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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. 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.}

  3. 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.

  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. 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.

  6. 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...

  7. 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.

  8. 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.

  9. 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.

  10. 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...

  11. The features of identifying lines in a diffraction image formed by a widely divergent X-ray beam

    SciTech Connect

    Avetyan, K. T. Levonyan, L. V.; Arakelyan, M. M. Semerjian, H. S.; Grigoryan, P. A.; Hovhannisyan, G. M.

    2009-05-15

    A method for identifying lines in a diffraction image formed by a widely divergent X-ray beam and a technique for measuring the crystal structure parameters in the case of asymmetric crystal position have been developed. It is established that, once the distances between a crystal and a photographic plate and between the points of intersection of the hyperbola branches in a diffraction image are known, one can determine the angle between the crystal's zone axis and the wave vector, which leads to multiwave diffraction. Relations linking this angle with the parameters of two atomic planes are obtained. It is found that, to measure the parameters of atomic planes belonging to a given zone, one can use different sets of crossed hyperbolas formed by radiations K{sub {alpha}} and K{sub {beta}}. The measurements and calculations performed for the same sample (Si crystal), mounted symmetrically and asymmetrically, confirm the reliability of the proposed method.

  12. 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.

  13. 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

  14. 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.

  15. Medipix 2 in X-ray diffraction

    NASA Astrophysics Data System (ADS)

    de Vries, R. I.; Weijers, S.; Bethke, K.; Kogan, V.; Vasterink, J.; Kharchenko, A.; Fransen, M.; Bethke, J.

    2007-06-01

    The Medipix 2 detector is a detector with a high dynamic range and, in principle, no intrinsic detector noise. This makes the detector perfectly suitable for use in X-ray diffraction experiments. For X-ray diffraction systems used in materials science, it is common to use X-rays with an energy of 8 keV. When the Medipix 2 read-out chip is bump-bonded to a 300 ?m silicon sensor it is able to detect these X-rays with a high efficiency. The Medipix 2 detector has been integrated into a PANalytical X'Pert PRO X-ray diffraction system. Details about this integration will be discussed and measurements performed with this system will be shown.

  16. A comparison between different X-ray diffraction line broadening analysis methods for nanocrystalline ball-milled FCC powders

    NASA Astrophysics Data System (ADS)

    Soleimanian, V.; Mojtahedi, M.

    2015-06-01

    The microstructural characteristics of aluminum, copper and nickel powders are investigated using different X-ray diffraction line broadening analysis approaches. Prior to analysis, the powders were ball-milled to produce a nanocrystalline structure with high density of probable types of lattice defects. A variety of methods, including Scherrer, Williamson-Smallman, Williamson-Hall, Warren-Averbach, modified Williamson-Hall, modified Warren-Averbach, Rietveld refinement and whole powder pattern modeling (WPPM) approaches are applied. In this way, microstructural characteristics such as crystallite size, microstrain, dislocation density, effective outer cut-off radius of dislocations and the probability of twining and stacking faults are calculated. On the other hand, the results of conventional and advanced line broadening analysis methods are compared. It is revealed that the density of linear and planar defects in the mechanically deformed aluminum powder is significantly smaller than that of copper and nickel, as well as the level of anisotropic strain broadening. Moreover, the WPPM procedure provided a better profile fitting with more accurate results.

  17. 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.

  18. X-Ray Diffraction Analysis Program

    NASA Technical Reports Server (NTRS)

    Wiedemann, K. E.; Unnam, J.; Naidu, S. V. N.; Houska, C. R.

    1986-01-01

    SOPAD separates overlapping peaks and analyzes derivatives of X-ray diffraction data. SOPAD helps analyst get most information out of available diffraction data. SOPAD uses Marquardt-type nonlinear regression routine to refine initial estimates of individual peak positions, intensities, shapes, and half-widths.

  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. 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.

  1. 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)

  2. 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.

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

    PubMed

    Authier, Andr

    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: Pendellsung, 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

  4. X-ray line emission from Capella

    NASA Technical Reports Server (NTRS)

    Holt, S. S.; Boldt, E. A.; Serlemitsos, P. J.; White, N. E.; Becker, R. H.; Mushotzky, R. F.; Smith, B. W.

    1979-01-01

    X-ray emission-line components from Mg, Si, S, and Fe are unambiguously detected from Capella with the solid-state spectrometer onboard the Einstein Observatory. The X-ray spectrum is inconsistent with an isothermal corona, and requires components between 6-million K and at least 24-million K for an adequate fit. An inhomogeneous corona in which the X-ray emitting plasma is confined to magnetically contained loops appears to be reconcilable with all of the experimental evidence.

  5. 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.

  6. Studies on X-ray diffraction microscopy

    NASA Astrophysics Data System (ADS)

    Miao, Huijie

    This dissertation includes three main parts: studies on coherence requirements for the diffraction microscopy experiments, ice formation on frozen-hydrated sample during data collection, and centering of the diffraction data sets. These three subjects are all in support of our groups overall goal of high resolution 3D imaging of frozen hydrated eukaryotic cells via x-ray diffraction microscopy. X-ray diffraction microscopy requires coherent illumination. However, the actual degree of coherence at some beamlines has never been tested. In research on coherence, our first aim is to determine the transverse coherence width at the sample plane at BL 9.0.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory. An analytical calculation of the coherence at the sample plane is presented. Experimental diffraction patterns of pinhole-pair samples were also taken at the beamline to determine the coherence. Due to the irregular shape of the pinholes and other optics complexity, it was very difficult to fit the data with known theoretical equations as it was traditionally done with 1D data. However, we found out that the auto-correlation function shows clearly three spots. Theoretical calculation have been carried out to show that the degree of coherence can be obtained from the intensities of the three spots. These results are compared with the results from the analytical calculation. We then perform a simulation, showing the required transverse coherence width for reconstructing samples with a given size. Ice accumulation has been a major problem in X-ray diffraction microscopy with frozen hydrated samples. Since the ice structure is different from point to point, we cannot subtract the scattering from ice, nor assume a completely "empty" region outside the finite support constraint area as required for reconstruction. Ice forms during the sample preparation and transfer. However, from the tests we did in September 2007, we found that the ice layer thickens significantly during the data collecting process. One of the tests we did was putting a dry room-temperature grid into the beam, cooling it down to liquid nitrogen temperature, and then collecting the diffraction pattern of it over time. This test showed that, after the cold grid remained in the chamber for a while, a ring could be observed in the diffraction pattern. The time necessary for this ring to be visible is highly dependent on the pressure and vacuum history of the chamber. We will discuss how the chamber pressure influences the ice accumulation rate, how an anti-contamination device can help to reduce the rate, and how this ring forms. The last part of the research is based on simulations and a real data set collected on beamline 9.0.1 at the ALS in Berkeley. In X-ray diffraction microscopy, one of the major challenges when processing the data is to accurately determine the true center of the recorded data; that is, the zero spatial frequency position. Simulations of reconstructing shifted data show that if the center of a 2D diffraction pattern is shifted by more than 3 pixels from its true center, the positivity constraint to the phase, which otherwise might be applied to improve the convergence of the reconstruction algorithm, cannot be imposed. Moreover, the phase unwrapping problem may appear during the reconstruction. These issues undermine the quality of the reconstruction of 2D data. Furthermore, the individual shift in each 2D pattern will lead to errors when assembling a 3D diffraction data cube, making the 3D reconstruction very difficult. We developed a method which uses power spectra of the partial diffraction pattern to pre-align the data. A reconstruction without severe phase unwrapping can then be obtained from the pre-aligned data. Next, the precise zero spatial frequency position can be found by examining the linear ramp present in the reconstructed phase. This method was applied to a freeze-dried yeast data set to show that this approach is effective with experimental data.

  7. 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.

  8. 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.

  9. Dynamical x-ray diffraction from an icosahedral quasicrystal

    SciTech Connect

    Kycia, S.W.; Goldman, A.I. ); Lograsso, T.A.; Delaney, D.W. ); Black, D. ); Sutton, M.; Dufresne, E.; Bruening, R. ); Rodricks, B. )

    1993-08-01

    We present direct evidence of dynamical diffraction of x rays from a quasicrystal. High-resolution x-ray-diffraction measurements of the Al-Pd-Mn face-centered icosahedral quasicrystal were performed, revealing a mosaic full width at half maximum of less than 0.001[degree]. In a second experiment, the anomalous transmission of x rays (the Borrmann effect) was observed. These measurements show that nearly perfect quasicrystals may be grown to centimeter-size dimensions allowing x-ray techniques based upon dynamical diffraction to be brought to bear on the analysis of icosahedral structures.

  10. 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.

  11. Atomic structure and faulted boundaries in the GaAs(001) ?(24) surface as derived from x-ray diffraction and line-shape analysis

    NASA Astrophysics Data System (ADS)

    Garreau, Y.; Sauvage-Simkin, M.; Jedrecy, N.; Pinchaux, R.; Veron, M. B.

    1996-12-01

    The atomic structure of the 24 reconstructed GaAs (001) surface, prepared in optimized molecular beam epitaxy growth conditions, has been fully determined by in situ grazing incidence x-ray diffraction measurements. The structure involves only two dimers in the As top layer, in agreement with recent scanning tunnel microscopy experiments by Avery et al. and Hashizume et al. and, in addition, the presence of an As dimer in the third layer as a consequence of a missing Ga row in the second layer is clearly established. Full agreement is obtained for the atomic displacements down to the fourth atomic layer below the surface with state-of-the-art first-principles total-energy calculations by Schmidt and Bechstedt. A quantitative line-shape analysis using diffuse scattering formalism demonstrates the influence on the intensity distribution of the most frequent faults in the reconstruction propagation and enables to understand the variations observed in the reflection high-energy electron-diffraction patterns with the surface preparation without need of a new surface structure.

  12. 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.

  13. Diffraction peaks in x-ray spectroscopy: Friend or foe?

    SciTech Connect

    Tissot, R.G.; Goehner, R.P.

    1992-11-01

    Diffraction peaks can occur as unidentifiable peaks in the energy spectrum of an x-ray spectrometric analysis. Recently, there has been increased interest in oriented polycrystalline films and epitaxial films on single crystal substrates for electronic applications. Since these materials diffract x-rays more efficiently than randomly oriented polycrystalline materials, diffraction peaks are being observed more frequently in x-ray fluorescent spectra. In addition, micro x-ray spectrometric analysis utilizes a small, intense, collimated x-ray beam that can yield well defined diffraction peaks. In some cases these diffraction peaks can occur at the same position as elemental peaks. These diffraction peaks, although a possible problem in qualitative and quantitative elemental analysis, can give very useful information about the crystallographic structure and orientation of the material being analyzed. The observed diffraction peaks are dependent on the geometry of the x-ray spectrometer, the degree of collimation and the distribution of wavelengths (energies) originating from the x-ray tube and striking the sample.

  14. Diffraction peaks in x-ray spectroscopy: Friend or foe

    SciTech Connect

    Tissot, R.G.; Goehner, R.P.

    1992-01-01

    Diffraction peaks can occur as unidentifiable peaks in the energy spectrum of an x-ray spectrometric analysis. Recently, there has been increased interest in oriented polycrystalline films and epitaxial films on single crystal substrates for electronic applications. Since these materials diffract x-rays more efficiently than randomly oriented polycrystalline materials, diffraction peaks are being observed more frequently in x-ray fluorescent spectra. In addition, micro x-ray spectrometric analysis utilizes a small, intense, collimated x-ray beam that can yield well defined diffraction peaks. In some cases these diffraction peaks can occur at the same position as elemental peaks. These diffraction peaks, although a possible problem in qualitative and quantitative elemental analysis, can give very useful information about the crystallographic structure and orientation of the material being analyzed. The observed diffraction peaks are dependent on the geometry of the x-ray spectrometer, the degree of collimation and the distribution of wavelengths (energies) originating from the x-ray tube and striking the sample.

  15. 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

  16. 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.

  17. Ultrahigh-Resolution Soft-X-Ray Microscopy with Zone Plates in High Orders of Diffraction

    SciTech Connect

    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{sup 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.

  18. High-Resolution Detector For X-Ray Diffraction

    NASA Technical Reports Server (NTRS)

    Carter, Daniel C.; Withrow, William K.; Pusey, Marc L.; Yost, Vaughn H.

    1988-01-01

    Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

  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. Precise rotational alignment of x-ray transmission diffraction gratings

    SciTech Connect

    Hill, S.L.

    1988-03-28

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

  3. 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.

  4. In Situ X-ray diffraction of Mo on a light gas gun

    NASA Astrophysics Data System (ADS)

    Akin, Minta; Maddox, Brian; Holmes, Neil

    2015-06-01

    We report on recent results using a newly developed x-ray diffraction system on a two stage light gas gun. Using slightly focusing polycapillary x-ray optics we are able to significantly reduce the background noise, improving diffraction lines, while keeping the x-ray source over 1 meter away and away from possible shrapnel sources. Using this system we obtained diffraction patterns for molybdenum and tin, and will discuss these results. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  5. 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.

  6. Transient x-ray diffraction to measure the dynamic response of shocked lithium fluoride single crystal

    NASA Astrophysics Data System (ADS)

    Wang, Hai-rong; Ye, Yan; Yang, Qing-guo; Li, Mu; Xiao, Sha-li; Li, Ze-ren

    2013-08-01

    Transient x-ray diffraction, also called time-resolved x-ray diffraction and dynamic x-ray diffraction, is one novel diagnostic technique for probing shocked solids. It can provide direct information about microscopic mechanisms governing shock-induced deformation and structural changes at atomistic scales with nanosecond and picoseconds resolution, and lately, it has become possible to measure the structure of transients with sub-picoseconds and sub-Angstrom resolution with the development of ultrafast lasers which can produce femtosecond electron and x-ray pulses in the form of characteristics emission lines as well as x-ray continua in the keV range. In this paper, we detect and measure directly the dynamic response of lithium fluoride single crystal shocked compressed by laser irradiation in SHENGUANG II. In our experiments, high-intensity lasers irradiated a thin Cu foil to generate helium-like rays as x-ray source. Film (IP--image plate) recorded x rays diffracted from multiple lattice planes both perpendicular and oblique angles to the shock loading direction [100]. We gained the diffraction signals of the lattice planes (200) shocked and unshocked, what's more, other lattices (113), (1-13). The positions of the diffraction lines associated with the (200) lattice plane indicated compression of the lattice along [100] direction by 13%. In the experiment, a large-angle detector consists of two films-one rectangular in shape,one triangular in shape that are positioned to record x rays diffracted from a shocked single crystal nearly within a full ? steradian. The experiment shows that transient x-ray diffraction can diagnose the dynamical response of solid with higher resolution.

  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. X-ray Lines in Stellar Coronae

    NASA Astrophysics Data System (ADS)

    Mewe, R.

    Because the emission line spectra and continua from optically thin plasmas are fairly well known, high-resolution X-ray spectroscopy has its most obvious application in the measurement of optically thin sources such as the coronae of stars. In particular X-ray observations with the EINSTEIN observatory have demonstrated that soft X-ray emitting coronae are a common feature among stars on the cool side of the Hertzsprung-Russell diagram, with the probable exception of single very cool giant and supergiant stars and A-type dwarfs. Observations with the spectrometers aboard EINSTEIN and EXOSAT have shown that data of even modest spectral resolution (/= 10-100 permit the identification of coronal material at different temperatures whose existence may relate to a range of possible magnetic loop structures in the outer atmospheres of these stars. The improved spectral resolution of the next generation of spectrometers aboard XMM and AXAF is needed to fully resolve the temperature structure of stellar coronae and to enable density and velocity diagnostics. In this paper spectral results from EINSTEIN and EXOSAT are discussed. A few simulations of high-resolution re L, K, and 2s-2p spectra with AXAF, XMM, and several detectors such as calorimeter and Nb-junction are shown to demonstrate the capabilities for plasma diagnostics.

  11. 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.

  12. 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.

  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. 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.

  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.; et al.

    2005-01-01

    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. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. Applied possibilities for x-ray diffraction interferometry

    NASA Astrophysics Data System (ADS)

    Raransky, M. D.; Struk, J. M.; Fodchuk, Igor M.; Shafraniuk, V. P.; Raransky, A. M.

    1995-11-01

    Among existing x ray diffraction diagnostics nonperfections of crystals the specific location take methods are based on use of x-ray dynamic diffraction effects. From them the most sensitive are based on interferention. The Pendellosung and Moire fringes methods arise in consequence of coherent dynamic interaction of wave fields in single crystals. One of the main advantages of the Moire method is the extraordinary high sensitivity to insignificant deformations of crystal lattice ((Delta) d/d approximately 10-8) and atomic planes turns ((delta) approximately 0.01'). Created by a method of x-ray diffraction Moire the unique phase magnification permits us to directly observe the nuclear rows of crystal lattice. Until recently the attention of researchers attracted, basically, precise measurements of refraction parameters and dispersion amendments to nuclear scattering amplitudes, measurement of movy with large accuracy and refinement of Avogadro number, and the creation of new multi crystal interferometers. At the same time, little opportunities of x-ray interferometry at research of crystal structure defects were used. For the first time the opportunity of definition by method x-ray diffraction Moire of Burgers vectors of individual dislocation was demonstrated by M. Hart, Christiansen has studied the series of 60 degree(s) dislocation in Si on Moire images. Tensions in Si, caused by Ar ions implantation, were defined in the work. The purpose, which the authors of given reviews pursue consists in demonstration of new opportunities of x-ray three crystal interferometry in the investigation of single and complex defects.

  4. Bioimaging by X-Ray Laser Diffraction at SACLA

    NASA Astrophysics Data System (ADS)

    Bessho, Y.

    2013-11-01

    The XFEL facility, SACLA is soon expected to be useful for new bioimaging method with an accuracy on the order of ten femto-seconds. We recorded coherent X-ray diffraction patterns from intact Microbacterium cells in solution at SACLA.

  5. 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)

  6. 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.

  7. 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)

  8. 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.

  9. 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.

  10. X-Ray Diffraction from Live Muscle Fibres

    NASA Astrophysics Data System (ADS)

    Svensson, A.; Bordas, J.; de La Cuesta, F. B.

    The previous chapter shows how small-angle X-ray Diffraction can be used to study the organization of collagen fibres in tissue, proposing this technique as a diagnosis tool. In this chapter, synchrotron small-angle X-ray diffraction (SAXD) by using high-angle and temporal resolution is presented as an essential tool in structural functional studies of skeletal muscle tissues. SAXD studies of muscle fibres involve the combination of mechanical and diffraction methods and provide insights into the molecular mechanisms responsible for the generation of force and motion in active muscle. These studies are made possible because of the highly ordered arrangement of the contractile proteins, myosin and actin, in the sarcomere, the smallest functional repeating unit of the muscle cell. The possibility to collect diffraction diagrams with high angular and temporal resolutions at modern third-generation synchrotron radiation sources together with new data processing algorithms together and two-dimensional photon counting detectors allow structural and functional studies of live muscle tissues. The review covers the basics of X-ray small-angle diffraction, instrumentation and mathematical methods used in data analysis. A general description of each of these points has been presented in Chap.1 and 2. It provides new results on the axial disposition of the myosin heads and their interpretation from analysing the interference fringes that carve the diffraction orders into clusters of peaks.

  11. 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 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.

  12. 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, Sbastien; 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 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.

  13. 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.

  14. Illicit drug detection using energy dispersive x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

    2009-05-01

    Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

  15. 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.

  16. Automated identification and classification of single particle serial femtosecond X-ray diffraction data.

    PubMed

    Andreasson, Jakob; Martin, Andrew V; Liang, Meng; Timneanu, Nicusor; Aquila, Andrew; Wang, Fenglin; Iwan, Bianca; Svenda, Martin; Ekeberg, Tomas; Hantke, Max; Bielecki, Johan; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Hartmann, Robert; Erk, Benjamin; Rudek, Benedikt; Chapman, Henry N; Hajdu, Janos; Barty, Anton

    2014-02-10

    The first hard X-ray laser, the Linac Coherent Light Source (LCLS), produces 120 shots per second. Particles injected into the X-ray beam are hit randomly and in unknown orientations by the extremely intense X-ray pulses, where the femtosecond-duration X-ray pulses diffract from the sample before the particle structure is significantly changed even though the sample is ultimately destroyed by the deposited X-ray energy. Single particle X-ray diffraction experiments generate data at the FEL repetition rate, resulting in more than 400,000 detector readouts in an hour, the data stream during an experiment contains blank frames mixed with hits on single particles, clusters and contaminants. The diffraction signal is generally weak and it is superimposed on a low but continually fluctuating background signal, originating from photon noise in the beam line and electronic noise from the detector. Meanwhile, explosion of the sample creates fragments with a characteristic signature. Here, we describe methods based on rapid image analysis combined with ion Time-of-Flight (ToF) spectroscopy of the fragments to achieve an efficient, automated and unsupervised sorting of diffraction data. The studies described here form a basis for the development of real-time frame rejection methods, e.g. for the European XFEL, which is expected to produce 100 million pulses per hour. PMID:24663542

  17. 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.

  18. 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.

  19. Anomalous X-ray diffraction with soft X-ray synchrotron radiation.

    PubMed

    Carpentier, P; Berthet-Colominas, C; Capitan, M; Chesne, M L; Fanchon, E; Lequien, S; Stuhrmann, H; Thiaudire, D; Vicat, J; Zielinski, P; Kahn, R

    2000-07-01

    Anomalous diffraction with soft X-ray synchrotron radiation opens new possibilities in protein crystallography and materials science. Low-Z elements like silicon, phosphorus, sulfur and chlorine become accessible as new labels in structural studies. Some of the heavy elements like uranium exhibit an unusually strong dispersion at their M(V) absorption edge (lambdaMV = 3.497 A, E(MV) = 3545 eV) and so does thorium. Two different test experiments are reported here showing the feasibility of anomalous X-ray diffraction at long wavelengths with a protein containing uranium and with a salt containing chlorine atoms. With 110 electrons the anomalous scattering amplitude of uranium exceeds by a factor of 4 the resonance scattering of other strong anomalous scatterers like that of the lanthanides at their L(III) edge. The resulting exceptional phasing power of uranium is most attractive in protein crystallography using the multi-wavelength anomalous diffraction (MAD) method. The anomalous dispersion of an uranium derivative of asparaginyl-tRNA synthetase (hexagonal unit cell; a = 123.4 A, c = 124.4 A) has been measured for the first time at 4 wavelengths near the M(V) edge using the beamline ID1 of ESRF (Grenoble, France). The present set up allowed to measure only 30% of the possible reflections at a resolution of 4 A, mainly because of the low sensitivity of the CCD detector. In the second experiment, the dispersion of the intensity of 5 X-ray diffraction peaks from pentakismethylammonium undecachlorodibismuthate (PMACB, orthorhombic unit cell; a = 13.003 A, b = 14.038 A, c = 15.450 A) has been measured at 30 wavelengths near the K absorption edge of chlorine (lambdaK = 4.397 A, EK= 2819.6 eV). All reflections within the resolution range from 6.4 A to 3.4 A expected in the 20 degree scan were observed. The chemical state varies between different chlorine atoms of PMACB, and so does the dispersion of different Bragg peaks near the K-edge of chlorine. The results reflect the performance of the beamline ID1 of ESRF at wavelengths beyond 3 A at the end of 1998. A gain by a factor 100 for diffraction experiments with 4.4 A photons was achieved in Autumn 1999 when two focusing mirrors had been added to the X-ray optics. Further progress is expected from area detectors more sensitive to soft X-rays. Both CCD detectors and image plates would provide a gain of two orders of measured intensity. Image plates would have the additional advantage that they can be bent cylindrically and thus cover a larger solid angle in reciprocal space. In many cases, samples need to be cooled: closed and open systems are presented. A comparison with the state of art of soft X-ray diffraction, as it had been reached at HASYLAB (Hamburg, Germany), and as it is developing at the Brookhaven National Laboratory (USA), is given. PMID:10976874

  20. 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.

  1. High energy transmission annular beam X-ray diffraction.

    PubMed

    Dicken, Anthony; Shevchuk, Alex; Rogers, Keith; Godber, Simon; Evans, Paul

    2015-03-01

    We demonstrate material phase retrieval by linearly translating extended polycrystalline samples along the symmetry axis of an annular beam of high-energy X-rays. A series of pseudo-monochromatic diffraction images are recorded from the dark region encompassed by the beam. We measure Bragg maxima from different annular gauge volumes in the form of bright spots in the X-ray diffraction intensity. We present the experiment data from three materials with different crystallographic structural properties i.e. near ideal, large grain size and preferred orientation. This technique shows great promise for analytical inspection tasks requiring highly penetrating radiation such as security screening, medicine and non-destructive testing. PMID:25836851

  2. 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.

  3. 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 6070 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

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. X-ray diffraction analysis of barton oxides

    NASA Astrophysics Data System (ADS)

    de la Torre, A.; Torralba, M.; Garca, A.; Adeva, P.

    In consequence of the influence of the composition of Barton oxides on the behaviour of batteries, a method has been developed for the quantitative determination of orthorhombic and tetragonal monoxides. An X-ray diffraction, internal standard method was used. Factors such as diffraction peak overlapping and its method of measurement, type of radiation, particle size as a function of the mass absorption coefficient, and the wavelength used, were all taken into account. An operational method was established and a statistical error analysis was carried out. Although the error varies with both chemical species and concentration, it can be considered as acceptable.

  9. X-ray diffraction studies of amorphous materials

    NASA Astrophysics Data System (ADS)

    Palma, Joseph J., Jr.

    This thesis presents a study on two types of X-ray diffraction methodologies applied to the characterization of amorphous materials. The purpose of this study was to assess the feasibility of measuring the diffractive spectrum of amorphous materials by Energy-Dispersive X-ray Diffraction (EDXRD) utilizing Cadmium Zinc Telluride detectors. The total scattering intensity (coherent plus incoherent scatter) spectra precisely measured by high-energy Wide-Angle X-ray Scattering (WAXS) were compared to the EDXRD spectra to determine the level of agreement between the two techniques. The EDXRD spectra were constructed by applying a spectra fusing technique which combined the EDXRD spectra collected at different scattering angles rendering a continuous total scattering spectrum. The spectra fusing technique extended the momentum transfer range of the observed scattered spectrum beyond the limitations of the X-ray source and CZT detection efficiencies. Agreement between the WAXS and fused EDXRD spectra was achieved. In addition, this thesis presents the atomic pair correlation functions and coordination numbers of the first coordination shell for four hydrogen peroxide solutions of varying mass concentrations using Empirical Potential Structural Refinement (EPSR). The results are compared to the state-of-the art ad initio quantum mechanical charge field molecular dynamics (QMCF MD) model of the hydrogen peroxide in solution to support the model's predictions on why hydrogen peroxide is stable in water. The EPSR results using the coherent scattering intensity calculated from the WAXS data set predicts a hydration shell of 6.4 molecules of water surrounding hydrogen peroxide. The results also indicate that hydrogen peroxide is more likely to behave as a proton donor than acceptor. These findings are in agreement with QMCF MD model of aqueous hydrogen peroxide.

  10. 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.

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

    SciTech Connect

    Kuang Longyu; Wang Chuanke; Wang Zhebin; Cao Leifeng; Liu Shenye; Ding Yongkun; Zhu Xiaoli; Xie Changqing

    2010-07-15

    A gold transmission grating is used routinely to disperse the x-ray spectrum at the Z soft x-ray facility to measure the spectrum and temporal history of the absolute soft x-ray power emitted from z-pinch and hohlraum radiation sources. A quantum-dot-array diffraction grating (QDADG) of 250 lines/mm for soft x-ray is designed and fabricated for the first time according to the principle of binary sinusoidal transmission grating. The diffraction efficiencies of the grating are measured in the 150-300 eV photon energy range on the Beamline 3W1B of Beijing Synchrotron Radiation Facility. This article describes the basic concept and calibration techniques and presents calibration results. It is shown that the 250 lines/mm QDADG can be used to disperse light without higher-order diffractions in soft x-ray range, and the diffraction efficiencies of this grating are nearly constant (about 25%), which is beneficial in the spectrum analysis.

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

    PubMed

    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. PMID:20687723

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. A Computational Algorithm to Produce Virtual X-ray and Electron Diffraction Patterns from Atomistic Simulations

    NASA Astrophysics Data System (ADS)

    Coleman, Shawn P.; Sichani, Mehrdad M.; Spearot, Douglas E.

    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. This algorithm advances beyond previous virtual diffraction methods by using a high-resolution mesh of reciprocal space that eliminates the need for a priori knowledge of the crystal structure being modeled or other assumptions concerning the diffraction conditions. At each point on the reciprocal space mesh, the diffraction intensity is computed via explicit computation of the structure factor equation. To construct virtual selected-area electron diffraction patterns, a hemispherical slice of the reciprocal lattice mesh lying on the surface of the Ewald sphere is isolated and viewed along a specified zone axis. X-ray diffraction line profiles are created by binning the intensity of each reciprocal lattice point by its associated scattering angle, effectively mimicking powder diffraction conditions. The virtual diffraction algorithm is sufficiently generic to be applied to atomistic simulations of any atomic species. In this article, the capability and versatility of the virtual diffraction algorithm is exhibited by presenting findings from atomistic simulations of <100> symmetric tilt Ni grain boundaries, nanocrystalline Cu models, and a heterogeneous interface formed between ?-Al2O3 (0001) and ?-Al2O3 (111).

  18. 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.

  19. Identifications studies of Lauha Bhasma by X-ray diffraction and X-ray fluorescence

    PubMed Central

    Bhargava, S. C.; Reddy, K. R. C; Sastry, G. V. S

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe3O4 of magnetite is undergoing oxidation to Fe2O3. The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc. PMID:23049200

  20. Identifications studies of Lauha Bhasma by X-ray diffraction and X-ray fluorescence.

    PubMed

    Bhargava, S C; Reddy, K R C; Sastry, G V S

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe(3)O(4) of magnetite is undergoing oxidation to Fe(2)O(3). The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc. PMID:23049200

  1. X-ray spectroscopy to determine line coincidences

    SciTech Connect

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

    1983-01-31

    X-ray spectroscopy in the 12 to 15 A region of L-shell lines from selected transition elements was performed in a joint Naval Research Laboratory - KMS Fusion, Inc. experiment. The accurate wavelengths determined in this work will be utilized in selecting potential pumping candidates in future x-ray lasing schemes. Specifically, high-resolution x-ray spectra were collected under controlled geometric and target conditions using both red and green light laser excitation in the KMS Chroma laser. Three groups of x-ray spectra were collected with highly-dispersive x-ray crystals at wavelengths centered at 12.543, 13.781 and 14.458 A corresponding to He- and H-like lines from fluorine. Two specially-designed flat crystal spectrographs employing film shutters were used with pairs of beryl and TAP crystals. The spectra from potential lasant and pump candidates could be recorded on the same spectrogram to aid in identifying x-ray line coincidences. In cases where wavelengths were measured in both the red and green laser work, agreement within 1 to 3 mA was obtained for the L-series x-ray lines. Within this accuracy range, five L series x-ray lines, mostly 2p-3d transitions from the metals Cr, Mn, and Ni, had wavelength values coincident to K-series lines in fluorine.

  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. 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.

  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. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  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. X-ray Diffraction Studies of Striated Muscles

    SciTech Connect

    Squire, J.M.; Knupp, C.; Roessle, M.; Al-Khayat, H.A.; Irving, T.C.; Eakins, F.; Mok, N.-S.; Harford, J.J.; Reedy, M.K.

    2006-04-24

    In this short review a number of recent X-ray diffraction results on the highly ordered striated muscles in insects and in bony fish have been briefly described. What is clear is that this technique applied to muscles which are amenable to rigorous analysis, taken together with related data from other sources (e.g. protein crystallography, biochemistry, mechanics, computer modelling) can provide not only the best descriptions yet available on the myosin head organisations on different myosin filaments in the relaxed state, but can also show the sequence of molecular events that occurs in the contractile cycle, and may also help to explain such phenomena as stretch-activation. X-ray diffraction is clearly an enormously powerful tool in studies of muscle. It has already provided a wealth of detail on muscle ultrastructure; it is providing ever more fascinating insights into molecular events in the 50-year old sliding filament mechanism, and there remains a great deal more potential that is as yet untapped.

  15. Diffraction and holography of photoelectrons and fluorescent x-rays

    SciTech Connect

    Fadley, C.S. |

    1993-04-01

    Photoelectron diffraction is by now a powerful technique for studying surface structures, with special capabilities for resolving chemical and magnetic states of atoms and deriving direct structural information from both forward scattering and backscattering. Fitting experiment to theory can lead to structural accuracies in the 0.03 {Angstrom} range. Holographic inversions of such diffraction data also show considerable promise for deriving local three-dimensional structures around a given emitter with accuracies of 0.2--0.3 {Angstrom}. Resolving the photoelectron spin in some way and using circularly polarized radiation for excitation provide added dimensions for the study of magnetic systems and chiral experimental geometries. Synchrotron radiation with the highest brightness and energy resolution, as well as variable polarization, is crucial to the full exploitation of these techniques. X-ray fluorescence holography also has promise for structural studies, but will require intense excitation sources and multichannel detection to be feasible.

  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. (Diffraction gratings used in x-ray spectroscopy): Final report

    SciTech Connect

    Smith, H.I.

    1988-11-01

    This subcontract was initiated in order to facilitate the development at MIT of technologies for fabricating the very fine diffraction grating required in x-ray spectroscopy at Lawrence Livermore Laboratory (LLL). These gratings are generally gold transmission gratings with spatial periods of 200 nm or less. The major focus of our efforts was to develop a means of fabricating gratings of 100 nm period. We explored two approaches: e-beam fabrication of x-ray lithography masks, and achromatic holographic lithography. This work was pursued by Erik Anderson as a major component of his Ph.D. thesis. Erik was successful in both the e-beam and holographic approaches. However, the e-beam method proved to be highly impractical: exposure times of about 115 days would be required to cover an area of 1 cm/sup 2/. The achromatic holography, on the other hand, should be capable of exposing areas well in excess of 1 cm/sup 2/ in times under 1 hour. Moreover, 100 nm-period gratings produced by achromatic holography are coherent over their entire area whereas gratings produced by e-beam lithography are coherent only over areas /approximately/100 ..mu..m. The remainder of this report consists of portions excerpted from Erik Anderson's thesis. These contain all the details of our work on 100 nm period gratings. 26 refs., 17 figs.

  20. 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.

  1. X-ray diffraction characterization of thin superconductive films

    SciTech Connect

    Kozaczek, K.J.; Watkins, T.R.; Book, G.W.; Carter, W.B.

    1995-12-31

    The physical and mechanical properties of thin films are often different from the properties of bulk material and are dictated by the film/substrate orientation relationship, crystal anisotropy and crystalgraphic texture of the film. X-ray diffraction texture analysis provides information about preferential film growth and can be used for optimization of deposition parameters and prediction of properties of thin films. An x-ray back reflection technique using the Braga-Brentano geometry with experimental corrections for absorption and defocusing was used to study thin ceramic films deposited by combustion chemical vapor deposition (CCVD). The film/substrate orientation relationships of YBa{sub 2}Cu{sub 3}O{sub x} (YBCO) superconducting thin films deposited via CCVD on single crystal MgO and polycrystalline silver substrates were studied. The as-deposited films on single crystal (100) MgO substrates showed strong preferential growth with the basal plane parallel to the substrate surface (c-axis up growth). Texture analysis showed two in-plane alignment orientations of the film with respect to the substrate, with YBCO [100] and [110] aligned with the [100] MgO substrate. YBCO films deposited on cold-rolled polycrystalline silver displayed c-axis up growth indicating that the orientation of the polycrystalline substrate (brass type texture) did not induce detectable in-plane preferential growth of the YBCO.

  2. 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

  3. 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

  4. 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

  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 ? 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. 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.

  8. 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.

  9. 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.

  10. X-ray diffraction diagnostic design for the National Ignition Facility

    NASA Astrophysics Data System (ADS)

    Ahmed, Maryum F.; House, Allen; Smith, R. F.; Ayers, Jay; Lamb, Zachary S.; Swift, David W.

    2013-09-01

    This paper describes the design considerations for Target Diffraction In-Situ (TARDIS), an x-ray diffraction diagnostic at the National Ignition Facility. A crystal sample is ramp-compressed to peak pressures between 10 and 30 Mbar and, during a pressure hold period, is probed with quasi-monochromatic x-rays emanating from a backlighter source foil. The crystal spectrography diffraction lines are recorded onto image plates. The crystal sample, filter, and image plates are packaged into one assembly, allowing for accurate and repeatable target to image plate registration. Unconverted laser light impinges upon the device, generating debris, the effects of which have been mitigated. Dimpled blast shields, high strength steel alloy, and high-z tungsten are used to shield and protect the image plates. A tapered opening was designed to provide adequate thickness of shielding materials without blocking the drive beams or x-ray source from reaching the crystal target. The high strength steel unit serves as a mount for the crystal target and x-ray source foil. A tungsten body contains the imaging components. Inside this sub-assembly, there are three image plates: a 160 degree field of view curved plate directly opposite the target opening and two flat plates for the top and bottom. A polycarbonate frame, coated with the appropriate filter material and embedded with registration features for image plate location, is inserted into the diagnostic body. The target assembly is metrologized and then the diagnostic assembly is attached.

  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 from Point-Like Imperfection

    NASA Astrophysics Data System (ADS)

    He, Baoping

    1992-01-01

    Displacement fields from point-like defects are investigated by x-ray diffraction. The atomic volume changes in the interstitial compounds using crystallographic information has been found to correlate with the size of filled octahedral sites. Systematic correlations enable estimates to be made of the components of the dipole tensor for interstitials in octahedral sites for binary systems containing N, C, and O in V, Nb, Ta, Cr, Mo, W, and Fe lattices. X-ray diffraction analysis of the concentration and residual stress gradients in N implanted Mo crystals and Nb films show that the dominant source of internal strain arises from N located in octahedral sites. For Nb implanted at LNT, these distortion centers are aligned equally along three mutually perpendicular directions to maintain cubic symmetry. Large biaxial residual strains are developed after a 5at% implantation of N into Nb and Mo. Radiation damage is present as small vacancy and interstitial loops. A method was developed to obtain the orientation function for samples containing a fiber texture. A slit correction is included and the final results from this simplified approach are compared with the pole figure measured by direct chi-scanning. Knowing the orientation function allows one to correct the integrated intensities to that for an ideal powder, thereby allowing thermal and static displacements to be obtained from textured samples. Anisotropic displacements about coherent Be rich GP zones were investigated in a Cu-11-at%Be alloy. The results indicate that the attenuation factor 2M which determines the relative integrated intensities of Bragg, quasiline, and static diffuse scattering can be expressed in a simplified form. Experimental data of 2M for aged Cu-Be samples show an anisotropy. The anisotropy increases with increasing aging time when the equiaxed-GP zones formed in the early stage collapse into platelike GP zones.

  13. Phosphor Scanner For Imaging X-Ray Diffraction

    NASA Technical Reports Server (NTRS)

    Carter, Daniel C.; Hecht, Diana L.; Witherow, William K.

    1992-01-01

    Improved optoelectronic scanning apparatus generates digitized image of x-ray image recorded in phosphor. Scanning fiber-optic probe supplies laser light stimulating luminescence in areas of phosphor exposed to x rays. Luminescence passes through probe and fiber to integrating sphere and photomultiplier. Sensitivity and resolution exceed previously available scanners. Intended for use in x-ray crystallography, medical radiography, and molecular biology.

  14. 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.

  15. Coherent X-ray diffraction investigation of twinnedmicrocrystals.

    PubMed

    Aranda, Miguel A G; Berenguer, Felisa; Bean, Richard J; Shi, Xiaowen; Xiong, Gang; Collins, Stephen P; Nave, Colin; Robinson, Ian K

    2010-11-01

    Coherent X-ray diffraction has been used to study pseudo-merohedrally twinned manganite microcrystals. The analyzed compositions were Pr(5/8)Ca(3/8)MnO(3) and La(0.275)Pr(0.35)Ca(3/8)MnO(3). The prepared loose powder was thermally attached to glass (and quartz) capillary walls by gentle heating to ensure positional stability during data collection. Many diffraction data sets were recorded and some of them were split as expected from the main observed twin law: 180 rotation around [101]. The peak splitting was measured with very high precision owing to the high-resolution nature of the diffraction data, with a resolution (?d/d) better than 2.0 10(-4). Furthermore, when these microcrystals are illuminated coherently, the different crystallographic phases of the structure factors induce interference in the form of a speckle pattern. The three-dimensional speckled Bragg peak intensity distribution has been measured providing information about the twin domains within the microcrystals. Research is ongoing to invert the measured patterns. Successful phase retrieval will allow mapping out the twin domains and twin boundaries which play a key role in the physical properties. PMID:20975220

  16. 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.

  17. 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 1020 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.

  18. 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

  19. 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.

  20. 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.

  1. 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.

  2. X-Ray Diffraction of Shock Compressed H2O

    NASA Astrophysics Data System (ADS)

    Gleason, A. E.

    2014-12-01

    H2O, critical for life and ubiquitous in biology, is one of the most abundant molecules in the solar system and is relevant to many fields, including fundamental physics and chemistry. Phase transformation information of H2O is also important to applied areas like planetary science where it is a constituent of giant planets Neptune and Uranus, icy satellites (e.g., Europa, Ganymede), and extrasolar planets (icy "super-Earths"). Using the MEC (Matter in Extreme Conditions) hutch at LCLS, we reach simultaneous high pressure (P) and temperature (T) with laser-driven shock waves and the capability of taking snapshots during a dynamic process with the X-ray Free Electron Laser (xFEL). We report the only shock-driven diffraction data on H2O ever collected to date, and examine time-resolved diffraction from ice Ih to high pressure ice VII. At 2 Mbar we find evidence of ice X - this has significant implications for planetary interiors and providing a bound for the onset of the superionic phase.

  3. A study of monochromatic x-ray area beam for application in diffraction enhanced imaging

    NASA Astrophysics Data System (ADS)

    Kim, Chang Hyeuk

    Synchrotron-based Diffraction Enhanced Imaging (DEI) system has shown improved contrast images on low attenuation material. In a previous DEI study great potential to detect earlier stage breast cancer was reported. However, to apply DEI technique at the clinical level, a synchrotron source is not feasible for clinically-approved systems due to the size of the accelerator, and hence a compact x-ray source that can replace synchrotron is desirable. Development of an x-ray source compatible to synchrotron radiation is an essential part for a clinical DEI system. Some important features for the design of an x-ray source, based on synchrotron radiation, are the photon flux and beam collimation. The NCSU research group suggested a wide-beam x-ray source, which consists of concentric circular filaments producing electron flux onto a cylindrically-shaped oxygen-free copper stationary target with a thin layer of Molybdenum for x-ray production. This source design emphasizes large field of view, which can eliminate the line by line scanning process experienced in a DEI experimental setup. In this study, the proof of principle model of a wide beam x-ray source was used to study for control electron trajectory of the concentric filaments design, calculations of the produced x-ray flux, simulation of the DEI imaging, and estimation of the operation time with target's active cooling system. The DEI images from the electron distribution were computationally generated by adopting a monochromator and an analyzer with a computationally generated dual cylindrical object. The image simulation showed that the wide-beam x-ray source based DEI images are highly dependent on the electron distribution at the target. Uniform electron distribution by electron trajectory optimization is carried out through independent powering of the filaments inside the focusing cup. For higher electron beam current the x-ray flux satisfies obtaining a successful DEI image scan, but such high current increases the heat loading on the target. The target cooling with a contact cold finger does not provide sufficient thermal management, and hence not enough scanning time. The impinging jet nozzle cooling option was investigated to maximize convective heat transfer, and has shown feasible thermal management and adequate operation time for DEI imaging.

  4. 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.

  5. Unit cell determination in CuZr martensite by electron microscopy and X-ray diffraction

    SciTech Connect

    Schryvers, D.; Seo, J.W.; Firstov, G.S.; Koval, Yu.N.; Humbeeck, J. Van

    1997-05-15

    As several other binary alloy compounds, stoichiometric CuZr has a B2 phase with a CsCl type bcc based structure. In the present system this phase appears as a line compound between 715 C and 935 C. Rapid cooling to below 140 C transforms this phase into at least two monoclinic structures which have been shown to have martensitic characteristics, not unusual for B2 phase alloys, including shape memory behavior. Unit cell dimensions for both monoclinic phases, one about twice the size of the other, were previously suggested on the basis of powder X-ray diffractometry and limited electron microscopy results. The aim of the current investigation was to confirm or correct these unit cells by extensive selected area electron diffraction (SAED), high resolution electron microscopy (HREM) and improved fitting procedures of the existing X-ray diffraction data. The crystallographic relation between parent and product phases will also be discussed.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. Flash X-Ray Diffraction System for Fast, Single-PulseTemperature and Phase Transition Measurements (Pre-print)

    SciTech Connect

    Michael J. Madlener; Dane V. Morgan

    2007-06-12

    A new, fast, single-pulse diagnostic for determining phase transitions and measuring the bulk temperature of polycrystalline metal objects has been developed. The diagnostic consists of a 37-stage Marx bank with a cable-coupled X-ray diode that produces a 35-ns pulse of mostly 0.71-{angstrom} monochromatic X rays and a P-43 fluor coupled to a cooled, charge-coupled device camera by a coherent fiber-optic bundle for detection of scattered X rays. The X-ray beam is collimated to a 1{sup o} divergence in the scattering plane with the combination of a 1.5-mm tungsten pinhole and a 1.5-mm-diameter molybdenum anode. X rays are produced by a high-energy electron beam transiting inward from the cathode to the anode in a needle-and-washer configuration. The anode's characteristic K-{alpha} X-ray emission lines are utilized for this diffraction system. The X-ray anode is heavily shielded in all directions other than the collimated beam. The X-ray diode has a sealed reentrant system, allowing X rays to be produced inside a vacuum containment vessel, close to the sample under study.

  11. 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

  12. Cinnamomin: separation, crystallization and preliminary X-ray diffraction study.

    PubMed

    Wang, T; Zou, Y-S; Zhu, D-W; Azzi, A; Liu, W-Y; Lin, S-X

    2008-02-01

    Cinnamomin from Cinnamonum camphora seeds, a type II ribosome-inactivating protein that interferes with protein biosynthesis in mammalian cells, can induce the apoptosis of carcinoma cells and be used as an insecticide. A rapid and improved method has been developed for the extraction and purification of cinnamomin from camphora seed. Purification of cinnamomin is achieved with two successive steps of hydrophobic interaction chromatography carried out on a fast protein liquid chromatography (FPLC) system. Crystals suitable for X-ray diffraction analysis were obtained by vapor diffusion method. A complete data set at 2.8 A resolution has been collected. Data indexation and refinement indicate that the crystal is orthorhombic with space group P2(1)2(1)2(1) and unit cell dimensions a = 52.39 A, b = 126.33 A, c = 161.45 A. There are two molecules per asymmetric unit. Initial phasing by molecular replacement method yielded a solution, which will contribute to the structure determination. A molecular model will further the understanding of the mechanism of cinnamomin function. The latter will be combined with bio-informatics to facilitate the medical and other applications of cinnamomin. PMID:17404804

  13. 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.

  14. 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.

  15. X-ray diffraction and extended X-ray absorption fine structure study using synchrotron radiation of cobalt (II) complexes

    NASA Astrophysics Data System (ADS)

    Mishra, Ashotosh; Shukla, Kritika; Dwivedi, Jagrati; Ninama, Samrath

    2014-09-01

    XRD and EXAFS investigation of cobalt (II) macro cyclic complexes were carried out. These complexes were synthesised by chemical rout method. On the analysis of the complexes with X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS), XRD analysis shows that complexes are crystalline in nature and having particle size and lattice parameter in the rang of few micro meter and EXAFS technique extract the local structure of complexes. The nearest neighbouring atom distance commonly known as 'bond length' were calculated using Fourier transform method. The bond lengths determined from these methods were also compared with the bond length obtained from several other known technique.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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).

  2. 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....

  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. 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

  6. X-ray Line Profile Variations During Quasar Microlensing

    NASA Astrophysics Data System (ADS)

    Heyrovsky, David; Ledvina, Lukas; Dovciak, Michal

    2016-01-01

    Observations of gravitationally lensed quasars have revealed X-ray line profile variations occurring during microlensing events. We simulate the effect using a simple model: a microlensing fold caustic crossing a spatially resolved model of Fe K? line emission from a thin accretion disk around a Kerr black hole. We demonstrate the appearance of additional peaks and edges in the line profile. We illustrate the underlying mechanism of their generation and derive analytical expressions for their shape.

  7. 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.

  8. 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.

  9. 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.

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

    PubMed

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

    2014-11-01

    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

  11. 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

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

    NASA Astrophysics Data System (ADS)

    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 ?m) aluminum foil as X-ray window as a non-toxic alternative to conventional beryllium windows. Owing to the reduced thickness, diffraction patterns and their changes during cycling can be observed with excellent quality, which was demonstrated for two cathode materials for sodium-ion batteries in a half-cell set-up, P2-Na0.7MnO2 and Na2.55V6O16 ? 0.6H2O.

  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. 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.

  15. Lensless Diffractive Imaging Using Tabletop Coherent High-Harmonic Soft-X-Ray Beams

    SciTech Connect

    Sandberg, Richard L.; Paul, Ariel; Raymondson, Daisy A.; Haedrich, Steffen; Gaudiosi, David M.; Holtsnider, Jim; Tobey, Ra'anan I.; Cohen, Oren; Murnane, Margaret M.; Kapteyn, Henry C.; Song, Changyong; Miao Jianwei; Liu Yanwei; Salmassi, Farhad

    2007-08-31

    We present the first experimental demonstration of lensless diffractive imaging using coherent soft x rays generated by a tabletop soft-x-ray source. A 29 nm high harmonic beam illuminates an object, and the subsequent diffraction is collected on an x-ray CCD camera. High dynamic range diffraction patterns are obtained by taking multiple exposures while blocking small-angle diffraction using beam blocks of varying size. These patterns reconstruct to images with 214 nm resolution. This work demonstrates a practical tabletop lensless microscope that promises to find applications in materials science, nanoscience, and biology.

  16. 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

  17. Chromium Environment within Cr-Doped BaAl2O4: Correlation of X-ray Diffraction and X-ray Absorption Spectroscopy Investigations.

    PubMed

    Vranki?, Martina; Greta, Biserka; Ltzenkirchen-Hecht, Dirk; Bosnar, Sanja; ari?, Ankica

    2015-12-01

    Powder BaAl2O4 samples doped with 0 and 1.76 atom % Cr in relation to Al were hydrothermally prepared. Both samples were characterized by X-ray diffraction and synchrotron based X-ray absorption spectroscopy at the Cr K- and the Ba L3-edge. Diffraction patterns indicated that samples were nanocrystalline with a hexagonal crystal structure, space group P63. Chromium doping of barium aluminate caused an increase of the unit-cell volume and diffraction line broadening. The doped sample contained a small amount of an impurity phase, namely, BaCrO4. Analyzed Cr K-edge X-ray absorption near edge structure for the doped sample showed the presence of chromium in 6+ and 3+ oxidation states: Cr(6+) was characteristic for chromium in the impurity phase BaCrO4, while Cr(3+) participated in the formation of the doped phase BaAl2O4:Cr. Extended X-ray absorption fine structure suggested an unusual tetrahedral coordination of Cr(3+) ions within the BaAl2O4 host phase. The structure of samples was refined by the Rietveld method, simultaneously with the analysis of diffraction line broadening. Rietveld structure refinement showed that in doping the Cr(3+) ions likely substituted for Al(3+) ions on Al1 tetrahedral sites of barium aluminate crystal lattice. Crystallite sizes in the samples decreased with chromium doping, from 32 nm for pure BaAl2O4 to 24 nm for Cr-doped BaAl2O4. The dopant Cr(3+) cations acted as defects in the barium aluminate structure that increased lattice strain from 0.02% for pure BaAl2O4 to 0.14% for doped BaAl2O4 and disturbed the crystallites to grow. PMID:26588707

  18. Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum

    NASA Astrophysics Data System (ADS)

    Morgan, Dane V.; Macy, Don; Stevens, Gerald

    2008-11-01

    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 K? 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 K? line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 36 mm2 spot and 1 full width half maximum 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 camera through a coherent fiber-optic 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 aluminum lattice with no phase transformation.

  19. 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.

  20. Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

    PubMed

    Morgan, Dane V; Macy, Don; Stevens, Gerald

    2008-11-01

    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 K(alpha) 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 K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum 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 degrees . 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 camera through a coherent fiber-optic 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 aluminum lattice with no phase transformation. PMID:19045900

  1. 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.

  2. 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.

  3. (X-ray diffraction experiments with condenser matter)

    SciTech Connect

    Coppens, P.

    1990-01-01

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

  4. 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.

  5. 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.

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

    PubMed Central

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

    2011-01-01

    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. PMID:21547016

  7. 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.

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

    NASA Astrophysics Data System (ADS)

    Matulkov, Irena; Holec, Petr; N?mec, Ivan; Kitazawa, Hideaki; Furubayashi, Takao; Vejpravov, Jana

    2015-06-01

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

  9. 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.

  10. 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.

  11. 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.

  12. 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...

  13. Determination of structural chirality of berlinite and quartz using resonant x-ray diffraction with circularly polarized x-rays

    NASA Astrophysics Data System (ADS)

    Tanaka, Yoshikazu; Kojima, Taro; Takata, Yasutaka; Chainani, Ashish; Lovesey, Stephen W.; Knight, Kevin S.; Takeuchi, Tomoyuki; Oura, Masaki; Senba, Yasunori; Ohashi, Haruhiko; Shin, Shik

    2010-04-01

    Many proteins, sugars, and pharmaceuticals crystallize into two forms that are mirror images of each other (enantiomers) such as our right and left hands (chiral). Berlinite (AlPO4) and low quartz (SiO2) have enantiomers belonging to a space-group pair, P3121 (right-handed screw) and P3221 (left-handed screw). We use circularly polarized resonant x-ray diffraction to study structural chirality. Our results demonstrate that positive and negative circularly polarized x-rays at the resonant energy of berlinite ( Al1s edge) and low quartz ( Si1s edge) can distinguish the absolute structure (right or left-handed screw) of an enantiomer. The advantage of our method is that the measurement of only one space-group forbidden reflection is enough to determine the chirality. This method is applicable to chiral motifs that occur in biomolecules, liquid crystals, ferroelectrics and antiferroelectrics, multiferroics, etc.

  14. 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.

  15. Curved anode wire chambers for x-ray diffraction applications

    SciTech Connect

    Perez-Mendez, V.; Wiedenbeck, P.; Wagner, C.N.J.; Woelfel, E.

    1983-01-01

    Curved position sensitive proportional detectors are described. The first has a radius of curvature of 135 mm and a 60/sup 0/ angular range. The second has a radius of curvature of 360 mm and a 45/sup 0/ angular range. For high quantum efficiency for x-ray energies up to 60 keV, a relatively large x-ray path and high gas pressure are required. The anode wires are suspended in circular arcs by the interaction of a current flowing through them and a magnetic field provided by two permanent magnets placed above and below the wire running parallel to it over the full length of the curved chambers. Anode wire stability under the combined action of the magnetic and electrostatic forces is discussed. (LEW)

  16. 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

  17. 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.

  18. Electrochemical in situ reaction cell for X-ray scattering, diffraction and spectroscopy.

    PubMed

    Braun, A; Shrout, S; Fowlks, A C; Osaisai, B A; Seifert, S; Granlund, E; Cairns, E J

    2003-07-01

    A versatile electrochemical in situ reaction cell for long-term hard X-ray experiments on battery electrodes is described. Applications include the small-angle scattering, diffraction and absorption spectroscopy of lithium manganese oxide electrodes. PMID:12824932

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

    NASA Astrophysics Data System (ADS)

    Andreeva, N. S.

    2006-12-01

    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.

  20. Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

    NASA Astrophysics Data System (ADS)

    Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffire, J. Y.

    2010-12-01

    The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

  1. 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.

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

    DOEpatents

    Berman, Robert M. (Pittsburgh, PA); Cohen, Isadore (Pittsburgh, PA)

    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.

  3. 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.

  4. 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.

  5. X-Ray Fiber Diffraction Recordings from Oriented Demembranated Chlamydomonas Flagellar Axonemes.

    PubMed

    Toba, Shiori; Iwamoto, Hiroyuki; Kamimura, Shinji; Oiwa, Kazuhiro

    2015-06-16

    The high homology of its axonemal components with humans and a large repertoire of axonemal mutants make Chlamydomonas a useful model system for experiments on the structure and function of eukaryotic cilia and flagella. Using this organism, we explored the spatial arrangement of axonemal components under physiological conditions by small-angle x-ray fiber diffraction. Axonemes were oriented in physiological solution by continuous shear flow and exposed to intense and stable x rays generated in the synchrotron radiation facility SPring-8, BL45XU. We compared diffraction patterns from axonemes isolated from wild-type and mutant strains lacking the whole outer arm (oda1), radial spoke (pf14), central apparatus (pf18), or the ?-chain of the outer arm dynein (oda11). Diffraction of the axonemes showed a series of well-defined meridional/layer-line and equatorial reflections. Diffraction patterns from mutant axonemes exhibited a systematic loss/attenuation of meridional/layer-line reflections, making it possible to determine the origin of various reflections. The 1/24 and 1/12nm(-1) meridional reflections of oda1 and oda11 were much weaker than those of the wild-type, suggesting that the outer dynein arms are the main contributor to these reflections. The weaker 1/32 and 1/13.7nm(-1) meridional reflections from pf14 compared with the wild-type suggest that these reflections come mainly from the radial spokes. The limited contribution of the central pair apparatus to the diffraction patterns was confirmed by the similarity between the patterns of the wild-type and pf18. The equatorial reflections were complex, but a comparison with electron micrograph-based models allowed the density of each axonemal component to be estimated. Addition of ATP to rigor-state axonemes also resulted in subtle changes in equatorial intensity profiles, which could report nucleotide-dependent structural changes of the dynein arms. The first detailed description of axonemal reflections presented here serves as a landmark for further x-ray diffraction studies to monitor the action of constituent proteins in functional axonemes. PMID:26083924

  6. 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.

  7. Measurement of piezoelectric constants of lanthanum-gallium tantalate crystal by X-ray diffraction methods

    SciTech Connect

    Blagov, A. E.; Marchenkov, N. V. Pisarevsky, Yu. V.; Prosekov, P. A.; Kovalchuk, M. V.

    2013-01-15

    A method for measuring piezoelectric constants of crystals of intermediate systems by X-ray quasi-multiple-wave diffraction is proposed and implemented. This technique makes it possible to determine the piezoelectric coefficient by measuring variations in the lattice parameter under an external electric field. This method has been approved, its potential is evaluated, and a comparison with high-resolution X-ray diffraction data is performed.

  8. X-ray diffraction characterization of suspended structures forMEMS applications

    SciTech Connect

    Goudeau, P.; Tamura, N.; Lavelle, B.; Rigo, S.; Masri, T.; Bosseboeuf, A.; Sarnet, T.; Petit, J.-A.; Desmarres, J.-M.

    2005-09-15

    Mechanical stress control is becoming one of the major challenges for the future of micro and nanotechnologies. Micro scanning X-ray diffraction is one of the promising techniques that allows stress characterization in such complex structures at sub micron scales. Two types of MEMS structure have been studied: a bilayer cantilever composed of a gold film deposited on poly-silicon and a boron doped silicon bridge. X-ray diffraction results are discussed in view of numerical simulation experiments.

  9. Second order x-ray in-line phase-contrast imaging

    NASA Astrophysics Data System (ADS)

    Cong, Wenxiang; Wang, Ge

    2014-09-01

    X-ray phase imaging is sensitive to structural variation of soft tissue, and offers excellent contrast resolution for characterization of cancerous tissues. Also, the cross-section of x-ray phase shift is a thousand times greater than that of x-ray attenuation in soft tissue over the diagnostic energy range, allowing a much higher signal-to-noise ratio at a substantially lower radiation dose than attenuation-based x-ray imaging. In this paper, we present a second order approximation model with respect to phase shift based on the paraxial Fresnel-Kirchhoff diffraction theory, and also discuss in-line dark-field imaging based on the second order model. This proposed model accurately establishes a quantitative correspondence between phases and recorded intensity images, outperforming the linear phase approximation model widely used in the conventional methods of x-ray in-line phase-contrast imaging. This new model can be iteratively solved using the algebraic reconstruction technique (ART). The state of the art compressive sensing ingredients can be incorporated to achieve high quality image reconstruction. Our numerical simulation studies demonstrate the feasibility of the proposed approach that is more accurate and stable, and more robust against noise than the conventional approach.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. Bragg diffraction using a 100ps 17.5 keV x-ray backlighter and the Bragg Diffraction Imager

    SciTech Connect

    Maddox, B R; Park, H; Hawreliak, J; Comley, A; Elsholz, A; Van Maren, R; Remington, B A; Wark, J

    2010-05-13

    A new diagnostic for measuring Bragg diffraction from a laser-driven crystal using a 100ps 17.5 kV x-ray backlighter source is designed and tested successfully at the Omega EP laser facility on static Mo and Ta single crystal samples using a Mo Ka backlighter. The Bragg Diffraction Imager (BDI) consists of a heavily shielded enclosure and a precisely positioned beam block, attached to the main enclosure by an Aluminum arm. Image plate is used as the x-ray detector. The diffraction lines from Mo and Ta <222> planes are clearly detected with a high signal-to-noise using the 17.5 keV and 19.6 keV characteristic lines generated by a petawatt-driven Mo foil. This technique will be applied to shock and ramp-loaded single crystals on the Omega EP laser. Pulsed x-ray diffraction of shock- and ramp-compressed materials is an exciting new technique that can give insight into the dynamic behavior of materials at ultra-high pressure not achievable by any other means to date. X-ray diffraction can be used to determine not only the phase and compression of the lattice at high pressure, but by probing the lattice compression on a timescale equal to the 3D relaxation time of the material, information about dislocation mechanics, including dislocation multiplication rate and velocity, can also be derived. Both Bragg, or reflection, and Laue, or transmission, diffraction have been developed for shock-loaded low-Z crystalline structures such as Cu, Fe, and Si using nano-second scale low-energy implosion and He-{alpha} x-ray backlighters. However, higher-Z materials require higher x-ray probe energies to penetrate the samples, such as in Laue, or probe deep enough into the target, as in the case of Bragg diffraction. Petawatt laser-generated K{alpha} x-ray backlighters have been developed for use in high-energy radiography of dense targets and other HED applications requiring picosecond-scale burst of hard x-rays. While short pulse lasers are very efficient at producing high-energy x-rays, the characteristic x-rays produced in these thin foil targets are superimposed on a broad bremsstrahlung background and can easily saturate a detector if careful diagnostic shielding and experimental geometry are not implemented. A new diagnostic has been designed to measure Bragg diffraction from laser-driven crystal targets using characteristic x-rays from a short-pulse laser backlighter on the Omega EP laser. The Bragg Diffraction Imager, or BDI, is a TIM-mounted instrument consisting of a heavily shielded enclosure made from 3/8-inch thick Heavymet (W-Fe-Ni alloy) and a precisely positioned beam bock, attached to the main enclosure by an Aluminum arm. The beam block is made of 1-inch thick, Al-coated Heavymet and serves to block the x-rays directly from the petawatt backlight, while allowing the diffraction x-rays from the crystal to pass to the enclosure. A schematic of the BDI is shown in Fig. 1a. Image plates are used as the x-ray detector and are loaded through the top of the diagnostic in an Aluminum, light-tight cartridge. The front of the enclosure can be fitted with various filters to maximize the diffraction signal-to-noise.

  17. The Use of Transient X-ray Diffraction for Shock Wave and High Pressure Materials Science

    NASA Astrophysics Data System (ADS)

    Hauer, A.; Kyrala, G.; Kopp, R.; Thoma, D.; Chen, K.; Chu, F.; Wilson, D.; Cobble, J.; Gobby, P.; Foreman, L.; Wark, J.; Loveridge, A.; Kalantar, D.; Remington, B.; Weber, S.; Asay, J.; Hall, C.; Trucano, T.

    1998-11-01

    Transient x-ray diffraction is powerful tool for the study of shock wave propagation and materials effects in the condensed state. Some of the phenomena that can be studied are plastic wave propagation, and the dynamics of phase transitions. We report on an on-going series of experiments on the Trident laser at Los Alamos and the Nova laser at Livermore that illustrate the value of transient diffraction. If significant plastic deformation occurs a diffracted signal from planes orthogonal to the shock propagation might be expected. We have observed such a signal in experiments with LiF crystals. Similar experiments with silicon exhibit other interesting phenomena such as the splitting of diffracted lines which may give temporally resolved information on phase changes. We have applied transient diffraction to the study of Be which is one of the most promising materials for the fuel containing capsule in inertial confinement fusion (ICF) target designs that may achieve ignition. We report on time resolved diffraction measurements using Be crystals that will help to clarify the behavior of Be in laser driven implosions. This work was performed under the auspices of the U. S. Department of Energy by the Los Alamos National Laboratory under contract No. W-7405-Eng-36.

  18. 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.

  19. 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.

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

    SciTech Connect

    LeBeau, J. M.; Engel-Herbert, R.; Jalan, B.; Cagnon, J.; Moetakef, P.; Stemmer, S.; Stephenson, G. B.; Materials Science Division; Univ. of California at Santa Barbara

    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.

  1. 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 K? 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 K? radiation (0.834 nm, 1.49 keV). PMID:23632552

  2. 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

  3. 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

  4. 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.

  5. 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.

  6. 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.

  7. First results from a next-generation off-plane X-ray diffraction grating

    NASA Astrophysics Data System (ADS)

    McEntaffer, Randall; DeRoo, Casey; Schultz, Ted; Gantner, Brennan; Tutt, James; Holland, Andrew; O'Dell, Stephen; Gaskin, Jessica; Kolodziejczak, Jeffrey; Zhang, William W.; Chan, Kai-Wing; Biskach, Michael; McClelland, Ryan; Iazikov, Dmitri; Wang, Xinpeng; Koecher, Larry

    2013-08-01

    Future NASA X-ray spectroscopy missions will require high throughput, high resolving power grating spectrometers. Off-plane reflection gratings are capable of meeting the performance requirements needed to realize the scientific goals of these missions. We have identified a novel grating fabrication method that utilizes common lithographic and microfabrication techniques to produce the high fidelity groove profile necessary to achieve this performance. Application of this process has produced an initial pre-master that exhibits a radial (variable line spacing along the groove dimension), high density (> 6000 grooves/mm), laminar profile. This pre-master has been tested for diffraction efficiency at the BESSY II synchrotron light facility and diffracts up to 55 % of incident light into usable spectral orders. Furthermore, tests of spectral resolving power show that these gratings are capable of obtaining resolving powers well above 1300 ( ?/? ?) with limitations due to the test apparatus, not the gratings. Obtaining these results has provided confidence that this fabrication process is capable of producing off-plane reflection gratings for the next generation of X-ray observatories.

  8. 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.

  9. 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.

  10. 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.

  11. Versatile wide angle diffraction setup for simultaneous wide and small angle x-ray scattering measurements with synchrotron radiation

    SciTech Connect

    Rueda, D.R.; Garcia-Gutierrez, M.C.; Nogales, A.; Capitan, M.J.; Ezquerra, T.A.; Labrador, A.; Fraga, E.; Beltran, D.; Juanhuix, J.; Herranz, J.F.; Bordas, J.

    2006-03-15

    Here we present a novel, simple, and versatile experimental setup aimed to perform wide angle x-ray scattering (WAXS) measurements alone or in simultaneous combination with small angle x-ray scattering measurements. The design of the WAXS goniometer allows one to obtain high resolution diffraction patterns in a broad angular range. The setup can incorporate a hot stage in order to evaluate temperature resolved experiments. The performance of the equipment has been verified in the BM16 beam line of the European Synchrotron Radiation Facility with different well known samples such as alumina, isotropic film of high density polyethylene (HDPE), and oriented HPDE fiber.

  12. 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.

  13. Stress measurement with two-dimensional X-ray diffraction

    NASA Astrophysics Data System (ADS)

    He, Bob B.

    2002-05-01

    2D diffraction systems, when used for residual stress measurement, have many advantages over the conventional 1D diffraction systems in dealing with highly textured materials, large grain size, small sample area, and weak diffraction systems in dealing with highly textured materials, large grain size, small sample area, and weak diffraction. The stress measurement is based on the fundamental relationship between the stress tensor and the diffraction cone distortion. The benefit of the 2D method is that all the data points on diffraction rings are used to calculate stresses so as to get better measurement result with less data collection time. The present paper introduces the recent development in the theory and applications of stress measurement using 2D detectors.

  14. 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

  15. 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.

  16. Closing the gap to the diffraction limit: Near wavelength limited tabletop soft x-ray coherent diffractive imaging

    NASA Astrophysics Data System (ADS)

    Sandberg, Richard Lunt

    Light microscopy has greatly advanced our understanding of nature. The achievable resolution, however, is limited by optical wavelengths to around 200 nm. Using novel imaging and labeling technologies, resolutions beyond the diffraction limit can be achieved for specialized specimens using techniques such as near-field scanning optical microscopy, stimulated emission depletion microscopy and structured illumination microscopy [1--3]. This dissertation presents a versatile soft x-ray diffraction microscope with 50 nm resolution using tabletop coherent soft x-ray sources. This work represents the first high resolution demonstrations of coherent diffractive or lensless imaging using tabletop extreme ultraviolet and soft x-ray sources [4, 5]. This dissertation also presents the first use of field curvature correction in x-ray coherent imaging which allows high numerical aperture imaging and near-diffraction-limited resolution of 1.5lambda. The relevant theory behind high harmonic generation, the primary tabletop source used in this work, will be discussed as well as the theory behind coherent diffractive imaging. Additionally, the first demonstration of tabletop soft x-ray Fourier Transform holography is shown with important applications to shorter wavelength imaging with high harmonic generation with limited flux. A tabletop soft x-ray diffraction microscope should find broad applications in biology, nanoscience, and materials science due to its simple optical design, high resolution, large depth of field, 3D imaging capability, scalability to shorter wavelengths, and ultrafast temporal resolution.

  17. Comparison of a CCD and an APS for soft X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Stewart, Graeme; Bates, R.; Blue, A.; Clark, A.; Dhesi, S. S.; Maneuski, D.; Marchal, J.; Steadman, P.; Tartoni, N.; Turchetta, R.

    2011-12-01

    We compare a new CMOS Active Pixel Sensor (APS) to a Princeton Instruments PIXIS-XO: 2048B Charge Coupled Device (CCD) with soft X-rays tested in a synchrotron beam line at the Diamond Light Source (DLS). Despite CCDs being established in the field of scientific imaging, APS are an innovative technology that offers advantages over CCDs. These include faster readout, higher operational temperature, in-pixel electronics for advanced image processing and reduced manufacturing cost. The APS employed was the Vanilla sensor designed by the MI3 collaboration and funded by an RCUK Basic technology grant. This sensor has 520 x 520 square pixels, of size 25 ?m on each side. The sensor can operate at a full frame readout of up to 20 Hz. The sensor had been back-thinned, to the epitaxial layer. This was the first time that a back-thinned APS had been demonstrated at a beam line at DLS. In the synchrotron experiment soft X-rays with an energy of approximately 708 eV were used to produce a diffraction pattern from a permalloy sample. The pattern was imaged at a range of integration times with both sensors. The CCD had to be operated at a temperature of -55C whereas the Vanilla was operated over a temperature range from 20C to -10C. We show that the APS detector can operate with frame rates up to two hundred times faster than the CCD, without excessive degradation of image quality. The signal to noise of the APS is shown to be the same as that of the CCD at identical integration times and the response is shown to be linear, with no charge blooming effects. The experiment has allowed a direct comparison of back thinned APS and CCDs in a real soft x-ray synchrotron experiment.

  18. X-ray line formation in radiation dominated astrophysical plasmas

    NASA Astrophysics Data System (ADS)

    Loisel, G.; Bailey, J. E.; Hansen, S. B.; Nagayama, T.; Rochau, G. A.; Liedahl, D.; Mancini, R.; Koepke, M.

    2014-10-01

    A remarkable opportunity to observe matter in a regime where the effects of General Relativity are significant has arisen through measurements of strongly red-shifted iron x-ray lines emitted from black hole accretion disks. A major uncertainty in the spectral formation models is the efficiency of Resonant Auger Destruction (RAD), in which fluorescent Ka photons are resonantly absorbed by neighbor ions. The absorbing ion preferentially decays by Auger ionization, thus reducing the emerging Ka intensity. If Ka lines from L-shell ions are not observed in iron spectral emission, why are such lines observed from silicon plasma surrounding other accretion powered objects? To help answer this question, we are investigating photoionized silicon plasmas produced using intense x-rays from the Z facility. For the first time in a terrestrial lab, we measured simultaneous absorption and emission spectra from these plasmas at high resolution. The charge state distribution, electron temperature, and electron density are determined through space-resolved absorption spectra. The emission spectra have been recorded at different column densities thus testing different radiative transport regime. These should allow us to answer quantitatively the original RAD hypothesis. Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under Contract DE-AC04-94AL85000.

  19. 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.

  20. In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell.

    PubMed

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

    2007-06-01

    We report a first combination of diamond anvil cell radial x-ray diffraction with in situ laser heating. The laser-heating setup of ALS beamline 12.2.2 was modified to allow one-sided heating of a sample in a diamond anvil cell with an 80 W yttrium lithium fluoride laser while probing the sample with radial x-ray diffraction. The diamond anvil cell is placed with its compressional axis vertical, and perpendicular to the beam. The laser beam is focused onto the sample from the top while the sample is probed with hard x-rays through an x-ray transparent boron-epoxy gasket. The temperature response of preferred orientation of (Fe,Mg)O is probed as a test experiment. Recrystallization was observed above 1500 K, accompanied by a decrease in stress. PMID:17614626

  1. In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell

    SciTech Connect

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

    2007-06-15

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

  2. Diffraction of a focused X-ray beam by surface acoustic waves

    NASA Astrophysics Data System (ADS)

    Tucoulou, R.; Schelokov, I. A.; Roschchupkin, D. V.; Brunel, M.; Ortega, L.; Chevallier, P.

    1995-02-01

    This paper reports the first attempt to carry out a focusing followed by a space-time scanning of a synchrotron X-ray beam. The focusing is performed through an elliptical multilayer Bragg-Fresnel lens while the space-time scanning is due to the grazing incidence diffraction on the YZ-cut of a LiNbO 3 crystal modulated by pulsed surface acoustic waves. It opens the field of a new generation of X-ray beam control devices which should be of interest for X-ray scanning microscopy or time resolved spectroscopy. These experiments were carried out at LURE (Orsay, France).

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

    NASA Astrophysics Data System (ADS)

    Li, Youli; Yasa, Mario; Pelletier, Olivier; Safinya, Cyrus R.; Caine, Ernie; Hu, Evelyn E.; Fernandez, Patricia

    2003-04-01

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

  4. Microstructure of heteroepitaxial GaN revealed by x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Chierchia, R.; Bttcher, T.; Heinke, H.; Einfeldt, S.; Figge, S.; Hommel, D.

    2003-06-01

    The mosaicity of GaN layers grown by metalorganic vapor phase epitaxy, on (0001) sapphire and exhibiting different grain diameters is studied using high-resolution x-ray diffraction. The coherence lengths, the tilt, and the twist of the mosaic structure are determined utilizing data taken in different x-ray scattering geometries. The results of different models, which were applied, are then compared and discussed. The dislocation densities, obtained from the x-ray data, are compared with the results of plan-view transmission electron microscopy and atomic force microscopy.

  5. 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).

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

    DOEpatents

    Pawloski, Gayle A. (Livermore, CA)

    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.

  7. X-ray diffraction and EXAFS analysis of materials for lithium-based rechargeable batteries

    SciTech Connect

    Sharkov, M. D. Boiko, M. E.; Bobyl, A. V.; Ershenko, E. M.; Terukov, E. I.; Zubavichus, Y. V.

    2013-12-15

    Lithium iron phosphate LiFePO{sub 4} (triphylite) and lithium titanate Li{sub 4}Ti{sub 5}O{sub 12} are used as components of a number of active materials in modern rechargeable batteries. Samples of these materials are studied by X-ray diffraction and extended X-ray absorption fine structure (EXAFS) spectroscopy. Hypotheses about the phase composition of the analyzed samples are formulated.

  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. 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.

  10. Study on quasiperiodic Ta/Al multilayer films by x-ray diffraction

    SciTech Connect

    Peng, R.W.; Hu, A.; Jiang, S.S. )

    1991-11-11

    Quasiperiodic (Fibonacci) Ta/Al multilayer films with Ta(110) and Al(111) textures were fabricated by magnetron sputtering. The structure of the multilayers was characterized in detail by x-ray diffraction. The diffraction peaks at low and high angles can be indexed by the projection method from the high-dimension periodic structure. The experimental results were in good agreement with the numerical calculation using the model for the compositionally modulated multilayers. The diffraction spectrum of the quasiperiodic Ta/Al multilayers is totally different from that of periodic structure, and the possible application of Fibonacci films as optical elements in a soft x-ray region is discussed.

  11. X-ray diffraction experiments on the Materials in Extreme Conditions (MEC) LCLS x-ray FEL beamline

    NASA Astrophysics Data System (ADS)

    Smith, Raymond; Fratanduono, Dayne; Wicks, June; Duffy, Tom; Lee, Hae Ja; Granados, Eduardo; Heimann, Philip; Gleason, Arianna; Bolme, Cynthia; Swift, Damian; Coppari, Federica; Eggert, Jon; Collins, Rip

    2015-06-01

    The experiments described here were conducted on the MEC beamline hutch at the SLAC Linac Coherent Light Source. A 10 ns 527 nm laser pulse was used to shock compress 60-100 ?m thick NaCl and Graphite samples. LCLS x-rays (40 fs, 8 keV), scattered off the shocked sample, were recorded on several pixel array detectors positioned downstream. The diffracted x-ray pattern allows us to determine changes in crystal structure at Mbar pressures and over nanosecond timescales. In this talk we detail the experimental setup, the current capabilities of the MEC laser and the considerations for optimizing the target design. We will describe the wave interactions within the shock-compressed target and the use of a 1D hydrocode to describe the pressure, temperature and density conditions within the target assembly as a function of time and Lagrangian position. We present observations of the B1-B2 phase transition in NaCl and subsequent back transformation during release to ambient pressure, and compare these findings to gas gun and static data. We also present results from a preliminary study of the shock-induced graphite to diamond transformation.

  12. Takagi-taupin description of x-ray dynamical diffraction from diffractive optics with large numerical aperture.

    SciTech Connect

    Yan, H.; Maser, J.; Macrander, A.; Shen, Q.; Vogt, S.; Stephenson, B.; Kang, H. C.; Advanced Photonics Research Inst.; Gwangju Inst. of Science and Technology

    2007-09-01

    We present a formalism of x-ray dynamical diffraction from volume diffractive optics with large numerical aperture and high aspect ratio, in an analogy to the Takagi-Taupin equations [Acta Crystallogr. 15, 1311 (1962); Bull. Soc. Fr. Mineral. Crystallogr. 87, 469 (1964)] for strained single crystals. We derive a set of basic equations for dynamical diffraction from volume diffractive optics, which enable us to study the focusing property of these optics with various grating profiles. We study volume diffractive optics that satisfy the Bragg condition to various degrees, namely, flat, tilted, and wedged geometries, and derive the curved geometries required for ultimate focusing. We show that the curved geometries satisfy both the Bragg condition everywhere and phase requirement for point focusing and effectively focus hard x rays to a scale close to the wavelength. Our calculations were made for an x-ray wavelength of 0.064 nm (19.5 keV).

  13. 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.

  14. 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…

  15. 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

  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. Structural studies of tropomyosin by cryoelectron microscopy and x-ray diffraction.

    PubMed Central

    Cabral-Lilly, D; Phillips, G N; Sosinsky, G E; Melanson, L; Chacko, S; Cohen, C

    1991-01-01

    A comparison has been made between cryoelectron microscope images and the x-ray structure of one projection of the Bailey tropomyosin crystal. The computed transforms of the electron micrographs extend to a resolution of approximately 18 A compared with the reflections from x-ray crystallography which extend to 15 A. After correction of the images for lattice distortions and the contrast transfer function, the structure factors were constrained to the plane group (pmg) symmetry of this projection. Amplitude and phase data for five images were compared with the corresponding view from the three-dimensional x-ray diffraction data (Phillips, G.N., Jr., J.P. Fillers, and C. Cohen. 1986. J. Mol. Biol. 192: 111-131). The average R factor between the electron microscopy and x-ray amplitudes was 15%, with an amplitude-weighted mean phase difference of 4.8 degrees. The density maps derived from cryoelectron microscopy contain structural features similar to those from x-ray diffraction: these include the width and run of the filaments and their woven appearance at the crossover regions. Preliminary images obtained from frozen-hydrated tropomyosin/troponin cocrystals suggest that this approach may provide structural details not readily obtainable from x-ray diffraction studies. Images FIGURE 1 FIGURE 2 FIGURE 4 PMID:2065187

  18. Optomechanical design of a high-precision detector robot arm system for x-ray nano-diffraction with x-ray nanoprobe

    NASA Astrophysics Data System (ADS)

    Shu, D.; Kalbfleisch, S.; Kearney, S.; Anton, J.; Chu, Y. S.

    2014-03-01

    Collaboration between Argonne National Laboratory and Brookhaven National Laboratory has created a design for the high-precision detector robot arm system that will be used in the x-ray nano-diffraction experimental station at the Hard X-ray Nanoprobe (HXN) beamline for the NSLS-II project. The robot arm system is designed for positioning and manipulating an x-ray detector in three-dimensional space for nano-diffraction data acquisition with the HXN x-ray microscope. It consists of the following major component groups: a granite base with air-bearing support, a 2-D horizontal base stage, a vertical axis goniometer, a 2-D vertical plane robot arm, a 3-D fast scanning stages group, and a 2-D x-ray pixel detector. The design specifications and unique optomechanical structure of this novel high-precision detector robot arm system will be presented in this paper.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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).

  4. 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.

  5. 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.

  6. 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}.

  7. Method of X-Ray Anomalous Diffraction for Lipid Structures

    PubMed Central

    Wang, Wangchen; Pan, Deng; Song, Yang; Liu, Wenhan; Yang, Lin; Huang, Huey W.

    2006-01-01

    The structures of the unit cells of lipid phases that exhibit long-range crystalline order but short-range liquid-like disorder are of biological interests. In particular, the recently discovered rhombohedral phase has a unit cell containing either the structure of a membrane fusion intermediate state or that of a peptide-induced transmembrane pore, depending on the lipid composition and participating peptides. Diffraction from such systems generally presents a difficult phase problem. The existing methods of phase determination all have their limitations. Therefore it is of general interest to develop a new phasing method. The method of multi-wavelength anomalous dispersion is routinely used in protein crystallography, but the same method is difficult for lipid systems for the practical reason that the commonly used lipid samples for diffraction do not have a well-defined thickness. Here we describe a practical approach to use the multi-wavelength anomalous dispersion method for lipid structures. The procedure is demonstrated with the lamellar phase of a brominated lipid. The method is general to all phases as long as anomalous diffraction is applicable. PMID:16632507

  8. 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

  9. 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.

  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. Hard X-ray resonance in sapphire crystal cavities using back diffraction

    NASA Astrophysics Data System (ADS)

    Wu, Y.-H.; Tsai, Y.-W.; Chang, Y.-Y.; Chu, C.-H.; Mikolas, David G.; Fu, C.-C.; Chang, S.-L.

    2012-02-01

    The Fabry-Perot type resonators using back diffraction from sapphire crystals for hard X-ray was investigated. On the basis of its less absorption and hexagonal structure, the resonator in sapphire crystals underwent a pure 2-beam diffraction which could enhance the resonance interference and improve finesse compared with the one in silicon crystals. The resonators were manufactured from sapphire crystals using microelectronic lithography process with thickness of a few tens ?m. With synchrotron radiation of energy resolution ?E=0.82 meV at 14.315 keV, X-ray back diffraction from two monolithic sapphire crystal plates shows resonance fringes clearly resulting from coherent interaction inside the energy gap of the (0 0 30) reflection. These experimental results of sapphire cavities imply the potential application for X-ray optics.

  12. Crystallization and preliminary X-ray diffraction studies of cyanuric acid hydrolase from Azorhizobium caulinodans

    PubMed Central

    Cho, Seunghee; Shi, Ke; Wackett, Lawrence P.; Aihara, Hideki

    2013-01-01

    Cyanuric acid is synthesized industrially and forms during the microbial metabolism of s-triazine herbicides. Cyanuric acid is metabolized by some microorganisms via cyanuric acid hydrolase (CAH), which opens the s-triazine ring as a prelude to further metabolism. CAH is a member of the rare cyanuric acid hydrolase/barbiturase family. Here, the crystallization and preliminary X-ray diffraction analysis of CAH from Azorhizobium caulinodans are reported. CAH was cocrystallized with barbituric acid, a close analog of cyanuric acid that is a tight-binding competitive inhibitor. Crystals suitable for X-ray diffraction experiments were grown in conditions containing PEG 8K or magnesium sulfate as precipitants. An X-ray diffraction data set was collected from CAHbarbituric acid crystals to 2.7? resolution. The crystals were found to belong to space group I4122, with unit-cell parameters a = b = 237.9, c=105.3?, ? = ? = ? = 90. PMID:23908033

  13. Study of double barrier superlattice by synchrotron radiation and double-crystal x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Zhuang, Y.; Wang, Y. T.; Jiang, D. S.; Yang, X. P.; Jiang, X. M.; Wu, J. Y.; Xiu, L. S.; Zheng, W. L.

    1996-02-01

    An (AlAs/GaAs/AlAs/AlGaAs)/GaAs(001) double-barrier superlattice grown by molecular beam epitaxy (MBE) is studied by combining synchrotron radiation and double-crystal x-ray diffraction (DCD). The intensity of satellite peaks is modulated by the wave function of each sublayer in one superlattice period. Simulated by the x-ray dynamical diffraction theory, it is discovered that the intensity of the satellite peaks situated near the modulating wave node point of each sublayer is very sensitive to the variation of the layer structural parameters. The accurate layer thickness of each sublayer is obtained with an error less than 1 . Furthermore, x-ray kinematical diffraction theory is used to explain the modulation phenomenon.

  14. 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.

  15. 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.

  16. 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.

  17. Diffraction crystal for sagittally focusing x-rays

    DOEpatents

    Ice, Gene E. (Oak Ridge, TN); Sparks, Jr., Cullie J. (Oak Ridge, TN)

    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.

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. X-ray diffraction study of fluorene, 9-fluorenone, and 9-dicyanomethylenefluorene derivatives

    SciTech Connect

    Chetkina, L. A.; Belsky, V. K.

    2013-01-15

    The results of a single-crystal X-ray diffraction analysis of fluorene, 9-fluorenone, and 9-dicyanomethylenefluorene derivatives as individual compounds, as well as their crystal solvates, molecular complexes, and charge-transfer complexes, are generalized. The most interesting features of the molecular geometry and conformation and the molecular packing in the crystals are discussed. The structural formula of 95 compounds and the R factors for X-ray diffraction analysis, which characterize the reliability of determining the structure, are summarized in three tables.

  4. 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.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    Characterization of defects and/or disorder in biological macromolecular crystals presents much greater challenges than in conventional small-molecule crystals. The lack of sufficient contrast of defects is often a limiting factor in x-ray diffraction topography of protein crystals. This has seriously hampered efforts to understand mechanisms and origins of formation of imperfections, and the role of defects as essential entities in the bulk of macromolecular crystals. In this report, we employ a phase sensitive x-ray diffraction imaging approach for augmenting the contrast of defects in protein crystals.

  5. 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.

  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. Probing the Local Order of Single Phospholipid Membranes Using Grazing Incidence X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Miller, C. E.; Majewski, J.; Watkins, E. B.; Mulder, D. J.; Gog, T.; Kuhl, T. L.

    2008-02-01

    We report the first grazing incidence x-ray diffraction measurements of a single phospholipid bilayer at the solid-liquid interface. Our grazing incidence x-ray diffraction and reflectivity measurements reveal that the lateral ordering in a supported DPPE (1, 2-Dipalmitoyl-sn-Glycero-3-Phosphoethanolamine) bilayer is significantly less than that of an equivalent monolayer at the air-liquid interface. Our findings also indicate that the leaflets of the bilayer are uncoupled in contrast to the scattering from free standing phosphatidylcholine bilayers. The methodology presented can be readily implemented to study more complicated biomembranes and their interaction with proteins.

  8. PREFACE: XTOP 2004 -- 7th Biennial Conference on High Resolution X-Ray Diffraction and Imaging

    NASA Astrophysics Data System (ADS)

    Hol, 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 Hrtwig, 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 Hrd, 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 Schlli, 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 p

  9. 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

  10. 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.; Bnazeth, 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 ? 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.

  11. Compact ultrahigh vacuum sample environments for x-ray nanobeam diffraction and imaging

    SciTech Connect

    Evans, P. G. Spalenka, J. W.; Chahine, G.; Grifone, R.; Jacques, V. L. R.; Schlli, T. U.

    2013-11-15

    X-ray nanobeams present the opportunity to obtain structural insight in materials with small volumes or nanoscale heterogeneity. The effective spatial resolution of the information derived from nanobeam techniques depends on the stability and precision with which the relative position of the x-ray optics and sample can be controlled. Nanobeam techniques include diffraction, imaging, and coherent scattering, with applications throughout materials science and condensed matter physics. Sample positioning is a significant mechanical challenge for x-ray instrumentation providing vacuum or controlled gas environments at elevated temperatures. Such environments often have masses that are too large for nanopositioners capable of the required positional accuracy of the order of a small fraction of the x-ray spot size. Similarly, the need to place x-ray optics as close as 1 cm to the sample places a constraint on the overall size of the sample environment. We illustrate a solution to the mechanical challenge in which compact ion-pumped ultrahigh vacuum chambers with masses of 12 kg are integrated with nanopositioners. The overall size of the environment is sufficiently small to allow their use with zone-plate focusing optics. We describe the design of sample environments for elevated-temperature nanobeam diffraction experiments demonstrate in situ diffraction, reflectivity, and scanning nanobeam imaging of the ripening of Au crystallites on Si substrates.

  12. 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.

  13. Normalization schemes for ultrafast x-ray diffraction using a table-top laser-driven plasma source

    SciTech Connect

    Schick, D.; Bojahr, A.; Herzog, M.; Korff Schmising, C. von; Shayduk, R.; Leitenberger, W.; Gaal, P.; Bargheer, M.

    2012-02-15

    We present an experimental setup of a laser-driven x-ray plasma source for femtosecond x-ray diffraction. Different normalization schemes accounting for x-ray source intensity fluctuations are discussed in detail. We apply these schemes to measure the temporal evolution of Bragg peak intensities of perovskite superlattices after ultrafast laser excitation.

  14. 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.

  15. 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.

  16. 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.

  17. Optimized performance of graded multilayer optics for x-ray single-crystal diffraction

    NASA Astrophysics Data System (ADS)

    Michaelsen, Carsten; Wiesmann, Joerg; Hoffmann, Christian; Oehr, A.; Storm, A. B.; Seijbel, L. J.

    2004-01-01

    We present recent developments in the production of X-ray multilayer optics for Cu K? laboratory single crystal diffraction equipment for protein crystallography and structural proteomics. The paper shows design, simulations and properties of Montel optics comprised of two elliptically bent focusing multilayers, optimized for the use with modern rotating anode X-ray generators. The multilayers are sputter deposited with a graded d-spacing along the length of the substrate. The various beam properties such as flux density and divergence are investigated in detail. After optimization of the optic for a state-of-the-art rotating anode x-ray generator, we obtain a flux density of 1 x 1010 photons/s/mm2. Results for a typical protein structure will be shown, illustrating the advantage of Montel optics in the field of single-crystal diffraction and protein crystallography for life sciences.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. 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-?m-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

  4. 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.

  5. 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.

  6. Magnetic symmetries in neutron and resonant x-ray Bragg diffraction patterns of four iridium oxides

    NASA Astrophysics Data System (ADS)

    Lovesey, S. W.; Khalyavin, D. D.; Manuel, P.; Chapon, L. C.; Cao, G.; Qi, T. F.

    2012-12-01

    The magnetic properties of Sr2IrO4, Na2IrO3, Sr3Ir2O7 and CaIrO3 are discussed, principally in the light of experimental data in recent literature for Bragg intensities measured in x-ray diffraction with enhancement at iridium L-absorption edges. The electronic structure factors we report, which incorporate parity-even and acentric entities, serve the immediate purpose of making full use of crystal and magnetic symmetry to refine our knowledge of the magnetic properties of the four iridates from resonant x-ray diffraction data. They also offer a platform on which to interpret future investigations, using dichroic signals, resonant x-ray diffraction and neutron diffraction, for example, as well as ab initio calculations of electronic structure. Unit-cell structure factors, suitable for x-ray Bragg diffraction enhanced by an electric dipole-electric dipole (E1-E1) event, reveal exactly which iridium multipoles are visible, e.g., a magnetic dipole parallel to the crystal c-axis (z-axis) and an electric quadrupole with yz-like symmetry in the specific case of CaIrO3. Magnetic space-groups are assigned to Sr2IrO4, Sr3Ir2O7 and CaIrO3, namely, PIcca, PAban and Cm?cm?, respectively, in the Belov-Neronova-Smirnova notation. The assignment for Sr2IrO4 is possible because of our new high-resolution neutron diffraction data, gathered on a powder sample. In addition, the new data are used to show that the ordered magnetic moment of an Ir4+ ion in Sr2IrO4 does not exceed 0.29(4) ?B. Na2IrO3 has two candidate magnetic space-groups that are not resolved with currently available resonant x-ray data.

  7. 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.

  8. 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...

  9. Growth of Strained Epitaxial Cu Films on Ru(0001) Monitored by Surface X-Ray Diffraction

    SciTech Connect

    Baddord, A.P.; Gibbs, D.; Zajonz, H.; Zehner, D.M.

    1998-10-19

    The growth of Cu Layers deposited on Ru(0001) substrates at temperatures between 500 K and 850 K was studied using surface x-ray diffraction. Results are consistent with a Stransky-Krastanov growth mode with a two layer critical thickness.

  10. 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…

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

    NASA Astrophysics Data System (ADS)

    Colao, 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 LaboratoryLNLS, 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.

  12. 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.

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

    DOEpatents

    Smither, Robert K. (Hinsdale, IL)

    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.

  14. 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.

  15. 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.

  16. 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.

  17. X-ray diffraction studies of polyaniline doped with Zn(NO3)2

    NASA Astrophysics Data System (ADS)

    Goyal, Sneh Lata; Sharma, Smriti; Kumar, Devinder; Kishore, Nawal

    2013-06-01

    Polyaniline (PANI) and PANI/zinc nitrate composites were synthesized by in situ chemical oxidative polymerization of aniline with Zn(NO3)2 using ammonium peroxidisulphate (APS) as an oxidant. These composites were characterized by X-ray diffraction (XRD) and the results were compared with pure Polyaniline and zinc nitrate.

  18. 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.

  19. 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 ...

  20. 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.

  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. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Progress report on the development of an area detector data acquisition system for X-ray crystallography and other X-ray diffraction experiments

    NASA Astrophysics Data System (ADS)

    Phizackerley, R. P.; Cork, C. W.; Hamlin, R. C.; Nielsen, C. P.; Vernon, W.; Xuong, Ng. H.; Perez-Mendez, V.

    1980-05-01

    A relatively inexpensive data acquisition system, incorporating a flat MWPC, with an anticipated count rate of approximately 130 kHz is currently being developed at SSRL in collaboration with research groups at UCSD and LBL. It will be primarily used for X-ray crystallographic studies of macromolecules using synchrotron radiation but will also be used for other X-ray diffraction experiments at SSRL. This system, controlled by a PDP 11-34 computer running under the RSX-11M operating system, incorporates the MWPC area detector, a fast display system, a 3-circle single-crystal goniometer, an alignment carriage, an incident-beam intensity monitor and a tunable monochromator. A progress report and future plans will be presented. The detector dimensions are 28 cm 28 cm with a spatial resolution of 128 256 elements. The absorption depth at normal incidence is 1 cm and the fill gas is a mixture of 90% Xe and 10% CO 2 at a pressure of 1 atmosphere. Fast printed-circuit delay-lines (? 170 ns) are used for read-out. It is anticipated that the complete system will be ready for initial testing in the Spring of 1980.

  10. Scanning acoustic microscopy and X-ray diffraction investigation of near crack tip stresses

    SciTech Connect

    Sathish, S.; Martin, R.W.

    2000-07-01

    Scanning Acoustic Microscopy has been used to measure and map the Rayleigh wave velocity and the Surface Skimming Longitudinal wave velocities near a crack tip in a sample of Ti-6Al-4V. X-ray diffraction measurements have been performed to map the stress in the same region of the sample. The differences in the contrast between the two acoustic velocity images and their sensitivity to stress are examined. Similarities between x-ray stress images and acoustic velocity images are discussed.

  11. Coherent Atomic Motions in a Nanostructure Studied by Femtosecond X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Bargheer, M.; Zhavoronkov, N.; Gritsai, Y.; Woo, J. C.; Kim, D. S.; Woerner, M.; Elsaesser, T.

    2004-12-01

    Reversible structural changes of a nanostructure were measured nondestructively with subpicometer spatial and subpicosecond temporal resolution via x-ray diffraction (XRD). The spatially periodic femtosecond excitation of a gallium arsenide/aluminum gallium arsenide superlattice results in coherent lattice motions with a 3.5-picosecond period, which was directly monitored by femtosecond x-ray pulses at a 1-kilohertz repetition rate. Small changes (?R/R = 0.01) of weak Bragg reflexes (R = 0.005) were detected. The phase and amplitude of the oscillatory XRD signal around a new equilibrium demonstrate that displacive excitation of the zone-folded acoustic phonons is the dominant mechanism for strong excitation.

  12. 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 77 superstructure on a Si(111) surface and at a SiO2/Si(111) interface.

  13. 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.

  14. 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

  15. 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.

  16. 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

  17. The catalytic mechanism of an aspartic proteinase explored with neutron and X-ray diffraction

    SciTech Connect

    Kovalevsky, Andrey; Erskine, Peter T.; Cooper, Jon

    2008-01-01

    Hydrogen atoms play key roles in enzyme mechanism, but as this study shows, even high-quality X-ray data to a resolution of 1 {angstrom} cannot directly visualize them. Neutron diffraction, however, can locate deuterium atoms even at resolutions around 2 {angstrom}. Both neutron and X-ray diffraction data have been used to investigate the transition state of the aspartic proteinase endothiapepsin. The different techniques reveal a different part of the story, revealing the clearest picture yet of the catalytic mechanism by which the enzyme operates. Room temperature neutron and X-ray diffraction data were used in a newly developed joint refinement software package to visualize deuterium atoms within the active site of the enzyme when a gem-diol transition state analogue inhibitor is bound at the active site. These data were also used to estimate their individual occupancy, while analysis of the differences between the bond lengths of the catalytic aspartates was performed using atomic resolution X-ray data. The two methods are in agreement on the protonation state of the active site with a transition state analogue inhibitor bound confirming the catalytic mechanism at which the enzyme operates.

  18. 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.

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

    PubMed

    Krko?lu, Gne? Sheyla; Kiraz, Fulya etinkaya; Say?n, 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. PMID:25919408

  20. 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.

  1. X-ray diffraction techniques for in-situ measurements of the dynamic flow stress of shock compressed Ta

    NASA Astrophysics Data System (ADS)

    Wehrenberg, Christopher; Barton, Nathan; Comley, Andrew; McGonegle, David; Maddox, Brian; McNaney, James; Park, Hye-Sook; Plechaty, Chris; Prisbrey, Shon; Remington, Bruce; Rudd, Rob

    2015-06-01

    A range of experimental techniques using in-situ x-ray diffraction have been developed to study the dynamic flow stress and underlying deformation of shock compressed samples. Experiments performed at the Omega and Omega EP facilities can generate both a high pressure drive, ranging from 0.3 Mbar up to and beyond the Hugoniot melt line, while simultaneous providing a short, bright x-ray source. Single crystal samples were studied either by Laue diffraction, using a broadband x-ray source created by an imploding CH capsule, or by Bragg diffraction, using a short pulse driven metal foil backlighter. The strength of polycrystalline samples can be determined using a pinhole camera setup and a quasi-monochromatic source. For highly-textured polycrystalline samples, additional strength information can be inferred from the azimuthal position of the texture spots on the Debye ring. Through measurements of the 1D-to-3D relaxation time or changes in the observed texture, information about the deformation mechanics of shock loading can be inferred. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

  2. A regularized iterative reconstruction algorithm for x-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Chen, Ke; Castan, David A.

    2012-06-01

    Material discrimination based on conventional or dual energy X-ray computed tomography (CT) imaging can be ambiguous. X-ray diraction imaging (XDI) can be used to construct diraction proles of objects, providing molecular signature information that can be used to characterize the presence of specic materials. Combining X-ray CT and diraction imaging can lead to enhanced detection and identication of explosives in luggage screening. Current XDI scan systems are based on direct imaging rather than tomographic imaging, which require the use of line collimators to localize scattering location and thus result in slow scan performance. In an eort to gain faster scan times and better signal-to-noise ratio, we focus on tomographic inversion techniques for X-ray Diraction Tomography (XDT) and look for joint reconstruction of CT absorption and X-ray diraction prole images of object. We present a fast reconstruction algorithm with geometric feature preserving regularization (IREP) using image-wise based iterative coordinate descent (ICD).We validate the initial results via Monte Carlo simulation of X-ray absorption and coherent scattering in 2 dimensions (2D), and compare the performance of the IREP algorithm with existing inversion techniques such as the ltered backprojection method and the algebraic reconstruction technique. The experimental results show that the IREP method oers improved image quality for enhanced material identication.

  3. Study of carbon steel corrosion layer by X-ray diffraction and absorption methods

    NASA Astrophysics Data System (ADS)

    Malinovschi, V.; Ducu, C.; Aldea, N.; Fulger, M.

    2006-06-01

    To predict the behavior of structural metallic materials into the CANDU nuclear reactor, the oxide films on the surface were growth in a controlled manner using an autoclave simulating the environment specific to the nuclear reactor. In order to establish the structural changes of the oxide films, the X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX) and extended X-ray absorption fine structure spectroscopy (EXAFS) analysis were used. Analysis performed showed differences in morphology of the oxide films from carbon steel samples exposed under different conditions corresponding to primary and secondary circuits in CANDU nuclear reactor. The oxide phases were identified and the thicknesses of the films were calculated. The agreement between results obtained by these methods was discussed according to the microstructure of the samples.

  4. 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.

  5. Investigations into rapid uniaxial compression of polycrystalline targets using femtosecond X-ray diffraction

    NASA Astrophysics Data System (ADS)

    McGonegle, David; Higginbotham, Andrew; Galtier, Eric; McBride, Emma E.; McMahon, Malcolm I.; Milathianaki, Despina; Lee, Hae Ja; Nagler, Bob; Vinko, Sam M.; Wark, Justin S.

    2014-05-01

    Although the pressures achievable in laser experiments continue to increase, the mechanisms underlying how solids deform at high strain rates are still not well understood. In particular, at higher pressures, the assumption that the difference between the longitudinal and transverse strains in a sample remains small becomes increasingly invalid. In recent years, there has been an increasing interest in simulating compression experiments on a granular level. In situ X-ray diffraction, where a target is probed with X-rays while a shock is propagating through it, is an excellent tool to test these simulations. We present data from the first long-pulse laser experiment at the MEC instrument of LCLS, the world's first hard X-ray Free Electron Laser, demonstrating large strain anisotropies. From this we infer shear stresses in polycrystalline copper of up to 1.75 GPa at a shock pressure of 32 GPa.

  6. Coherent hard x-ray diffractive imaging of nonisolated objects confined by an aperture

    SciTech Connect

    Kim, Sunam; Kim, Chan; Lee, Suyong; Marathe, Shashidhara; Noh, D. Y.; Kang, H. C.; Kim, S. S.; Sandy, A.; Narayanan, S.

    2010-04-15

    Coherent hard x-ray imaging of nonisolated weak phase objects is demonstrated by confining x-ray beam in a region of a few micrometers in cross section using a micrometer-sized aperture. Two major obstacles in the hard x-ray coherent diffraction imaging, isolating samples and obtaining central speckles, are addressed by using the aperture. The usefulness of the proposed method is illustrated by reconstructing the exit wave field of a nanoscale trench structure fabricated on silicon which serves as a weak phase object. The quantitative phase information of the exit wave field was used to reconstruct the depth profile of the trench structure. The scanning capability of this method was also briefly discussed.

  7. Collagen imaged by Coherent X-ray Diffraction: towards a complementary tool to conventional scanning SAXS

    NASA Astrophysics Data System (ADS)

    Berenguer de la Cuesta, Felisa; Bean, Richard J.; McCallion, Catriona; Wallace, Kris; Bozec, Laurent; Hiller, Jen C.; Terrill, Nicholas J.; Robinson, Ian K.

    2010-10-01

    Third generation x-ray sources offer unique possibilities for exploiting coherence in the study of materials. New insights in the structure and dynamics of soft condensed matter and biological samples can be obtained by coherent x-ray diffraction (CXD). However, the experimental procedures for applying these methods to collagen tissues are still under development. We present here an investigation for the optimal procedure in order to obtain high quality CXD data from collagen tissues. Sample handling and preparation and adequate coherence defining apertures are among the more relevant factors to take into account. The impact of the results is also discussed, in particular in comparison with the information that can be extracted from conventional scanning small angle x-ray scattering (SAXS). Images of collagen tissues obtained by CXD reconstructions will give additional information about the local structure with higher resolution and will complement scanning SAXS images.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. HRTEM and X-ray diffraction analysis of Au wire bonding interface in microelectronics packaging

    NASA Astrophysics Data System (ADS)

    Junhui, Li; Ruishan, Wang; Lei, Han; Fuliang, Wang; Zhili, Long

    2011-01-01

    Interfacial microstructures of thermosonic Au wire bonding to an Al pad of die were investigated firstly by high-resolution transmission electron microscopy (HRTEM) and X-ray micro-diffractometer. The equal-thickness interference structures were observed by HRTEM due to diffusion and reaction activated by ultrasonic and thermal at the Au/Al bond interface. And X-ray diffraction results showed that three different interplanar crystal spacings ('d' value) of the interfacial microstructures were 2.2257 , 2.2645 , and 2.1806 respectively from the high intensity of diffraction to the low intensity of diffraction. These indicated that the intermetallic phase AlAu 2 formed within a very short time. It would be helpful to further research wire bonding technology.

  13. 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

  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; Strder, 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. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

    PubMed Central

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-01-01

    Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27?724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b=49.9, c = 56.3?, ? = 95.2. Diffraction images were processed to a resolution of 1.74? with an R merge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase. PMID:21139221

  16. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto.

    PubMed

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-12-01

    Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27,724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a=74.3, b=49.9, c=56.3?, ?=95.2. Diffraction images were processed to a resolution of 1.74? with an Rmerge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase. PMID:21139221

  17. 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 23 ?s, and the frame interval is 26.762.5 ?s. 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.

  18. 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

  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. 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.

  1. 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.

  2. Imaging outside the box: Resolution enhancement in X-ray coherent diffraction imaging by extrapolation of diffraction patterns

    NASA Astrophysics Data System (ADS)

    Latychevskaia, Tatiana; Chushkin, Yuriy; Zontone, Federico; Fink, Hans-Werner

    2015-11-01

    Coherent diffraction imaging is a high-resolution imaging technique whose potential can be greatly enhanced by applying the extrapolation method presented here. We demonstrate the enhancement in resolution of a non-periodical object reconstructed from an experimental X-ray diffraction record which contains about 10% missing information, including the pixels in the center of the diffraction pattern. A diffraction pattern is extrapolated beyond the detector area and as a result, the object is reconstructed at an enhanced resolution and better agreement with experimental amplitudes is achieved. The optimal parameters for the iterative routine and the limits of the extrapolation procedure are discussed.

  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. 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.

  5. 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.

  6. X-Ray Diffraction Study of the Internal Structure of Supercooled Water

    NASA Technical Reports Server (NTRS)

    Dorsch, Robert G.; Boyd, Bemrose

    1951-01-01

    A Bragg X-ray spectrometer equipped with a volume-sensitive Geiger counter and Soller slits and employing filtered molybdenum Ka radiation was used to obtain a set of diffracted intensity curves as a Punction of angle for supercooled water. Diffracted intensity curves in the temperature region of 21 to -16 C were obtained. The minimum between the two main diffraction peaks deepened continuously with lowering temperature, indicating a gradual change in the internal structure of the water. No discontinuity in this trend was noted at the melting point. The internal structure of supercooled water was concluded to become progressively more ice-like as the temperature is lowered.

  7. Spectral x-ray diffraction using a 6 megapixel photon counting array detector

    NASA Astrophysics Data System (ADS)

    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.

    2015-03-01

    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.

  8. 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.

  9. 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.

  10. 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

  11. 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)

  12. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    PubMed Central

    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

    2015-01-01

    In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecond X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2? resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser. PMID:26798805

  13. 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, poly?-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

  14. 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.

  15. 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.

  16. 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

  17. A nearly on-axis spectroscopic system for simultaneouslymeasuring UV-visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline.

    PubMed

    Sakaguchi, Miyuki; Kimura, Tetsunari; Nishida, Takuma; Tosha, Takehiko; Sugimoto, Hiroshi; Yamaguchi, Yoshihiro; Yanagisawa, Sachiko; Ueno, Go; Murakami, Hironori; Ago, Hideo; Yamamoto, Masaki; Ogura, Takashi; Shiro, Yoshitsugu; Kubo, Minoru

    2016-01-01

    UV-visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2 off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probed via caged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis. PMID:26698082

  18. 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.

  19. 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.

  20. 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.

  1. Calcinosis Circumscripta. A Case Report with X-ray Diffraction Studies

    PubMed Central

    Grice, H. C.; Hutchison, J. A.; Cloutier, J. A. R.

    1962-01-01

    A small subcutaneous mass located on the right foreleg of a 3 months old Brittany spaniel was observed to progressively enlarge over a 2 month period. The lesion which had not affected locomotion was removed at 5 months of age and was diagnosed as calcinosis circumscripta. The chalk-like material contained in the lesion was studied by x-ray diffraction and from the crystallographic view point, the structure of this growth was not different from that of normal or abnormal calcification. As there is no agreement on the exact chemical arrangement of bone salts (13), the observed x-ray powder diffraction pattern may be taken as that corresponding to a calcium phosphate hydrated (14), a calcium phosphate of apatite structure (15), a pseudo-apatite (16), or a hydroxy apatite (17). ImagesFigure 1.Figure 2.Figure 3.Figure 4. PMID:17649393

  2. 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, Jos Andrs; Aparicio, Ricardo

    2007-11-01

    Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 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 and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 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.

  3. Ultrafast lattice response of photoexcited thin films studied by X-ray diffraction.

    PubMed

    Schick, Daniel; Herzog, Marc; Bojahr, Andr; Leitenberger, Wolfram; Hertwig, Andreas; Shayduk, Roman; Bargheer, Matias

    2014-11-01

    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

  4. X-ray diffraction analysis of uranium tritide after aging for 420 days

    NASA Astrophysics Data System (ADS)

    Ao, B. Y.; Wang, X. L.; Zhang, Y. Z.; Wei, Y. J.

    2009-02-01

    Uranium tritide aging leads to continuous creation of decayed product 3He, vacancies, vacancy clusters, self interstitials, dislocations and helium bubbles. These defects result in the changes of material properties such as degradation of tritium storage, swelling, hardening and intergranular embrittlement. In our previous study, a simple hermetic sample holder that fits the Philip X'Pert Pro X-ray diffractometer has been developed for X-ray diffraction (XRD) analysis of uranium hydride. In order to help resolve unknowns regarding aging effects of uranium during long-term storage of tritium, XRD techniques with the hermetic method are applied to obtain the structural changes of aged uranium tritide. XRD analysis of uranium tritide aged for 420 days have shown that noticeable peak shifts appear in the diffraction patterns of uranium tritide, which indicate lattice distortion occurrence during the formation and growth of helium bubbles and other associated defects.

  5. Ultrafast lattice response of photoexcited thin films studied by X-ray diffraction

    PubMed Central

    Herzog, Marc; Bojahr, Andr; 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.

  6. 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.

  7. [Studies on X-ray diffraction pattern of traditional Chinese medicinal materials].

    PubMed

    Lu, Y; Zheng, Q T; Wu, N; Wang, G L; Tian, J G; Zhang, J; Chen, D C

    1997-01-01

    Traditional Chinese medicine(TCM) as prescribed by Chinese traditional physicians is usually available as "decoction slices" which calls for a ready method for assessment of quantity or even genuineness. Three groups of TCM drugs (radix Rubiae, bulbus Fritillariae and rhizoma Dioscoreae) were selected by using powder X-ray diffraction analysis with complete absorption profile. Topological regularity and characteristic peaks of the absorption profile were obtained as fingerprint in X-ray diffraction diagrams of the pertinent medicinal materials. We have discovered the similarities of 3 radix Rubiae samples gathered from different localities and their differences with Rubia tinctorum, the similarities and differences between 7 species belonging to Fritillaria Genus, the similarities of 2 rhizoma Dioscoreae samples from different localities and their differences with 2 counterfeits. The result points to a promising prospect in achieving an objective assessment of genuineness at TCM drugs. PMID:11327020

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. X-ray diffraction studies of inhomogeneity of Langmuir-Blodgett films

    SciTech Connect

    Lider, V.V.; Soroka, I.L.

    1994-12-31

    The inhomogeneity of a Langmuir-Blodgett film was evaluated from the halfwidth and the maximum intensity of the Bragg reflection peak measured in double-crystal X-ray diffraction studies. The mean square values of the internal stresses and the angle between mosaic blocks were determined, as well as the film roughness. The effect of internal elastic stress relaxation due to the change in the mosaic-block misorientation is established. 11 refs., 4 figs.

  15. Surface x-ray speckles : coherent surface diffraction from Au(0 01).

    SciTech Connect

    Pierce, M. S.; Chang, K. C.; Hennessy, D.; Komanicky, V.; Sprung, M.; Sandy, A.; You, H.; Safarik Univ.; HASYLAB

    2009-10-16

    We present coherent speckled x-ray diffraction patterns obtained from a monolayer of surface atoms. We measured both the specular anti-Bragg reflection and the off-specular hexagonal reconstruction peak for the Au(001) surface reconstruction. We observed fluctuations of the speckle patterns even when the integrated intensity appears static. By autocorrelating the speckle patterns, we were able to identify two qualitatively different surface dynamic behaviors of the hex reconstruction depending on the sample temperature.

  16. 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.

  17. Quantitative characterization of epitaxial superlattices by x-ray diffraction and high resolution electron microscopy

    SciTech Connect

    Fullerton, E.E. ); Cao, W.; Thomas, G. ); Schuller, I.K. ); Carey, M.J.; Berkowitz, A.E. )

    1993-07-26

    Quantitative x-ray diffraction (XRD) and high resolution electron microscopy (HREM) have been applied to the analysis of an epitaxial CoO/NiO superlattice. This example shows that the qualitative information determined directly from a XRD spectrum or HREM image is limited and can even be misleading. However, by a combination of quantitative intensity measurements and structural modeling, a detailed quantitative characterization of the superlattice structure is possible.

  18. 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

  19. 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.

  20. Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

    PubMed Central

    Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

    2003-01-01

    Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (?-XRD) techniques. Rietveld refinement analyses of XRD and ?-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

  1. Realizing in-plane surface diffraction by x-ray multiple-beam diffraction with large incidence angle

    SciTech Connect

    Huang, Xian-Rong Gog, Thomas; Assoufid, Lahsen; Peng, Ru-Wen; Siddons, D. P.

    2014-11-03

    Based on rigorous dynamical-theory calculations, we demonstrate the principle of an x-ray multiple-beam diffraction (MBD) scheme that overcomes the long-lasting difficulties of high-resolution in-plane diffraction from crystal surfaces. This scheme only utilizes symmetric reflection geometry with large incident angles but activates the out-of-plane and in-plane diffraction processes simultaneously and separately in the continuous MBD planes. The in-plane diffraction is realized by detoured MBD, where the intermediate diffracted waves propagate parallel to the surface, which corresponds to an absolute Bragg surface diffraction configuration that is extremely sensitive to surface structures. A series of MBD diffraction and imaging techniques may be developed from this principle to study surface/interface (misfit) strains, lateral nanostructures, and phase transitions of a wide range of (pseudo)cubic crystal structures, including ultrathin epitaxial films and multilayers, quantum dots, strain-engineered semiconductor or (multi)ferroic materials, etc.

  2. 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.

  3. Femtosecond diffractive imaging with a soft-X-ray free-electron laser

    NASA Astrophysics Data System (ADS)

    Chapman, Henry N.; Barty, Anton; Bogan, Michael J.; Boutet, Sbastien; Frank, Matthias; Hau-Riege, Stefan P.; Marchesini, Stefano; Woods, Bruce W.; Bajt, Saa; Benner, W. Henry; London, Richard A.; Plnjes, Elke; Kuhlmann, Marion; Treusch, Rolf; Dsterer, Stefan; Tschentscher, Thomas; Schneider, Jochen R.; Spiller, Eberhard; Mller, Thomas; Bostedt, Christoph; Hoener, Matthias; Shapiro, David A.; Hodgson, Keith O.; van der Spoel, David; Burmeister, Florian; Bergh, Magnus; Caleman, Carl; Huldt, Gsta; Seibert, M. Marvin; Maia, Filipe R. N. C.; Lee, Richard W.; Szke, Abraham; Timneanu, Nicusor; Hajdu, Janos

    2006-12-01

    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 25fs, 41013Wcm-2 pulse, containing 1012 photons at 32nm wavelength, produced a coherent diffraction pattern from a nanostructured non-periodic object, before destroying it at 60,000K. 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 is reconstructed at the 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.

  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 (1020 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??s) 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. 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.

  6. 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.

  7. 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

  8. 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.

  9. X-ray diffraction from thin film structures: Characterization and modeling

    NASA Astrophysics Data System (ADS)

    Liu, Ge

    InAs/GaSb superlattices grown via molecular beam epitaxy, and containing InSb-like interfacial layers, were analyzed with a combination of x-ray diffraction (XRD) and structural refinement techniques. The superlattice refinement from x-rays (SUPREX) method determines with high accuracy the average thicknesses and d-spacings of the individual InAs and GaSb layers in addition to standard structural parameters usually obtained by XRD, such as the modulation length (periodicity), average out-of-plane interplanar spacings, and total thickness. The combined SUPREX/XRD experiments show that the absence of certain odd order satellite features in the x-ray data is due to asymmetric and inhomogeneous lattice strain. Ex situ-annealed InAs/GaSb superlattices were studied using atomic force microscopy (AFM) and XRD methods. Results show that annealing at temperatures between 200C and 350C for 1 hour in HVAC improves the structural quality of these superlattices. Strain relaxation occurs during the annealing process indicating that there are chemical intermixing and anion segregation in the superlattices. The effect of the inner-molecular electron density on the x-ray diffraction profile of a layer-stacked thin film is studied. Important phase information contained in the x-ray diffraction profile of highly anisotropic molecular-based thin films is charaterized. The experimental and calculated results show that the intensity distribution of the diffraction peaks belonging to the same lattice orientation provides important structural information. For example, tilt angle and core electron density of a molecule can be determined from the intensity distribution. The out-of-plane tilt angle relaxation is studied numerically. The results show that the relaxation can only occur at the first phthalocyanine monolayer above the substrate. The lateral grain size effect and the polar angle anisotropy are studied using a three-dimensional model. The FWHM of the center peak in associated rocking curves gives lateral coherence length or lateral grain size, and the ratio of the intensities from the diffraction peaks in normal diffraction curves shows the uniaxial angular anisotropy of the phthalocyanine thin films.

  10. X-ray structure of perdeuterated diisopropyl fluorophosphatase (DFPase): perdeuteration of proteins for neutron diffraction.

    PubMed

    Blum, Marc Michael; Tomanicek, Stephen J; John, Harald; Hanson, B Leif; Rterjans, Heinz; Schoenborn, Benno P; Langan, Paul; Chen, Julian C H

    2010-04-01

    The signal-to-noise ratio is one of the limiting factors in neutron macromolecular crystallography. Protein perdeuteration, which replaces all H atoms with deuterium, is a method of improving the signal-to-noise ratio of neutron crystallography experiments by reducing the incoherent scattering of the hydrogen isotope. Detailed analyses of perdeuterated and hydrogenated structures are necessary in order to evaluate the utility of perdeuterated crystals for neutron diffraction studies. The room-temperature X-ray structure of perdeuterated diisopropyl fluorophosphatase (DFPase) is reported at 2.1 A resolution. Comparison with an independently refined hydrogenated room-temperature structure of DFPase revealed no major systematic differences, although the crystals of perdeuterated DFPase did not diffract neutrons. The lack of diffraction is examined with respect to data-collection and crystallographic parameters. The diffraction characteristics of successful neutron structure determinations are presented as a guideline for future neutron diffraction studies of macromolecules. X-ray diffraction to beyond 2.0 A resolution appears to be a strong predictor of successful neutron structures. PMID:20383004

  11. 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

  12. Theoretical study of the properties of X-ray diffraction moir fringes. I

    PubMed Central

    Yoshimura, Jun-ichi

    2015-01-01

    A detailed and comprehensive theoretical description of X-ray diffraction moir 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, 810812] on the two-dimensionality of diffraction moir patterns is restated on a thorough calculation of the moir interference phase. Then, the properties of moir fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellsung intensity oscillation on the moir pattern when the crystal is strained is described in detail with theoretically simulated moir images. Although such plane-wave moir images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moir fringes in general. PMID:25970298

  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. Tensile behavior of bulk metallic glasses by in situ x-ray diffraction

    SciTech Connect

    Wang, X. D.; Bednarcik, J.; Saksl, K.; Franz, H.; Cao, Q. P.; Jiang, J. Z.

    2007-08-20

    The authors report the use of in situ high-energy x-ray diffraction to detect the tensile behavior of two Zr- and La-based bulk metallic glasses (BMGs). Based on the diffraction data, the tensile elastic modulus and Poisson's ratio can be accurately evaluated. No excess free volume appears in the fractured region. However, a drastic change in atomic-level strains is found in the La-based BMG along the tensile direction, while a tiny crystalline component is detected in the fracture region of Zr-based BMG, which may be the different factors leading to the catastrophic failure of them, respectively.

  16. Time-resolved coherent X-ray diffraction imaging of surface acoustic waves

    PubMed Central

    Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schlein, 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

  17. Crystallization and preliminary X-ray diffraction studies of Escherichia coli glyceraldehyde-3-phosphate dehydrogenase.

    PubMed

    Olivier, L; Buisson, G; Fanchon, E; Corbier, C; Branlant, G; Dideberg, O

    1995-03-01

    Phosphorylating glyceraldehyde-3-phosphate dehydrogenase (GAPDH) is a key enzyme in glycolysis. Single crystals of NAD-dependent GAPDH from Escherichia coli have been obtained by vapour diffusion at room temperature using trisodium citrate as precipitant. In almost the same crystallization conditions, two kinds of crystals were found to be suitable for X-ray diffraction. The crystals with only one half of a tetramer in the asymmetric unit were chosen for high- resolution analysis. They belonged to space group C222(1), with cell dimensions a = 79.1, b = 189.6 and c = 122.2 A. These crystals diffracted to 1.8 A resolution. PMID:15299328

  18. 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.

  19. Commissioning of Angle Dispersive X-ray Diffraction Beamline on Indus-2

    SciTech Connect

    Sinha, A. K.; Sagdeo, Archna; Gupta, Pooja; Kumar, Ashok; Singh, M. N.; Gupta, R. K.; Kane, S. R.; Deb, S. K.

    2011-07-15

    An Angle dispersive x-ray diffraction (ADXRD) beamline on bending magnet source of Indus-2 synchrotron (2.5 GeV, 300 mA) has been commissioned, for the study of single and polycrystalline samples. The beamline optics is based on vertically focusing Pt-coated pre and post mirrors and sagittal focusing Si (311) based double crystal monochromator. Experimental station consists of a six circle diffractometer equipped with scintillation detector and an image plate area detector for powder diffraction. XRD experiments have been performed to study single crystal and polycrystalline samples.

  20. 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.

  1. On the microstructure of nanoporous gold: an x-ray diffraction study

    SciTech Connect

    Van Petegem, S; Brandstetter, S; Maa?, R; Schmitt, B; Borca, C; Van Swygenhoven, H; Hodge, A M; El-Dasher, B S; Biener, J

    2008-08-26

    The evolution of the grain structure, internal stresses, and the lattice misorientations of nanoporous gold (npAu) during dealloying of bulk (3D) Ag-Au alloy samples was studied by various in-situ and ex-situ X-ray diffraction techniques including powder and Laue diffraction. The experiments reveal that the dealloying process preserves the original crystallographic structure, but leads to a small spread in orientations within individual grains. Furthermore, most grains develop in-plane tensile stress. The feature size of the developing nanoporous structure increases with increasing dealloying time.

  2. Compression studies of TiB2 using synchrotron x-ray diffraction and ultrasonic techniques

    NASA Astrophysics Data System (ADS)

    Amulele, George M.; Manghnani, Murli H.

    2005-01-01

    The compressibility of TiB2 has been determined separately by synchrotron x-ray diffraction and ultrasonic measurements on samples loaded in diamond-anvil cells and in multianvil high-pressure apparatus up to pressures of 65.9GPa and 13.9GPa, respectively, at ambient temperature. The high-pressure x-ray diffraction measurements, carried out on a pure polycrystalline sample, show a monotonic decrease of the lattice parameters with pressure, with the c /a ratio variation suggesting an increase in the structural rigidity along the c direction. No structural transition is observed even after laser heating of the sample up to 2200K at 40GPa, indicating a phase stability of TiB2 in this pressure range. The ultrasonic measurements of compressional Vp and shear Vs velocities on a cylindrical specimen show linear pressure dependencies. Using the third-order Eulerian finite strain equation to fit the pressure-volume x-ray data, we obtain an isothermal bulk modulus of KTo=232.94.2GPa and its pressure derivative KTo'=3.860.23. Similarly, the parameters derived from fitting the finite strain equation to the ultrasonic data give an adiabatic bulk modulus of KSo=232.91.6GPa and KSo'=3.020.24, in good agreement with the x-ray diffraction measurements. The shear modulus and its pressure derivative derived from the ultrasonic measurements are GSo=259.80.4 and GSo'=2.520.01, respectively.

  3. Hybrid quantitative simulation on the in-line phase-contrast x-ray imaging of three dimensional samples under actual clinic imaging parameters

    SciTech Connect

    Yu Hong; Han Shensheng; Ding Jianhui; Jiang Zhaoxia; Peng Weijun

    2009-07-06

    A hybrid model combining Monte Carlo method with diffraction theory of wave optics has been developed and applied to quantitatively simulate the in-line diffractive phase-contrast x-ray imaging of three dimensional tissue samples under actual clinic imaging parameters. The primary microcosmic interactions of medical-energy x-ray within matter including photoabsorption, Compton scattering, and coherent scattering, have been taken into account in the Monte Carlo simulation. A diffraction processing based on Fresnel diffraction theory is carried out to simulate the macroscopic diffraction effect. A comparison with experiment results has also been performed.

  4. 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.

  5. Wedge-Driven and Miniature Diamond-Anvil Cells for High-Pressure Optical and X-Ray Diffraction Studies

    NASA Astrophysics Data System (ADS)

    Aoki, Katsutoshi; Kakudate, Yozo; Yoshida, Masatake; Usuba, Shu; Tanaka, Katsumi; Fujiwara, Syuzo

    1987-12-01

    This paper describes two newly designed diamond-anvil cells. The first one, applicable to powder X-ray diffraction and optical measurements, employs a wedge-driven thrust mechanism for pressure generation. This mechanism enables the fine control of the pressure and remote operation of the cell. The second one, designed for single-crystal X-ray diffraction studies, employs a screw-clamped mechanism for the sake of compactness. The operations for loading and compressing samples with this cell are facilitated by combining it with a wedge-driven cell. Their applications to X-ray diffraction measurements are presented.

  6. 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

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

    PubMed

    Giewekemeyer, K; Hackenberg, C; Aquila, A; Wilke, R N; Groves, M R; Jordanova, R; Lamzin, V S; Borchers, G; Saksl, K; Zozulya, A V; Sprung, M; Mancuso, A P

    2015-11-01

    The structural investigation of noncrystalline, soft biological matter using x-rays is of rapidly increasing interest. Large-scale x-ray sources, such as synchrotrons and x-ray free electron lasers, are becoming ever brighter and make the study of such weakly scattering materials more feasible. Variants of coherent diffractive imaging (CDI) are particularly attractive, as the absence of an objective lens between sample and detector ensures that no x-ray photons scattered by a sample are lost in a limited-efficiency imaging system. Furthermore, the reconstructed complex image contains quantitative density information, most directly accessible through its phase, which is proportional to the projected electron density of the sample. If applied in three dimensions, CDI can thus recover the sample's electron density distribution. As the extension to three dimensions is accompanied by a considerable dose applied to the sample, cryogenic cooling is necessary to optimize the structural preservation of a unique sample in the beam. This, however, imposes considerable technical challenges on the experimental realization. Here, we show a route toward the solution of these challenges using ptychographic CDI (PCDI), a scanning variant of coherent imaging. We present an experimental demonstration of the combination of three-dimensional structure determination through PCDI with a cryogenically cooled biological sample--a budding yeast cell (Saccharomyces cerevisiae)--using hard (7.9 keV) synchrotron x-rays. This proof-of-principle demonstration in particular illustrates the potential of PCDI for highly sensitive, quantitative three-dimensional density determination of cryogenically cooled, hydrated, and unstained biological matter and paves the way to future studies of unique, nonreproducible biological cells at higher resolution. PMID:26536275

  8. 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-K? radiation with the sin2? 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, ?1m, and perpendicular to the fiber direction, ?2m, and shear stress ?12m can be expressed as the functions of the applied (macro-) stresses, ?1A, ?2A , ?12A as follows: ?1m = ?11?1A +?12?2A, ?2m = ?21?1A + ?22?2A, ?12m = ?66?12A, where ?11 ,?12, ?21, ?22, ?66 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.

  9. Ultrafast structural dynamics with table top femtosecond hard X-ray and electron diffraction setups

    NASA Astrophysics Data System (ADS)

    Hada, M.; Pichugin, K.; Sciaini, G.

    2013-07-01

    The following tutorial review is directed to graduate students willing to be part of the emerging field of ultrafast structural dynamics. It provides them with an introduction to the field and all the very basic assumptions and experimental tricks involved in femtosecond (fs) diffraction techniques. The concept of stroboscopic photography and its implication in ultrafast science are introduced. Special attention is paid to the generation of ultrashort electron and hard X-ray pulses in table top setups, and a direct comparison in terms of brightness and temporal resolution between current table top and facility-based methodologies is given for proper calibration. This review is focused on ultrafast X-ray and electron diffraction techniques. The progress in the development of fs-structural probes during the last twenty years has been tremendous. Current ultrafast structural probes provide us with the temporal and spatial resolutions required to observe atoms in motion. Different compression approaches have made it possible the generation of ultrashort and ultrabright electron pulses with an effective brightness close to that of fs-hard X-ray pulses produced by free electron lasers. We now have in hand a variety of ultrafast structural cameras ready to be applied for the study of an endless list of dynamical phenomena at the atomic level of inspection.

  10. 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.

  11. 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.

  12. 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.

  13. 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 ?,?-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.

  14. DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

    NASA Astrophysics Data System (ADS)

    Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

    2012-03-01

    X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

  15. Glancing Angle Dependence of the X-Ray Emission Measured under Total Reflection Angle X-Ray Spectroscopy (TRAXS) Condition during Reflection High Energy Electron Diffraction Observation

    NASA Astrophysics Data System (ADS)

    Yamanaka, Toshiro; Hanada, Takashi; Ino, Shozo; Daimon, Hiroshi

    1992-10-01

    We measured the glancing angle (?g) dependence of the X-ray emission from Si(111)-\\sqrt{3}\\sqrt{3}-Ag and ?-\\sqrt{3}\\sqrt{3}-Au surfaces during Reflection High Energy Electron Diffraction observation under the Total Reflection Angle X-ray Spectroscopy condition. The characteristic X-rays AgL and AuM decreased according to 1/sin ?g. The function 1/\\sin?g is easily understood in terms of Ag and Au atoms located at the top layer of the surface. The SiK and the bremsstrahlung showed broad peaks around 8. These trends of the curves are explained by an analysis using Monte Carlo electron trajectory simulation. By measuring the glancing angle dependence we can easily distinguish whether or not a specific kind of atom is confined at the top layer of the surface.

  16. 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.

  17. 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.

  18. Synchrotron X-ray diffraction and fluorescence study of the astrolabe

    NASA Astrophysics Data System (ADS)

    Notis, Michael; Newbury, Brian; Stephenson, Bruce; Stephenson, G. Brian

    2013-04-01

    The astrolabe is an ancient analogue astronomical computing device used for calculations relating to position and time of the observer's location. In its most common form (the planispheric astrolabe), it consists of an engraved plate or series of plates held together and pinned in a housing, the assembly usually being made of brass. The present study describes the use of X-ray diffraction (XRD) and X-ray fluorescence (XRF) in a synchrotron to elucidate the composition of, and fabrication techniques used for, the major component parts of the astrolabe. The synchrotron XRF studies are compared to similar studies made with a handheld XRF instrument and the advantages and disadvantages of both approaches are discussed.

  19. Mesoscale X-ray diffraction measurement of stress relaxation associated with buckling in compressed thin films

    SciTech Connect

    Goudeau, Philippe; Villain, Pascale; Tamura, Nobumichi; Padmore, Howard A.

    2003-07-01

    Compressed thin films deposited on substrates may buckle depending on the geometrical and mechanical properties of the film/substrate set. Until recently, the small dimensions of the buckling have prevented measurements of their local in plane internal stress distribution. Using a Scanning X-ray Micro diffraction (mSXRD) technique developed at a 3rd generation x-ray synchrotron source, we obtained thin film internal stress maps for circular blisters and telephone chord buckling with micrometric spatial resolution. A fair agreement was found between the film delamination topology observed by optical microscopy and the measured stress maps. We evidenced residual stress relaxation associated with the film buckling: the top is essentially stress-free while adherent region exhibits large compressive stresses.

  20. 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.

  1. X-ray Diffraction Results from Mars Science Laboratory: Mineralogy of Rocknest at Gale Crater

    NASA Astrophysics Data System (ADS)

    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.; Achilles, Cherie; Agard, Christophe; Verdasca, Jos Alexandre Alves; Anderson, Robert; Anderson, Ryan; Archer, Doug; Armiens-Aparicio, Carlos; Arvidson, Ray; Atlaskin, Evgeny; Atreya, Sushil; Aubrey, Andrew; Baker, Burt; Baker, Michael; Balic-Zunic, Tonci; Baratoux, David; Baroukh, Julien; Barraclough, Bruce; Bean, Keri; Beegle, Luther; Behar, Alberto; Bell, James; Bender, Steve; Benna, Mehdi; Bentz, Jennifer; Berger, Gilles; Berger, Jeff; Berman, Daniel; Bish, David; Blake, David F.; Avalos, Juan J. Blanco; Blaney, Diana; Blank, Jen; Blau, Hannah; Bleacher, Lora; Boehm, Eckart; Botta, Oliver; Bttcher, Stephan; Boucher, Thomas; Bower, Hannah; Boyd, Nick; Boynton, Bill; Breves, Elly; Bridges, John; Bridges, Nathan; Brinckerhoff, William; Brinza, David; Bristow, Thomas; Brunet, Claude; Brunner, Anna; Brunner, Will; Buch, Arnaud; Bullock, Mark; Burmeister, Snke; Cabane, Michel; Calef, Fred; Cameron, James; Campbell, John "Iain"; Cantor, Bruce; Caplinger, Michael; Rodrguez, Javier Caride; Carmosino, Marco; Blzquez, Isaas Carrasco; Charpentier, Antoine; Chipera, Steve; Choi, David; Clark, Benton; Clegg, Sam; Cleghorn, Timothy; Cloutis, Ed; Cody, George; Coll, Patrice; Conrad, Pamela; Coscia, David; Cousin, Agns; Cremers, David; Crisp, Joy; Cros, Alain; Cucinotta, Frank; d'Uston, Claude; Davis, Scott; Day, Mackenzie "Kenzie"; Juarez, Manuel de la Torre; DeFlores, Lauren; DeLapp, Dorothea; DeMarines, Julia; DesMarais, David; Dietrich, William; Dingler, Robert; Donny, Christophe; Downs, Bob; Drake, Darrell; Dromart, Gilles; Dupont, Audrey; Duston, Brian; Dworkin, Jason; Dyar, M. Darby; Edgar, Lauren; Edgett, Kenneth; Edwards, Christopher; Edwards, Laurence; Ehlmann, Bethany; Ehresmann, Bent; Eigenbrode, Jen; Elliott, Beverley; Elliott, Harvey; Ewing, Ryan; Fabre, Ccile; Fairn, Alberto; Farley, Ken; Farmer, Jack; Fassett, Caleb; Favot, Laurent; Fay, Donald; Fedosov, Fedor; Feldman, Jason; Feldman, Sabrina; Fisk, Marty; Fitzgibbon, Mike; Flesch, Greg; Floyd, Melissa; Flckiger, Lorenzo; Forni, Olivier; Fraeman, Abby; Francis, Raymond; Franois, Pascaline; Franz, Heather; Freissinet, Caroline; French, Katherine Louise; Frydenvang, Jens; Gaboriaud, Alain; Gailhanou, Marc; Garvin, James; Gasnault, Olivier; Geffroy, Claude; Gellert, Ralf; Genzer, Maria; Glavin, Daniel; Godber, Austin; Goesmann, Fred; Goetz, Walter; Golovin, Dmitry; Gmez, Felipe Gmez; Gmez-Elvira, Javier; Gondet, Brigitte; Gordon, Suzanne; Gorevan, Stephen; Grant, John; Griffes, Jennifer; Grinspoon, David; Grotzinger, John; Guillemot, Philippe; Guo, Jingnan; Gupta, Sanjeev; Guzewich, Scott; Haberle, Robert; Halleaux, Douglas; Hallet, Bernard; Hamilton, Vicky; Hardgrove, Craig; Harker, David; Harpold, Daniel; Harri, Ari-Matti; Harshman, Karl; Hassler, Donald; Haukka, Harri; Hayes, Alex; Herkenhoff, Ken; Herrera, Paul; Hettrich, Sebastian; Heydari, Ezat; Hipkin, Victoria; Hoehler, Tori; Hollingsworth, Jeff; Hudgins, Judy; Huntress, Wesley; Hurowitz, Joel; Hviid, Stubbe; Iagnemma, Karl; Indyk, Steve; Isral, Guy; Jackson, Ryan; Jacob, Samantha; Jakosky, Bruce; Jensen, Elsa; Jensen, Jaqueline Klvgaard; Johnson, Jeffrey; Johnson, Micah; Johnstone, Steve; Jones, Andrea; Jones, John; Joseph, Jonathan; Jun, Insoo; Kah, Linda; Kahanp, Henrik; Kahre, Melinda; Karpushkina, Natalya; Kasprzak, Wayne; Kauhanen, Janne; Keely, Leslie; Kemppinen, Osku; Keymeulen, Didier; Kim, Myung-Hee; Kinch, Kjartan; King, Penny; Kirkland, Laurel; Kocurek, Gary; Koefoed, Asmus; Khler, Jan; Kortmann, Onno; Kozyrev, Alexander; Krezoski, Jill; Krysak, Daniel; Kuzmin, Ruslan; Lacour, Jean Luc; Lafaille, Vivian; Langevin, Yves; Lanza, Nina; Lasue, Jeremie; Le Moulic, Stphane; Lee, Ella Mae; Lee, Qiu-Mei; Lees, David; Lefavor, Matthew; Lemmon, Mark; Malvitte, Alain Lepinette; Leshin, Laurie; Lveill, Richard; Lewin-Carpintier, ric; Lewis, Kevin; Li, Shuai; Lipkaman, Leslie; Little, Cynthia; Litvak, Maxim; Lorigny, Eric; Lugmair, Guenter; Lundberg, Angela; Lyness, Eric; Madsen, Morten; Mahaffy, Paul; Maki, Justin; Malakhov, Alexey; Malespin, Charles; Malin, Michael; Mangold, Nicolas; Manhes, Grard; Manning, Heidi; Marchand, Genevive; Jimnez, Mercedes Marn; Garca, Csar Martn; Martin, Dave; Martin, Mildred; Martnez-Fras, Jess; Martn-Soler, Javier; Martn-Torres, F. Javier; Mauchien, Patrick

    2013-09-01

    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 Fe3+- 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.

  2. 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

  3. 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.

  4. 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.

  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. 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

  7. Determination of the absolute chirality of tellurium using resonant diffraction with circularly polarized x-rays

    NASA Astrophysics Data System (ADS)

    Tanaka, Y.; Collins, S. P.; Lovesey, S. W.; Matsumami, M.; Moriwaki, T.; Shin, S.

    2010-03-01

    Many proteins, sugars and pharmaceuticals crystallize into two forms that are mirror images of each other (enantiomers) like our right and left hands. Tellurium is one enantiomer having a space group pair, P3121 (right-handed screw) and P3221 (left-handed screw). X-ray diffraction with dispersion correction terms has been playing an important role in determining the handedness of enantiomers for a long time. However, this approach is not applicable for an elemental crystal such as tellurium or selenium. We have demonstrated that positive and negative circularly polarized x-rays at the resonant energy of tellurium can be used to absolutely distinguish right from left tellurium. This method is applicable to chiral motifs that occur in biomolecules, liquid crystals, ferroelectrics and antiferroelectrics, multiferroics, etc.

  8. 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.

  9. 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.

  10. 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.

  11. KOTOBUKI-1 apparatus for cryogenic coherent X-ray diffraction imaging

    NASA Astrophysics Data System (ADS)

    Nakasako, Masayoshi; Takayama, Yuki; Oroguchi, Tomotaka; Sekiguchi, Yuki; Kobayashi, Amane; Shirahama, Keiya; Yamamoto, Masaki; Hikima, Takaaki; Yonekura, Koji; Maki-Yonekura, Saori; Kohmura, Yoshiki; Inubushi, Yuichi; Takahashi, Yukio; Suzuki, Akihiro; Matsunaga, Sachihiro; Inui, Yayoi; Tono, Kensuke; Kameshima, Takashi; Joti, Yasumasa; Hoshi, Takahiko

    2013-09-01

    We have developed an experimental apparatus named KOTOBUKI-1 for use in coherent X-ray diffraction imaging experiments of frozen-hydrated non-crystalline particles at cryogenic temperature. For cryogenic specimen stage with small positional fluctuation for a long exposure time of more than several minutes, we here use a cryogenic pot cooled by the evaporation cooling effect for liquid nitrogen. In addition, a loading device is developed to bring specimens stored in liquid nitrogen to the specimen stage in vacuum. The apparatus allows diffraction data collection for frozen-hydrated specimens at 66 K with a positional fluctuation of less than 0.4 ?m and provides an experimental environment to easily exchange specimens from liquid nitrogen storage to the specimen stage. The apparatus was developed and utilized in diffraction data collection of non-crystalline particles with dimensions of ?m from material and biological sciences, such as metal colloid particles and chloroplast, at BL29XU of SPring-8. Recently, it has been applied for single-shot diffraction data collection of non-crystalline particles with dimensions of sub-?m using X-ray free electron laser at BL3 of SACLA.

  12. KOTOBUKI-1 apparatus for cryogenic coherent X-ray diffraction imaging

    SciTech Connect

    Nakasako, Masayoshi; Takayama, Yuki; Oroguchi, Tomotaka; Sekiguchi, Yuki; Kobayashi, Amane; RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo, Hyogo 679-5148 ; Shirahama, Keiya; Yamamoto, Masaki; Hikima, Takaaki; Yonekura, Koji; Maki-Yonekura, Saori; Kohmura, Yoshiki; Inubushi, Yuichi; Takahashi, Yukio; Suzuki, Akihiro; Department of Precision Science and Technology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 ; Matsunaga, Sachihiro; Inui, Yayoi; Tono, Kensuke; Kameshima, Takashi; Joti, Yasumasa; Hoshi, Takahiko

    2013-09-15

    We have developed an experimental apparatus named KOTOBUKI-1 for use in coherent X-ray diffraction imaging experiments of frozen-hydrated non-crystalline particles at cryogenic temperature. For cryogenic specimen stage with small positional fluctuation for a long exposure time of more than several minutes, we here use a cryogenic pot cooled by the evaporation cooling effect for liquid nitrogen. In addition, a loading device is developed to bring specimens stored in liquid nitrogen to the specimen stage in vacuum. The apparatus allows diffraction data collection for frozen-hydrated specimens at 66 K with a positional fluctuation of less than 0.4 ?m and provides an experimental environment to easily exchange specimens from liquid nitrogen storage to the specimen stage. The apparatus was developed and utilized in diffraction data collection of non-crystalline particles with dimensions of ?m from material and biological sciences, such as metal colloid particles and chloroplast, at BL29XU of SPring-8. Recently, it has been applied for single-shot diffraction data collection of non-crystalline particles with dimensions of sub-?m using X-ray free electron laser at BL3 of SACLA.

  13. 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.

  14. Hard X-ray Diffractive Focusing Properties of GaAs Linear Bragg-Fresnel Lenses

    NASA Astrophysics Data System (ADS)

    Li, Youli; Wong, Gerard C. L.; Case, Ryan; Caine, Ernie; Hu, Evelyn; Safinya, Cyrus R.; Fernandez, Patricia; Haeffner, Dean

    2000-03-01

    We investigated the diffractive focusing properties of linear Bragg-Fresnel Lenses (BFLs), which are being developed for hard x-ray microscopy and spectromicroscopy. The lenses were fabricated on GaAs substrates using e-beam lithography and reactive ion etching methods. We demonstrated that the use of GaAs resulted in much reduced (compared to Si) zone depth and significant gains in processing control.(Li, Y., G.C.L. Wong, C.R. Safinya, et al, Rev. of Sci. Instrum.),69(8), p. 2844-8 (1998) Linear BFLs with 0.3 ? m diffraction-limited resolution and zone length up to 10 mm were characterized at the Advanced Photon Source using an undulator source in the energy range of 8 keV - 40 keV. Focal plane diffraction patterns were measured using a x-ray fluorescence probe. The data were in good agreement with a model based on Kirchhoff-Fresnel diffraction theory by considering the undulator emission as a partially coherent and spatially extended source.

  15. KOTOBUKI-1 apparatus for cryogenic coherent X-ray diffraction imaging.

    PubMed

    Nakasako, Masayoshi; Takayama, Yuki; Oroguchi, Tomotaka; Sekiguchi, Yuki; Kobayashi, Amane; Shirahama, Keiya; Yamamoto, Masaki; Hikima, Takaaki; Yonekura, Koji; Maki-Yonekura, Saori; Kohmura, Yoshiki; Inubushi, Yuichi; Takahashi, Yukio; Suzuki, Akihiro; Matsunaga, Sachihiro; Inui, Yayoi; Tono, Kensuke; Kameshima, Takashi; Joti, Yasumasa; Hoshi, Takahiko

    2013-09-01

    We have developed an experimental apparatus named KOTOBUKI-1 for use in coherent X-ray diffraction imaging experiments of frozen-hydrated non-crystalline particles at cryogenic temperature. For cryogenic specimen stage with small positional fluctuation for a long exposure time of more than several minutes, we here use a cryogenic pot cooled by the evaporation cooling effect for liquid nitrogen. In addition, a loading device is developed to bring specimens stored in liquid nitrogen to the specimen stage in vacuum. The apparatus allows diffraction data collection for frozen-hydrated specimens at 66 K with a positional fluctuation of less than 0.4 ?m and provides an experimental environment to easily exchange specimens from liquid nitrogen storage to the specimen stage. The apparatus was developed and utilized in diffraction data collection of non-crystalline particles with dimensions of ?m from material and biological sciences, such as metal colloid particles and chloroplast, at BL29XU of SPring-8. Recently, it has been applied for single-shot diffraction data collection of non-crystalline particles with dimensions of sub-?m using X-ray free electron laser at BL3 of SACLA. PMID:24089834

  16. The determination of electric field gradients from X-ray diffraction data

    NASA Astrophysics Data System (ADS)

    Brown, Anthony S.; Spackman, Mark A.

    The electric field gradient (EFG) tensors for Al and O atoms in corundum and for C and D(2H) in hexadeuterobenzene (C6D6) are determined from accurate X-ray diffraction data using four independent computational strategies. Two of the strategies capitalize on the fact that the electric field gradient is the second derivative of the electrostatic potential, a simple relationship which has not been exploited previously in analyses of diffraction data. The convergence behaviour of the tensor components calculated by each strategy is examined for both systems, and the fully converged results obtained with each computational strategy are shown to be identical. It is found that the orientation of the tensors and the signs of their components are well determined from diffraction data, but the magnitudes and asymmetry of the components are not. Discrepancies in previous analyses of the corundum data are resolved, and it is shown that the origin of the EFG at hydrogen is quite different from that at heavier nuclei. Successful determination of EFGs from X-ray diffraction data appears within reach, but will require precise knowledge of atomic position and thermal parameters, more extensive data sets than are currently available, and a more flexible pseudoatom model than presently used.

  17. 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.

  18. 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 1050C 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 ?m. The complex of X-ray diffraction techniques includes a measurement of ?-2? 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 ?-2? 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.

  19. Vibrational Spectroscopy and X-ray Diffraction of Cd(OH)2 to 28GPa at 300 K

    SciTech Connect

    Shim, Sang-Heon; Rekhi, Sandeep; Martin, Michael C.; Jeanloz,Raymond

    2006-03-20

    We report Raman and infrared absorption spectroscopy alongwith X-ray diffraction for brucite-type beta-Cd(OH)2 to 28 GPa at 300 K.The OH-stretching modes soften with pressure and disappear at 21 GPa withtheir widths increasing rapidly above 5 GPa, consistent with a gradualdisordering of the H sublattice at 5 20 GPa similar to that previouslyobserved for Co(OH)2.Asymmetry in the peak shapes of the OH-stretchingmodes suggests the existence of diverse disordered sitesfor H atoms inCd(OH)2 under pressure. Above 15 GPa, the A1g(T) lattice mode showsnon-linear behavior and softens to 21 GPa, at which pressure significantchanges are observed: new Raman modes appear, two Raman-active latticemodes and the OH-stretching modes of the low-pressure phase disappears,and the positions of some X-ray diffraction lines change abruptly withthe appearance of weak new diffraction features. These observationssuggest that amorphization of the H sublattice is accompanied by acrystalline-to-crystalline transition at 21 GPa in Cd(OH)2, which has notbeen previously observed in the brucite-type hydroxides. The Ramanspectra of the high-pressure phase of Cd(OH)2 is similar to those of thehigh-pressure phase of single-crystal Ca(OH)2 of which structure has beententatively assigned to the Sr(OH)2 type.

  20. 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 l) 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 (1015 m) loaded into the chips yielded a complete, high-resolution (<1.6 ) 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.

  1. 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.

  2. Single-crystal X-ray diffraction studies of photo-induced molecular species.

    PubMed

    Cole, Jacqueline M

    2004-10-20

    This tutorial review gathers together the recent developments in single-crystal X-ray diffraction that are starting to enable one to quantify directly the nature of light-induced electronic perturbations in chemical structures. Such structural information is key to understanding many photo-activated chemical processes and physical properties, and a description of the scientific impetus behind this incipient area of structural science, from academic and industrial perspectives, is given. Photoisomerism processes, solid-state photochemical reactions and spin-cross-over magnetic transitions, that have long-lived or irreversible light-induced states, are best understood by unravelling their three-dimensional structures measured in situ in their photo-converted state. A review of steady-state laser-induced single-crystal X-ray diffraction studies conducted, to date, and the experimental methodologies used in order to realise such structures, is presented. The structural characterisation of more transient photo-induced species (down to picosecond lifetimes) is paramount to a better understanding of the materials that undergo high-speed electronic switching, which make operative much of the electronics and optics industry, since there exists an inherent relationship between the excited-state structure and the physical properties exhibited. Prime examples include excited-state structures of molecular conductors and luminescent materials with potential applications as molecular wires, light-emitting diodes, non-linear optics, triboluminescence and electroluminescence. Previously, only indirect and qualitative interpretations of the nature of these excited-states could be formulated via spectroscopic techniques, but the developments in ms-ps time-resolved laser pump, X-ray probe single-crystal diffraction techniques, described herein, are overcoming this barrier, affording results that are entirely quantitative via a three-dimensional structural representation. In this regard, a review of structures of transient species studied to date is presented along with a discussion of the key experimental parameters that are required for a successful experiment, in terms of the X-ray, laser and sample characteristics. The importance of auxiliary spectroscopic work and complementary theoretical calculations is also briefly discussed. The paper concludes with a future outlook on new possible X-ray sources that will facilitate such work and extend it to structural studies on even more ephemeral species in the future. PMID:15480474

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. X-ray diffraction studies and equation of state of methane at 200 GPa

    SciTech Connect

    Sun, L.

    2010-02-24

    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. X-ray images of the solid CH{sub 4} at three pressures, showing the high pressure phase with cubic structure persisting up to 202 GPa. At high pressure the XRD from the sample became increasingly weaker. To improve the quality of XRD pattern, we reduced the X-ray focus spot size and clean-up slits at 171 GPa, and increased the exposure time for each measurement.

  8. 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

  9. Tracking the motion of charges in a terahertz light field by femtosecond X-ray diffraction.

    PubMed

    Cavalleri, A; Wall, S; Simpson, C; Statz, E; Ward, D W; Nelson, K A; Rini, M; Schoenlein, R W

    2006-08-10

    In condensed matter, light propagation near resonances is described in terms of polaritons, electro-mechanical excitations in which the time-dependent electric field is coupled to the oscillation of charged masses. This description underpins our understanding of the macroscopic optical properties of solids, liquids and plasmas, as well as of their dispersion with frequency. In ferroelectric materials, terahertz radiation propagates by driving infrared-active lattice vibrations, resulting in phonon-polariton waves. Electro-optic sampling with femtosecond optical pulses can measure the time-dependent electrical polarization, providing a phase-sensitive analogue to optical Raman scattering. Here we use femtosecond time-resolved X-ray diffraction, a phase-sensitive analogue to inelastic X-ray scattering, to measure the corresponding displacements of ions in ferroelectric lithium tantalate, LiTaO(3). Amplitude and phase of all degrees of freedom in a light field are thus directly measured in the time domain. Notably, extension of other X-ray techniques to the femtosecond timescale (for example, magnetic or anomalous scattering) would allow for studies in complex systems, where electric fields couple to multiple degrees of freedom. PMID:16900195

  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. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. Purification, crystallization, small-angle X-ray scattering and preliminary X-ray diffraction analysis of the SH2 domain of the Csk-homologous kinase.

    PubMed

    Gunn, Natalie J; Gorman, Michael A; Dobson, Renwick C J; Parker, Michael W; Mulhern, Terrence D

    2011-03-01

    The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2?M sodium bromide, 0.1?M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ?1.6? resolution. The crystals belonged to space group P2, with unit-cell parameters a=25.8, b=34.6, c=63.2?, ?=99.4. PMID:21393838

  18. 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.

  19. X-ray diffraction analysis of a crystal of HscA from Escherichia coli

    SciTech Connect

    Aoto, Phillip C.; Ta, Dennis T.; Cupp-Vickery, Jill R. Vickery, Larry E.

    2005-07-01

    A truncated form of HscA (52 kDa) containing both nucleotide- and substrate-binding domains has been crystallized and analyzed by X-ray diffraction. The crystal belongs to space group P2{sub 1}2{sub 1}2{sub 1} and diffracts to 2.9 . HscA is a constitutively expressed Hsp70 that interacts with the ironsulfur cluster assembly protein IscU. Crystals of a truncated form of HscA (52 kDa; residues 17505) grown in the presence of an IscU-recognition peptide, WELPPVKI, have been obtained by hanging-drop vapor diffusion using ammonium sulfate as the precipitant. A complete native X-ray diffraction data set was collected from a single crystal at 100 K to a resolution of 2.9 . The crystal belongs to the orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 158.35, b = 166.15, c = 168.26 , and contains six molecules per asymmetric unit. Phases were determined by molecular replacement using the nucleotide-binding domain from DnaK and the substrate-binding domain from HscA as models. This is the first reported crystallization of an Hsp70 containing both nucleotide- and substrate-binding domains.

  20. 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, 13601366]. 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 . The crystals belong to the trigonal space group P3{sub 1}21, with unit-cell parameters a = b = 116.83, c = 92.24 , and contain one protein molecule per asymmetric unit. The V{sub M} value and solvent content are 4.07 {sup 3} Da{sup ?1} and 69.8%, respectively.

  1. 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.

  2. 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.

  3. 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.

  4. Quantum oscillations and beats in X-ray diffraction during film growth.

    PubMed

    Lee, Y-R; Gray, A; Tischler, J; Czoschke, P; Hong, H; Chang, S-L; Chiang, T-C

    2007-10-12

    X-ray diffraction from a growing film at an anti-Bragg point should exhibit bilayer oscillations caused by interference. In an experiment of TiN film growth by laser ablation onto sapphire, an unexpected beating envelope function is found to modulate the oscillations. The successive nodes and antinodes are identified with the development of new growth domains separated by one atomic layer in thickness. This effect allows atomic layer counting of the film thickness distribution. The results imply that the growth is not characterized by a continuum stochastic process, as usually assumed. PMID:17995191

  5. High Pressure X-ray Diffraction Study on Icosahedral Boron Arsenide (B12As2)

    SciTech Connect

    J Wu; H Zhu; D Hou; C Ji; C Whiteley; J Edgar; Y Ma

    2011-12-31

    The high pressure properties of icosahedral boron arsenide (B12As2) were studied by in situ X-ray diffraction measurements at pressures up to 25.5 GPa at room temperature. B12As2 retains its rhombohedral structure; no phase transition was observed in the pressure range. The bulk modulus was determined to be 216 GPa with the pressure derivative 2.2. Anisotropy was observed in the compressibility of B12As2-c-axis was 16.2% more compressible than a-axis. The boron icosahedron plays a dominant role in the compressibility of boron-rich compounds.

  6. 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.

  7. High-resolution x-ray diffraction study of single crystals of lead zirconate titanate

    NASA Astrophysics Data System (ADS)

    Gorfman, S.; Keeble, D. S.; Glazer, A. M.; Long, X.; Xie, Y.; Ye, Z.-G.; Collins, S.; Thomas, P. A.

    2011-07-01

    The symmetry of single-crystal piezoelectric PbZr1-xTixO3, with x?0.31 and x?0.46, has been investigated by high-resolution x-ray diffraction, both at room temperature and up to and above the Curie temperature. Reciprocal space maps around a selection of Bragg reflections were collected and self-consistent patterns showing Bragg splittings were observed. The analysis of the separation of peaks from different twin domains provides precise information on PbZr1-xTixO3 symmetry when approaching the morphotropic phase boundary at x=0.48 from the zirconium-rich side.

  8. 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

  9. 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.

  10. 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.

  11. Investigation of hepatic fibrosis in rats with x-ray diffraction enhanced imaging

    SciTech Connect

    Li Hui; Zhang Lu; Wang Xueyan; Luo Shuqian; Wang Tailing; Wang Baoen; Zhao Xinyan

    2009-03-23

    X-ray diffraction enhanced imaging (DEI) is a phase contrast technique that generates excellent contrast of biological soft tissues compared to conventional absorption radiography. We explore the application of DEI in the diagnosis of hepatic fibrosis. The produced refraction contrast images of fibrous rat liver samples show clearly abnormal liver architectures. Moreover, by comparing to histological pictures, different stages of fibrosis are discriminated, and the corresponding morphological features are analyzed. Besides, quantitative analyses of texture features are presented. The results reported herein show that DEI can be a potential noninvasive technique to diagnose and stage hepatic fibrosis.

  12. 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

  13. A scheme for lensless X-ray microscopy combining coherent diffraction imaging and differential corner holography.

    PubMed

    Capotondi, F; Pedersoli, E; Kiskinova, M; Martin, A V; Barthelmess, M; Chapman, H N

    2012-10-22

    We successfully use the corners of a common silicon nitride supporting window in lensless X-ray microscopy as extended references in differential holography to obtain a real space hologram of the illuminated object. Moreover, we combine this method with the iterative phasing techniques of coherent diffraction imaging to enhance the spatial resolution on the reconstructed object, and overcome the problem of missing areas in the collected data due to the presence of a beam stop, achieving a resolution close to 85 nm. PMID:23187281

  14. Structural investigation of Lisinopril by powder X-ray diffraction and solid-state NMR

    NASA Astrophysics Data System (ADS)

    Filip, Xenia; Tripon, Carmen; Borodi, Gheorghe; Oprean, Lumini?a; Filip, Claudiu

    2009-08-01

    Structural studies on polycrystalline Lisinopril (N-N-[(s)-1-carboxy-3-phenylpropyl]-L-lysil-L-proline) are performed by combined powder X-Ray diffraction and 13C solid-state nuclear magnetic resonance (NMR). The crystal structure of this drug, used primarily for the treatment of hypertension, has not yet been determined due to the impossibility of synthesizing single crystals of sufficient quality. It is shown here that valuable insights into the crystal and molecular structure of Lisinopril can be obtained on polycrystalline powder based on the complementary character of the information provided by the two techniques.

  15. High resolution x-ray and gamma ray imaging using diffraction lenses with mechanically bent crystals

    DOEpatents

    Smither, Robert K. (Hinsdale, IL)

    2008-12-23

    A method for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation is provided. High quality mechanically bent diffracting crystals of 0.1 mm radial width are used for focusing the radiation and directing the radiation to an array of detectors which is used for analyzing their addition to collect data as to the location of the source of radiation. A computer is used for converting the data to an image. The invention also provides for the use of a multi-component high resolution detector array and for narrow source and detector apertures.

  16. X-ray Diffraction Measurements in a Rotational Diamond Anvil Cell

    SciTech Connect

    Ma,Y.; Levitas, V.; Hashemi, J.

    2006-01-01

    We have established an experimental method to perform synchrotron X-ray diffraction in a rotational diamond anvil cell to study the properties of a material under pressure and shear by achieving a quasi-homogeneous pressure distribution. The uniform distribution of pressure eliminates the peak widening caused by pressure deviation in the sample chamber. This enables us to explore the effects of shear on the physical and chemical properties such as the structural disorder, phase transformation, and chemical bonding. The method has been applied in studying the shear-induced stacking fault, phase transition-induced plasticity, and the shear-induced formation of bonding between diamond and hexagonal boron nitride.

  17. Crystallization and preliminary X-ray diffraction analysis of alanine racemase from Pseudomonas putida YZ-26.

    PubMed

    Liu, Junlin; Feng, Lei; Shi, Yawei; Feng, Wei

    2012-10-01

    A recombinant form of alanine racemase (Alr) from Pseudomonas putida YZ-26 has been crystallized by the sitting-drop vapour diffusion method. X-ray diffraction data were collected to 2.4? resolution. The crystals belong to the space group C222(1), with unit-cell parameters a = 118.08, b = 141.86, c = 113.83?, and contain an Alr dimer in the asymmetric unit. The Matthews coefficient and the solvent content were calculated to be 2.8?(3)?Da(-1) and approximately 50%, respectively. PMID:23027757

  18. 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.

  19. Sample cell for powder x-ray diffraction at up to 500 bars and 200 C

    NASA Astrophysics Data System (ADS)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-11-01

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube.

  20. Directly Observing Squeezed Phonon States with Femtosecond X-Ray Diffraction

    SciTech Connect

    Johnson, S. L.; Beaud, P.; Vorobeva, E.; Ingold, G.; Milne, C. J.; Murray, E. D.; Fahy, S.

    2009-05-01

    Squeezed states are quantum states of a harmonic oscillator in which the variance of two conjugate variables each oscillate out of phase. Ultrafast optical excitation of crystals can create squeezed phonon states, where the variance of the atomic displacements oscillates due to a sudden change in the interatomic bonding strength. With femtosecond x-ray diffraction we measure squeezing oscillations in bismuth and conclude that they are consistent with a model in which electronic excitation softens all phonon modes by a constant scaling factor.