction analysis of a nickel superalloy subjected to barothermal treatment (BTT) at 1235, 1260, and 1320°C is performed using a high-power synchrotron radiation source. The alloy is found to contain two types of γ' phase and two types of γ solid solution, which are likely to be located in dendrite arms and the interdendritic space, respectively. The averaged lattice misfits of the γ' phases and the γ solid solutions change with the BTT temperature at a constant pressure and exposure time, which substantially affects the high-temperature characteristics of the alloy.

  13. Darwin's approach to X-ray diffraction on lateral crystalline structures.

    PubMed

    Punegov, Vasily I; Kolosov, Sergey I; Pavlov, Konstantin M

    2014-01-01

    Darwin's dynamical theory of X-ray diffraction is extended to the case of lateral (i.e., having a finite length in the lateral direction) crystalline structures. This approach allows one to calculate rocking curves as well as reciprocal-space maps for lateral crystalline structures having a rectangular cross section. Numerical modelling is performed for these structures with different lateral sizes. It is shown that the kinematical approximation is valid for thick crystalline structures having a small length in the lateral direction. PMID:24419171

  14. Massive Submandibular Sialolith: Complete Radiographic Registration and Biochemical Analysis through X-Ray Diffraction

    PubMed Central

    de Carvalho Mattos, Mayara Jessica; Ferrari, Francine; dos Reis Neto, José Manoel; Carta Gambus, Luiz Carlos; Couto Souza, Paulo Henrique; Berti-Couto, Soraya de Azambuja

    2014-01-01

    Sialolithiasis is a pathologic condition that affects 60 million people per year, which is caused by the presence of calcified structures, named sialoliths, inside the salivary glands and their salivary ducts. Despite the large incidence of sialolithiasis, its etiology is still unknown. In the present case report, a 47-year-old female patient, presenting with local pain and hampered mouth opening, underwent a surgical approach for the removal of a 20 mm sialolith, which was further analyzed through X-ray diffraction. In parallel, a radiographic registration of 8 years, covering all the period for sialolith formation, is presented along the case report. PMID:25258693

  15. Quantitative X-ray diffraction analysis of oxides formed on superalloys

    NASA Technical Reports Server (NTRS)

    Garlick, R. G.

    1972-01-01

    Methods were developed for quantitative analysis by X-ray diffraction of the oxides Al2O3, NiO, Cr2O3, CoO, and CoCr2O4 within a standard deviation of about 10 percent of the weight fraction reported or within 1 percent absolute. These error limits assume that the sample oxides are well characterized and that the physiochemical structure of the oxides in the samples are identical with those in the synthesized standards. Results are given for the use of one of the techniques in the analysis of spalls from a series of oxidation tests of the cobalt base alloy WI-52.

  16. X-ray diffraction study of elemental thulium at pressures up to 86 GPa

    SciTech Connect

    Pravica, Michael; Quine, Zachary; Romano, Edward

    2006-09-01

    We have performed a high-pressure synchrotron x-ray diffraction experiment on elemental thulium in a diamond anvil cell to 86 GPa. A series of phase transitions was observed as a function of pressure that follow the expected hexagonal-close-packed{yields}Samarium-type{yields}double hexagonal-close-packed{yields}distorted distorted face-centered cubic sequence. In particular, we present evidence for the predicted double hexagonal close packed{yields}distorted face-centered cubic phase transition near 68 GPa. Equation of state data for thulium are also reported up to 86 GPa.

  17. X-ray diffraction investigation of 1-phenyl-3-isopropyl-5-(benzothiazol-2-yl)formazan

    SciTech Connect

    Slepukhin, P. A. Pervova, I. G.; Rezinskikh, Z. G.; Lipunova, G. N.; Gorbatenko, Yu. A.; Lipunov, I. N.

    2008-01-15

    The crystal structure of 1-phenyl-3-isopropyl-5-(benzothiazol-2-yl)formazan is investigated using X-ray diffraction. The compound crystallizes in the form of two crystallographically independent molecules (A and B) in identical conformations that are stabilized by intermolecular hydrogen bonds. The intermolecular hydrogen bonds N-H-N (N-N, 2.892 and 2.939 A) link molecules into AB dimers. Both molecules have a flattened structure, except for the isopropyl fragment. The bonds in the formazan chains are delocalized. Molecules A and B have close geometric characteristics.

  18. Quantitative mineralogical analysis of hydraulic limes by X-ray diffraction

    SciTech Connect

    Mertens, G. Madau, P.; Durinck, D.; Blanpain, B.; Elsen, J.

    2007-11-15

    A combined selective dissolution/quantitative X-ray diffraction (QXRD) approach is proposed for the quantitative mineralogical phase analysis of hydraulic limes. The proposed methodology is validated by the analysis of two model mixtures. Afterwards two commercial hydraulic binders and one self-burned hydraulic quicklime were analysed. Chemical, thermal and microprobe analyses were performed to check the results. It is shown that the proposed selective dissolution/QXRD approach yields reliable quantitative mineralogical information for hydraulic limes in spite of their complex phase composition and the presence of amorphous material.

  19. X-ray diffraction studies and equation of state of methane at 202 GPa

    SciTech Connect

    Sun, Liling; Yi, Wei; Wang, Lin; Shu, Jinfu; Sinogeikin, Stas; Meng, Yue; Shen, Guoyin; Bai, Ligang; Li, Yanchuan; Liu, Jing; Mao, Ho-kwang; Mao, Wendy L.

    2009-04-22

    Solid methane (CH{sub 4}) was compressed up to 202 GPa at 300 K in a diamond-anvil cell. The crystal structure and equation of state over this entire range were determined from angle dispersive X-ray diffraction results. CH{sub 4} undergoes phase transitions from rhombohedral to a simple cubic phase at 19 GPa and from simple cubic to a higher pressure cubic phase at approximately 94 GPa. This higher pressure cubic phase was stable to the maximum pressure investigated. Combined with previous optical measurements, it was found that at room temperature compressed CH{sub 4} remains an insulator with cubic structure to 202 GPa.

  20. Crystallization and preliminary X-ray diffraction analysis of red clover necrotic mosaic virus

    SciTech Connect

    Martin, Stanton L.; Guenther, Richard H.; Sit, Tim L.; Swartz, Paul D.; Meilleur, Flora; Lommel, Steven A.; Rose, Robert B.

    2010-11-12

    Red clover necrotic mosaic virus (RCNMV) is a species that belongs to the Tombusviridae family of plant viruses with a T = 3 icosahedral capsid. RCNMV virions were purified and were crystallized for X-ray analysis using the hanging-drop vapor-diffusion method. Self-rotation functions and systematic absences identified the space group as I23, with two virions in the unit cell. The crystals diffracted to better than 4 {angstrom} resolution but were very radiation-sensitive, causing rapid decay of the high-resolution reflections. The data were processed to 6 {angstrom} in the analysis presented here.