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Sample records for x-ray diffraction line

  1. X-Ray Diffraction.

    ERIC Educational Resources Information Center

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

    1980-01-01

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

  2. 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...

  3. 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

  4. X-ray diffraction line profile analysis of KBr thin films

    NASA Astrophysics Data System (ADS)

    Rai, R.; Triloki, Triloki; Singh, B. K.

    2016-08-01

    In the present work, the microcrystalline characteristics of KBr thin films have been investigated by evaluating the breadth of diffraction peak. The Williamson-Hall, the Size-Strain plot and the single-line Voigt methods are employed to deconvolute the finite crystallite size and microstrain contribution from the broaden X-ray profile. The texture coefficient and dislocation density have been determined along each diffraction peak. Other relevant physical parameters such as stress, Young's modulus and energy density are also estimated using uniform stress deformation and uniform deformation energy density approximation of Williamson-Hall method.

  5. 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.

  6. 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...

  7. 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.

  8. Phase-targeted X-ray diffraction

    PubMed Central

    Hansford, G. M.

    2016-01-01

    A powder X-ray diffraction (XRD) method to enhance the signal of a specific crystalline phase within a mixture is presented for the first time. Specificity to the targeted phase relies on finding coincidences in the ratios of crystal d spacings and the ratios of elemental characteristic X-ray energies. Such coincidences can be exploited so that the two crystal planes diffract through the same scattering angle at two different X-ray energies. An energy-resolving detector placed at the appropriate scattering angle will detect a significantly enhanced signal at these energies if the target mineral or phase is present in the sample. When implemented using high scattering angles, for example 2θ > 150°, the method is tolerant to sample morphology and distance on the scale of ∼2 mm. The principle of the method is demonstrated experimentally using Pd Lα1 and Pd Lβ1 emission lines to enhance the diffraction signal of quartz. Both a pure quartz powder pellet and an unprepared mudstone rock specimen are used to test and develop the phase-targeted method. The technique is further demonstrated in the sensitive detection of retained austenite in steel samples using a combination of In Lβ1 and Ti Kβ emission lines. For both these examples it is also shown how the use of an attenuating foil, with an absorption edge close to and above the higher-energy characteristic X-ray line, can serve to isolate to some degree the coincidence signals from other fluorescence and diffraction peaks in the detected spectrum. The phase-targeted XRD technique is suitable for implementation using low-cost off-the-shelf components in a handheld or in-line instrument format. PMID:27738415

  9. Diffractive Imaging Using Partially Coherent X Rays

    NASA Astrophysics Data System (ADS)

    Whitehead, L. W.; Williams, G. J.; Quiney, H. M.; Vine, D. J.; Dilanian, R. A.; Flewett, S.; Nugent, K. A.; Peele, A. G.; Balaur, E.; McNulty, I.

    2009-12-01

    The measured spatial coherence characteristics of the illumination used in a diffractive imaging experiment are incorporated in an algorithm that reconstructs the complex transmission function of an object from experimental x-ray diffraction data using 1.4 keV x rays. Conventional coherent diffractive imaging, which assumes full spatial coherence, is a limiting case of our approach. Even in cases in which the deviation from full spatial coherence is small, we demonstrate a significant improvement in the quality of wave field reconstructions. Our formulation is applicable to x-ray and electron diffraction imaging techniques provided that the spatial coherence properties of the illumination are known or can be measured.

  10. X-ray diffraction: instrumentation and applications.

    PubMed

    Bunaciu, Andrei A; Udriştioiu, Elena Gabriela; Aboul-Enein, Hassan Y

    2015-01-01

    X-ray diffraction (XRD) is a powerful nondestructive technique for characterizing crystalline materials. It provides information on structures, phases, preferred crystal orientations (texture), and other structural parameters, such as average grain size, crystallinity, strain, and crystal defects. X-ray diffraction peaks are produced by constructive interference of a monochromatic beam of X-rays scattered at specific angles from each set of lattice planes in a sample. The peak intensities are determined by the distribution of atoms within the lattice. Consequently, the X-ray diffraction pattern is the fingerprint of periodic atomic arrangements in a given material. This review summarizes the scientific trends associated with the rapid development of the technique of X-ray diffraction over the past five years pertaining to the fields of pharmaceuticals, forensic science, geological applications, microelectronics, and glass manufacturing, as well as in corrosion analysis.

  11. 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

  12. 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.

  13. X-ray dynamical diffraction Fraunhofer holography.

    PubMed

    Balyan, Minas

    2013-09-01

    An X-ray dynamical diffraction Fraunhofer holographic scheme is proposed. Theoretically it is shown that the reconstruction of the object image by visible light is possible. The spatial and temporal coherence requirements of the incident X-ray beam are considered. As an example, the hologram recording as well as the reconstruction by visible light of an absolutely absorbing wire are discussed.

  14. 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.

  15. 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.

  16. Interlaced X-ray diffraction computed tomography

    PubMed Central

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

    2016-01-01

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

  17. 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.

  18. Single particle X-ray diffractive imaging.

    PubMed

    Bogan, Michael J; Benner, W Henry; Boutet, Sébastien; Rohner, Urs; Frank, Matthias; Barty, Anton; Seibert, M Marvin; Maia, Filipe; Marchesini, Stefano; Bajt, Sasa; Woods, Bruce; Riot, Vincent; Hau-Riege, Stefan P; Svenda, Martin; Marklund, Erik; Spiller, Eberhard; Hajdu, Janos; Chapman, Henry N

    2008-01-01

    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 suboptical 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.

  19. 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)

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

    DOEpatents

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

    2016-08-09

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

  1. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Fabrication of 11-nm-Wide Silica-Like Lines Using X-Ray Diffraction Exposure

    NASA Astrophysics Data System (ADS)

    Zhu, Xiao-Li; Xie, Chang-Qing; Zhang, Man-Hong; Liu, Ming; Chen, Bao-Qin; Pan, Feng

    2009-08-01

    Fine silica-like lines with 11 nm width are successfully fabricated using x-ray Fresnel diffraction exposure. X-rays pass a mask of 175-nm-wide lines and 125-nm-wide spaces and form sharp peaks on a wafer coated with a layer of hydrogen silsesquioxane resist (HSQ). By precisely controlling the mask-wafer gap at 10 μm using the laser interferogram method, the fine structures are defined on HSQ. Experimental images are reproduced by a simulation using the one-dimensional beam propagation method. This lithographic technique presents a novel and convenient way to fabricate fine silica-like structures and devices in nano-optical and nanoelectronic applications.

  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. X-ray microimaging by diffractive techniques

    SciTech Connect

    Kirz, Janos; Jacobsen, Chris

    2001-07-31

    The report summarizes the development of soft x-ray microscopes at the National Synchrotron Light Source X-1A beamline. We have developed a soft x-ray microscopy beamline (X-1A) at the National Synchrotron Light Source at Brookhaven National Laboratory. This beamline has been upgraded recently to provide two endstations dedicated to microscopy experiments. One endstation hosts a brand new copy of the redesigned room temperature scanning x-ray microscope (STXM), and the other end station hosts a cryo STXM and the original redesigned room temperature microscope, which has been commissioned and has started operation. Cryo STXM and the new microscope use the same new software package, running under the LINUX operating system. The new microscope is showing improved image resolution and extends spectromicroscopy to the nitrogen, oxygen and iron edges. These microscopes are used by us, and by users of the facility, to image hydrated specimens at 50 nm or better spatial resolution and with 0.1-0.5 eV energy resolution. This allows us to carry out chemical state mapping in biological, materials science, and environmental and colloidal science specimens. In the cryo microscope, we are able to do chemical state mapping and tomography of frozen hydrated specimens, and this is of special importance for radiation-sensitive biological specimens. for spectromicroscopic analysis, and methods for obtaining real-space images from the soft x-ray diffraction patterns of non-crystalline specimens. The user program provides opportunities for collaborators and other groups to exploit the techniques available and to develop them further. We have also developed new techniques such as an automated method for acquiring ''stacks'' of images.

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

    PubMed

    Authier, André

    2012-01-01

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

  5. In-line x-ray phase-contrast tomography and diffraction-contrast tomography study of the ferrite-cementite microstructure in steel

    NASA Astrophysics Data System (ADS)

    Kostenko, Alexander; Sharma, Hemant; Dere, E. Gözde; King, Andrew; Ludwig, Wolfgang; Van Oel, Wim; Offerman, S. Erik; Stallinga, Sjoerd; Vliet, Lucas J. van

    2012-05-01

    This work presents the development of a non-destructive imaging technique for the investigation of the microstructure of cementite grains embedded in a ferrite matrix of medium-carbon steel. The measurements were carried out at the material science beamline of the European Synchrotron Radiation Facility (ESRF) ID11. It was shown that in-line X-ray phase-contrast tomography (PCT) can be used for the detection of cementite grains of several microns in size. X-ray PCT of the cementite structure can be achieved by either a `single distance' or a `multiple distance' acquisition protocol. The latter permits quantitative phase retrieval. A second imaging technique, X-ray diffraction-contrast tomography (DCT), was employed to obtain information about the shapes and crystallographic orientations of the distinct ferrite grains surrounding the cementite structures. The initial results demonstrate the feasibility of determining the geometry of the cementite grains after the austenite-ferrite phase-transformation in a non-destructive manner. The results obtained with PCT and DCT are verified with ex-situ optical microscopy studies of the same specimen.

  6. 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.

  7. Liquids identification with x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Harding, G.; Delfs, J.

    2007-09-01

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

  8. 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

  9. Elimination of X-Ray Diffraction through Stimulated X-Ray Transmission.

    PubMed

    Wu, B; Wang, T; Graves, C E; Zhu, D; Schlotter, W F; Turner, J J; Hellwig, O; Chen, Z; Dürr, H A; Scherz, A; Stöhr, J

    2016-07-01

    X-ray diffractive imaging with laterally coherent x-ray free-electron laser (XFEL) pulses is increasingly utilized to obtain ultrafast snapshots of matter. Here we report the amazing disappearance of single-shot charge and magnetic diffraction patterns recorded with resonantly tuned, narrow bandwidth XFEL pulses. Our experimental results reveal the exquisite sensitivity of single-shot charge and magnetic diffraction patterns of a magnetic film to the onset of field-induced stimulated elastic x-ray forward scattering. The loss in diffraction contrast, measured over 3 orders of magnitude in intensity, is in remarkable quantitative agreement with a recent theory that is extended to include diffraction. PMID:27447522

  10. Elimination of X-Ray Diffraction through Stimulated X-Ray Transmission

    NASA Astrophysics Data System (ADS)

    Wu, B.; Wang, T.; Graves, C. E.; Zhu, D.; Schlotter, W. F.; Turner, J. J.; Hellwig, O.; Chen, Z.; Dürr, H. A.; Scherz, A.; Stöhr, J.

    2016-07-01

    X-ray diffractive imaging with laterally coherent x-ray free-electron laser (XFEL) pulses is increasingly utilized to obtain ultrafast snapshots of matter. Here we report the amazing disappearance of single-shot charge and magnetic diffraction patterns recorded with resonantly tuned, narrow bandwidth XFEL pulses. Our experimental results reveal the exquisite sensitivity of single-shot charge and magnetic diffraction patterns of a magnetic film to the onset of field-induced stimulated elastic x-ray forward scattering. The loss in diffraction contrast, measured over 3 orders of magnitude in intensity, is in remarkable quantitative agreement with a recent theory that is extended to include diffraction.

  11. X-ray diffraction microtomography using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Barroso, R. C.; Lopes, R. T.; de Jesus, E. F. O.; Oliveira, L. F.

    2001-09-01

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

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

    SciTech Connect

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

    2007-01-22

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

  13. 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.

  14. X-RAY DIFFRACTION STUDIES ON FROG MUSCLES

    PubMed Central

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

    1944-01-01

    1. X-ray diffraction studies of sartorius muscles of Rana pipiens were made in a new x-ray diffraction camera which permits exposures of 3 to 6 minutes. The object-film distance can be varied from 20 to 80 mm; the muscle inside the camera can be electrically stimulated while contracting isotonically or isometrically, and can be observed by a special device. After exposures up to 30 minutes (approximately 40,830 r) muscles are still alive and responsive. 2. Contrary to the x-ray diffraction pattern of powdered dry muscle, which pattern consists of two rings corresponding to spacings of 4.46 Å.u. and 9.66 Å.u., both moist and dried whole sartorius muscle show signs of orientation in both rings, consisting of two equatorial streaks (wet) or points (dry) and meridional sickles. The moist muscle shows in addition a diffuse water ring. The spacings corresponding to the orientation points and elliptical structure show only slight differences in moist and dried samples. Through statistical computations based on two different series consisting of thirteen moist and twenty-eight dried samples, and nine muscles before and after drying, it was shown that only the divergence in the smaller spacing has some real significance, which indicates that most water of the moist muscle is bound intermolecularly. Upon resoaking of dried muscle the x-ray diffraction pattern of the moist muscle is restored. 3. Stretching of muscle by weights below the breaking point produces an additional well defined diffraction line, corresponding to a spacing of 4.32 Å.u. A similar diffraction line can be produced in frog tendon upon stretching. 4. The influence of heat on the x-ray diffraction pattern of muscle depends upon the maximum temperature and the length of action; 5 minutes at 50° C. markedly reduces the orientation of the sample; 5 minutes' immersion in boiling Ringer's solution destroys the orientation and produces a ring corresponding to a spacing of 5.3 to 5.5 Å.u. in the moist and

  15. Diffractive imaging of highly focused X-ray fields

    NASA Astrophysics Data System (ADS)

    Quiney, H. M.; Peele, A. G.; Cai, Z.; Paterson, D.; Nugent, K. A.

    2006-02-01

    The rapid development of new sources of coherent X-rays, such as third-generation synchrotrons, high-harmonic-generation lasers and X-ray free-electron lasers, has led to the emergence of the new field of X-ray coherent science. The extension of coherent methods to the X-ray regime makes possible methods such as coherent diffraction, X-ray photon-correlation spectroscopy, speckle interferometry and ultrafast probing at atomic resolution and femtosecond timescales. Despite rapid improvements in the resolution that conventional X-ray optics can achieve, new methods for manipulating X-rays are required to push this to the atomic scale. Here we demonstrate a coherent imaging technique that enables us to image the complex field at the focus of an X-ray zone plate without the need for conventional X-ray lenses. There are no fundamental limits on the resolution of this lensless imaging technique other than the wavelength of the X-rays themselves. The ability to characterize the beam with one measurement makes the method ideally suited to characterizing the fields generated by pulsed coherent X-ray sources.

  16. High-Energy X-Ray Diffraction Analysis Tool

    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

  17. High-Energy X-Ray Diffraction Analysis Tool

    SciTech Connect

    2011-11-29

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

  18. X-ray powder diffraction study of polytetrafluoroethylene

    SciTech Connect

    Lebedev, Yu. A. Korolev, Yu. M.; Polikarpov, V. M.; Ignat'eva, L. N.; Antipov, E. M.

    2010-07-15

    Samples of polytetrafluoroethylene were studied by X-ray diffraction. A quantitative X-ray powder diffraction analysis of three components of the polymer was performed for the first time. All samples of polytetrafluoroethylene were found to be three-phase and consist of one crystalline and two amorphous phases. One of the amorphous phases is composed of low-molecular-weight products. The structure of the latter phase was established for the first time by X-ray diffraction methods and computer simulation.

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

    SciTech Connect

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

    2010-02-15

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

  20. 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.

  1. Detection of nonthermal melting by ultrafast X-ray diffraction.

    PubMed

    Siders, C W; Cavalleri, A; Sokolowski-Tinten, K; Tóth, C; Guo, T; Kammler, M; Horn von Hoegen, M; Wilson, K R; von der Linde, D; Barty, C P

    1999-11-12

    Using ultrafast, time-resolved, 1.54 angstrom x-ray diffraction, thermal and ultrafast nonthermal melting of germanium, involving passage through nonequilibrium extreme states of matter, was observed. Such ultrafast, optical-pump, x-ray diffraction probe measurements provide a way to study many other transient processes in physics, chemistry, and biology, including direct observation of the atomic motion by which many solid-state processes and chemical and biochemical reactions take place.

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

    SciTech Connect

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

    2004-05-12

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

  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. X-ray diffraction microscopy of magnetic structures.

    PubMed

    Turner, Joshua J; Huang, Xiaojing; Krupin, Oleg; Seu, Keoki A; Parks, Daniel; Kevan, Stephen; Lima, Enju; Kisslinger, Kim; McNulty, Ian; Gambino, Richard; Mangin, Stephane; Roy, Sujoy; Fischer, Peter

    2011-07-15

    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 L3 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.

  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. X-ray characterization by energy-resolved powder diffraction

    NASA Astrophysics Data System (ADS)

    Cheung, G.; Hooker, S. M.

    2016-08-01

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

  7. Cryogenic X-ray Diffraction Microscopy for Biological Samples

    SciTech Connect

    E Lima; L Wiegart; P Pernot; M Howells; J Timmins; F Zontone; A Madsen

    2011-12-31

    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.

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

    SciTech Connect

    Shen, Q.

    1996-09-01

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

  9. 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.

  10. Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment.

    PubMed

    Cha, Wonsuk; Liu, Wenjun; Harder, Ross; Xu, Ruqing; Fuoss, Paul H; Hruszkewycz, Stephan O

    2016-09-01

    A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load. PMID:27577782

  11. Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment.

    PubMed

    Cha, Wonsuk; Liu, Wenjun; Harder, Ross; Xu, Ruqing; Fuoss, Paul H; Hruszkewycz, Stephan O

    2016-09-01

    A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

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

    SciTech Connect

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

    2014-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Heimann, P. A.; Larsson, J.; Chang, Z.; Lindenberg, A.; Schuck, P. J.; Judd, E.; Padmore, H. A.; Bucksbaum, P. H.; Lee, R. W.; Murnane, M.; Kapteyn, H.; Wark, J. S.; Falcone, R. W.

    1997-07-01

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

  18. X-ray fiber diffraction studies on flagellar axonemes.

    PubMed

    Oiwa, Kazuhiro; Kamimura, Shinji; Iwamoto, Hiroyuki

    2009-01-01

    Eukaryotic cilia and flagella are highly ordered and precisely assembled cellular organelles. Here, to understand the mechanism of the orderly undulations of cilia and flagella, we shall draw a blueprint of their core structures and supporting scaffolds, that is, axonemes, and we shall describe the dynamic structural changes of components of the organelles. Small-angle X-ray scattering and diffraction are among the principal tools used to study protein polymers. These methods are now well established as indispensable tools that complement electron microscopy, providing information on the structure and dynamics of biological materials at atomic resolution in near-physiological environments. For instance, X-ray diffraction studies of skeletal muscles have contributed greatly to our understanding of the structure and molecular mechanisms of muscles. However, owing to the minute size and low diffracting power of axonemes, few attempts at X-ray diffraction of axonemes have been reported. The advent of third-generation synchrotron radiation facilities now makes these attempts feasible, because we now have stable and intense X-rays that enable us to obtain diffractions from the axonemes. In this chapter, we provide a concise practical guide to this new avenue for structural analysis of axonemes. PMID:20409782

  19. 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.

  20. Biological imaging by soft x-ray diffraction microscopy

    DOE PAGES

    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

  1. 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.

  2. 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)

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

  4. 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.

  5. 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)

  6. Single photon energy dispersive x-ray diffraction.

    PubMed

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

    2014-03-01

    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.

  7. Dynamical Effects in Resonant X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Macke, S.; Hamann-Borrero, J. E.; Green, R. J.; Keimer, B.; Sawatzky, G. A.; Haverkort, M. W.

    2016-09-01

    Using resonant magnetic diffraction at the Ni L2 ,3 edge in a LaNiO3 superlattice, we show that dynamical effects beyond the standard kinematic approximation can drastically modify the resonant scattering cross section. In particular, the combination of extinction and refraction convert maxima to minima in the azimuthal-angle dependence of the diffracted intensity, which is commonly used to determine orbital and magnetic structures by resonant x-ray diffraction. We provide a comprehensive theoretical description of these effects by numerically solving Maxwell's equations in three dimensions. The understanding and description of dynamical diffraction enhances the capabilities of resonant x-ray scattering as a probe of electronic ordering phenomena in solids.

  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. Dynamical Effects in Resonant X-Ray Diffraction.

    PubMed

    Macke, S; Hamann-Borrero, J E; Green, R J; Keimer, B; Sawatzky, G A; Haverkort, M W

    2016-09-01

    Using resonant magnetic diffraction at the Ni L_{2,3} edge in a LaNiO_{3} superlattice, we show that dynamical effects beyond the standard kinematic approximation can drastically modify the resonant scattering cross section. In particular, the combination of extinction and refraction convert maxima to minima in the azimuthal-angle dependence of the diffracted intensity, which is commonly used to determine orbital and magnetic structures by resonant x-ray diffraction. We provide a comprehensive theoretical description of these effects by numerically solving Maxwell's equations in three dimensions. The understanding and description of dynamical diffraction enhances the capabilities of resonant x-ray scattering as a probe of electronic ordering phenomena in solids. PMID:27661698

  10. 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.

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

    DOE PAGES

    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. Raman spectroscopy and X-ray diffraction studies on celestite

    NASA Astrophysics Data System (ADS)

    Chen, Yen-Hua; Yu, Shu-Cheng; Huang, Eugene; Lee, Pei-Lun

    2010-10-01

    High-pressure Raman spectroscopy and X-ray diffraction studies of celestite (SrSO 4) were carried out in a diamond anvil cell at room temperature. Variation in the Raman vibrational frequency and change of lattice parameters with pressure indicate that a transformation occurs in celestite. This transformation caused an adjustment in the Sr-O polyhedra that affected the stretching-force constant of SO 4. Moreover, compressibilities along the crystallographic axes decreased in the order a to c to b. From the compression data, the bulk modulus of the celestite was 87 GPa. Both X-ray and Raman data show that the transition in celestite is reversible.

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

    NASA Astrophysics Data System (ADS)

    Antunes, A.; Hönnicke, M. G.; Safatle, A. M. V.; Cusatis, C.; Moraes Barros, P. S.; Morelhão, S. L.

    2005-08-01

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

  14. 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.

  15. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction.

    PubMed

    Maddox, B R; Akin, M C; Teruya, A; Hunt, D; Hahn, D; Cradick, J; Morgan, D V

    2016-08-01

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10(7) molybdenum Kα photons.

  16. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction.

    PubMed

    Maddox, B R; Akin, M C; Teruya, A; Hunt, D; Hahn, D; Cradick, J; Morgan, D V

    2016-08-01

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10(7) molybdenum Kα photons. PMID:27587130

  17. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

    NASA Astrophysics Data System (ADS)

    Maddox, B. R.; Akin, M. C.; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J.; Morgan, D. V.

    2016-08-01

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 107 molybdenum Kα photons.

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

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

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

  19. Powder X-ray Diffraction Using the Omega Laser

    NASA Astrophysics Data System (ADS)

    Eggert, Jon; Rygg, Ryan; Smith, Raymond; Bastea, Marina; Ping, Yuan; Shepherd, Ronnie; Collins, Gilbert

    2009-06-01

    The past several years have seen dramatic improvements in dynamic ramp-compression experiments to measure stress-density using laser and pulsed-power drivers. Goals for future experiments center on achieving pressures over 1 TPa (10 Mbar), while keeping the samples in a solid phase and applying additional diagnostics to probe the nature of these states. X-ray scattering is a natural probe for such studies due to the copious x-ray energy produced by laser sources. Such experiments allow studies of the crystal structure, texture, strength, and possibly temperature of ramp-compressed solids at unprecedented density. With this in mind we have developed a powder x-ray diffraction diagnostic fielded at the Omega laser. We will report our results on ramp-driven iron, tin and copper. This work performed under the auspices of the U.S. DOE by LLNL under Contract DE-AC52-07NA27344.

  20. 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.

  1. 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.

  2. Wavefront aberrations of x-ray dynamical diffraction beams.

    PubMed

    Liao, Keliang; Hong, Youli; Sheng, Weifan

    2014-10-01

    The effects of dynamical diffraction in x-ray diffractive optics with large numerical aperture render the wavefront aberrations difficult to describe using the aberration polynomials, yet knowledge of them plays an important role in a vast variety of scientific problems ranging from optical testing to adaptive optics. Although the diffraction theory of optical aberrations was established decades ago, its application in the area of x-ray dynamical diffraction theory (DDT) is still lacking. Here, we conduct a theoretical study on the aberration properties of x-ray dynamical diffraction beams. By treating the modulus of the complex envelope as the amplitude weight function in the orthogonalization procedure, we generalize the nonrecursive matrix method for the determination of orthonormal aberration polynomials, wherein Zernike DDT and Legendre DDT polynomials are proposed. As an example, we investigate the aberration evolution inside a tilted multilayer Laue lens. The corresponding Legendre DDT polynomials are obtained numerically, which represent balanced aberrations yielding minimum variance of the classical aberrations of an anamorphic optical system. The balancing of classical aberrations and their standard deviations are discussed. We also present the Strehl ratio of the primary and secondary balanced aberrations.

  3. 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.

  4. 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

  5. X-Ray Line Measurements with High Efficiency Bragg Crystals

    SciTech Connect

    Pak, A; Gregori, G; Knight, J; Campbell, K; Landen, O; Glenzer, S

    2004-04-01

    We have studied the focusing properties of two highly oriented pyrolitic graphite (HOPG) spectrometers, which differ in the degree of the mosaic spread: ZYA with a low mosaic spread ({gamma}=0.4 degrees) and ZYH with a large mosaic spread ({gamma}=3.5 degrees). In order to assess the crystal performance for a variety of different experiments, various K{alpha} and K{beta} x-ray lines have been produced using a high-intensity ({approx}>10{sup 17} W/cm{sup 2}) short-pulse ({approx} 100 fs) laser beam focused onto Ti, V, Zn, and Cu foils. The measured spectral resolution of the HOPG crystals in both first and second order diffraction has been compared with theoretical predictions. Using known values for the peak reflectivity of HOPG crystals, we have also computed K{alpha} x-ray conversion efficiencies of Ti, V, Zn, and Cu. These results are important to estimate the optimal conditions under which different types of HOPG monochromators can be used for the detection of weak x-ray signals as the one encountered in x-ray Thomson/Compton scattering experiments.

  6. X-ray line measurements with high efficiency Bragg crystals

    SciTech Connect

    Pak, A.; Gregori, G.; Knight, J.; Campbell, K.; Price, D.; Hammel, B.; Landen, O.L.; Glenzer, S.H.

    2004-10-01

    We have studied the focusing properties of two highly oriented pyrolitic graphite (HOPG) spectrometers, which differ in the degree of the mosaic spread: ZYA with a low mosaic spread ({gamma}=0.4 deg.) and ZYH with a large mosaic spread ({gamma}=3.5 deg.). In order to asses the crystal performance for a variety of different experiments, various K{alpha} and K{beta} x-ray lines have been produced using a high-intensity (> or approx. 10{sup 17} W/cm{sup 2}) short-pulse ({approx}100 fs) laser beam focused onto Ti, V, Zn, and Cu foils. The measured spectral resolution of the HOPG crystals in both first and second order diffraction has been compared with theoretical predictions. Using known values for the peak reflectivity of HOPG crystals, we have also computed K{alpha} x-ray conversion efficiencies of Ti, V, Zn, and Cu. These results are important to estimate the optimal conditions under which different types of HOPG monochromators can be used for the detection of weak x-ray signals as the one encountered in x-ray Thomson/Compton scattering experiments.

  7. 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.

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

  9. Impulsive solvent heating probed by picosecond x-ray diffraction.

    PubMed

    Cammarata, M; Lorenc, M; Kim, T K; Lee, J H; Kong, Q Y; Pontecorvo, E; Lo Russo, M; Schiró, G; Cupane, A; Wulff, M; Ihee, H

    2006-03-28

    The time-resolved diffraction signal from a laser-excited solution has three principal components: the solute-only term, the solute-solvent cross term, and the solvent-only term. The last term is very sensitive to the thermodynamic state of the bulk solvent, which may change during a chemical reaction due to energy transfer from light-absorbing solute molecules to the surrounding solvent molecules and the following relaxation to equilibrium with the environment around the scattering volume. The volume expansion coefficient alpha for a liquid is typically approximately 1 x 10(-3) K(-1), which is about 1000 times greater than for a solid. Hence solvent scattering is a very sensitive on-line thermometer. The decomposition of the scattered x-ray signal has so far been aided by molecular dynamics (MD) simulations, a method capable of simulating the solvent response as well as the solute term and solute/solvent cross terms for the data analysis. Here we present an experimental procedure, applicable to most hydrogen containing solvents, that directly measures the solvent response to a transient temperature rise. The overtone modes of OH stretching and CH3 asymmetric stretching in liquid methanol were excited by near-infrared femtosecond laser pulses at 1.5 and 1.7 microm and the ensuing hydrodynamics, induced by the transfer of heat from a subset of excited CH3OH* to the bulk and the subsequent thermal expansion, were probed by 100 ps x-ray pulses from a synchrotron. The time-resolved data allowed us to extract two key differentials: the change in the solvent diffraction from a temperature change at constant density, seen at a very short time delay approximately 100 ps, and a term from a change in density at constant temperature. The latter term becomes relevant at later times approximately 1 mus when the bulk of liquid expands to accommodate its new temperature at ambient pressure. These two terms are the principal building blocks in the hydrodynamic equation of state

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

    PubMed

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

    2016-03-14

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

  11. 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.

  12. Melting curve of metals evidenced by X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Dewaele, Agnes

    2013-06-01

    There has been a consistent pattern of disagreement between the determinations of high pressure melting by two experimental techniques, the static laser-heated diamond anvil cell (LHDAC) and the dynamic shock wave compression. For several elements, ``high'' and ``low'' melting points have been measured by shock compression and LHDAC, respectively. The difference could exceed one thousand of K. We have re-visited the melting curve of a few metals in a LHDAC: lead, tantalum, beryllium and iron. We have used an alternative diagnostic of melting, based on X-ray diffraction instead of optical detection. The melting curves obtained with this diagnostic are in correct agreement with shock wave data. Movements of the sample surface, which were previously interpreted as a melting signature, could be due to a fast recrystallization of the solid sample. This fast recrystallization is evidenced by X-ray diffraction up to several hundreds of degrees below melting for some metals.

  13. Simulations of a Johann/Johansson diffraction spectrometer for x-ray experiments at an electron beam ion source

    NASA Astrophysics Data System (ADS)

    Jabłoński, Ł.; Jagodziński, P.; Banaś, D.; Pajek, M.

    2013-09-01

    The ray tracing simulations of x-ray spectra for a compact six-crystal Johann/Johansson diffraction spectrometer covering a wide photon energy range (70 eV-15 keV), i.e. from the extended ultraviolet to the hard x-ray region, are discussed in the context of x-ray experiments at an electron beam ion source facility. In particular, the x-ray line profiles and energy resolution for different diffraction crystals and multilayers were studied, and the effects of extension of x-ray source size and misalignment were investigated. The simulations were also performed for x-ray emission from solid targets bombarded by electrons, which will be used for calibration of the x-ray spectrometer.

  14. Coherent X-ray diffraction from collagenous soft tissues

    PubMed Central

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

    2009-01-01

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

  15. 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

  16. 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.

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

    NASA Astrophysics Data System (ADS)

    Mendoza Cuevas, Ariadna; Perez Gravie, Homero

    2011-03-01

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

  18. 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.

  19. 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, Sébastien; 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 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses. PMID:26798819

  20. 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.

  1. Synchrotron energy-dispersive X-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Hall, C.; Barnes, P.; Cockcroft, J. K.; Colston, S. L.; Häusermann, D.; Jacques, S. D. M.; Jupe, A. C.; Kunz, M.

    1998-04-01

    Energy-dispersive diffraction tomography using white-beam synchrotron X-rays with energies up to 140 keV yields images of the interior features of solid objects up to 50 mm thick. The volume sampled is determined by the geometry of the diffracting lozenge defined by the incident beam, the detector system collimation and the Bragg angle. Using conventional beam slits to form a highly collimated 50 μm × 50 μm incident beam and a 40 μm collimator aperture, we demonstrate on a PEEK phantom that a lateral resolution (transverse to the beam direction) of a few microns can be achieved. The resolution in the direction of the incident beam is necessarily poorer than this since the diffracting lozenge is elongated in this direction, with length increasing rapidly at small angles. There is no evidence of significant contamination of the diffracted intensity by the effects of multiple scattering from outside the primary lozenge.

  2. 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.

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

    PubMed

    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 × 10(5) cm(-2).

  4. 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

  5. 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

  6. 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.

  7. High pressure x-ray diffraction techniques with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Jing, Liu

    2016-07-01

    This article summarizes the developments of experimental techniques for high pressure x-ray diffraction (XRD) in diamond anvil cells (DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, time-resolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF (Beijing Synchrotron Radiation Facility) and some results are also presented. Project supported by the National Natural Science Foundation of China (Grant Nos. 10875142, 11079040, and 11075175). The 4W2 beamline of BSRF was supported by the Chinese Academy of Sciences (Grant Nos. KJCX2-SW-N20, KJCX2-SW-N03, and SYGNS04).

  8. X-ray diffraction properties of highly oriented pyrolytic graphite

    SciTech Connect

    Freund, A.K.; Munkholm, A.; Brennan, S.

    1996-12-31

    The x-ray diffraction properties of highly oriented pyrolytic graphite (HOPG) were studied for x-ray energies ranging from 4 to 60 keV. In particular, the secondary extinction thickness was determined by recording the peak and integrated reflectivity as a function of depth below the surface. The results showed that for the high quality material investigated a thickness of 200 to 300 {micro}m was sufficient to get 80% of the maximum reflectivity that is obtained for a very thick plate. Primary extinction was important for low energy and still persisted at higher energies. Inhomogeneities of the mosaic structure were observed, too, that make this material not a truly ideal mosaic monochromator crystal. However, quite high peak reflectivities between 35% and 58% were measured at FWHM of 0.25 to 0.45 degrees. A 200 {micro}m thick plate was then prepared and glued on a bending device to manufacture a monochromator or analyzer with variable curvature that works from flat down to a minimum bending radius of 10 cm. The successful tests of this device confirmed that HOPG plates much thinner than those commonly used as x-ray monochromators and analyzers still have high efficiency and can be curved to achieve dynamical focusing.

  9. Model-based reconstruction for x-ray diffraction imaging

    NASA Astrophysics Data System (ADS)

    Sridhar, Venkatesh; Kisner, Sherman J.; Skatter, Sondre; Bouman, Charles A.

    2016-05-01

    In this paper, we propose a novel 4D model-based iterative reconstruction (MBIR) algorithm for low-angle scatter X-ray Diffraction (XRD) that can substantially increase the SNR. Our forward model is based on a Poisson photon counting model that incorporates a spatial point-spread function, detector energy response and energy-dependent attenuation correction. Our prior model uses a Markov random field (MRF) together with a reduced spectral bases set determined using non-negative matrix factorization. We demonstrate the effectiveness of our method with real data sets.

  10. 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.

  11. 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.

  12. 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.

  13. Coherent x-ray diffraction imaging of silicon oxide growth

    NASA Astrophysics Data System (ADS)

    Robinson, I. K.; Libbert, J. L.; Vartanyants, I. A.; Pitney, J. A.; Smilgies, D. M.; Abernathy, D. L.; Grübel, G.

    1999-10-01

    We have measured the morphology of Si samples as a function of time in air after stripping of the native oxide. For this purpose we examined the reflectivity of a coherent beam of x rays, which produces a structured diffraction pattern. We have made further progress in the development of an inversion algorithm for conversion of these patterns into one-dimensional height images. Nanometer-sized features are found to grow and evolve in waves across the surface on the time scale of minutes to hours.

  14. 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.

  15. 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

  16. 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.

  17. Ex situ metrology of x-ray diffraction gratings

    NASA Astrophysics Data System (ADS)

    Yashchuk, Valeriy V.; McKinney, Wayne R.; Artemiev, Nikolay A.

    2013-05-01

    The idea of measurements of groove density distributions of diffraction gratings suggested and first realized in Proceedings of SPIE 5858, (2005) 58580A consists of determination of the spatial frequency of the first harmonic peak appearing in the power spectral density (PSD) distribution of the grating surface profile observed with a microscope. Using a MicroMap™-570 interferometric microscope, it was experimentally proven that this technique is capable of high precision measurements with x-ray gratings with groove densities of about 250 grooves/mm, varying along the grating by ±5%. In the present work, we provide analytical and experimental background for useful application of PSD characterization of groove densities of diffraction gratings. In particular, we analyze the shape of harmonic peaks and derive an analytical fitting function suitable for fitting the PSD peaks obtained with gratings with a variety of groove shapes. We demonstrate the capabilities of the method by application to the groove density distribution measurements with a 300-groove/mm grating suitable for soft x-ray applications.

  18. 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.

  19. 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.

  20. Characterization of X-Ray Diffraction System with a Microfocus X-Ray Source and a Polycapillary Optic

    NASA Technical Reports Server (NTRS)

    Gubarev, Mikhail; Marshall, Joy K.; Ciszak, Ewa; Ponomarev, Igor

    2000-01-01

    We present here an optimized microfocus x-ray source and polycapillary optic system designed for diffraction of small protein crystals. The x-ray beam is formed by a 5.5mm focal length capillary collimator coupled with a 40 micron x-ray source operating at 46Watts. Measurements of the x-ray flux, the divergence and the spectral characteristics of the beam are presented, This optimized system provides a seven fold greater flux than our recently reported configuration [M. Gubarev, et al., J. of Applied Crystallography (2000) 33, in press]. We now make a comparison with a 5kWatts rotating anode generator (Rigaku) coupled with confocal multilayer focusing mirrors (Osmic, CMF12- 38Cu6). The microfocus x-ray source and polycapillary collimator system delivers 60% of the x-ray flux from the rotating anode system. Additional ways to improve our microfocus x-ray system, and thus increase the x-ray flux will be discussed.

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

    SciTech Connect

    Noda, Daiji; Tokuoka, Atsushi; Katori, Megumi; Minamiyama, Yasuto; Yamashita, Kenji; Nishida, Satoshi; Hattori, Tadashi

    2012-07-31

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

  2. Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline.

    PubMed

    Jones, Michael W M; Phillips, Nicholas W; van Riessen, Grant A; Abbey, Brian; Vine, David J; Nashed, Youssef S G; Mudie, Stephen T; Afshar, Nader; Kirkham, Robin; Chen, Bo; Balaur, Eugeniu; de Jonge, Martin D

    2016-09-01

    Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated. PMID:27577770

  3. 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.

  4. 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

  5. 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.

  6. 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

  7. 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

  8. 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.

  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. Parts per Million Powder X-ray Diffraction.

    PubMed

    Newman, Justin A; Schmitt, Paul D; Toth, Scott J; Deng, Fengyuan; Zhang, Shijie; Simpson, Garth J

    2015-11-01

    Here we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect low crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.

  11. 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.

  12. 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.

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

    NASA Technical Reports Server (NTRS)

    Schmidt, Gary D.

    2005-01-01

    This award represents the second phase of an X-ray study of QSOs that are heavily obscured in the optical/near-IR. An earlier survey revealed that these active galactic nuclei (AGN) are also typically strongly absorbed at high photon energies, but the enhanced sensitivity of XMM-Newton provided for the first time the opportunity to measure the spectral indices of individual sources and to test the possibility that obscured AGN are responsible for a substantial portion of the cosmic X-ray background (CXRB). The new observations confirm and greatly extend the earlier results. Substantial intervening absorbing material is detected for 3 of the sources, and 2 additional targets show hard power-law continua. In addition, soft X-ray excesses are detected in 3 of sources, indicating the presence of extended regions of ionized gas. This component is-particularly well-defined in the Type 1 source 2MASS2344+1221, allowing analysis and modeling at a level of detail unusual for such distant sources. An important finding that parallels conclusions from optical polarimetry is the lack of dependence of absorption on optical spectral class (Type 1 or 2). The combination of strong polarization and X-ray absorption in sources that show strong, broad emission lines indicates either a very small (nuclear) absorber or a favored viewing angle which allows the X-ray source to be covered but the surrounding broad emission-line region to be largely exposed. The observed spectral also indicate that obscured AGN of both Type 1 and 2 contribute significantly to the CXRB at higher X-ray energies.

  15. 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.

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

    NASA Astrophysics Data System (ADS)

    Hambach, D.; Peuker, M.; Schneider, G.

    2001-07-01

    The new transmission X-ray microscope (TXM) installed at the BESSY II electron storage ring uses an off-axis transmission zone plate (OTZ) as diffractive and focusing element of the condenser-monochromator setup. A high resolution micro-zone plate (MZP) forms a magnified image on a CCD-detector. Both, the OTZ with an active area of up to 24 mm2 and the MZP with zone widths as small as 25 nm are generated by a process including electron beam lithography (EBL), dry etching and subsequent electroplating of nickel on top of silicon membrane substrates with about 100- 150 nm thickness. The combination of a larger zone width and the usage of nickel zone structures allows to increase the diffraction efficiency of the condenser element at least by a factor of 3 compared to the earlier used KZP7 condenser zone plate in the TXM at BESSY I. Groove diffraction efficiencies of 21.6% and 14.7% were measured for MZP objectives with 40 and 25 nm outermost zone width, respectively.

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

    SciTech Connect

    Shirokoff, J.; Lewis, J. Courtenay

    2010-10-29

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

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

    SciTech Connect

    Ichiyanagi, Kouhei; Sasaki, Yuji C.; 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

    2013-10-15

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

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

    PubMed

    Ichiyanagi, Kouhei; Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Hoshisashi, Kentaro; Chang, Jae-won; 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 (ΔE/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.

  20. 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

  1. Elimination of higher-order diffraction using zigzag transmission grating in soft x-ray region

    SciTech Connect

    Zang, H. P.; Wang, C. K.; Gao, Y. L.; Zhou, W. M.; Kuang, L. Y.; Wei, L.; Fan, W.; Zhang, W. H.; Zhao, Z. Q.; Cao, L. F.; Gu, Y. Q.; Zhang, B. H.; Jiang, G.; Zhu, X. L.; Xie, C. Q.; Zhao, Y. D.; Cui, M. Q.

    2012-03-12

    We present a realization of the sinusoidal transmission function using a series of zigzag-profiled strips where the transmission takes on the binary values 0 and 1 in a two-dimensional distribution. A zigzag transmission grating of 1000 line/mm has been fabricated and demonstrated on the soft x-ray beam of synchrotron radiation. The axial single-order diffraction indicates that the zigzag transmission grating is adequate for spectroscopic application.

  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. X-ray Diffraction Study of Molybdenum to 900 GPa

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

    Molybdenum (Mo) is a transition metal that is important as a high-pressure standard. Its equation of state, structure, and melting behavior have been explored extensively in both experimental and theoretical studies. Melting data up to the Mbar pressure region from static compression experiments in the diamond anvil cell [Errandonea et al. 2004] are inconsistent with shock wave sound velocity measurements [Hixson et al., 1989]. There are also conflicting reports as to whether body-centered cubic (BCC) Mo transforms to a face-centered cubic (FCC), hexagonal close packed (HCP) or double hexagonal close packed (DHCP) structure at either high pressure or high pressure and temperature conditions [Belonoshko et al. 2008, Mikhaylushkin et al., 2008 and Cazorla et al., 2008]. Recently, a phase transition from BCC to the DHCP phase at 660 GPa and 0 K was predicted using the particle swam optimization (PSO) method (Wang et al, 2013). Here we report an x-ray diffraction study of dynamically compressed molybdenum. Experiments were conducted using the Omega laser at the Laboratory for Laser Energetics at the University of Rochester. Mo targets were either ramp or shock compressed using a laser drive. In ramp loading, the sample is compressed sufficiently slowly that a shock wave does not form. This results in lower temperatures, keeping the sample in the solid state to higher pressures. X-ray diffraction measurements were performed using quasi-monochromatic x-rays from a highly ionized He-α Cu source and image plate detectors. Upon ramp compression, we found no evidence of phase transition in solid Mo up to 900 GPa. The observed peaks can be assigned to the (110) and (200) or (220) reflections of BCC Mo up to the highest pressure, indicating that Mo does not melt under ramp loading to maximum pressure reached. Under shock loading, we did not observe any evidence for the solid-solid phase transformation around 210 GPa as reported in previous work (Hixson et al, 1989). The BCC

  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. 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

  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.; 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.

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

    SciTech Connect

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

    2014-11-15

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

  9. Mapping a Mantle Xenolith Using Micro X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Harwood, B. P.; Flemming, R. L.; Stachel, T.

    2009-05-01

    With the advent of Micro X-ray diffraction (μXRD), mineral mapping is now possible at the thin section scale, using crystal structural rather than chemical properties. To test the effectiveness of this technique, a Brüker D8 Discover μXRD was used to create mineral maps from two garnet lherzolite xenoliths from the Bultfontein kimberlite recovered on the Boshof road dumps (Kimberley, South Africa). This technique generated a 2D representation of the major mineralogy (olivine + garnet + clinopyroxene + orthopyroxene + phlogopite); it also enabled estimation of the modal proportions of each mineral. For one polished section, two sets of μXRD data were collected along grids having spacing of 0.5 mm (1148 points) and 1.5 mm (516 points), respectively. The 0.5 mm spacing coincided with the X-ray beam diameter, leaving no gaps in coverage. Data were also collected using a grid of 1.5 mm spacing to examine the effectiveness of a low- resolution map, which would be advantageous to decrease the time required for data collection and processing. To test the potential for automation of the method, data were collected for a second polished thin section, using the high resolution grid (0.5 mm spacing, 3312 data points). General Area Diffraction Detection System (GADDS) images were collected and processed at each step. Debye rings were integrated along small "slices" of 2θ to yield the total number of counts in that area. The 2θ ranges used to identify each phase were chosen such that they coincided with regions where there was no overlap with peaks from any of the other four major phases. To compensate for variable orientation of the grains in the thin sections, several d-spacings (2θ ranges) were integrated for each mineral, and then added together to create five "overall" mineral maps. To create final maps, minerals were determined to be 'present' in cells where the number of counts was above a threshold level in the "overall" map for that mineral. The maps provided

  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. 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.

  12. Federated repositories of X-ray diffraction images.

    PubMed

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

    2008-07-01

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

  13. Spectral feature variations in x-ray diffraction imaging systems

    NASA Astrophysics Data System (ADS)

    Wolter, Scott D.; Greenberg, Joel A.

    2016-05-01

    Materials with different atomic or molecular structures give rise to unique scatter spectra when measured by X-ray diffraction. The details of these spectra, though, can vary based on both intrinsic (e.g., degree of crystallinity or doping) and extrinsic (e.g., pressure or temperature) conditions. While this sensitivity is useful for detailed characterizations of the material properties, these dependences make it difficult to perform more general classification tasks, such as explosives threat detection in aviation security. A number of challenges, therefore, currently exist for reliable substance detection including the similarity in spectral features among some categories of materials combined with spectral feature variations from materials processing and environmental factors. These factors complicate the creation of a material dictionary and the implementation of conventional classification and detection algorithms. Herein, we report on two prominent factors that lead to variations in spectral features: crystalline texture and temperature variations. Spectral feature comparisons between materials categories will be described for solid metallic sheet, aqueous liquids, polymer sheet, and metallic, organic, and inorganic powder specimens. While liquids are largely immune to texture effects, they are susceptible to temperature changes that can modify their density or produce phase changes. We will describe in situ temperature-dependent measurement of aqueous-based commercial goods in the temperature range of -20°C to 35°C.

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

    DOE PAGES

    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.

  15. Atomic calculations for the Fe XX X-ray lines

    NASA Technical Reports Server (NTRS)

    Mason, H. E.; Bhatia, A. K.

    1983-01-01

    The atomic data presented here and in Bhatia and Mason (1980) allow the calculation of theoretical intensity ratios for all the EUV, UV, and X-ray lines from Fe XX. Tabulations are presently given for the transitions between levels in the 2s2 2p3, 2s2 2p2 3s, and 2s2 2p2 3d configurations of Fe(19+), and electron collision strengths are calculated by means of the 'distorted wave' approximation. In addition to the theoretical X-ray line intensity ratios, new spectral line identifications from a solar flare are presented.

  16. 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.

  17. X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

    NASA Astrophysics Data System (ADS)

    Mahato, Dip Narayan

    This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles

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

    ERIC Educational Resources Information Center

    Blanchard, Frank N.

    1980-01-01

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

  19. 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…

  20. 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

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

    SciTech Connect

    Cao, L. F.; Foerster, E.; Fuhrmann, A.; Wang, C. K.; Kuang, L. Y.; Liu, S. Y.; Ding, Y. K.

    2007-01-29

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

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

    SciTech Connect

    Thoe, R.S.

    1986-06-01

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

  3. Direct modeling of x-ray diffraction pattern from skeletal muscle in rigor.

    PubMed Central

    Koubassova, Natalia A; Tsaturyan, A K

    2002-01-01

    Available high-resolution structures of F-actin, myosin subfragment 1 (S1), and their complex, actin-S1, were used to calculate a 2D x-ray diffraction pattern from skeletal muscle in rigor. Actin sites occupied by myosin heads were chosen using a "principle of minimal elastic distortion energy" so that the 3D actin labeling pattern in the A-band of a sarcomere was determined by a single parameter. Computer calculations demonstrate that the total off-meridional intensity of a layer line does not depend on disorder of the filament lattice. The intensity of the first actin layer A1 line is independent of tilting of the "lever arm" region of the myosin heads. Myosin-based modulation of actin labeling pattern leads not only to the appearance of the myosin and "beating" actin-myosin layer lines in rigor diffraction patterns, but also to changes in the intensities of some actin layer lines compared to random labeling. Results of the modeling were compared to experimental data obtained from small bundles of rabbit muscle fibers. A good fit of the data was obtained without recourse to global parameter search. The approach developed here provides a background for quantitative interpretation of the x-ray diffraction data from contracting muscle and understanding structural changes underlying muscle contraction. PMID:12124288

  4. Combined measurement of X-ray photon correlation spectroscopy and diffracted X-ray tracking using pink beam X-rays.

    PubMed

    Shinohara, Yuya; Watanabe, Akira; Kishimoto, Hiroyuki; Amemiya, Yoshiyuki

    2013-09-01

    Combined X-ray photon correlation spectroscopy (XPCS) and diffracted X-ray tracking (DXT) measurements of carbon-black nanocrystals embedded in styrene-butadiene rubber were performed. From the intensity fluctuation of speckle patterns in a small-angle scattering region (XPCS), dynamical information relating to the translational motion can be obtained, and the rotational motion is observed through the changes in the positions of DXT diffraction spots. Graphitized carbon-black nanocrystals in unvulcanized styrene-butadiene rubber showed an apparent discrepancy between their translational and rotational motions; this result seems to support a stress-relaxation model for the origin of super-diffusive particle motion that is widely observed in nanocolloidal systems. Combined measurements using these two techniques will give new insights into nanoscopic dynamics, and will be useful as a microrheology technique.

  5. 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.

  6. Applications of the Generalized X-ray Diffraction Enhanced Imaging in the Medical Imaging

    NASA Astrophysics Data System (ADS)

    Maksimenko, Anton; Hashimoto, Eiko; Ando, Masami; Sugiyama, Hiroshi

    2007-01-01

    The X-ray Diffraction Enhanced Imaging (DEI) is the analyzer-based X-ray imaging technique which allows extraction of the "pure refraction" and "apparent absorption" contrasts from two images taken on the opposite sides of the rocking curve of the analyzing crystal. The refraction contrast obtained by this method shows many advantages over conventional absorption contrast. It was successfully applied in medicine, technique and other fields of science. However, information provided by the method is rather qualitative than quantitative. This happens because either side of the rocking curve of the analyzer is approximated as a straight line what limits the ranges of applicability and introduces additional error. One can easily overcome this problem considering the rocking curve as is instead of it's Taylor's expansion. This report is dedicated to the application of this idea in medical imaging and especially computed tomography based on the refraction contrast. The results obtained via both methods are presented and compared.

  7. 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.

  8. 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.

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

    SciTech Connect

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

    2015-08-15

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

  10. 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.

  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. 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.

  13. X-ray diffraction and electron microscopy studies of frozen erythrocyte membrane preparations.

    PubMed

    Rzepecki, L M; Berriman, J; Finean, J B

    1980-07-16

    Well-defined X-ray diffraction patterns have been recorded from erythrocyte membranes in the frozen state. At -40 degrees C, lamellar periodicities range from 19 to 95 nm depending on the glycerol content (0--40%, respectively). Freeze-fracture electon micrographs of samples frozen in two stages to approximate to the diffraction conditions show ice formation external to membrane stacks. The membrane stacks have periodicities of the same order of magnitude as those obtained by X-ray diffraction.

  14. (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)

  15. A Bayesian Approach to Surface X-ray Diffraction

    SciTech Connect

    Lyman, Paul F.; Saldin, Dilano K.

    2006-11-17

    We report on the development of an iterative method to directly invert surface x-ray diffraction (SXRD) data and thereby provide a map of electron density in the near-surface region of a solid. We have termed this method PARADIGM, which stands for Phase and Amplitude Recovery And Diffraction Image Generation Method. Significant advances in the PARADIGM theory were made during the grant period, and experimental milestones have also been achieved. The two components of the research program worked in concert, each spurring progress in the other. The method works by iteratively recovering the phases of surface scattering factors. Initially, random phases are assigned to the structure factors. After subtracting off the known bulk component, a Fourier transform converts these factors into an estimate of the real-space electron density map. This map is subjected to a support constraint, which holds that the electron density may only be non-zero near the solid surface. The modified electron density is then subjected to an inverse Fourier transform, and the bulk contributions are added back in. This renders an improved estimate of the phases of the surface structure factors. A constraint in reciprocal space is then applied, namely, the amplitudes of the scattering factors are set equal to the experimentally observed ones. This cycle is repeated, transforming between real and reciprocal space and applying constraints in each, until convergence is reached. The result renders a good initial model of the unknown surface structure. Such a direct method is important because conventional structural refinement methods rely on having a guess of the starting structure that sufficiently good that it may be refined into a model with the correct atomic positions. If the starting model has, for example, the wrong number or identity of atoms in the surface unit cell, it can never refine to the correct model. Even in cases where the starting model contains the correct number and identity

  16. 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.

  17. 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.

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

    DOE PAGES

    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.

  19. 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.

  20. Nanofabrication of diffractive optics for soft X-ray and atom beam focusing

    NASA Astrophysics Data System (ADS)

    Rehbein, S.

    2003-03-01

    Nanostructuring processes are described for manufacturing diffractive optics for the condensermonochromator set-up of the transmission X-ray microscope (TXM) and for the scanning transmission X-ray microscope (STXM) at the BESSY II electron storage ring in Berlin. Furthermore, a process for manufacturing freestanding nickel zone plates for helium atom beam focusing experiments is presented.

  1. Fitting dynamical x-ray diffraction data over the World Wide Web.

    SciTech Connect

    Stepanov, S.; Forrest, R.; Biosciences Division; Univ. of Houston

    2008-01-01

    The first implementation of fitting X-ray Bragg diffraction profiles from strained multilayer crystals at a remote web-based X-ray software server is presented. The algorithms and the software solutions involved in the process are described. The suggested technology can be applied to a wide range of scientific research and has the potential to promote remote collaborations across scientific communities.

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

    PubMed

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

    2014-03-01

    X-ray diffraction patterns from two-dimensional (2-D) protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL) are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  3. X-Ray Spectrum of a Narrow-Line QSO

    NASA Technical Reports Server (NTRS)

    Halpern, Jules P.

    1998-01-01

    During the reporting period, seven papers using ASCA data, supported in whole or in part by this grant, were published or submitted to refereed journals. Their abstracts are given in this report, and the complete bibliographic references are listed in the Appendix. Titles include (1) A Broad-Band X-ray Study of the Geminga Pulsar; (2) ASCA Observations of PSR 1920+10 and PSR 0950+08; (3) X-ray and Optical Spectroscopy of IRAS 20181-2244: Not a Type 2 QSO, but a I Zw I Object; (4) Models for X-ray Emission from Isolated Pulsars; (5) Optical and X-ray Spectroscopy of 1E 0449.4-1823: Demise of the Original Type 2 QSO; (6) The ASCA Spectrum of the Broad-Line Radio Galaxy Pictor A: A Simple Power Law with No Fe Ka Line; and (7) ASCA Spectra of NGC 4388 and ESO 103-G35: Absorption, Reflection, and Variability in Intermediate Type Seyfert Galaxies.

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

    NASA Technical Reports Server (NTRS)

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

    1990-01-01

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

  5. A Fourier optics approach to the dynamical theory of X-ray diffraction--perfect crystals.

    PubMed

    Mana, Giovanni; Montanari, Francesco

    2004-01-01

    A new formalism is presented concerning the dynamics of X-rays in crystals. It is based on Takagi's equations and Fourier optics; it also offers an alternative to the usual Ewald-von Laue approach. The article does not give new results but shows a new way to formulate the dynamical theory of X-ray diffraction. In addition, it proposes a novel description of X-ray propagation based on the analogy between the dynamics of X-rays in crystals and that of two-level quantum systems.

  6. Mitigation of X-ray damage in macromolecular crystallography by submicrometre line focusing.

    PubMed

    Finfrock, Y Zou; Stern, Edward A; Alkire, R W; Kas, Joshua J; Evans-Lutterodt, Kenneth; Stein, Aaron; Duke, Norma; Lazarski, Krzysztof; Joachimiak, Andrzej

    2013-08-01

    Reported here are measurements of the penetration depth and spatial distribution of photoelectron (PE) damage excited by 18.6 keV X-ray photons in a lysozyme crystal with a vertical submicrometre line-focus beam of 0.7 µm full-width half-maximum (FWHM). The experimental results determined that the penetration depth of PEs is 5 ± 0.5 µm with a monotonically decreasing spatial distribution shape, resulting in mitigation of diffraction signal damage. This does not agree with previous theoretical predication that the mitigation of damage requires a peak of damage outside the focus. A new improved calculation provides some qualitative agreement with the experimental results, but significant errors still remain. The mitigation of radiation damage by line focusing was measured experimentally by comparing the damage in the X-ray-irradiated regions of the submicrometre focus with the large-beam case under conditions of equal exposure and equal volumes of the protein crystal, and a mitigation factor of 4.4 ± 0.4 was determined. The mitigation of radiation damage is caused by spatial separation of the dominant PE radiation-damage component from the crystal region of the line-focus beam that contributes the diffraction signal. The diffraction signal is generated by coherent scattering of incident X-rays (which introduces no damage), while the overwhelming proportion of damage is caused by PE emission as X-ray photons are absorbed.

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

    SciTech Connect

    Braun, Artur; Granlund, Eric; Cairns, Elton J.

    2003-01-27

    An electrochemical in-situ reaction cell for hard X-ray experiments with battery electrodes is described. Applications include the small angle scattering, diffraction, and near-edge spectroscopy of lithium manganese oxide electrodes.

  8. 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.

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

    DOEpatents

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

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

  10. 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.

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

    SciTech Connect

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

    2000-04-04

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

  12. 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.

  13. 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.

  14. Electron microscope and low-angle x-ray diffraction studies of the nerve myelin sheath.

    PubMed

    FERNANDEZ-MORAN, H; FINEAN, J B

    1957-09-25

    1. A close correlation has been obtained between high resolution electron microscopy and low-angle x-ray diffraction studies of the myelin sheath of frog and rat peripheral and central nerves. Extensive studies were performed by application of both techniques to the same specimens, prepared for examination by OsO(4) or KMnO(4) fixation, and embedding either in methacrylate or in gelatin employing a new procedure. Controlled physical and chemical modifications of the myelin sheath prior to fixation were also investigated. 2. A correspondence was established between the layer spacings observed in electron micrographs and the fundamental radial repeating unit indicated by the low-angle x-ray diffraction patterns. The variations in relative intensities of the low-angle x-ray reflections could be related to the radial density distributions seen in the electron micrographs. 3. An analysis of the preparation procedures revealed that OsO(4) fixation introduces a greater shrinkage of the layer spacings and more pronounced changes in the density distribution within the layers than KMnO(4) fixation. The effects of methacrylate and gelatin embedding are described, and their relative merits considered in relation to the preservation of myelin structure by OsO(4) fixation. 4. The experimental modifications introduced by freezing and thawing of fresh whole nerve are described, particularly the enhancement of the intermediate lines and the dissociation of the layer components in the myelin sheath. A characteristic collapsing of the radial period of the sheath is observed after subjecting fresh nerve trunks to prolonged and intense ultracentrifugation. 5. Controlled extraction of fresh nerve with acetone at 0 degrees C., which preferentially removes cholesterol, produces characteristic, differentiated modifications of the myelin sheath structure. Electron microscopy reveals several types of modifications within a single preparation, including both expanded and collapsed layer

  15. 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 α-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 1/12 nm(-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 1/13.7 nm(-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

  16. 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 α-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 1/12 nm(-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 1/13.7 nm(-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

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

    PubMed Central

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

    2015-01-01

    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 α-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 1/12 nm−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 1/13.7 nm−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

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

    SciTech Connect

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

    2009-01-09

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

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

    NASA Astrophysics Data System (ADS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

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

  20. 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.

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

    DOEpatents

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

    2007-06-26

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

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

    DOE PAGES

    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

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

    DOE PAGES

    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

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

    SciTech Connect

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

    2005-08-19

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

  5. 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.

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

    PubMed

    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

    2006-05-01

    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.

  8. 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 ( λ/Δ λ) 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.

  9. 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.

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

    PubMed Central

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

    2016-01-01

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

  11. 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

  12. 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.

  13. Advanced x-ray stress analysis method for a single crystal using different diffraction plane families

    SciTech Connect

    Imafuku, Muneyuki; Suzuki, Hiroshi; Sueyoshi, Kazuyuki; Akita, Koichi; Ohya, Shin-ichi

    2008-06-09

    Generalized formula of the x-ray stress analysis for a single crystal with unknown stress-free lattice parameter was proposed. This method enables us to evaluate the plane stress states with any combination of diffraction planes. We can choose and combine the appropriate x-ray sources and diffraction plane families, depending on the sample orientation and the apparatus, whenever diffraction condition is satisfied. The analysis of plane stress distributions in an iron single crystal was demonstrated combining with the diffraction data for Fe{l_brace}211{r_brace} and Fe{l_brace}310{r_brace} plane families.

  14. 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.

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

    SciTech Connect

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

    1998-12-31

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

  16. 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.

  17. An instrument for combining x-ray multiple diffraction and x-ray topographic imaging for examining crystal microcrystallography and perfection

    SciTech Connect

    Lai, X.; Ma, C. Y.; Roberts, K. J.; Cardoso, L. P.; Santos, A. O. dos; Bogg, D.; Miller, M. C.

    2009-03-15

    Diffraction imaging using x-ray topography (XRT) and x-ray multiple diffraction (XRMD) provide valuable tools for examining the growth defects in crystals and the distributions from ideal lattice symmetry (microcrystallography). The topographic x-ray multiple diffraction microprobe (TMDM) combines the complementary aspects of both techniques enabling XRT and XRMD studies within the same instrument providing a useful resource for the structural characterization of materials that are not very stable in vacuum and electron beam environments. The design of the TMDM instrument is described together with data taken on GaAs (001) and potassium dihydrogen phosphate (001)

  18. 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 μm 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 -55°C whereas the Vanilla was operated over a temperature range from 20°C to -10°C. 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.

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

    SciTech Connect

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

    2015-11-14

    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. CCD-based X-ray area detector for time-resolved diffraction experiments.

    PubMed

    Yagi, Naoto; Inoue, Katsuaki; Oka, Toshihiko

    2004-11-01

    A fast X-ray area detector for diffraction, scattering and imaging experiments at microsecond to millisecond time resolution has been developed. The key element of the detector is a fast (291 frames s(-1)) framing camera with three CCDs. A prism forms identical images on the CCDs and the frame rate is increased three times by reading them alternately. In order to convert X-rays into visible light that is detectable with the CCDs, an X-ray image intensifier is used. The camera can also be used with a high-resolution X-ray detector. In both cases it was found to be important to use a phosphor with a short decay time to fully make use of the high-speed framing capability of the camera. Preliminary results of a fibre diffraction experiment on a skeletal muscle and coronary angiography are presented.

  1. 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).

  2. Measurement of coronal X-ray emission lines from Capella

    NASA Technical Reports Server (NTRS)

    Vedder, P. W.; Canizares, C. R.

    1983-01-01

    The Einstein Observatory's Focal Plane Crystal Spectrometer has detected X-ray emission lines due to O VIII, Fe XVII, and Fe XX, from the binary star system Capella. Line luminosities are well fitted by an emitting plasma at a single temperature of 6.29 + or - 0.01 - 0.03 million K, and a volume emission measure of about 8.6 x 10 to the 52nd/cu cm, corresponding to the low temperature component previously observed. A high temperature component is undetectable, since the observed lines are not produced in plasma at temperatures above about 20 million K. Nearly isothermal plasma would be expected if many of the magnetically confined coronal loops have similar sizes and pressures, and a second population of longer loops would be required to account for the hotter component. An alternative interpretation of the observed X-ray line emission and upper limit is that the plasma contains a continuous distribution of emission measure versus temperature that rises sharply to 3 million K and then falls by nearly a decade to 16 million. An extrapolation of the loop sizes suggested by this alternative to hotter, longer loops may also account for the higher temperature emission.

  3. 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 μm 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.

  4. Thermal expansion in UO2 determined by high-energy X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Guthrie, M.; Benmore, C. J.; Skinner, L. B.; Alderman, O. L. G.; Weber, J. K. R.; Parise, J. B.; Williamson, M.

    2016-10-01

    Here we present crystallographic analyses of high-energy X-ray diffraction data on polycrystalline UO2 up to the melting temperature. The Rietveld refinements of our X-ray data are in agreement with previous measurements, but are systematically located around the upper bound of their uncertainty, indicating a slightly steeper trend of thermal expansion compared to established values. This observation is consistent with recent first principles calculations.

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

    DOEpatents

    Pawloski, Gayle A.

    1986-01-01

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

  6. 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.

  7. Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques.

    PubMed

    Mazaj, Matjaž; Kaučič, Venčeslav; Zabukovec Logar, Nataša

    2016-01-01

    The research on metal-organic frameworks (MOFs) experienced rapid progress in recent years due to their structure diversity and wide range of application opportunities. Continuous progress of X-ray and neutron diffraction methods enables more and more detailed insight into MOF's structural features and significantly contributes to the understanding of their chemistry. Improved instrumentation and data processing in high-resolution X-ray diffraction methods enables the determination of new complex MOF crystal structures in powdered form. By the use of neutron diffraction techniques, a lot of knowledge about the interaction of guest molecules with crystalline framework has been gained in the past few years. Moreover, in-situ time-resolved studies by various diffraction and scattering techniques provided comprehensive information about crystallization kinetics, crystal growth mechanism and structural dynamics triggered by external physical or chemical stimuli. The review emphasizes most relevant advanced structural studies of MOFs based on powder X-ray and neutron scattering. PMID:27640372

  8. Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques.

    PubMed

    Mazaj, Matjaž; Kaučič, Venčeslav; Zabukovec Logar, Nataša

    2016-01-01

    The research on metal-organic frameworks (MOFs) experienced rapid progress in recent years due to their structure diversity and wide range of application opportunities. Continuous progress of X-ray and neutron diffraction methods enables more and more detailed insight into MOF's structural features and significantly contributes to the understanding of their chemistry. Improved instrumentation and data processing in high-resolution X-ray diffraction methods enables the determination of new complex MOF crystal structures in powdered form. By the use of neutron diffraction techniques, a lot of knowledge about the interaction of guest molecules with crystalline framework has been gained in the past few years. Moreover, in-situ time-resolved studies by various diffraction and scattering techniques provided comprehensive information about crystallization kinetics, crystal growth mechanism and structural dynamics triggered by external physical or chemical stimuli. The review emphasizes most relevant advanced structural studies of MOFs based on powder X-ray and neutron scattering.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  10. 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.

  11. 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…

  12. 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

  13. On the calculation of the gauge volume size for energy-dispersive X-ray diffraction.

    PubMed

    Rowles, Matthew R

    2011-11-01

    Equations for the calculation of the dimensions of a gauge volume, also known as the active volume or diffraction lozenge, in an energy-dispersive diffraction experiment where the detector is collimated by two ideal slits have been developed. Equations are given for equatorially divergent and parallel incident X-ray beams, assuming negligible axial divergence. PMID:21997921

  14. 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

  15. 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.

  16. X-ray diffraction of slag-based sodium salt waste forms

    SciTech Connect

    Langton, C. A.; Missimer, D. M.

    2014-09-30

    The attached report documents sample preparation and x-ray diffraction results for a series of cement and blended cement matrices prepared with either water or a 4.4 M Na salt solution. The objective of the study was to provide initial phase characterization for the Cementitious Barriers Partnership reference case cementitious salt waste form. This information can be used to: 1) generate a base line for the evolution of the waste form as a function of time and conditions, 2) potentially to design new binders based on mineralogy of the binder, 3) understand and predict anion and cation leaching behavior of contaminants of concern, and 4) predict performance of the waste forms for which phase solubility and thermodynamic data are available.

  17. 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}.

  18. Direct Observation of Melting in Shock-Compressed Bismuth With Femtosecond X-ray Diffraction.

    PubMed

    Gorman, M G; Briggs, R; McBride, E E; Higginbotham, A; Arnold, B; Eggert, J H; Fratanduono, D E; Galtier, E; Lazicki, A E; Lee, H J; Liermann, H P; Nagler, B; Rothkirch, A; Smith, R F; Swift, D C; Collins, G W; Wark, J S; McMahon, M I

    2015-08-28

    The melting of bismuth in response to shock compression has been studied using in situ femtosecond x-ray diffraction at an x-ray free electron laser. Both solid-solid and solid-liquid phase transitions are documented using changes in discrete diffraction peaks and the emergence of broad, liquid scattering upon release from shock pressures up to 14 GPa. The transformation from the solid state to the liquid is found to occur in less than 3 ns, very much faster than previously believed. These results are the first quantitative measurements of a liquid material obtained on shock release using x-ray diffraction, and provide an upper limit for the time scale of melting of bismuth under shock loading.

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

    PubMed

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

    2009-08-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. This can be an important advantage for studying radiation-sensitive biological and soft matter specimens. PMID:19654762

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

  1. 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.

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

    SciTech Connect

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

    1986-05-29

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

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

    DOE PAGES

    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

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

    PubMed

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

    2016-09-16

    We present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional data cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. We demonstrate this 'big data' approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate. PMID:27505613

  5. Submicron X-Ray Diffraction and Its Applications to Problems in Materials and Environmental Science

    NASA Astrophysics Data System (ADS)

    Tamura, N.; Spolenak, R.; Valek, B. C.; Manceau, A.; Chang, N. M.

    2002-08-01

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

  6. 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; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.

    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.

  7. 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.

  8. 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

  9. 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.

  10. Diffraction crystal for sagittally focusing x-rays

    DOEpatents

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

    1984-01-01

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

  11. X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

    NASA Astrophysics Data System (ADS)

    Marshall, J.; Keaten, R.

    1999-09-01

    Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

  12. X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Keaten, R.

    1999-01-01

    Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

  13. 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.

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

    SciTech Connect

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

    2015-05-15

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

  15. 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.

  16. 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.

  17. Mössbauer, magnetization and X-ray diffraction characterization methods for iron oxide nanoparticles

    NASA Astrophysics Data System (ADS)

    Gabbasov, Raul; Polikarpov, Michael; Cherepanov, Valery; Chuev, Michael; Mischenko, Iliya; Lomov, Andrey; Wang, Andrew; Panchenko, Vladislav

    2015-04-01

    Water soluble magnetite iron oxide nanoparticles with oleic polymer coating and average diameters in the range of 5-25 nm, previously determined by TEM, were characterized using Mössbauer, magnetization and X-ray diffraction measurements. Comparative analysis of the results demonstrated a large diversity of magnetic relaxation regimes. Analysis showed the presence of an additional impurity component in the 25 nm nanoparticles, with principally different magnetic nature at the magnetite core. In some cases, X-ray diffraction measurements were unable to estimate the size of the magnetic core and Mössbauer data were necessary for the correct interpretation of the experimental results.

  18. Toward atomic resolution diffractive imaging of isolated molecules with X-ray free-electron lasers.

    PubMed

    Stern, S; Holmegaard, L; Filsinger, F; Rouzée, A; Rudenko, A; Johnsson, P; Martin, A V; Barty, A; Bostedt, C; Bozek, J; Coffee, R; Epp, S; Erk, B; Foucar, L; Hartmann, R; Kimmel, N; Kühnel, K-U; Maurer, J; Messerschmidt, M; Rudek, B; Starodub, D; Thøgersen, J; Weidenspointner, G; White, T A; Stapelfeldt, H; Rolles, D; Chapman, H N; Küpper, J

    2014-01-01

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

  19. Toward atomic resolution diffractive imaging of isolated molecules with X-ray free-electron lasers.

    PubMed

    Stern, S; Holmegaard, L; Filsinger, F; Rouzée, A; Rudenko, A; Johnsson, P; Martin, A V; Barty, A; Bostedt, C; Bozek, J; Coffee, R; Epp, S; Erk, B; Foucar, L; Hartmann, R; Kimmel, N; Kühnel, K-U; Maurer, J; Messerschmidt, M; Rudek, B; Starodub, D; Thøgersen, J; Weidenspointner, G; White, T A; Stapelfeldt, H; Rolles, D; Chapman, H N; Küpper, J

    2014-01-01

    We give a detailed account of the theoretical analysis and the experimental results of an X-ray-diffraction experiment on quantum-state selected and strongly laser-aligned gas-phase ensembles of the prototypical large asymmetric rotor molecule 2,5-diiodobenzonitrile, performed at the Linac Coherent Light Source [Phys. Rev. Lett.112, 083002 (2014)]. This experiment is the first step toward coherent diffractive imaging of structures and structural dynamics of isolated molecules at atomic resolution, i.e., picometers and femtoseconds, using X-ray free-electron lasers. PMID:25415561

  20. Femtosecond free-electron laser x-ray diffraction data sets for algorithm development.

    PubMed

    Kassemeyer, Stephan; Steinbrener, Jan; Lomb, Lukas; Hartmann, Elisabeth; Aquila, Andrew; Barty, Anton; Martin, Andrew V; Hampton, Christina Y; Bajt, Saša; Barthelmess, Miriam; Barends, Thomas R M; Bostedt, Christoph; Bott, Mario; Bozek, John D; Coppola, Nicola; Cryle, Max; DePonte, Daniel P; Doak, R Bruce; Epp, Sascha W; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Graafsma, Heinz; Gumprecht, Lars; Hartmann, Andreas; Hartmann, Robert; Hauser, Günter; Hirsemann, Helmut; Hömke, André; Holl, Peter; Jönsson, Olof; Kimmel, Nils; Krasniqi, Faton; Liang, Mengning; Maia, Filipe R N C; Marchesini, Stefano; Nass, Karol; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Schmidt, Carlo; Schulz, Joachim; Shoeman, Robert L; Sierra, Raymond G; Soltau, Heike; Spence, John C H; Starodub, Dmitri; Stellato, Francesco; Stern, Stephan; Stier, Gunter; Svenda, Martin; Weidenspointner, Georg; Weierstall, Uwe; White, Thomas A; Wunderer, Cornelia; Frank, Matthias; Chapman, Henry N; Ullrich, Joachim; Strüder, Lothar; Bogan, Michael J; Schlichting, Ilme

    2012-02-13

    We describe femtosecond X-ray diffraction data sets of viruses and nanoparticles collected at the Linac Coherent Light Source. The data establish the first large benchmark data sets for coherent diffraction methods freely available to the public, to bolster the development of algorithms that are essential for developing this novel approach as a useful imaging technique. Applications are 2D reconstructions, orientation classification and finally 3D imaging by assembling 2D patterns into a 3D diffraction volume.

  1. Femtosecond free-electron laser x-ray diffraction data sets for algorithm development.

    PubMed

    Kassemeyer, Stephan; Steinbrener, Jan; Lomb, Lukas; Hartmann, Elisabeth; Aquila, Andrew; Barty, Anton; Martin, Andrew V; Hampton, Christina Y; Bajt, Saša; Barthelmess, Miriam; Barends, Thomas R M; Bostedt, Christoph; Bott, Mario; Bozek, John D; Coppola, Nicola; Cryle, Max; DePonte, Daniel P; Doak, R Bruce; Epp, Sascha W; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Graafsma, Heinz; Gumprecht, Lars; Hartmann, Andreas; Hartmann, Robert; Hauser, Günter; Hirsemann, Helmut; Hömke, André; Holl, Peter; Jönsson, Olof; Kimmel, Nils; Krasniqi, Faton; Liang, Mengning; Maia, Filipe R N C; Marchesini, Stefano; Nass, Karol; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Schmidt, Carlo; Schulz, Joachim; Shoeman, Robert L; Sierra, Raymond G; Soltau, Heike; Spence, John C H; Starodub, Dmitri; Stellato, Francesco; Stern, Stephan; Stier, Gunter; Svenda, Martin; Weidenspointner, Georg; Weierstall, Uwe; White, Thomas A; Wunderer, Cornelia; Frank, Matthias; Chapman, Henry N; Ullrich, Joachim; Strüder, Lothar; Bogan, Michael J; Schlichting, Ilme

    2012-02-13

    We describe femtosecond X-ray diffraction data sets of viruses and nanoparticles collected at the Linac Coherent Light Source. The data establish the first large benchmark data sets for coherent diffraction methods freely available to the public, to bolster the development of algorithms that are essential for developing this novel approach as a useful imaging technique. Applications are 2D reconstructions, orientation classification and finally 3D imaging by assembling 2D patterns into a 3D diffraction volume. PMID:22418172

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

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

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

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

    PubMed

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

    2016-09-01

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

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

    PubMed

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

    2016-09-01

    X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration. PMID:27626076

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

    PubMed Central

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

    2016-01-01

    X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration. PMID:27626076

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

    PubMed Central

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

    2016-01-01

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

  7. High Resolution Triple Axis X-Ray Diffraction Analysis of II-VI Semiconductor Crystals

    NASA Technical Reports Server (NTRS)

    Volz, H. M.; Matyi, R. J.

    1999-01-01

    The objective of this research program is to develop methods of structural analysis based on high resolution triple axis X-ray diffractometry (HRTXD) and to carry out detailed studies of defect distributions in crystals grown in both microgravity and ground-based environments. HRTXD represents a modification of the widely used double axis X-ray rocking curve method for the characterization of grown-in defects in nearly perfect crystals. In a double axis rocking curve experiment, the sample is illuminated by a monochromatic X-ray beam and the diffracted intensity is recorded by a fixed, wide-open detector. The intensity diffracted by the sample is then monitored as the sample is rotated through the Bragg reflection condition. The breadth of the peak, which is often reported as the full angular width at half the maximum intensity (FWHM), is used as an indicator of the amount of defects in the sample. This work has shown that high resolution triple axis X-ray diffraction is an effective tool for characterizing the defect structure in semiconductor crystals, particularly at high defect densities. Additionally, the technique is complimentary to X-ray topography for defect characterization in crystals.

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

    PubMed

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

    2016-03-01

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

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

    DOE PAGES

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

    2016-02-17

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-09-01

    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/ΔE = 104 [1]. 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 [2]. 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.

  11. 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.

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

    PubMed Central

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

    2014-01-01

    X-ray diffraction patterns from two-dimensional (2-D) protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL) are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals. PMID:25075325

  13. Single-shot femtosecond x-ray diffraction from randomly oriented ellipsoidal nanoparticles

    NASA Astrophysics Data System (ADS)

    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.

    2010-09-01

    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 (250nm×50nm) 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.

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

    PubMed

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

    2014-03-01

    X-ray diffraction patterns from two-dimensional (2-D) protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL) are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals. PMID:25075325

  15. X-ray line from exciting dark matter

    NASA Astrophysics Data System (ADS)

    Finkbeiner, Douglas P.; Weiner, Neal

    2016-10-01

    The exciting dark matter (XDM) model was proposed as a mechanism to efficiently convert the kinetic energy (in sufficiently hot environments) of dark matter into e +e - pairs. The standard scenario invokes a doublet of nearly degenerate dark matter (DM) states and a dark force to mediate a large upscattering cross section between the two. For heavy (˜TeV ) DM, the kinetic energy of weakly interacting massive particles in large (galaxy-sized or larger) halos is capable of producing low-energy positrons. For lighter dark matter, this is kinematically impossible, and the unique observable signature becomes an x-ray line, arising from χ χ →χ*χ*, followed by χ*→χ γ . This variant of XDM is distinctive from other DM x-ray scenarios in that its signatures tend to be most present in more massive, hotter environments, such as clusters, rather than nearby dwarfs, and has different dependencies from decaying models. We find that it is capable of explaining the recently reported s-ray line at 3.56 keV. For very long lifetimes of the excited state, primordial decays can explain the signal without the presence of upscattering. Thermal models freeze out as in the normal XDM setup, via annihilations to the light boson ϕ . For suitable masses, the annihilation χ χ →ϕ ϕ followed by ϕ →SM can explain the reported gamma-ray signature from the Galactic center. Direct detection is discussed, including the possibility of explaining DAMA via the "luminous" dark matter approach. Quite generally, the proximity of the 3.56 keV line to the energy scale of DAMA motivates a reexamination of electromagnetic explanations. Other signals, including lepton jets and the modification of cores of dwarf galaxies are also considered.

  16. 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.

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

    SciTech Connect

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

    2005-06-15

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

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

    PubMed

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

    2014-10-01

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

  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. 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.

  2. 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.

  3. 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.

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

    DOEpatents

    Smither, Robert K.

    2011-05-17

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

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

    NASA Technical Reports Server (NTRS)

    Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.; Achilles, C. N.; Downs, R. T.; Farmer, J. D.; Crisp, J. A.; Morookian, J. M.; Des Marais, D. J.; Grotzinger, J. P.; Sarrazin, P.; Yen, A. S.

    2014-01-01

    To obtain detailed mineralogy information, the Mars Science Laboratory rover Curiosity carries CheMin, the first X-ray diffraction (XRD) instrument used on a planet other than Earth. CheMin has provided the first in situ XRD analyses of full phase assemblages on another planet.

  6. X-ray diffraction phase analysis of the crystalline phase of polytetrafluoroethylene

    SciTech Connect

    Lebedev, Yu. A. Korolev, Yu. M.; Rebrov, A. V.; Ignat'eva, L. N.; Antipov, E. M.

    2010-07-15

    Samples of ultradispersed polytetrafluoroethylene, which were prepared with the use of different technological approaches, were studied by X-ray diffraction. The samples were found to belong to the monoclinic system. For some samples, basal reflections, which can be related to paraffins, were found for the first time. This indicates that polymer chains can form yet another type of monoclinic structure.

  7. 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.

  8. 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…

  9. 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…

  10. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-10-01

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

  12. 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 ...

  13. Observation of parametric X-ray radiation in an anomalous diffraction region

    NASA Astrophysics Data System (ADS)

    Alexeyev, V. I.; Eliseyev, A. N.; Irribarra, E.; Kishin, I. A.; Kubankin, A. S.; Nazhmudinov, R. M.

    2016-08-01

    A new possibility to expand the energy region of diffraction processes based on the interaction of relativistic charged particles with crystalline structures is presented. Diffracted photons related to parametric X-ray radiation produced by relativistic electrons are detected below the low energy threshold for the X-ray diffraction mechanism in crystalline structures for the first time. The measurements were performed during the interaction of 7 MeV electrons with a textured polycrystalline tungsten foil and a highly oriented pyrolytic graphite crystal. The experiment results are in good agreement with a developed model based on the PXR kinematical theory. The developed experimental approach can be applied to separate the contributions of real and virtual photons to the total diffracted radiation generated during the interaction of relativistic charged particles with crystalline targets.

  14. High-pressure X-ray diffraction studies on β-Ni(OH) 2

    NASA Astrophysics Data System (ADS)

    Garg, Nandini; Karmakar, S.; Sharma, Surinder M.; Busseto, E.; Sikka, S. K.

    2004-06-01

    Using in situ X-ray diffraction, we have investigated the high-pressure behavior of β-Ni(OH) 2 upto 10 GPa. No phase transformation was observed in this pressure range. Our studies show that the diffraction peaks show inherent broadening on increase of pressure. This suggests that H-lattice may be already disordered at ambient conditions and further increase in pressure may increase the lattice disorder as observed in Co(OH) 2 (Phys. Rev. B 66 (2002) 134301).

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

    PubMed

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

    2014-11-17

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

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

    PubMed

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

    2014-11-17

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

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

    SciTech Connect

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

    2015-03-15

    We investigated the specific features of two diffraction schemes for a widely divergent X-ray beam that use a circular diaphragm 30–50 μm 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 = 2l (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{sub α} and K{sub β} 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.

  18. 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 μm 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 α and K β 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.

  19. 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

  20. High-resolution x-ray diffraction measurements of SiGe/Si structures

    SciTech Connect

    Jordan-Sweet, J.L.; Mooney, P.M.; Stephenson, G.B.

    1995-09-01

    High-resolution x-ray diffraction is an excellent probe of strain relaxation in complex SiGe structures. The high flux provided by synchrotron sources enables one to make extensive reciprocal space map measurements and evaluate many samples. The diffraction peak positions of each layer in a step-graded structure, measured for two different reflections, yield quantitative values for the relaxation and alloy composition in the layer. Grazing-incidence diffraction allows one to determine the in-plane structure of very thin layers, which have thickness-broadened peaks at conventional diffraction geometries. They demonstrate the power of these techniques with two examples.

  1. 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.

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2007-01-01

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

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

    PubMed Central

    Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C.H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

    2016-01-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

  5. 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.

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

    PubMed

    Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

    2016-01-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

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

    PubMed

    Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

    2016-01-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

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

    SciTech Connect

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

    2009-09-01

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

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

    SciTech Connect

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

    2014-11-15

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

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

    DOE PAGES

    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

  11. 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 Å, β=95.2°. Diffraction images were processed to a resolution of 1.74 Å 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.

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

    SciTech Connect

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

    2007-12-12

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

  13. 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.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

    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.

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

    PubMed

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

    2012-01-01

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

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

    PubMed

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

    2012-01-01

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

  18. 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.

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

    NASA Astrophysics Data System (ADS)

    Rago, P. B.; Ayers, J. E.

    2013-08-01

    High-resolution x-ray diffraction is an important nondestructive tool for structural characterization of semiconductor heterostructures, and the diffraction intensity profiles contain information on the depth profiles of strain, composition, and defect densities in device heterostructures. Much of this information remains inaccessible because the lack of phase information prevents direct inversion of the rocking curves. The current practice is to use dynamical simulations in conjunction with a curve-fitting procedure to indirectly extract the profiles of strain and composition, but such dynamical simulations have been based on perfect, dislocation-free laminar crystals, which renders the analysis inapplicable to highly mismatched structures containing dislocation densities greater than about 106 cm-2. In this work we present a dynamical model for Bragg x-ray diffraction in semiconductor device structures with nonuniform composition, strain, and dislocation density, which is based on the Takagi-Taupin equation for distorted crystals and accounts for the diffuse scattering arising from the strain mosaicity and angular mosaicity associated with dislocations. We show theoretically that the x-ray diffraction profiles from In x Ga1- x As/GaAs (001) heterostructures are strongly affected by the depth distribution of the dislocation density as well as the composition and strain, so that in principle all three distributions may be obtained by the analysis of the measured diffraction profiles.

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

    NASA Technical Reports Server (NTRS)

    Ko, Yuan-Kuen; Kallman, Timothy R.

    1994-01-01

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

  1. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements

    NASA Astrophysics Data System (ADS)

    Barty, Anton; Caleman, Carl; Aquila, Andrew; Timneanu, Nicusor; Lomb, Lukas; White, Thomas A.; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R. M.; Barthelmess, Miriam; Bogan, Michael J.; Bostedt, Christoph; Bozek, John D.; Coffee, Ryan; Coppola, Nicola; Davidsson, Jan; Deponte, Daniel P.; Doak, R. Bruce; Ekeberg, Tomas; Elser, Veit; Epp, Sascha W.; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Fromme, Petra; Graafsma, Heinz; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y.; Hartmann, Robert; Hartmann, Andreas; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Hunter, Mark S.; Johansson, Linda; Kassemeyer, Stephan; Kimmel, Nils; Kirian, Richard A.; Liang, Mengning; Maia, Filipe R. N. C.; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V.; Nass, Karol; Neutze, Richard; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Scott, Howard; Schlichting, Ilme; Schulz, Joachim; Seibert, M. Marvin; Shoeman, Robert L.; Sierra, Raymond G.; Soltau, Heike; Spence, John C. H.; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Ullrich, Joachim; Wang, X.; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia B.; Chapman, Henry N.

    2012-01-01

    X-ray free-electron lasers have enabled new approaches to the structural determination of protein crystals that are too small or radiation-sensitive for conventional analysis. For sufficiently short pulses, diffraction is collected before significant changes occur to the sample, and it has been predicted that pulses as short as 10 fs may be required to acquire atomic-resolution structural information. Here, we describe a mechanism unique to ultrafast, ultra-intense X-ray experiments that allows structural information to be collected from crystalline samples using high radiation doses without the requirement for the pulse to terminate before the onset of sample damage. Instead, the diffracted X-rays are gated by a rapid loss of crystalline periodicity, producing apparent pulse lengths significantly shorter than the duration of the incident pulse. The shortest apparent pulse lengths occur at the highest resolution, and our measurements indicate that current X-ray free-electron laser technology should enable structural determination from submicrometre protein crystals with atomic resolution.

  2. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements

    PubMed Central

    Barty, Anton; Caleman, Carl; Aquila, Andrew; Timneanu, Nicusor; Lomb, Lukas; White, Thomas A.; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R. M.; Barthelmess, Miriam; Bogan, Michael J.; Bostedt, Christoph; Bozek, John D.; Coffee, Ryan; Coppola, Nicola; Davidsson, Jan; DePonte, Daniel P.; Doak, R. Bruce; Ekeberg, Tomas; Elser, Veit; Epp, Sascha W.; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Fromme, Petra; Graafsma, Heinz; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y.; Hartmann, Robert; Hartmann, Andreas; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Hunter, Mark S.; Johansson, Linda; Kassemeyer, Stephan; Kimmel, Nils; Kirian, Richard A.; Liang, Mengning; Maia, Filipe R. N. C.; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V.; Nass, Karol; Neutze, Richard; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Scott, Howard; Schlichting, Ilme; Schulz, Joachim; Seibert, M. Marvin; Shoeman, Robert L.; Sierra, Raymond G.; Soltau, Heike; Spence, John C. H.; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Ullrich, Joachim; Wang, X.; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia B.; Chapman, Henry N.

    2013-01-01

    X-ray free-electron lasers have enabled new approaches to the structural determination of protein crystals that are too small or radiation-sensitive for conventional analysis1. For sufficiently short pulses, diffraction is collected before significant changes occur to the sample, and it has been predicted that pulses as short as 10 fs may be required to acquire atomic-resolution structural information1–4. Here, we describe a mechanism unique to ultrafast, ultra-intense X-ray experiments that allows structural information to be collected from crystalline samples using high radiation doses without the requirement for the pulse to terminate before the onset of sample damage. Instead, the diffracted X-rays are gated by a rapid loss of crystalline periodicity, producing apparent pulse lengths significantly shorter than the duration of the incident pulse. The shortest apparent pulse lengths occur at the highest resolution, and our measurements indicate that current X-ray free-electron laser technology5 should enable structural determination from submicrometre protein crystals with atomic resolution. PMID:24078834

  3. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements.

    PubMed

    Barty, Anton; Caleman, Carl; Aquila, Andrew; Timneanu, Nicusor; Lomb, Lukas; White, Thomas A; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R M; Barthelmess, Miriam; Bogan, Michael J; Bostedt, Christoph; Bozek, John D; Coffee, Ryan; Coppola, Nicola; Davidsson, Jan; Deponte, Daniel P; Doak, R Bruce; Ekeberg, Tomas; Elser, Veit; Epp, Sascha W; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Fromme, Petra; Graafsma, Heinz; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y; Hartmann, Robert; Hartmann, Andreas; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Hunter, Mark S; Johansson, Linda; Kassemeyer, Stephan; Kimmel, Nils; Kirian, Richard A; Liang, Mengning; Maia, Filipe R N C; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V; Nass, Karol; Neutze, Richard; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Scott, Howard; Schlichting, Ilme; Schulz, Joachim; Seibert, M Marvin; Shoeman, Robert L; Sierra, Raymond G; Soltau, Heike; Spence, John C H; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Ullrich, Joachim; Wang, X; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia B; Chapman, Henry N

    2012-01-01

    X-ray free-electron lasers have enabled new approaches to the structural determination of protein crystals that are too small or radiation-sensitive for conventional analysis(1). For sufficiently short pulses, diffraction is collected before significant changes occur to the sample, and it has been predicted that pulses as short as 10 fs may be required to acquire atomic-resolution structural information(1-4). Here, we describe a mechanism unique to ultrafast, ultra-intense X-ray experiments that allows structural information to be collected from crystalline samples using high radiation doses without the requirement for the pulse to terminate before the onset of sample damage. Instead, the diffracted X-rays are gated by a rapid loss of crystalline periodicity, producing apparent pulse lengths significantly shorter than the duration of the incident pulse. The shortest apparent pulse lengths occur at the highest resolution, and our measurements indicate that current X-ray free-electron laser technology(5) should enable structural determination from submicrometre protein crystals with atomic resolution.

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

    PubMed Central

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

    2014-01-01

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. PMID:24914153

  5. Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements.

    PubMed

    Barty, Anton; Caleman, Carl; Aquila, Andrew; Timneanu, Nicusor; Lomb, Lukas; White, Thomas A; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R M; Barthelmess, Miriam; Bogan, Michael J; Bostedt, Christoph; Bozek, John D; Coffee, Ryan; Coppola, Nicola; Davidsson, Jan; Deponte, Daniel P; Doak, R Bruce; Ekeberg, Tomas; Elser, Veit; Epp, Sascha W; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Fromme, Petra; Graafsma, Heinz; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y; Hartmann, Robert; Hartmann, Andreas; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Hunter, Mark S; Johansson, Linda; Kassemeyer, Stephan; Kimmel, Nils; Kirian, Richard A; Liang, Mengning; Maia, Filipe R N C; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V; Nass, Karol; Neutze, Richard; Reich, Christian; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Scott, Howard; Schlichting, Ilme; Schulz, Joachim; Seibert, M Marvin; Shoeman, Robert L; Sierra, Raymond G; Soltau, Heike; Spence, John C H; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Ullrich, Joachim; Wang, X; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia B; Chapman, Henry N

    2012-01-01

    X-ray free-electron lasers have enabled new approaches to the structural determination of protein crystals that are too small or radiation-sensitive for conventional analysis(1). For sufficiently short pulses, diffraction is collected before significant changes occur to the sample, and it has been predicted that pulses as short as 10 fs may be required to acquire atomic-resolution structural information(1-4). Here, we describe a mechanism unique to ultrafast, ultra-intense X-ray experiments that allows structural information to be collected from crystalline samples using high radiation doses without the requirement for the pulse to terminate before the onset of sample damage. Instead, the diffracted X-rays are gated by a rapid loss of crystalline periodicity, producing apparent pulse lengths significantly shorter than the duration of the incident pulse. The shortest apparent pulse lengths occur at the highest resolution, and our measurements indicate that current X-ray free-electron laser technology(5) should enable structural determination from submicrometre protein crystals with atomic resolution. PMID:24078834

  6. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg-Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position.

  7. 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.

  8. Small-angle x-ray scattering/diffraction system for studies of biological and other materials at the Stanford Synchrotron Radiation Laboratorya)

    NASA Astrophysics Data System (ADS)

    Wakatsuki, S.; Hodgson, K. O.; Eliezer, D.; Rice, M.; Hubbard, S.; Gillis, N.; Doniach, S.; Spann, U.

    1992-02-01

    A versatile small-angle x-ray diffraction/scattering system has been developed at Stanford Synchrotron Radiation Laboratory for studies of biological and other materials. The system includes two sets of collimation slits separated by an ionization chamber, a sample holder cooled by a circulation bath, a vacuum/He scattering path after the sample holder and a detector, either a linear one-dimensional position-sensitive proportional counter or a position-sensitive quadrant detector. Data aquisition is controlled by a VAXstation through a CAMAC interface. Menu-driven data acquisition and on-line analysis software has been developed. The system can be used to collect small- to intermediate-angle x-ray scattering and diffraction data. Monochromatic, anomalous, and time-resolved scattering/diffraction experiments are possible. A time-resolved spectrophotometer using photodiode arrays has also been developed for simultaneous measurements of optical absorption spectra and x-ray scattering/diffraction.

  9. Small-angle x-ray scattering/diffraction system for studies of biological and other materials at the Stanford Synchrotron Radiation Laboratory (abstract)a)

    NASA Astrophysics Data System (ADS)

    Wakatsuki, S.; Hodgson, K. O.; Eliezer, D.; Rice, M.; Hubbard, S.; Gillis, N.; Doniach, S.; Spann, U.

    1992-01-01

    A versatile small-angle x-ray diffraction/scattering system has been developed at Stanford Synchrotron Radiation Laboratory for studies of biological and other materials. The system includes two sets of collimation slits separated by an ionization chamber, a sample holder cooled by a circulation bath, a vacuum/He scattering path after the sample holder and a detector, either a linear one-dimensional position-sensitive proportional counter or a position-sensitive quadrant detector. Data aquisition is controlled by a VAXstation through a CAMAC interface. Menu-driven data acquisition and on-line analysis software has been developed. The system can be used to collect small- to intermediate-angle x-ray scattering and diffraction data. Monochromatic, anomalous, and time-resolved diffraction/scattering experiments are possible. A time-resolved spectrophotometer using photodiode arrays has also been developed for simultaneous measurements of optical absorption spectra and x-ray scattering/diffraction.

  10. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    SciTech Connect

    McGonegle, David Wark, Justin S.; Higginbotham, Andrew; Milathianaki, Despina; Remington, Bruce A.

    2015-08-14

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as may occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.

  11. The Scherrer equation and the dynamical theory of X-ray diffraction.

    PubMed

    Muniz, Francisco Tiago Leitão; Miranda, Marcus Aurélio Ribeiro; Morilla Dos Santos, Cássio; Sasaki, José Marcos

    2016-05-01

    The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6 and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm(-1) the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm. PMID:27126115

  12. 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.

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

    DOE PAGES

    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

  14. 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)

  15. 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.

  16. X-Ray Continua of Broad Absorption Line Quasars

    NASA Technical Reports Server (NTRS)

    Mathur, S.

    1999-01-01

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

  17. 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.

  18. 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.

  19. Modeling X-ray emission line profiles from massive star winds - A review

    NASA Astrophysics Data System (ADS)

    Ignace, Richard

    2016-09-01

    The Chandra and XMM-Newton X-ray telescopes have led to numerous advances in the study and understanding of astrophysical X-ray sources. Particularly important has been the much increased spectral resolution of modern X-ray instrumentation. Wind-broadened emission lines have been spectroscopically resolved for many massive stars. This contribution reviews approaches to the modeling of X-ray emission line profile shapes from single stars, including smooth winds, winds with clumping, optically thin versus thick lines, and the effect of a radius-dependent photoabsorption coefficient.

  20. X-ray diffraction imaging of metal–oxide epitaxial tunnel junctions made by optical lithography: use of focused and unfocused X-ray beams

    PubMed Central

    Mocuta, Cristian; Barbier, Antoine; Stanescu, Stefan; Matzen, Sylvia; Moussy, Jean-Baptiste; Ziegler, Eric

    2013-01-01

    X-ray diffraction techniques are used in imaging mode in order to characterize micrometre-sized objects. The samples used as models are metal–oxide tunnel junctions made by optical lithography, with lateral sizes ranging from 150 µm down to 10 µm and various shapes: discs, squares and rectangles. Two approaches are described and compared, both using diffraction contrast: full-field imaging (topography) and raster imaging (scanning probe) using a micrometre-sized focused X-ray beam. It is shown that the full-field image gives access to macroscopic distortions (e.g. sample bending), while the local distortions, at the micrometre scale (e.g. tilts of the crystalline planes in the vicinity of the junction edges), can be accurately characterized only using focused X-ray beams. These local defects are dependent on the junction shape and larger by one order of magnitude than the macroscopic curvature of the sample. PMID:23412494

  1. Structural characterisation of Ni clusters in AlN via X-ray absorption, X-ray diffraction and transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Zanghi, D.; Traverse, A.; Dallas, J.-P.; Snoeck, E.

    Ni ions were implanted in bulk AlN with the goal to form embedded metallic clusters. Combining several characterisation techniques such as X-ray absorption spectroscopy, X-ray diffraction and high resolution transmission electron microscopy, we determined the lattice parameter of the Ni clusters that display a fcc crystalline structure. The average size increases when the ion fluence is increased or after a thermal treatment. Thanks to moiré fringes observed by high resolution transmission electron microscopy and to satellite peaks seen on the diffraction patterns, we concluded that the annealed Ni clusters orientate their (002) planes on the (101) of AlN. Moreover, the satellite positions allowed us to calculate Ni cluster average diameters, that are in agreement with average sizes deduced by X-ray absorption spectroscopy.

  2. A nearly on-axis spectroscopic system for simultaneously measuring 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.

  3. 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.

  4. Diffraction theory applied to X-ray imaging with clessidra prism array lenses.

    PubMed

    De Caro, Liberato; Jark, Werner

    2008-03-01

    Clessidra (hourglass) lenses, i.e. two large prisms each composed of smaller identical prisms or prism-like objects, can focus X-rays. As these lenses have a periodic structure perpendicular to the incident radiation, they will diffract the beam like a diffraction grating. Refraction in the prisms is responsible for blazing, i.e. for the concentration of the diffracted intensity into only a few diffraction peaks. It is found that the diffraction of coherent radiation in clessidra lenses needs to be treated in the Fresnel, or near-field, regime. Here, diffraction theory is applied appropriately to the clessidra structure in order to show that blazing in a perfect structure with partly curved prisms can indeed concentrate the diffracted intensity into only one peak. When the lens is entirely composed of identical perfect prisms, small secondary peaks are found. Nevertheless, the loss in intensity in the central peak will not lead to any significant widening of this peak. Clessidras with perfect prisms illuminated by full coherent X-ray radiation can then provide spatial resolutions, which are consistent with the increased aperture, and which are far below the height of the single small prisms.

  5. 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.

  6. Crystallization and preliminary X-ray diffraction analysis of maize aldose reductase

    SciTech Connect

    Kiyota, Eduardo; Sousa, Sylvia Morais de; Santos, Marcelo Leite dos; Costa Lima, Aline da; Menossi, Marcelo; Yunes, José Andrés; Aparicio, Ricardo

    2007-11-01

    Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 Å resolution are reported. Maize aldose reductase (AR) is a member of the aldo-keto reductase superfamily. In contrast to human AR, maize AR seems to prefer the conversion of sorbitol into glucose. The apoenzyme was crystallized in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 47.2, b = 54.5, c = 100.6 Å and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 Å was obtained after data reduction. Phasing was carried out by an automated molecular-replacement procedure and structural refinement is currently in progress. The refined structure is expected to shed light on the functional/enzymatic mechanism and the unusual activities of maize AR.

  7. Time Resolved X-Ray Diffraction of Reactive Solids Under Dynamic Loadings

    NASA Astrophysics Data System (ADS)

    Yoo, Choong-Shik

    2015-06-01

    We present novel time-resolved (TR) x-ray diffraction and TR Raman spectroscopy capable of probing structural and chemical evolutions of solids undergoing chemical and phase transformations. These methods are applicable to a wide range of dynamic experiments to study both single event phenomena of solids under thermal, electric or mechanical impact conditions and non-single event phenomena under dynamic-diamond anvil cell (d-DAC) and high frequency pulse (or ramp) laser-heated DAC. In this talk, relevant technology developments are described with several examples of our recent studies on reactive metals and dense molecular systems, which are synergistic to many proposed activities to develop dynamic synchrotron x-ray diffraction capabilities centered at advanced third and fourth generation light sources.

  8. Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

    NASA Technical Reports Server (NTRS)

    Hagiya, Kenji; Mikouchi, Takashi; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Yamaguchi, Shoki; Hirata, Arashi; Kurokawa, Ayaka; Zolensky, Michael E. (Principal Investigator)

    2016-01-01

    We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

  9. High pressure phase transformations in α-AlPO4: an x-ray diffraction investigation

    NASA Astrophysics Data System (ADS)

    Sharma, Surinder M.; Garg, Nandini; Sikka, S. K.

    2000-07-01

    We have re-investigated the high pressure behaviour of berlinite AlPO4 (α-AlPO4) with x-ray diffraction using a powerful synchrotron x-ray source SPring-8. Our results show that it transforms to a crystalline phase beyond ~13 GPa. Our data seem to be consistent with a CrVO4 type of structure in the Cmcm space group, similar to the high pressure phase observed in some isostructural phosphate compounds. The persistence of the diffraction pattern up to 40 GPa establishes that the previously accepted amorphization of AlPO4 around 12-18 GPa is incorrect. Experimental results suggest that the so-called memory glass effect observed earlier may in fact be the reversibility of the α-phase←⇔crystalline phase transformation. Comparisons of our experimental and theoretical results raise serious doubts about the theoretical understanding of the high pressure behaviour of α-AlPO4.

  10. Equation of state for technetium from X-ray diffraction and first-principle calculations

    NASA Astrophysics Data System (ADS)

    Mast, Daniel S.; Kim, Eunja; Siska, Emily M.; Poineau, Frederic; Czerwinski, Kenneth R.; Lavina, Barbara; Forster, Paul M.

    2016-08-01

    The ambient temperature equation of state (EoS) of technetium metal has been measured by X-ray diffraction. The metal was compressed using a diamond anvil cell and using a 4:1 methanol-ethanol pressure transmitting medium. The maximum pressure achieved, as determined from the gold pressureEquation of state for technetium from X-ray diffraction and first-principle calculations scale, was 67 GPa. The compression data shows that the HCP phase of technetium is stable up to 67 GPa. The compression curve of technetium was also calculated using first-principles total-energy calculations. Utilizing a number of fitting strategies to compare the experimental and theoretical data it is determined that the Vinet equation of state with an ambient isothermal bulk modulus of B0T=288 GPa and a first pressure derivative of B‧=5.9(2) best represent the compression behavior of technetium metal.

  11. Single-crystal X-ray diffraction studies on structural transformations of porous coordination polymers.

    PubMed

    Zhang, Jie-Peng; Liao, Pei-Qin; Zhou, Hao-Long; Lin, Rui-Biao; Chen, Xiao-Ming

    2014-08-21

    X-Ray single-crystal diffraction has been the most straightforward and important technique in structural determination of crystalline materials for understanding their structure-property relationships. This powerful tool can be used to directly visualize the precise and detailed structural information of porous coordination polymers or metal-organic frameworks at different states, which are unique for their flexible host frameworks compared with conventional adsorbents. With a series of selected recent examples, this review gives a brief overview of single-crystal X-ray diffraction studies and single-crystal to single-crystal transformations of porous coordination polymers under various chemical and physical stimuli such as solvent and gas sorption/desorption/exchange, chemical reaction and temperature change.

  12. X-ray diffraction analysis of multilayer porous InP(001) structure

    SciTech Connect

    Lomov, A. A.; Punegov, V. I.; Vasil'ev, A. L.; Nohavica, D.; Gladkov, P.; Kartsev, A. A.; Novikov, D. V.

    2010-03-15

    Multilayer structures composed of four porous bilayers have been studied by high-resolution X-ray diffraction using synchrotron radiation, and the photoluminescence of these structures has been investigated at 4 K. The porous structures were formed by anodic oxidation of InP(001) substrates in aqueous HCl solution. The structural parameters of the sublayers were varied by changing the electrochemical etching mode (potentiostatic/galvanostatic). The X-ray scattering intensity maps near the InP 004 reflection are obtained. A model for scattering from such systems is proposed based on the statistical dynamical diffraction theory. Theoretical scattering maps have been fitted to the experimental ones. It is shown that a mathematical analysis of the scattering intensity maps makes it possible to determine the structural parameters of sublayers. The reconstructed parameters (thickness, strain, and porosity of sublayers and the shape and arrangement of pores) are in satisfactory agreement with the scanning electron microscopy data.

  13. Ultrafast self-gating Bragg diffraction of exploding nanocrystals in an X-ray laser.

    PubMed

    Caleman, Carl; Tîmneanu, Nicuşor; Martin, Andrew V; Jönsson, H Olof; Aquila, Andrew; Barty, Anton; Scott, Howard A; White, Thomas A; Chapman, Henry N

    2015-01-26

    In structural determination of crystalline proteins using intense femtosecond X-ray lasers, damage processes lead to loss of structural coherence during the exposure. We use a nonthermal description for the damage dynamics to calculate the ultrafast ionization and the subsequent atomic displacement. These effects degrade the Bragg diffraction on femtosecond time scales and gate the ultrafast imaging. This process is intensity and resolution dependent. At high intensities the signal is gated by the ionization affecting low resolution information first. At lower intensities, atomic displacement dominates the loss of coherence affecting high-resolution information. We find that pulse length is not a limiting factor as long as there is a high enough X-ray flux to measure a diffracted signal.

  14. Low temperature single crystal X-ray diffraction: advantages, instrumentation and applications.

    PubMed

    Goeta, A E; Howard, J A K

    2004-10-20

    The benefits of carrying out single crystal X-ray diffraction (SXRD) experiments at low temperatures have long been recognised by the scientific community, as clearly demonstrated by the massive increase in publications reporting the use of low temperature SXRD in the past 15 years. This tutorial review will summarise the advantages, many of them now often forgotten by its practitioners or never known by the newcomers to the field, of performing single crystal X-ray diffraction experiments at low temperatures. The instrumentation currently available to university laboratories, which has been greatly improved over the past 5 years, will also be briefly described and a few different examples covering a range of applications will be presented.

  15. Ultrafast self-gating Bragg diffraction of exploding nanocrystals in an X-ray laser.

    PubMed

    Caleman, Carl; Tîmneanu, Nicuşor; Martin, Andrew V; Jönsson, H Olof; Aquila, Andrew; Barty, Anton; Scott, Howard A; White, Thomas A; Chapman, Henry N

    2015-01-26

    In structural determination of crystalline proteins using intense femtosecond X-ray lasers, damage processes lead to loss of structural coherence during the exposure. We use a nonthermal description for the damage dynamics to calculate the ultrafast ionization and the subsequent atomic displacement. These effects degrade the Bragg diffraction on femtosecond time scales and gate the ultrafast imaging. This process is intensity and resolution dependent. At high intensities the signal is gated by the ionization affecting low resolution information first. At lower intensities, atomic displacement dominates the loss of coherence affecting high-resolution information. We find that pulse length is not a limiting factor as long as there is a high enough X-ray flux to measure a diffracted signal. PMID:25835880

  16. Shock Melting of Forsterite by In-Situ X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Newman, M.; Kraus, R. G.; Wicks, J. K.; Coppari, F.; Smith, R.; Duffy, T. S.

    2015-12-01

    The equation of state of magnesium silicates at pressures and temperatures near the solid-liquid coexistence curve is important for understanding the thermal evolution and interior structure of rocky planets. Here, we present a series of laser driven shock-melt experiments on single crystal Mg_2SiO_4 forsterite, conducted at the Omega EP laser facility. Particle velocities in the Mg_2SiO_4 samples were measured using a line VISAR and used to infer the thermodynamic state of the shocked samples. In situ X-ray diffraction measurements are used to probe the melting transition and investigate the potential decomposition of Mg_2SiO_4 in to MgO and MgSiO_3 upon melt. This work examines potential kinetic effects of decomposition due to the short time scale of laser-shock experiments. In addition, the thermodynamic data collected in these experiments adds to a limited body of information regarding the equation of state of Mg_2SiO_4, which is the dominant end member composition in Earth's upper mantle. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  19. Thermoluminescence and X-ray diffraction studies on sliced ancient porcelain samples

    NASA Astrophysics Data System (ADS)

    Leung, P. L.; Yang, B.

    1999-09-01

    The thermal activation characteristics (TACs) of the sensitivity of the '110°C' peak in 14 sliced ancient Chinese porcelain samples are studied. Comparing with the TACs of natural quartz and synthetic mullite, the relation between the TACs and the composition of the sample is discussed with reference to the X-ray diffraction (XRD) spectra. It is suggested that in some cases, contribution of the porcelain components other than quartz to the TACs is not negligible.

  20. Rietveld refinement on x-ray diffraction patterns of bioapatite in human fetal bones.

    PubMed

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

    2003-03-01

    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 ( micro -XRD) techniques. Rietveld refinement analyses of XRD and micro -XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age.

  1. 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.

  2. 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.

  3. Estimating mean crystallite size of magnetite using multivariate calibration and powder x-ray diffraction analysis.

    PubMed

    Lemes, Maykon A; Godinho, Mariana S; Rabelo, Denilson; Martins, Felipe T; Mesquita, Alexandre; Neto, Francisco N De Souza; Araujo, Olacir A; Oliveira, Anselmo E De

    2014-01-01

    Powder X-ray diffraction patterns for 29 samples of magnetite, acquired using a conventional diffractometer, were used to build PLS calibration-based methods and variable selection to estimate mean crystallite size of magnetite directly from powder X-ray diffraction patterns. The best IPLS model corresponds to the Bragg reflections at 35.4° (h k l = 3 1 1), 43.0° (h k l = 4 0 0), 53.6° (h k l = 4 2 2), and 57.0° (h k l = 5 1 1) in 2θ. The best model was a GA-PLS which produced a model with RMSEP of 0.9 nm, and a correlation coefficient of 0.9976 between mean crystallite sizes calculated using Williamson-Hall approach and the ones predicted by GA-PLS method. These results indicate that magnetite mean crystallite sizes can be predicted directly from Powder X-Ray Diffraction and multivariate calibration using PLS variable selection approach.

  4. 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

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

    DOE PAGES

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

    2016-08-09

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

  6. 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.

  7. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

    SciTech Connect

    Lambert, P. K.; Hustedt, C. J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C.; Vecchio, K. S.; Huskins, E. L.; Casem, D. T.; Gruner, S. M.; Tate, M. W.; Philipp, H. T.; Purohit, P.; Weiss, J. T.; Woll, A. R.; Kannan, V.; Ramesh, K. T.; Kenesei, P.; Okasinski, J. S.; Almer, J.

    2014-09-15

    We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼10{sup 3}–10{sup 4} s{sup −1} in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10–20 keV) and is well suited to weakly absorbing materials such as magnesium alloys. The second technique is useful for more strongly absorbing materials, and uses high-energy x-rays (86 keV) and a fast shutter synchronized with the Kolsky bar to produce short (∼40 μs) pulses timed with the arrival of the strain pulse at the specimen, recording the diffraction pattern on a large-format amorphous silicon detector. For both techniques we present sample data demonstrating the ability of these techniques to characterize elastic strains and polycrystalline texture as a function of time during high-rate deformation.

  8. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading.

    PubMed

    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

    2014-09-01

    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 ~10(3)-10(4) 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.

  9. 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.

  10. 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.

  11. Femtosecond Diffractive Imaging with a Soft-X-ray Free-Electron Laser

    SciTech Connect

    Chapman, H N; Barty, A; Bogan, M; Boutet, S; Frank, M; Hau-Riege, S P; Marchesini, S; Woods, B; Bajt, S; Benner, W H; London, R; Ploenjes-Palm, E; Kuhlmann, M; Treusch, R; Dusterer, S; Tschentscher, T; Schneider, J; Spiller, E; Moller, T; Bostedt, C; Hoener, M; Shapiro, D; Hodgson, K O; der Spoel, D v; Burmeister, F; Bergh, M; Caleman, C; Huldt, G; Seibert, M; Maia, F; Lee, R; Szoke, A; Timneanu, N; Hajdu, J

    2006-03-13

    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.

  12. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques. PMID:21615981

  13. 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.

  14. Formation of x-ray vortex dipoles using a single diffraction pattern and direct phase measurement using interferometry

    SciTech Connect

    Kohmura, Yoshiki; Sawada, Kei; Taguchi, Munetaka; Ishikawa, Tetsuya; Ohigashi, Takuji; Suzuki, Yoshio

    2009-03-09

    We have devised a method for generating x-ray vortices by using a diffraction pattern from a simple aperture with illumination wave fronts with spherical curvatures. The interferometry visualized the x-ray vortex dipoles by the direct phase measurement. Our interference technique enabled us to sensitively detect and quantitatively measure various phase dislocations on the x-ray wave fronts, providing useful methodologies for beam diagnostics and materials science.

  15. Grazing-incidence X-ray diffraction from a crystal with subsurface defects

    SciTech Connect

    Gaevskii, A. Yu. Golentus, I. E.

    2015-03-15

    The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaks are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.

  16. 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.

  17. Time-Domain X-ray Diffraction in the Pulsed Laser Heated Diamond Anvil Cell

    NASA Astrophysics Data System (ADS)

    Prakapenka, V.; Goncharov, A. F.; Struzhkin, V.; Kantor, I.; Rivers, M. L.; Dalton, D. A.

    2011-12-01

    We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell (DAC) at pressure up to 100 GPa and 3500 K. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 microseconds pulse width synchronized with a gated x-ray detector (Pilatus) and time resolved radiometric temperature measurements. For the special APS hybrid mode, the measurements were also synchronized with a 500 ns long bunch carrying 88% of the ring current. This setup enables time domain measurements as a function of temperature in a micrometers time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration samples 4 micrometers thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformity as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. We will show examples of studies of the melting, thermal equation of state, and chemical reactivity. We acknowledge support from NSF EAR-0842057, DOE/ NNSA (CDAC), and EFree, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Award No. DESC0001057. X-ray diffraction measurements were performed at GSECARS (APS) supported by DOE Contract No.W-31-109- Eng-38.

  18. 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.

  19. Crystallization and preliminary X-ray diffraction studies of ferredoxin reductase from Leptospira interrogans

    SciTech Connect

    Nascimento, Alessandro S.; Ferrarezi, Thiago; Catalano-Dupuy, Daniela L.; Ceccarelli, Eduardo A.; Polikarpov, Igor

    2006-07-01

    Crystals adequate for X-ray diffraction analysis have been prepared from L. interrogans ferredoxin-NADP{sup +} reductase. Ferredoxin-NADP{sup +} reductase (FNR) is an FAD-containing enzyme that catalyzes electron transfer between NADP(H) and ferredoxin. Here, results are reported of the recombinant expression, purification and crystallization of FNR from Leptospira interrogans, a parasitic bacterium of animals and humans. The L. interrogans FNR crystals belong to a primitive monoclinic space group and diffract to 2.4 Å resolution at a synchrotron source.

  20. X-ray diffraction of molybdenum under ramp compression to 1 TPa

    NASA Astrophysics Data System (ADS)

    Wang, Jue; Coppari, Federica; Smith, Raymond F.; Eggert, Jon H.; Lazicki, Amy E.; Fratanduono, Dayne E.; Rygg, J. Ryan; Boehly, Thomas R.; Collins, Gilbert W.; Duffy, Thomas S.

    2016-09-01

    Molybdenum (Mo) is a transition metal with a wide range of technical applications. There has long been strong interest in its high-pressure behavior, and it is often used as standard for high-pressure experiments. Combining powder x-ray diffraction and dynamic ramp compression, structural and equation of state data were collected for solid Mo to 1 TPa (10 Mbar). Diffraction results are consistent with Mo remaining in the body-centered-cubic structure into the TPa regime. Stress-density data show that Mo under ramp loading is less compressible than the room-temperature isotherm but more compressible than the single-shock Hugoniot.

  1. Simulating picosecond X-ray diffraction from crystals using FFT methods on MD output

    SciTech Connect

    Kimminau, Giles; Nagler, Bob; Higginbotham, Andrew; Murphy, William; Wark, Justin; Park, Nigel; Hawreliak, James; Kalantar, Dan; Lorenzana, Hector; Remington, Bruce

    2007-12-12

    Multi-million atom non-equilibrium molecular dynamics (MD) simulations give significant insight into the transient processes that occur under shock compression. Picosecond X-ray diffraction enables the probing of materials on a timescale fast enough to test such effects. In order to simulate diffraction patterns, Fourier methods are required to gain a picture of reciprocal lattice space. We present here results of fast Fourier transforms of atomic coordinates of shocked crystals simulated by MD, and comment on the computing power required as a function of problem size. The relationship between reciprocal space and particular experimental geometries is discussed.

  2. X-ray third-order nonlinear dynamical diffraction in a crystal

    SciTech Connect

    Balyan, M. K.

    2015-12-15

    The dynamic diffraction of an X-ray wave in a crystal with a third-order nonlinear response to external field strength has been theoretically investigated. General equations for the wave propagation in crystal and nonlinear Takagi equations for both ideal and deformed crystals are derived. Integrals of motion are determined for the nonlinear problem of dynamic diffraction. The results of the numerical calculations of reflectivity in the symmetric Laue geometry for an incident plane wave and the intensity distributions on the output crystal surface for a point source are reported as an example.

  3. 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.

  4. [A quantitation method for andrographolide and dehydroandrographolide by X-ray powder diffraction Fourier fingerprint pattern technique].

    PubMed

    Gong, Ning-Bo; Lü, Li-Juan; Liu, Chao; Ma, Lin; Chen, Ruo-Yun; Lü, Yang

    2010-05-01

    The powder X-ray diffraction Fourier fingerprint pattern technique was used to develop a new quantitation method for the analysis of andrographolide and dehydroandrographolide. And the high performance liquid chromatography method was used to evaluate the quantity of andrographolide and dehydroandrographolide. The relationship of diffraction peak intensity and content of andrographolide and dehydroandrographolide was investigated. The powder X-ray diffraction Fourier fingerprint pattern analysis technique can be used to evaluate the quantity of andrographolide and dehydroandrographolide in the herb simultaneously.

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

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

  6. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility.

    PubMed

    Gupta, Y M; Turneaure, Stefan J; Perkins, K; Zimmerman, K; Arganbright, N; Shen, G; Chow, P

    2012-12-01

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization∕x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  7. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    SciTech Connect

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-15

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  8. A study of X-ray multiple diffraction by means of section topography.

    PubMed

    Kohn, V G; Smirnova, I A

    2015-09-01

    The results of theoretical and experimental study are presented for the question of how the X-ray multiple diffraction in a silicon single crystal influences the interference fringes of section topography for the 400 reflection in the Laue case. Two different cases of multiple diffraction are discovered for zero and very small values of the azimuthal angle for the sample in the form of a plate with the surface normal to the 001 direction. The cases are seen on the same topogram without rotation of the crystal. Accurate computer simulations of the section topogram for the case of X-ray multiple diffraction are performed for the first time. It is shown that the structure of interference fringes on the section topogram in the region of multiple diffraction becomes more complicated. It has a very sharp dependence on the azimuthal angle. The experiment is carried out using a laboratory source under conditions of low resolution over the azimuthal angle. Nevertheless, the characteristic inclination of the interference fringes on the tails of the multiple diffraction region is easily seen. This phenomenon corresponds completely to the computer simulations. PMID:26317194

  9. Peculiarities of section topograms for the multiple diffraction of X rays

    NASA Astrophysics Data System (ADS)

    Kohn, V. G.; Smirnova, I. A.

    2016-07-01

    The distortion of interference fringes on the section topograms of single crystal due to the multiple diffraction of X rays has been investigated. The cases of the 220 and 400 reflections in a silicon crystal in the form of a plate with a surface oriented normally to the [001] direction are considered both theoretically and experimentally. The same section topogram exhibits five cases of multiple diffraction at small azimuthal angles for the 400 reflection and Mo K α radiation, while the topogram for the 220 reflection demonstrates two cases of multiple diffraction. All these cases correspond to different combinations of reciprocal lattice vectors. Exact theoretical calculations of section topograms for the aforementioned cases of multiple diffraction have been performed for the first time. The section topograms exhibit two different distortion regions. The distortions in the central region of the structure are fairly complex and depend strongly on the azimuthal angle. In the tails of the multiple diffraction region, there is a shift of two-beam interference fringes, which can be observed even with a laboratory X-ray source.

  10. Imaging Whole Escherichia Coli Bacteria by Using Single-Particle X-Ray Diffraction

    SciTech Connect

    Miao, J.

    2004-06-04

    We report the first experimental recording, to our knowledge, of the diffraction pattern from intact Escherichia coli bacteria using coherent x-rays with a wavelength of 2 {angstrom}. By using the over-sampling phasing method, a real space image at a resolution of 30 nm was directly reconstructed from the diffraction pattern. An R factor used for characterizing the quality of the reconstruction was in the range of 5%, which demonstrated the reliability of the reconstruction process. The distribution of proteins inside the bacteria labeled with manganese oxide has been identified and this distribution confirmed by fluorescence microscopy images. Compared with lens-based microscopy, this diffraction-based imaging approach can examine thicker samples, such as whole cultured cells, in three dimensions with resolution limited only by radiation damage. Looking forward, the successful recording and reconstruction of diffraction patterns from biological samples reported here represent an important step toward the potential of imaging single biomolecules at near-atomic resolution by combining single-particle diffraction with x-ray free electron lasers.

  11. 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.

  12. Nondestructive evaluation of residual stress in short-fiber reinforced plastics by x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Tanaka, Keisuke; Tokoro, Syouhei; Akiniwa, Yoshiaki; Egami, Noboru

    2014-06-01

    The X-ray diffraction method is used to measure the residual stress in injection-molded plates of short-fiber reinforced plastics (SFRP) made of crystalline thermoplastics, polyphenylene sulphide (PPS), reinforced by carbon fibers with 30 mass%. Based on the orientation of carbon fibers, injection molded plates can be modeled as three-layered lamella where the core layer is sandwiched by skin layers. The stress in the matrix in the skin layer was measured using Cr-Kα radiation with the sin2Ψ method. Since the X-ray penetration depth is shallow, the state of stresses measured by X-rays in FRP can be assumed to be plane stress. The X-ray measurement of stress in carbon fibers was not possible because of high texture. A new method was proposed to evaluate the macrostress in SFRP from the measurement of the matrix stress. According to micromechanics analysis of SFRP, the matrix stresses in the fiber direction, σ1m, and perpendicular to the fiber direction, σ2m, and shear stress τ12m can be expressed as the functions of the applied (macro-) stresses, σ1A, σ2A , τ12A as follows: σ1m = α11σ1A +α12σ2A, σ2m = α21σ1A + α22σ2A, τ12m = α66τ12A, where α11 ,α12, α21, α22, α66 are stress-partitioning coefficients. Using skin-layer strips cut parallel, perpendicular and 45° to the molding direction, the stress in the matrix was measured under the uniaxial applied stress and the stress-partitioning coefficients of the above equations were determined. Once these relations are established, the macrostress in SFRP can be determined from the measurements of the matrix stresses by X-rays.

  13. 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.

  14. 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.

  15. 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.

  16. X-ray diffraction imaging--a multi-generational perspective.

    PubMed

    Harding, G

    2009-02-01

    A brief description is given of some applications of X-ray diffraction imaging (XDI) in security screening, including detection of narcotics and a wide range of explosives: organic (plastic) explosives, liquids, home-made explosives (HMEs) and special nuclear materials (SNMs). A Bayesian formulation of the "rare event scenario" is presented, allowing the probability to be quantified that an unlikely threat is indeed present when an uncertain detection system raises an alarm. Granted the utility of X-ray diffraction (XRD) as a significant screening modality for false-alarm resolution, the topic of its technological feasibility is addressed. It is shown that, in analogy to computed tomography, XDI permits a significant reduction to be achieved in measurement time per object volume element (voxel) compared with that of a classical X-ray diffractometer. This reduction can be accomplished by designing the XDI system to record energy-dispersive XRD profiles from many volume elements (object voxels) in parallel. A general scheme for designing "massively-parallel" (MP) XDI systems is presented. XDI configurations of the first generation (1 voxels(-1)), second generation (100 voxelss(-1)) and third generation (10(4) voxelss(-1)) are presented and discussed. Three alternative 3rd Generation XDI geometries, namely: direct fan-beam; parallel (waterfall) beam; and inverse fan-beam are compared with respect to technological realization. Directions for future development of XDI in screening applications are outlined. PMID:18805014

  17. Imaging live cell in micro-liquid enclosure by X-ray laser diffraction

    NASA Astrophysics Data System (ADS)

    Kimura, Takashi; Joti, Yasumasa; Shibuya, Akemi; Song, Changyong; Kim, Sangsoo; Tono, Kensuke; Yabashi, Makina; Tamakoshi, Masatada; Moriya, Toshiyuki; Oshima, Tairo; Ishikawa, Tetsuya; Bessho, Yoshitaka; Nishino, Yoshinori

    2014-01-01

    Emerging X-ray free-electron lasers with femtosecond pulse duration enable single-shot snapshot imaging almost free from sample damage by outrunning major radiation damage processes. In bioimaging, it is essential to keep the sample close to its natural state. Conventional high-resolution imaging, however, suffers from severe radiation damage that hinders live cell imaging. Here we present a method for capturing snapshots of live cells kept in a micro-liquid enclosure array by X-ray laser diffraction. We place living Microbacterium lacticum cells in an enclosure array and successively expose each enclosure to a single X-ray laser pulse from the SPring-8 Angstrom Compact Free-Electron Laser. The enclosure itself works as a guard slit and allows us to record a coherent diffraction pattern from a weakly-scattering submicrometre-sized cell with a clear fringe extending up to a 28-nm full-period resolution. The reconstructed image reveals living whole-cell structures without any staining, which helps advance understanding of intracellular phenomena.

  18. 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.

  19. 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.

  20. Object image correction using an X-ray dynamical diffraction Fraunhofer hologram.

    PubMed

    Balyan, Minas K

    2014-03-01

    Taking into account background correction and using Fourier analysis, a numerical method of an object image correction using an X-ray dynamical diffraction Fraunhofer hologram is presented. An example of the image correction of a cylindrical beryllium wire is considered. A background correction of second-order iteration leads to an almost precise reconstruction of the real part of the amplitude transmission coefficient and improves the imaginary part compared with that without a background correction. Using Fourier analysis of the reconstructed transmission coefficient, non-physical oscillations can be avoided. This method can be applied for the determination of the complex amplitude transmission coefficient of amplitude as well as phase objects, and can be used in X-ray microscopy.

  1. 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.

  2. 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.

  3. Use of x-ray fluorescence and diffraction techniques in studying ancient ceramics of Sri Lanka

    NASA Astrophysics Data System (ADS)

    Karunaratne, B. S. B.

    2012-07-01

    Ceramics were produced for centuries in Sri Lanka for various purposes. Ancient ceramic articles such as pottery, bricks, tiles, sewer pipes, etc, were made from naturally occurring raw materials. Use of X-ray fluorescence (XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) in characterizing of two ancient ceramic samples from two different archaeological sites in Sri Lanka is presented. The information obtained in this manner is used to figure out the ancient ceramic technology, particularly to learn about the raw materials used, the source of raw materials, processing parameters such as firing temperature or binders used in ceramic production. This information then can be used to explore the archaeometric background such as the nature and extent of cultural and technological interaction between different periods of history in Sri Lanka.

  4. 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

  5. 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.

  6. 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.

  7. 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.

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

    SciTech Connect

    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

    2013-09-15

    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 μm 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 μm 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-μm using X-ray free electron laser at BL3 of SACLA.

  9. A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

    SciTech Connect

    Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

    2015-09-26

    A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.

  10. Advanced combined application of micro-X-ray diffraction/micro-X-ray fluorescence with conventional techniques for the identification of pictorial materials from Baroque Andalusia paintings.

    PubMed

    Herrera, L K; Montalbani, S; Chiavari, G; Cotte, M; Solé, V A; Bueno, J; Duran, A; Justo, A; Perez-Rodriguez, J L

    2009-11-15

    The process of investigating paintings includes the identification of materials to solve technical and historical art questions, to aid in the deduction of the original appearance, and in the establishment of the chemical and physical conditions for adequate restoration and conservation. In particular, we have focused on the identification of several samples taken from six famous canvases painted by Pedro Atanasio Bocanegra, who created a very special collection depicting the life of San Ignacio, which is located in the church of San Justo y Pastor of Granada, Spain. The characterization of the inorganic and organic compounds of the textiles, preparation layers, and pictorial layers have been carried out using an XRD diffractometer, SEM observations, EDX spectrometry, FT-IR spectrometry (both in reflection and transmission mode), pyrolysis/gas chromatography/mass spectrometry and synchrotron-based micro-X-ray techniques. In this work, the advantages over conventional X-ray diffraction of using combined synchrotron-based micro-X-ray diffraction and micro-X-ray fluorescence in the identification of multi-layer paintings is demonstrated. PMID:19782194

  11. 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.

  12. 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.

  13. X-Ray Diffraction from Isolated and Strongly Aligned Gas-Phase Molecules with a Free-Electron Laser

    NASA Astrophysics Data System (ADS)

    Küpper, Jochen; Stern, Stephan; Holmegaard, Lotte; Filsinger, Frank; Rouzée, Arnaud; Rudenko, Artem; Johnsson, Per; Martin, Andrew V.; Adolph, Marcus; Aquila, Andrew; Bajt, Saša; Barty, Anton; Bostedt, Christoph; Bozek, John; Caleman, Carl; Coffee, Ryan; Coppola, Nicola; Delmas, Tjark; Epp, Sascha; Erk, Benjamin; Foucar, Lutz; Gorkhover, Tais; Gumprecht, Lars; Hartmann, Andreas; Hartmann, Robert; Hauser, Günter; Holl, Peter; Hömke, Andre; Kimmel, Nils; Krasniqi, Faton; Kühnel, Kai-Uwe; Maurer, Jochen; Messerschmidt, Marc; Moshammer, Robert; Reich, Christian; Rudek, Benedikt; Santra, Robin; Schlichting, Ilme; Schmidt, Carlo; Schorb, Sebastian; Schulz, Joachim; Soltau, Heike; Spence, John C. H.; Starodub, Dmitri; Strüder, Lothar; Thøgersen, Jan; Vrakking, Marc J. J.; Weidenspointner, Georg; White, Thomas A.; Wunderer, Cornelia; Meijer, Gerard; Ullrich, Joachim; Stapelfeldt, Henrik; Rolles, Daniel; Chapman, Henry N.

    2014-02-01

    We report experimental results on x-ray diffraction of quantum-state-selected and strongly aligned ensembles of the prototypical asymmetric rotor molecule 2,5-diiodobenzonitrile using the Linac Coherent Light Source. The experiments demonstrate first steps toward a new approach to diffractive imaging of distinct structures of individual, isolated gas-phase molecules. We confirm several key ingredients of single molecule diffraction experiments: the abilities to detect and count individual scattered x-ray photons in single shot diffraction data, to deliver state-selected, e.g., structural-isomer-selected, ensembles of molecules to the x-ray interaction volume, and to strongly align the scattering molecules. Our approach, using ultrashort x-ray pulses, is suitable to study ultrafast dynamics of isolated molecules.

  14. Kinetic products in coordination networks: ab initio X-ray powder diffraction analysis.

    PubMed

    Martí-Rujas, Javier; Kawano, Masaki

    2013-02-19

    Porous coordination networks are materials that maintain their crystal structure as molecular "guests" enter and exit their pores. They are of great research interest with applications in areas such as catalysis, gas adsorption, proton conductivity, and drug release. As with zeolite preparation, the kinetic states in coordination network preparation play a crucial role in determining the final products. Controlling the kinetic state during self-assembly of coordination networks is a fundamental aspect of developing further functionalization of this class of materials. However, unlike for zeolites, there are few structural studies reporting the kinetic products made during self-assembly of coordination networks. Synthetic routes that produce the necessary selectivity are complex. The structural knowledge obtained from X-ray crystallography has been crucial for developing rational strategies for design of organic-inorganic hybrid networks. However, despite the explosive progress in the solid-state study of coordination networks during the last 15 years, researchers still do not understand many chemical reaction processes because of the difficulties in growing single crystals suitable for X-ray diffraction: Fast precipitation can lead to kinetic (metastable) products, but in microcrystalline form, unsuitable for single crystal X-ray analysis. X-ray powder diffraction (XRPD) routinely is used to check phase purity, crystallinity, and to monitor the stability of frameworks upon guest removal/inclusion under various conditions, but rarely is used for structure elucidation. Recent advances in structure determination of microcrystalline solids from ab initio XRPD have allowed three-dimensional structure determination when single crystals are not available. Thus, ab initio XRPD structure determination is becoming a powerful method for structure determination of microcrystalline solids, including porous coordination networks. Because of the great interest across scientific

  15. 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

  16. Ab initio simulation of diffractometer instrumental function for high-resolution X-ray diffraction1

    PubMed Central

    Mikhalychev, Alexander; Benediktovitch, Andrei; Ulyanenkova, Tatjana; Ulyanenkov, Alex

    2015-01-01

    Modeling of the X-ray diffractometer instrumental function for a given optics configuration is important both for planning experiments and for the analysis of measured data. A fast and universal method for instrumental function simulation, suitable for fully automated computer realization and describing both coplanar and noncoplanar measurement geometries for any combination of X-ray optical elements, is proposed. The method can be identified as semi-analytical backward ray tracing and is based on the calculation of a detected signal as an integral of X-ray intensities for all the rays reaching the detector. The high speed of calculation is provided by the expressions for analytical integration over the spatial coordinates that describe the detection point. Consideration of the three-dimensional propagation of rays without restriction to the diffraction plane provides the applicability of the method for noncoplanar geometry and the accuracy for characterization of the signal from a two-dimensional detector. The correctness of the simulation algorithm is checked in the following two ways: by verifying the consistency of the calculated data with the patterns expected for certain simple limiting cases and by comparing measured reciprocal-space maps with the corresponding maps simulated by the proposed method for the same diffractometer configurations. Both kinds of tests demonstrate the agreement of the simulated instrumental function shape with the measured data. PMID:26089760

  17. 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.

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

    DOE PAGES

    Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; et al

    2016-04-12

    Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

  19. An x-ray diffraction microscope at the Advanced Photon Source.

    SciTech Connect

    Cai, Z.; Lai, B.; Xiao, Y.; Xu, S.; Experimental Facilities Division

    2003-03-01

    An instrument capable of high-resolution spatial mapping of crystallographic phase, lattice strain, and lattice distortion with x-rays of energies from 6 to 20 keV has been constructed and commissioned at the 2-ID-D. beamline of the Advanced Photon Source. By integrating a hard x-ray Fresnel zone-plate-based microprobe and a six-circle diffractometer, the instrument provides a spatial resolution better than 250 nm, angular resolution of diffractometer circles better than 0.000, angular repeatability of the sample circles better than 0.001 degrees, and almost full accessibility to the entire reciprocal space. The microprobe employs 10 cm and 40 cm (focal length at 8 keV) zone plates to provide high and moderate focusing power, respectively. Each zone-plate assembly has two identical zone plates stacked together to provide higher efficiency for higher energy (up to 30 keV) applications. The x-ray diffraction microscope has been applied to studies of the microstructures of bicrystal-supported magnetoresistive films.

  20. 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.

  1. 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.

  2. Investigation of the neptunium-zirconium system by X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Gensini, Michel M.; Haire, Richard G.; Gibson, John K.

    1994-10-01

    X-ray powder diffraction analysis at 25 C has been used to further characterize the Np-Zr phase diagram. We have studied a variety of Np-Zr aggregate compositions obtained by different preparative methods, including arc melting of the components. For the materials at ambient temperature, obtained by either slow cooling or quenching from elevated temperatures, we observed one or more of the following product phases: alpha-Np, alpha-Zr, NpZr2 and one new phase. The last was interpreted tentatively to be either Np4Zr or Np6Zr. Calculations based on the X-ray data suggested a limited solubility of Np in alpha-Zr and an even lower solubility of Zr in alpha-Np. The X-ray data for the NpZr2 phase showed that it possesses hexagonal symmetry and is isostructural with UZr2 and PuZr2. Annealing of Np-Zr composites at selected temperatures did not enhance the formation of NpZr2.

  3. 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.

  4. 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.

  5. Characterization of GaAs/Si interface structure by x-ray diffraction

    SciTech Connect

    Specht, E.D.; Ice, G.E.; Peters, C.J.; Sparks, C.J. ); Lucas, N.; Zhu, X.-M.; Moret, R.; Morkoc, H. )

    1990-01-01

    By measuring the intensity profiles along the crystal truncation rods of a Si(001) substrate, we obtain the depth sensitivity necessary for x-ray diffraction measurements of the structure of its interface with a thick GaAs overlayer which is epitaxial to, but not in registry with the substrate. By comparing the diffraction with a model based on a grid of misfit dislocations, we find that the atoms at the interface have a root mean square displacement of 1.09 {plus minus} 0.1 {angstrom} from this ideal structure, and that the interface has a roughness of 2.9 {plus minus} 1 {angstrom}. The diffraction indicates an anomalously small strain perpendicular to the interface in the GaAs near the interface. 19 refs., 4 figs.

  6. 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.

  7. Spectral X-Ray Diffraction using a 6 Megapixel Photon Counting Array Detector

    PubMed Central

    Muir, Ryan D.; Pogranichniy, Nicholas R.; Muir, J. Lewis; Sullivan, Shane Z.; Battaile, Kevin P.; Mulichak, Anne M.; Toth, Scott J.; Keefe, Lisa J.; Simpson, Garth J.

    2016-01-01

    Pixel-array array detectors allow single-photon counting to be performed on a massively parallel scale, with several million counting circuits and detectors in the array. Because the number of photoelectrons produced at the detector surface depends on the photon energy, these detectors offer the possibility of spectral imaging. In this work, a statistical model of the instrument response is used to calibrate the detector on a per-pixel basis. In turn, the calibrated sensor was used to perform separation of dual-energy diffraction measurements into two monochromatic images. Targeting applications include multi-wavelength diffraction to aid in protein structure determination and X-ray diffraction imaging. PMID:27041789

  8. Data preparation and evaluation techniques for x-ray diffraction microscopy

    DOE PAGES

    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

  9. Structural characterization of the N-terminal part of the MERS-CoV nucleocapsid by X-ray diffraction and small-angle X-ray scattering.

    PubMed

    Papageorgiou, Nicolas; Lichière, Julie; Baklouti, Amal; Ferron, François; Sévajol, Marion; Canard, Bruno; Coutard, Bruno

    2016-02-01

    The N protein of coronaviruses is a multifunctional protein that is organized into several domains. The N-terminal part is composed of an intrinsically disordered region (IDR) followed by a structured domain called the N-terminal domain (NTD). In this study, the structure determination of the N-terminal region of the MERS-CoV N protein via X-ray diffraction measurements is reported at a resolution of 2.4 Å. Since the first 30 amino acids were not resolved by X-ray diffraction, the structural study was completed by a SAXS experiment to propose a structural model including the IDR. This model presents the N-terminal region of the MERS-CoV as a monomer that displays structural features in common with other coronavirus NTDs. PMID:26894667

  10. UV and X-ray variability of the narrow-line Seyfert 1 galaxy Ark 564

    NASA Astrophysics Data System (ADS)

    Ezhikode, Savithri H.; Dewangan, Gulab C.; Misra, Ranjeev; Tripathi, Shruti; Sajeeth Philip, Ninan; Kembhavi, Ajit K.

    2016-07-01

    We analyze eight XMM-Newton observations of the bright Narrow Line Seyfert 1 galaxy Arakelian 564 (Ark 564). These observations, separated by ∼ 6 days, allow us to look for correlations between the simultaneous ultraviolet (UV) emission (from the Optical Monitor) with not only the X-ray flux but also with different X-ray spectral parameters. The X-ray spectra from all the observations are found to be adequately fitted by a double Comptonization model where the soft excess and the hard X-ray power law are represented by thermal Comptonization in a low temperature plasma and hot corona, respectively. Apart from the fluxes of each component, the hard X-ray power law index is found to be variable. These results suggest that the variability is associated with changes in the geometry of the inner region. The UV emission is found to be variable and well correlated with the high energy index while the correlations with the fluxes of each component are found to be weaker. Using viscous timescale arguments we rule out the possibility that the UV variation is due to the fluctuating accretion rate in the outer disk. If the UV variation is driven by X-ray reprocessing, then our results indicate that the strength of the X-ray reprocessing depends more on the geometry of the X-ray producing inner region rather than on the X-ray luminosity alone.

  11. 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.

  12. Purification, crystallization and preliminary X-ray diffraction analysis of royal palm tree (Roystonea regia) peroxidase

    SciTech Connect

    Watanabe, Leandra; Nascimento, Alessandro S.; Zamorano, Laura S.; Shnyrov, Valery L.; Polikarpov, Igor

    2007-09-01

    The purification, crystallization, X-ray diffraction data acquisition and molecular-replacement results of royal palm tree (R. regia) peroxidase are described. Royal palm tree peroxidase (RPTP), which was isolated from Roystonea regia leaves, has an unusually high stability that makes it a promising candidate for diverse applications in industry and analytical chemistry [Caramyshev et al. (2005 ▶), Biomacromolecules, 6, 1360–1366]. Here, the purification and crystallization of this plant peroxidase and its X-ray diffraction data collection are described. RPTP crystals were obtained by the hanging-drop vapour-diffusion method and diffraction data were collected to a resolution of 2.8 Å. The crystals belong to the trigonal space group P3{sub 1}21, with unit-cell parameters a = b = 116.83, c = 92.24 Å, and contain one protein molecule per asymmetric unit. The V{sub M} value and solvent content are 4.07 Å{sup 3} Da{sup −1} and 69.8%, respectively.

  13. Estimating nanoscale deformation in bone by X-ray diffraction imaging method.

    PubMed

    Tadano, Shigeru; Giri, Bijay; Sato, Takuya; Fujisaki, Kazuhiro; Todoh, Masahiro

    2008-01-01

    Knowledge of internal stress-strain in bone tissue is important for clinical diagnosis and remedies. The inorganic mineral phase of apatite crystals in bone composite, because of its crystalline nature, provides a reliable way of measurement through X-ray diffraction system. Use of two-dimensional detector, imaging plate (IP), is considered to expedite the process with much more information, hence, is widely applied in the study of organization, stress, strain, etc. for crystalline substance. The distortion of Debye rings in the image obtained by IP can be directly related to the deformation in lattice plane of the crystals. Since X-ray diffraction method involves measurement at nano-level, proper focus on the extraction of data and corresponding analysis is needed. In the current work, we considered weighted average value of intensity to locate radius vectors along azimuthal direction in the diffracted rings from the primary array of digital data in steps of pixels. The widely applied approaches for profile shift measurement--peak shift and full width at half maximum (FWHM) of a peak, and shift of center of gravity of profile--were compared with a new concept of segmental shift (SS) proposed previously by the authors. We observed reliable and effective outcomes with higher precision in the consideration of SS while using IP as a detector. Our approach in this work for intensity integration and radius vector positioning especially add precision in such applications.

  14. Picosecond X-Ray Diffraction from Laser-Shocked Copper and Iron

    SciTech Connect

    Wark, J. S.; Hawreliak, J.; Higginbotham, A.; Rosolankova, K.; Sheppard, J.; Belak, J. F.; Collins, G. W.; Colvin, J. D.; Duchaineau, M.; Eggert, J. H.; Kalantar, D. H.; Lorenzana, H. E.; Remington, B. A.; Rudd, R. E.; Stolken, J. S.; Davies, H. M.; Germann, T. C.; Holian, B. L.; Kadau, K.; Lomdahl, P. S.

    2006-07-28

    In situ X-ray diffraction allows the determination of the structure of transient states of matter. We have used laser-plasma generated X-rays to study how single crystals of metals (copper and iron) react to uniaxial shock compression. We find that copper, as a face-centred-cubic material, allows rapid generation and motion of dislocations, allowing close to hydrostatic conditions to be achieved on sub-nanosecond timescales. Detailed molecular dynamics calculations provide novel information about the process, and point towards methods whereby the dislocation density might be measured during the passage of the shock wave itself. We also report on recent experiments where we have obtained diffraction images from shock-compressed single-crystal iron. The single crystal sample transforms to the hcp phase above a critical pressure, below which it appears to be uniaxially compressed bcc, with no evidence of plasticity. Above the transition threshold, clear evidence for the hcp phase can be seen in the diffraction images, and via a mechanism that is also consistent with recent multi- million atom molecular dynamics simulations that use the Voter- Chen potential. We believe these data to be of import, in that they constitute the first conclusive in situ evidence of the transformed structure of iron during the passage of a shock wave.

  15. X-ray diffraction recording from single axonemes of eukaryotic flagella.

    PubMed

    Nishiura, Masaya; Toba, Shiori; Takao, Daisuke; Miyashiro, Daisuke; Sakakibara, Hitoshi; Matsuo, Tatsuhito; Kamimura, Shinji; Oiwa, Kazuhiro; Yagi, Naoto; Iwamoto, Hiroyuki

    2012-06-01

    We report the first X-ray diffraction patterns recorded from single axonemes of eukaryotic flagella with a diameter of only <0.2 μm, by using the technique of cryomicrodiffraction. A spermatozoon isolated from the testis of a fruit fly, Drosophila melanogaster, either intact or demembranated, was mounted straight in a glass capillary, quickly frozen and its 800-μm segment was irradiated end-on with intense synchrotron radiation X-ray microbeams (diameter, ~2 μm) at 74 K. Well-defined diffraction patterns were recorded, consisting of a large number of isolated reflection spots, extending up to 1/5 nm(-1). These reflections showed a tendency to peak every 20°, i.e., the patterns had features of an 18-fold rotational symmetry as expected from the 9-fold rotational symmetry of axonemal structure. This means that the axonemes remain untwisted, even after the manual mounting procedure. The diffraction patterns were compared with the results of model calculations based on a published electron micrograph of the Drosophila axoneme. The comparison provided information about the native state of axoneme, including estimates of axonemal diameter, interdoublet spacing, and masses of axonemal components relative to those of microtubules (e.g., radial spokes, dynein arms, and proteins associated with accessory singlet microtubules). When combined with the genetic resource of Drosophila, the technique presented here will serve as a powerful tool for studying the structure-function relationship of eukaryotic flagella in general. PMID:22503702

  16. X-ray diffraction recording from single axonemes of eukaryotic flagella.

    PubMed

    Nishiura, Masaya; Toba, Shiori; Takao, Daisuke; Miyashiro, Daisuke; Sakakibara, Hitoshi; Matsuo, Tatsuhito; Kamimura, Shinji; Oiwa, Kazuhiro; Yagi, Naoto; Iwamoto, Hiroyuki

    2012-06-01

    We report the first X-ray diffraction patterns recorded from single axonemes of eukaryotic flagella with a diameter of only <0.2 μm, by using the technique of cryomicrodiffraction. A spermatozoon isolated from the testis of a fruit fly, Drosophila melanogaster, either intact or demembranated, was mounted straight in a glass capillary, quickly frozen and its 800-μm segment was irradiated end-on with intense synchrotron radiation X-ray microbeams (diameter, ~2 μm) at 74 K. Well-defined diffraction patterns were recorded, consisting of a large number of isolated reflection spots, extending up to 1/5 nm(-1). These reflections showed a tendency to peak every 20°, i.e., the patterns had features of an 18-fold rotational symmetry as expected from the 9-fold rotational symmetry of axonemal structure. This means that the axonemes remain untwisted, even after the manual mounting procedure. The diffraction patterns were compared with the results of model calculations based on a published electron micrograph of the Drosophila axoneme. The comparison provided information about the native state of axoneme, including estimates of axonemal diameter, interdoublet spacing, and masses of axonemal components relative to those of microtubules (e.g., radial spokes, dynein arms, and proteins associated with accessory singlet microtubules). When combined with the genetic resource of Drosophila, the technique presented here will serve as a powerful tool for studying the structure-function relationship of eukaryotic flagella in general.

  17. Continuous-scan capability at SSRL and applications to X-ray diffraction.

    PubMed

    Li, Chunlei; Kiss, Andrew M; Van Campen, Douglas G; Garachtchenko, Alex; Kolotovsky, Yuriy; Stone, Kevin; Xu, Yahong; Zhang, Wenjun; Corbett, Jeff

    2016-07-01

    Typical X-ray diffraction measurements are made by moving a detector to discrete positions in space and then measuring the signal at each stationary position. This step-scanning method can be time-consuming, and may induce vibrations in the measurement system when the motors are accelerated and decelerated at each position. Furthermore, diffraction information between the data points may be missed unless a fine step-scanning is used, which further increases the total measurement time. To utilize beam time efficiently, the motor acceleration and deceleration time should be minimized, and the signal-to-noise ratio should be maximized. To accomplish this, an integrated continuous-scan system was developed at the Stanford Synchrotron Radiation Lightsource (SSRL). The continuous-scan system uses an in-house integrated motor controller system and counter/timer electronics. SPEC software is used to control both the hardware and data acquisition systems. The time efficiency and repeatability of the continuous-scan system were tested using X-ray diffraction from a ZnO powder and compared with the step-scan technique. Advantages and limitations of the continuous-scan system and a demonstration of variable-velocity continuous scan are discussed. PMID:27359139

  18. 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 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å 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

  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 Å. HscA is a constitutively expressed Hsp70 that interacts with the iron–sulfur cluster assembly protein IscU. Crystals of a truncated form of HscA (52 kDa; residues 17–505) 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 Å. 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 Å, 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. Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

    DOEpatents

    Green, Lanny A.; Heck, Jr., Joaquim L.

    1987-01-01

    A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

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

    DOEpatents

    Smither, Robert K.

    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.

  3. 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.

  4. Darwin's approach to X-ray diffraction on lateral crystalline structures.

    PubMed

    Punegov, Vasily I; Kolosov, Sergey I; Pavlov, Konstantin M

    2014-01-01

    Darwin's dynamical theory of X-ray diffraction is extended to the case of lateral (i.e., having a finite length in the lateral direction) crystalline structures. This approach allows one to calculate rocking curves as well as reciprocal-space maps for lateral crystalline structures having a rectangular cross section. Numerical modelling is performed for these structures with different lateral sizes. It is shown that the kinematical approximation is valid for thick crystalline structures having a small length in the lateral direction. PMID:24419171

  5. 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

  6. Snapshot full-volume coded aperture x-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Greenberg, Joel A.; Brady, David J.

    2016-05-01

    X-ray diffraction tomography (XRDT) is a well-established technique that makes it possible to identify the material composition of an object throughout its volume. We show that using coded apertures to structure the measured scatter signal gives rise to a family of imaging architectures than enables snapshot XRDT in up to 4-dimensions. We consider pencil, fan, and cone beam snapshot XRDT and show results from both experimental and simulation-based studies. We find that, while lower-dimensional systems typically result in higher imaging fidelity, higher-dimensional systems can perform adequately for a specific task at orders of magnitude faster scan times.

  7. Load transfer in bovine plexiform bone determined by synchrotron x-ray diffraction.

    SciTech Connect

    Akhtar, R.; Daymond, M.; Almer, J.; Mummery, P.; The Univ. of Manchester; Queen's Univ.

    2008-02-01

    High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.

  8. Quantitative X-ray diffraction analysis of oxides formed on superalloys

    NASA Technical Reports Server (NTRS)

    Garlick, R. G.

    1972-01-01

    Methods were developed for quantitative analysis by X-ray diffraction of the oxides Al2O3, NiO, Cr2O3, CoO, and CoCr2O4 within a standard deviation of about 10 percent of the weight fraction reported or within 1 percent absolute. These error limits assume that the sample oxides are well characterized and that the physiochemical structure of the oxides in the samples are identical with those in the synthesized standards. Results are given for the use of one of the techniques in the analysis of spalls from a series of oxidation tests of the cobalt base alloy WI-52.

  9. Aortic valvular tophus: identification by X-ray diffraction of urate and calcium phosphates.

    PubMed Central

    Gawoski, J M; Balogh, K; Landis, W J

    1985-01-01

    A typical gouty tophus with birefringent, dichroic, needle shaped crystals was found in a resected calcified aortic valve on routine histological examination. The patient, an elderly man, had a long history of gout. X-ray diffraction confirmed the presence of sodium acid urate monohydrate and identified hydroxyapatite and whitlockite in the accompanying dystrophic calcification of the aortic valves. Previous reports indicate that gouty tophi of the cardiac valves are rare: of the nine cases reported, eight occurred in the mitral valve. Images PMID:4031099

  10. 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.

  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. Structural characterization of phosphatidylcholine-diacylglycerol system by neutron scattering and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Takahashi, H.; Nagura, K.; Imai, M.; Matsushita, Y.; Hatta, I.

    Diacylglycerol (DAG) is recognized as one of the most important lipids for biological functions of cell membranes. In order to understand the functions of DAG, it is indispensable to study the effect of DAG on phosphatidylcholine (PC), which is a main lipid component of biomembranes. Here we report neutron-scattering data of sonicated PC/DAG vesicles and X-ray-diffraction data of oriented PC/DAG multilamellar systems. These data imply that addition of DAG induces a change in the tilt angle of lipid molecules and that, as a result, an increase of the membrane thickness is induced.

  13. MEASURING THE PLASTIC RESPONSE IN POLYCRSYTALLINE MATERIALS USING IN-SITU X-RAY DIFFRACTION

    SciTech Connect

    Hawreliak, J; Butterfield, M; El-Dasher, B; McNaney, J; Lorenzana, H

    2008-10-01

    The insight provided by ultra-fast lattice level measurements during high strain rate high pressure experiments is key to understanding kinetic material properties like plasticity. In-situ x-ray diffraction provides a diagnostic technique which can be used to study the governing physical phenomena of plasticity at the relevant time and spatial scale. Here we discuss the recent development of a geometry capable of investigating plasticity in polycrystalline foils. We also present some preliminary data of investigations into shock compressed rolled copper foils.

  14. Atomic motion of resonantly vibrating quartz crystal visualized by time-resolved X-ray diffraction

    SciTech Connect

    Aoyagi, Shinobu; Osawa, Hitoshi; Sugimoto, Kunihisa; Fujiwara, Akihiko

    2015-11-16

    Transient atomic displacements during a resonant thickness-shear vibration of AT-cut α-quartz are revealed by time-resolved X-ray diffraction under an alternating electric field. The lattice strain resonantly amplified by the alternating electric field is ∼10{sup 4} times larger than that induced by a static electric field. The resonantly amplified lattice strain is achieved by fast displacements of oxygen anions and collateral resilient deformation of Si−O−Si angles bridging rigid SiO{sub 4} tetrahedra, which efficiently transduce electric energy into elastic energy.

  15. 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.

  16. Phasing of coherent femtosecond X-ray diffraction from size-varying nanocrystals.

    PubMed

    Spence, John C H; Kirian, Richard A; Wang, Xiaoyu; Weierstall, Uwe; Schmidt, Kevin E; White, Thomas; Barty, Anton; Chapman, Henry N; Marchesini, Stefano; Holton, James

    2011-02-14

    The scattering between Bragg reflections from nanocrystals is used to aid solution of the phase problem. We describe a method for reconstructing the charge density of a typical molecule within a single unit cell, if sufficiently finely-sampled "snap-shot" diffraction data (as provided a free-electron X-ray laser) are available from many nanocrystals of different sizes lying in random orientations. By using information on the particle-size distribution within the patterns, this digital method succeeds, using all the data, without knowledge of the distribution of particle size or requiring atomic-resolution data.

  17. Anharmonic lattice dynamics in germanium measured with ultrafast x-ray diffraction.

    PubMed

    Cavalleri, A; Siders, C W; Brown, F L; Leitner, D M; Tóth, C; Squier, J A; Barty, C P; Wilson, K R; Sokolowski-Tinten, K; Horn Von Hoegen, M; von der Linde, D; Kammler, M

    2000-07-17

    Damping of impulsively generated coherent acoustic oscillations in a femtosecond laser-heated thin germanium film is measured as a function of fluence by means of ultrafast x-ray diffraction. By simultaneously measuring picosecond strain dynamics in the film and in the unexcited silicon substrate, we separate anharmonic damping from acoustic transmission through the buried interface. The measured damping rate and its dependence on the calculated temperature of the thermal bath is consistent with estimated four-body, elastic dephasing times (T2) for 7-GHz longitudinal acoustic phonons in germanium.

  18. Phasing of coherent femtosecond X-ray diffraction from size-varying nanocrystals.

    PubMed

    Spence, John C H; Kirian, Richard A; Wang, Xiaoyu; Weierstall, Uwe; Schmidt, Kevin E; White, Thomas; Barty, Anton; Chapman, Henry N; Marchesini, Stefano; Holton, James

    2011-02-14

    The scattering between Bragg reflections from nanocrystals is used to aid solution of the phase problem. We describe a method for reconstructing the charge density of a typical molecule within a single unit cell, if sufficiently finely-sampled "snap-shot" diffraction data (as provided a free-electron X-ray laser) are available from many nanocrystals of different sizes lying in random orientations. By using information on the particle-size distribution within the patterns, this digital method succeeds, using all the data, without knowledge of the distribution of particle size or requiring atomic-resolution data. PMID:21369108

  19. Discovery of an X-ray Violently Variable Broad Absorption Line Quasar

    NASA Technical Reports Server (NTRS)

    Ghosh, Kajal K.; Gutierrez, Carlos M.; Punsly, Brian; Chevallier, Loic; Goncalves, Anabela C.

    2006-01-01

    In this letter, we report on a quasar that is violently variable in the X-rays, XVV. It is also a broad absorption line quasar (BALQSO) that exhibits both high ionization and low ionization UV absorption lines (LoBALQSO). It is very luminous in the X-rays (approximately 10(exp 46) ergs s(sup -l) over the entire X-ray band). Surprisingly, this does not over ionize the LoBAL outflow. The X-rays vary by a factor of two within minutes in the quasar rest frame, which is shorter than 1/30 of the light travel time across a scale length equal to the black hole radius. We concluded that the X-rays are produced in a relativistic jet beamed toward earth in which variations in the Doppler enhancement produce the XVV behavior.

  20. X-ray Spectroscopy of the most extreme Balmer-line disk-emission AGN

    NASA Astrophysics Data System (ADS)

    Eracleous, Michael

    2005-10-01

    We propose to obtain simultaneous X-ray and UV observations of the most extreme AGN with double-peaked Balmer emission lines (FWHM > 19000km/s). We will use the XMM-Newton data to measure their X-ray spectral shapes and construct spectral energy distributions. We will combine these with measurements of the optical emission line profiles (from simultaneous HET observations) and luminosities to (a) test models for illumination of the outer disk by the central X-ray source, (b) test models for the structure of the inner accretion disk (radiatively inefficient accretion vs. standard disk), and (c) compare the X-ray-to-optical properties of these broadest Balmer-line objects to those of broad and narrow line AGN to test models for the origin of the low-ionization broad lines.

  1. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

    SciTech Connect

    Szlachetko, J.; Nachtegaal, M.; Boni, E. de; Willimann, M.; Safonova, O.; Sa, J.; Smolentsev, G.; Szlachetko, M.; Bergamaschi, A.; Schmitt, B.; David, C.; Luecke, A.; Bokhoven, J. A. van; Dousse, J.-Cl.; Hoszowska, J.; Kayser, Y.; Jagodzinski, P.

    2012-10-15

    We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

  2. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies.

    PubMed

    Szlachetko, J; Nachtegaal, M; de Boni, E; Willimann, M; Safonova, O; Sa, J; Smolentsev, G; Szlachetko, M; van Bokhoven, J A; Dousse, J-Cl; Hoszowska, J; Kayser, Y; Jagodzinski, P; Bergamaschi, A; Schmitt, B; David, C; Lücke, A

    2012-10-01

    We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

  3. Micro-X-ray diffraction assessment of shock stage in enstatite chondrites

    NASA Astrophysics Data System (ADS)

    Izawa, Matthew R. M.; Flemming, Roberta L.; Banerjee, Neil R.; McCausland, Philip J. A.

    2011-05-01

    A new method for assessing the shock stage of enstatite chondrites has been developed, using in situ micro-X-ray diffraction (μXRD) to measure the full width at half maximum (FWHMχ) of peak intensity distributed along the direction of the Debye rings, or chi angle (χ), corresponding to individual lattice reflections in two-dimensional XRD patterns. This μXRD technique differs from previous XRD shock characterization methods: it does not require single crystals or powders. In situ μXRD has been applied to polished thin sections and whole-rock meteorite samples. Three frequently observed orthoenstatite reflections were measured: (020), (610), and (131); these were selected as they did not overlap with diffraction lines from other phases. Enstatite chondrites are commonly fine grained, stained or darkened by weathering, shock-induced oxidation, and metal/sulfide inclusions; furthermore, most E chondrites have little olivine or plagioclase. These characteristics inhibit transmitted-light petrography, nevertheless, shock stages have been assigned MacAlpine Hills (MAC) 02837 (EL3) S3, Pecora Escarpment (PCA) 91020 (EL3) S5, MAC 02747 (EL4) S4, Thiel Mountains (TIL) 91714 (EL5) S2, Allan Hills (ALHA) 81021 (EL6) S2, Elephant Moraine (EET) 87746 (EH3) S3, Meteorite Hills (MET) 00783 (EH4) S4, EET 96135 (EH4-5) S2, Lewis Cliff (LEW) 88180 (EH5) S2, Queen Alexandra Range (QUE) 94204 (EH7) S2, LaPaz Icefield (LAP) 02225 (EH impact melt) S1; for the six with published shock stages, there is agreement with the published classification. FWHMχ plotted against petrographic shock stage demonstrates positive linear correlation. FWHMχ ranges corresponding to shock stages were assigned as follows: S1 < 0.7°, S2 = 0.7-1.2°, S3 = 1.2-2.3°, S4 = 2.3-3.5°, S5 > 3.5°, S6—not measured. Slabs of Abee (EH impact-melt breccia), and Northwest Africa (NWA) 2212 (EL6) were examined using μXRD alone; FWHMχ values place both in the S2 range, consistent with literature values. Micro

  4. Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA.

    PubMed

    Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

    2016-07-01

    Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed. PMID:27359147

  5. TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA.

    PubMed

    Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

    2016-05-01

    Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens. PMID:27250394

  6. TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

    NASA Astrophysics Data System (ADS)

    Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

    2016-05-01

    Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.

  7. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies

    SciTech Connect

    Zucchini, F.; Chauvin, C.; Combes, P.; Sol, D.; Loyen, A.; Roques, B.; Grunenwald, J.; Bland, S. N.

    2015-03-15

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2–5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium.

  8. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies.

    PubMed

    Zucchini, F; Bland, S N; Chauvin, C; Combes, P; Sol, D; Loyen, A; Roques, B; Grunenwald, J

    2015-03-01

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2-5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium. PMID:25832229

  9. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies

    NASA Astrophysics Data System (ADS)

    Zucchini, F.; Bland, S. N.; Chauvin, C.; Combes, P.; Sol, D.; Loyen, A.; Roques, B.; Grunenwald, J.

    2015-03-01

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2-5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium.

  10. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies.

    PubMed

    Zucchini, F; Bland, S N; Chauvin, C; Combes, P; Sol, D; Loyen, A; Roques, B; Grunenwald, J

    2015-03-01

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2-5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium.

  11. Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

    SciTech Connect

    Nam, Daewoong; Park, Jaehyun; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong; Gallagher-Jones, Marcus

    2013-11-15

    This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10{sup −2} Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

  12. Strength and structural phase transitions of gadolinium at high pressure from radial X-ray diffraction

    SciTech Connect

    Xiong, Lun Liu, Jing; Bai, Ligang; Li, Xiaodong; Lin, Chuanlong; Lin, Jung-Fu

    2014-12-28

    Lattice strength and structural phase transitions of gadolinium (Gd) were determined under nonhydrostatic compression up to 55 GPa using an angle-dispersive radial x-ray diffraction technique in a diamond-anvil cell at room temperature. Three new phases of fcc structure, dfcc structure, and new monoclinic structure were observed at 25 GPa, 34 GPa, and 53 GPa, respectively. The radial x-ray diffraction data yield a bulk modulus K{sub 0} = 36(1) GPa with its pressure derivate K{sub 0}′ = 3.8(1) at the azimuthal angle between the diamond cell loading axis and the diffraction plane normal and diffraction plane ψ = 54.7°. With K{sub 0}′ fixed at 4, the derived K{sub 0} is 34(1) GPa. In addition, analysis of diffraction data with lattice strain theory indicates that the ratio of differential stress to shear modulus (t/G) ranges from 0.011 to 0.014 at pressures of 12–55 GPa. Together with estimated high-pressure shear moduli, our results show that Gd can support a maximum differential stress of 0.41 GPa, while it starts to yield to plastic deformation at 16 GPa under uniaxial compression. The yield strength of Gd remains approximately a constant with increasing pressure, and reaches 0.46 GPa at 55 GPa.

  13. Ionised Iron Lines in X-ray Reflection Spectra

    NASA Astrophysics Data System (ADS)

    Ballantyne, D. R.; Ross, R. R.; Fabian, A. C.

    2000-10-01

    We present results from new calculations of the reflected X-ray spectrum from ionised accretion disks in Active Galactic Nuclei (AGN). These calculations improve on our previous models by including the condition of hydrostatic balance in the vertical direction, following the work of Nayakshin, Kazanas & Kallman (2000). Our results show that, for gas pressure dominated accretion discs, ionised iron features are found in the reflection spectrum over a range of conditions. We also explore extending our results into radiation pressure dominated discs, and discuss the limitations of the current models.

  14. Time-resolved x-ray diffraction and calorimetric studies at low scan rates

    PubMed Central

    Yao, Haruhiko; Hatta, Ichiro; Koynova, Rumiana; Tenchov, Boris

    1992-01-01

    The phase transitions of dipalmitoylphosphatidylethanolamine (DPPE) in excess water have been examined by low-angle time-resolved x-ray diffraction and calorimetry at low scan rates. The lamellar subgel/lamellar liquid-crystalline (Lc → Lα), lamellar gel/lamellar liquid-crystalline (Lβ → Lα), and lamellar liquid-crystalline/lamellar gel (Lα → Lβ) phase transitions proceed via coexistence of the initial and final phases with no detectable intermediates at scan rates 0.1 and 0.5°C/min. At constant temperature within the region of the Lβ → Lα transition the ratio of the two coexisting phases was found to be stable for over 30 min. The state of stable phase coexistence was preceded by a 150-s relaxation taking place at constant temperature after termination of the heating scan in the transition region. While no intermediate structures were present in the coexistence region, a well reproducible multipeak pattern, with at least four prominent heat capacity peaks separated in temperature by 0.4-0.5°C, has been observed in the cooling transition (Lα → Lβ) by calorimetry. The multipeak pattern became distinct with an increase of incubation time in the liquid-crystalline phase. It was also clearly resolved in the x-ray diffraction intensity versus temperature plots recorded at slow cooling rates. These data suggest that the equilibrium state of the Lα phase of hydrated DPPE is represented by a mixture of domains that differ in thermal behavior, but cannot be distinguished structurally by x-ray scattering. Imagesp689-aFIGURE 9 PMID:19431820

  15. X-ray diffraction from flight muscle with a headless myosin mutation: implications for interpreting reflection patterns

    PubMed Central

    Iwamoto, Hiroyuki; Trombitás, Károly; Yagi, Naoto; Suggs, Jennifer A.; Bernstein, Sanford I.

    2014-01-01

    Fruit fly (Drosophila melanogaster) is one of the most useful animal models to study the causes and effects of hereditary diseases because of its rich genetic resources. It is especially suitable for studying myopathies caused by myosin mutations, because specific mutations can be induced to the flight muscle-specific myosin isoform, while leaving other isoforms intact. Here we describe an X-ray-diffraction-based method to evaluate the structural effects of mutations in contractile proteins in Drosophila indirect flight muscle. Specifically, we describe the effect of the headless myosin mutation, Mhc10-Y97, in which the motor domain of the myosin head is deleted, on the X-ray diffraction pattern. The loss of general integrity of the filament lattice is evident from the pattern. A striking observation, however, is the prominent meridional reflection at d = 14.5 nm, a hallmark for the regularity of the myosin-containing thick filament. This reflection has long been considered to arise mainly from the myosin head, but taking the 6th actin layer line reflection as an internal control, the 14.5-nm reflection is even stronger than that of wild-type muscle. We confirmed these results via electron microscopy, wherein image analysis revealed structures with a similar periodicity. These observations have major implications on the interpretation of myosin-based reflections. PMID:25400584

  16. Determination of line profiles on photomasks using DUV, EUV, and x-ray scattering

    NASA Astrophysics Data System (ADS)

    Scholze, F.; Bodermann, B.; Burger, S.; Endres, J.; Haase, A.; Krumrey, M.; Laubis, C.; Soltwisch, V.; Ullrich, A.; Wernecke, J.

    2014-10-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. GISAXS provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range which allow for much steeper angles of incidence but preserve the large range of momentum transfer that can be observed. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, a finite element method (FEM) Maxwell solver and least-squares optimization yielded consistent results for EUV and deep ultraviolet (DUV) scatterometry. For EUV photomasks, the actinic wavelength EUV scatterometry yields particular advantages. A significant polarization dependence of the diffraction intensities for 0th and +1st orders in the geometry with the grating lines perpendicular to the plane of reflection is observed and the 0th order intensity shows sufficient sensitivity to the line width such that a CD-resolution below 0.1 nm is within reach. In this contribution we present scatterometry data for line gratings using GISAXS, and EUV and DUV scatterometry and consistent reconstruction results of the line geometry for EUV and DUV scatterometry.

  17. On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

    SciTech Connect

    Tolchard, Julian Richard; Sømme, Astri; Solberg, Jan Ketil; Solheim, Karl Gunnar

    2015-01-15

    Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction in the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.

  18. High-pressure powder x-ray diffraction study of EuVO{sub 4}

    SciTech Connect

    Garg, Alka B.; Errandonea, D.

    2015-03-15

    The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon–scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite–fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measurements. A partial decomposition of EuVO{sub 4} was also observed from 8.1 to 12.8 GPa; however, this fact did not preclude the identification of the different crystal structures of EuVO{sub 4}. The crystal structures of the different phases have been Rietveld refined and their equations of state (EOS) have been determined. The results are compared with the previous experimental data and theoretical calculations. - Graphical abstract: The high-pressure structural sequence of EuVO{sub 4}. - Highlights: • EuVO{sub 4} is studied under pressure up to 35 GPa using synchrotron XRD. • The zircón–scheelite–fergusonite structural sequence is observed. • Crystal structures are refined and equations of state determined.

  19. Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

    NASA Astrophysics Data System (ADS)

    Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

    Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

  20. Identification of inversion domains in KTiOPO4 via resonant X-ray diffraction.

    PubMed

    Fabrizi, Federica; Thomas, Pamela A; Nisbet, Gareth; Collins, Stephen P

    2015-07-01

    A novel method is presented for the identification of the absolute crystallographic structure in multi-domain polar materials such as ferroelectric KTiOPO4. 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). PMID:25970297

  1. X-ray diffraction study of defects in zinc-diffusion-doped silicon

    SciTech Connect

    Privezentsev, V. V.

    2013-12-15

    Samples of CZ n-Si〈Zn〉(111) are prepared by high-temperature zinc-diffusion annealing followed by quenching and are studied by X-ray diffraction. The silicon contains an initial phosphorus impurity and zinc-compensating admixture at concentrations N{sub P} = 1.5 × 10{sup 14} cm{sup −3} and N{sub Zn} = 1 × 10{sup 14} cm{sup −3}; i.e., the relation N{sub P}/2 < N{sub Zn} < N{sub P} is fulfilled. Microdefects are studied by double- and triple-crystal X-ray diffraction in the dispersion free modes (n, −n) and (n, −n, +n). The samples are found to contain microdefects with two characteristic sizes (average sizes of about 1 μm and 70 nm). The interplanar distance in the near-surface layer with a thickness of 0.1 μm is smaller than this parameter in the remaining matrix, the difference being equal to d{sub 0} Δd/d{sub 0} ≈ 2 × 10{sup −5}. This layer contains mainly vacancy-type microdefects. The angle between the reflecting planes and the local surface relief is Δψ = (7 ± 1) arcmin.

  2. Crystallization and preliminary X-ray diffraction study of phosphoribosyl pyrophosphate synthetase from E. Coli

    SciTech Connect

    Timofeev, V. I. Abramchik, Yu. A. Zhukhlistova, N. E. Kuranova, I. P.

    2015-09-15

    Enzymes of the phosphoribosyl pyrophosphate synthetase family (PRPPS, EC 2.7.6.1) catalyze the formation of 5-phosphoribosyl pyrophosphate (5-PRPP) from adenosine triphosphate and ribose 5-phosphate. 5-Phosphoribosyl pyrophosphate is an important intermediate in the synthesis of purine, pyrimidine, and pyridine nucleotides, as well as of the amino acids histidine and tryptophan. The crystallization conditions for E. coli PRPPS were found by the vapor-diffusion technique and were optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals grown by the counter-diffusion technique using a synchrotron radiation source to 3.1-Å resolution. The crystals of PRPPS belong to sp. gr. P6{sub 3}22 and have the following unit-cell parameters: a = b = 104.44 Å, c = 124.98 Å, α = β = 90°, γ = 120°. The collected X-ray diffraction data set is suitable for the solution of the three-dimensional structure of PRPPS at 3.1-Å resolution.

  3. Crystallization and X-ray diffraction of virus-like particles from a piscine betanodavirus.

    PubMed

    Luo, Yu-Chun; Wang, Chun-Hsiung; Wu, Yi-Min; Liu, Wangta; Lu, Ming-Wei; Lin, Chan-Shing

    2014-08-01

    Dragon grouper nervous necrosis virus (DGNNV), a member of the genus Betanodavirus, causes high mortality of larvae and juveniles of the grouper fish Epinephelus lanceolatus. Currently, there is no reported crystal structure of a fish nodavirus. The DGNNV virion capsid is derived from a single open reading frame that encodes a 338-amino-acid protein of approximately 37 kDa. The capsid protein of DGNNV was expressed to form virus-like particles (VLPs) in Escherichia coli. The VLP shape is T = 3 quasi-symmetric with a diameter of ∼38 nm in cryo-electron microscopy images and is highly similar to the native virion. In this report, crystals of DGNNV VLPs were grown to a size of 0.27 mm within two weeks by the hanging-drop vapour-diffusion method at 283 K and diffracted X-rays to ∼7.5 Å resolution. In-house X-ray diffraction data of the DGNNV VLP crystals showed that the crystals belonged to space group R32, with unit-cell parameters a = b = 353.00, c = 800.40 Å, α = β = 90, γ = 120°. 23 268 unique reflections were acquired with an overall Rmerge of 18.2% and a completeness of 93.2%. Self-rotation function maps confirmed the fivefold, threefold and twofold symmetries of the icosahedron of DGNNV VLPs. PMID:25084387

  4. Automatic processing of macromolecular crystallography X-ray diffraction data at the ESRF

    PubMed Central

    Monaco, Stéphanie; Gordon, Elspeth; Bowler, Matthew W.; Delagenière, Solange; Guijarro, Matias; Spruce, Darren; Svensson, Olof; McSweeney, Sean M.; McCarthy, Andrew A.; Leonard, Gordon; Nanao, Max H.

    2013-01-01

    The development of automated high-intensity macromolecular crystallography (MX) beamlines at synchrotron facilities has resulted in a remarkable increase in sample throughput. Developments in X-ray detector technology now mean that complete X-ray diffraction datasets can be collected in less than one minute. Such high-speed collection, and the volumes of data that it produces, often make it difficult for even the most experienced users to cope with the deluge. However, the careful reduction of data during experimental sessions is often necessary for the success of a particular project or as an aid in decision making for subsequent experiments. Automated data reduction pipelines provide a fast and reliable alternative to user-initiated processing at the beamline. In order to provide such a pipeline for the MX user community of the European Synchrotron Radiation Facility (ESRF), a system for the rapid automatic processing of MX diffraction data from single and multiple positions on a single or multiple crystals has been developed. Standard integration and data analysis programs have been incorporated into the ESRF data collection, storage and computing environment, with the final results stored and displayed in an intuitive manner in the ISPyB (information system for protein crystallography beamlines) database, from which they are also available for download. In some cases, experimental phase information can be automatically determined from the processed data. Here, the system is described in detail. PMID:23682196

  5. Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells

    DOE PAGES

    Rodriguez, Jose A.; Xu, Rui; Chen, Chien -Chun; Huang, Zhifeng; Jiang, Huaidong; Chen, Allan L.; Raines, Kevin S.; Pryor, Jr., Alan; Nam, Daewoong; Wiegart, Lutz; et al

    2015-09-01

    Here, a structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 Kev X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and themore » three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. Finally, it is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres.« less

  6. Which orbital and charge ordering in transition metal oxides can resonant X-ray diffraction detect?

    NASA Astrophysics Data System (ADS)

    Di Matteo, Sergio

    2009-11-01

    The present article is a brief critical review about the possibility of detecting charge and/or orbital order in transition-metal oxides by means of resonant x-ray diffraction. Many recent models of transition-metal oxides are based on charge and/or orbitally ordered ground-states and it has been claimed in the past that resonant x-ray diffraction is able to confirm or reject them. However, in spite of the many merits of this technique, such claims are ambiguous, because the interpretative frameworks used to analyze such results in transition-metal oxides, where structural distortions are always associated to the claimed charged/orbitally ordered transition, strongly influence (not to say suggest) the answer. In order to clarify this point, I discuss the two different definitions of orbital and charge orderings which are often used in the literature without a clear distinction. My conclusion is that the answer to the question of the title depends on which definition is adopted.

  7. Mossbauer spectroscopy and X-ray diffraction of samples from the Santa Catharina iron meteorite

    NASA Technical Reports Server (NTRS)

    Roy-Poulsen, H.; Clarke, R. S., Jr.; Jensen, G. B.; Knudsen, J. M.; Larsen, L.; Roy-Poulsen, N. O.; Vistisen, L.

    1984-01-01

    Conversion electron Mossbauer spectroscopy (CEMS) of samples from the Santa Catharina iron meteorite shows the presence of the ordered iron-nickel phase with 50% Ni, tetrataenite, and of the paramagnetic iron-nickel phase with 25% Ni. The FeNi phase with 50% Ni amounts to 70% of the iron-nickel alloys. Futhermore, the CEM spectra show the presence of small peaks from one or more spinel compounds. These small peaks are more pronounced when regions near the rim of the samples are analyzed. The X-ray diffraction of different areas of the samples, both optically dark and optically light areas, shows the presence of a diffraction pattern from a single f.c.c. lattice with a lattice parameter of a=3.58A This means that the two different Fe-Ni phases seen in the CEMS analysis occupy the same lattice. The X-ray photographs also show the presence of super-structure reflections from the ordered FeNi phase, and that the orientation of the f.c.c. lattice is the same within the whole sample.

  8. Crystallization and X-ray diffraction of virus-like particles from a piscine betanodavirus.

    PubMed

    Luo, Yu-Chun; Wang, Chun-Hsiung; Wu, Yi-Min; Liu, Wangta; Lu, Ming-Wei; Lin, Chan-Shing

    2014-08-01

    Dragon grouper nervous necrosis virus (DGNNV), a member of the genus Betanodavirus, causes high mortality of larvae and juveniles of the grouper fish Epinephelus lanceolatus. Currently, there is no reported crystal structure of a fish nodavirus. The DGNNV virion capsid is derived from a single open reading frame that encodes a 338-amino-acid protein of approximately 37 kDa. The capsid protein of DGNNV was expressed to form virus-like particles (VLPs) in Escherichia coli. The VLP shape is T = 3 quasi-symmetric with a diameter of ∼38 nm in cryo-electron microscopy images and is highly similar to the native virion. In this report, crystals of DGNNV VLPs were grown to a size of 0.27 mm within two weeks by the hanging-drop vapour-diffusion method at 283 K and diffracted X-rays to ∼7.5 Å resolution. In-house X-ray diffraction data of the DGNNV VLP crystals showed that the crystals belonged to space group R32, with unit-cell parameters a = b = 353.00, c = 800.40 Å, α = β = 90, γ = 120°. 23 268 unique reflections were acquired with an overall Rmerge of 18.2% and a completeness of 93.2%. Self-rotation function maps confirmed the fivefold, threefold and twofold symmetries of the icosahedron of DGNNV VLPs.

  9. Destruction-and-diffraction by X-ray free-electron laser.

    PubMed

    Wang, Jimin

    2016-09-01

    It is common knowledge that macromolecular crystals are damaged by the X-rays they are exposed to during conventional data collection. One of the claims made about the crystallographic data collection now being collected using X-ray free-electron lasers (XFEL) is that they are unaffected by radiation damage. XFEL data sets are assembled by merging data obtained from a very large number of crystals, each of which is exposed to a single femtosecond pulse of radiation, the duration of which is so short that diffraction occurs before the damage done to the crystal has time to become manifest, i.e. "diffraction-before-destruction." However, recent theoretical studies have shown that many of the elemental electronic processes that ultimately result in the destruction of such crystals occur during a single pulse. It is predicted that the amplitudes of atomic scattering factor could be reduced by as much as 75% within the first 5 femtoseconds of such pulses, and that different atoms will respond in different ways. Experimental evidence is provided here that these predictions are correct.

  10. In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Ferrari, S.; Kumar, R. S.; Grinblat, F.; Aphesteguy, J. C.; Saccone, F. D.; Errandonea, D.

    2016-06-01

    We have studied the high-pressure structural behavior of zinc ferrite (ZnFe2O4) nanoparticles by powder X-ray diffraction measurements up to 47 GPa. We found that the cubic spinel structure of ZnFe2O4 remains up to 33 GPa and a phase transition is induced beyond this pressure. The high-pressure phase is indexed to an orthorhombic CaMn2O4-type structure. Upon decompression the low- and high-pressure phases coexist. The compressibility of both structures was also investigated. We have observed that the lattice parameters of the high-pressure phase behave anisotropically upon compression. Further, we predict possible phase transition around 55 GPa. For comparison, we also studied the compression behavior of magnetite (Fe3O4) nanoparticles by X-ray diffraction up to 23 GPa. Spinel-type ZnFe2O4 and Fe3O4 nanoparticles have a bulk modulus of 172 (20) GPa and 152 (9) GPa, respectively. This indicates that in both cases the nanoparticles do not undergo a Hall-Petch strengthening.

  11. Taking snapshots of photosynthetic water oxidation using femtosecond X-ray diffraction and spectroscopy

    NASA Astrophysics Data System (ADS)

    Kern, Jan; Tran, Rosalie; Alonso-Mori, Roberto; Koroidov, Sergey; Echols, Nathaniel; Hattne, Johan; Ibrahim, Mohamed; Gul, Sheraz; Laksmono, Hartawan; Sierra, Raymond G.; Gildea, Richard J.; Han, Guangye; Hellmich, Julia; Lassalle-Kaiser, Benedikt; Chatterjee, Ruchira; Brewster, Aaron S.; Stan, Claudiu A.; Glöckner, Carina; Lampe, Alyssa; Difiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Seibert, M. Marvin; Koglin, Jason E.; Gallo, Erik; Uhlig, Jens; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H.; Skinner, David E.; Bogan, Michael J.; Messerschmidt, Marc; Glatzel, Pieter; Williams, Garth J.; Boutet, Sébastien; Adams, Paul D.; Zouni, Athina; Messinger, Johannes; Sauter, Nicholas K.; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K.

    2014-07-01

    The dioxygen we breathe is formed by light-induced oxidation of water in photosystem II. O2 formation takes place at a catalytic manganese cluster within milliseconds after the photosystem II reaction centre is excited by three single-turnover flashes. Here we present combined X-ray emission spectra and diffraction data of 2-flash (2F) and 3-flash (3F) photosystem II samples, and of a transient 3F’ state (250 μs after the third flash), collected under functional conditions using an X-ray free electron laser. The spectra show that the initial O-O bond formation, coupled to Mn reduction, does not yet occur within 250 μs after the third flash. Diffraction data of all states studied exhibit an anomalous scattering signal from Mn but show no significant structural changes at the present resolution of 4.5 Å. This study represents the initial frames in a molecular movie of the structural changes during the catalytic reaction in photosystem II.

  12. Mechanics of Microelectronics Structures as Revealed by X-ray Diffraction

    SciTech Connect

    Murray,C.; Yan, H.; Noyan, I.

    2007-01-01

    The presence of strain distributions within semiconductor features influences many aspects of their behavior. For example, microelectronic technology that incorporates strained silicon improves device performance by increasing carrier mobility in the Si channels. Because current semiconductor fabrication contains multiple levels of metallic and dielectric structures, an understanding of the mechanical response of the constituent elements is critical to the prediction of the overall device performance. In addition, the interaction of strain fields between adjacent structures becomes greater as feature sizes decrease and the corresponding feature density increases. The use of synchrotron-based X-ray methods allows one to determine the interaction between strained features and their environment at a submicron resolution. Real-space mapping of strain distributions in pseudomorphically strained, raised SiGe structures revealed that elastic relaxation extends approximately 20 times the feature thickness from their edges. X-ray topographic methods were also applied to map the substrate deformation induced by overlying SiGe features. A formulation based on the classical Ewald-von Laue theory of dynamical diffraction was derived to match the measured diffraction profiles.

  13. Taking Snapshots of Photosynthetic Water Oxidation Using Femtosecond X-ray Diffraction and Spectroscopy

    PubMed Central

    Kern, Jan; Tran, Rosalie; Alonso-Mori, Roberto; Koroidov, Sergey; Echols, Nathaniel; Hattne, Johan; Ibrahim, Mohamed; Gul, Sheraz; Laksmono, Hartawan; Sierra, Raymond G.; Gildea, Richard J.; Han, Guangye; Hellmich, Julia; Lassalle-Kaiser, Benedikt; Chatterjee, Ruchira; Brewster, Aaron S.; Stan, Claudiu A.; Glöckner, Carina; Lampe, Alyssa; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Seibert, M. Marvin; Koglin, Jason E.; Gallo, Erik; Uhlig, Jens; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H.; Skinner, David E.; Bogan, Michael J.; Messerschmidt, Marc; Glatzel, Pieter; Williams, Garth J.; Boutet, Sébastien; Adams, Paul D.; Zouni, Athina; Messinger, Johannes; Sauter, Nicholas K.; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K.

    2014-01-01

    The dioxygen we breathe is formed from water by its light-induced oxidation in photosystem II. O2 formation takes place at a catalytic manganese cluster within milliseconds after the photosystem II reaction center is excited by three single-turnover flashes. Here we present combined X-ray emission spectra and diffraction data of 2 flash (2F) and 3 flash (3F) photosystem II samples, and of a transient 3F′ state (250 μs after the third flash), collected under functional conditions using an X-ray free electron laser. The spectra show that the initial O-O bond formation, coupled to Mn-reduction, does not yet occur within 250 μs after the third flash. Diffraction data of all states studied exhibit an anomalous scattering signal from Mn but show no significant structural changes at the present resolution of 4.5 Å. This study represents the initial frames in a molecular movie of the structural changes during the catalytic reaction in photosystem II. PMID:25006873

  14. Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells

    SciTech Connect

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

    2015-09-01

    Here, a structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 Kev X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and the three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. Finally, it is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres.

  15. Identification of inversion domains in KTiOPO4 via resonant X-ray diffraction.

    PubMed

    Fabrizi, Federica; Thomas, Pamela A; Nisbet, Gareth; Collins, Stephen P

    2015-07-01

    A novel method is presented for the identification of the absolute crystallographic structure in multi-domain polar materials such as ferroelectric KTiOPO4. 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).

  16. Structure of phospholipid-cholesterol membranes: An x-ray diffraction study

    NASA Astrophysics Data System (ADS)

    Karmakar, Sanat; Raghunathan, V. A.

    2005-06-01

    We have studied the phase behavior of mixtures of cholesterol with dipalmitoyl phosphatidylcholine (DPPC), dimyristoyl phosphatidylcholine (DMPC), and dilauroyl phosphatidylethanolamine (DLPE), using x-ray diffraction techniques. Phosphatidylcholine (PC)-cholesterol mixtures are found to exhibit a modulated phase for cholesterol concentrations around 15mol% at temperatures below the chain melting transition. Lowering the relative humidity from 98% to 75% increases the temperature range over which it exists. An electron density map of this phase in DPPC-cholesterol mixtures, calculated from the x-ray diffraction data, shows bilayers with a periodic height modulation, as in the ripple phase observed in many PCs in between the main- and pretransitions. However, these two phases differ in many aspects, such as the dependence of the modulation wavelength on the cholesterol content and thermodynamic stability at reduced humidities. This modulated phase is found to be absent in DLPE-cholesterol mixtures. At higher cholesterol contents the gel phase does not occur in any of these three systems, and the fluid lamellar phase is observed down to the lowest temperature studied (5°C) .

  17. Crystallization and preliminary X-ray diffraction analysis of recombinant hepatitis E virus-like particle

    SciTech Connect

    Wang, Che-Yen; Miyazaki, Naoyuki; Yamashita, Tetsuo; Higashiura, Akifumi; Nakagawa, Atsushi; Li, Tian-Cheng; Takeda, Naokazu; Xing, Li; Hjalmarsson, Erik; Friberg, Claes; Liou, Der-Ming; Sung, Yen-Jen; Tsukihara, Tomitake; Matsuura, Yoshiharu; Miyamura, Tatsuo; Cheng, R. Holland

    2008-04-01

    A recombinant virus-like particle that is a potential oral hepatitis E vaccine was crystallized. Diffraction data were collected to 8.3 Å resolution and the X-ray structure was phased with the aid of a low-resolution density map determined using cryo-electron microscopy data. Hepatitis E virus (HEV) accounts for the majority of enterically transmitted hepatitis infections worldwide. Currently, there is no specific treatment for or vaccine against HEV. The major structural protein is derived from open reading frame (ORF) 2 of the viral genome. A potential oral vaccine is provided by the virus-like particles formed by a protein construct of partial ORF3 protein (residue 70–123) fused to the N-terminus of the ORF2 protein (residues 112–608). Single crystals obtained by the hanging-drop vapour-diffusion method at 293 K diffract X-rays to 8.3 Å resolution. The crystals belong to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 337, b = 343, c = 346 Å, α = β = γ = 90°, and contain one particle per asymmetric unit.

  18. Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array

    SciTech Connect

    Lyubimov, Artem Y.; Murray, Thomas D.; Koehl, Antoine; Araci, Ismail Emre; Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Cohen, Aina E.; Soltis, S. Michael; Baxter, Elizabeth L.; Brewster, Aaron S.; Sauter, Nicholas K.; Brunger, Axel T.; Berger, James M.

    2015-04-01

    A microfluidic platform has been developed for the capture and X-ray analysis of protein microcrystals, affording a means to improve the efficiency of XFEL and synchrotron experiments. X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat for conducting diffraction experiments at room temperature without the need for flash-cooling. Proof-of-principle tests with a model system (hen egg-white lysozyme) demonstrated the high efficiency of the microfluidic approach for crystal harvesting, permitting the collection of sufficient data from only 265 single-crystal still images to permit determination and refinement of the structure of the protein. This work shows that microfluidic capture devices can be readily used to facilitate data collection from protein microcrystals grown in traditional laboratory formats, enabling analysis when cryopreservation is problematic or when only small numbers of crystals are available. Such microfluidic capture devices may also be useful for data collection at synchrotron sources.

  19. Crystallization and X-ray diffraction studies of glutathione S-transferase from Escherichia coli

    NASA Astrophysics Data System (ADS)

    Nishida, Motohiko; Harada, Shigeharu; Satow, Yoshinori; Inoue, Hideshi; Takahashi, Kenji

    1996-10-01

    Crystals of glutathione S-transferase from Escherichia coli have been obtained by use of polyethylene glycol 6000 as a precipitant. The crystallization was performed in the presence of a glutathione sulfonate inhibitor under the acidic condition, with combination of the sitting-drop vapour-diffusion and the macro-seeding procedures. The crystals are of a thin-plate shape with typical sizes of 1.0 × 0.5 × 0.1 mm, and are stable against X-ray irradiation. They belong to the space group P2 12 12 1 with cell parameters of a = 90.47 Å, b = 93.87 Å and c = 51.10 Å, and diffract X-rays at least up to 2.3 Å resolution. The solvent content is 48% in volume, when a homodimeric molecule of the enzyme is assumed to occupy an asymmetric unit of the crystal. The crystals are suitable for three-dimensional structural studies. Diffraction data of the native crystal have been collected.

  20. Application of biochemical and X-ray diffraction analyses to establish the postmortem interval.

    PubMed

    Prieto-Castelló, M J; Hernández del Rincón, J P; Pérez-Sirvent, C; Alvarez-Jiménez, P; Pérez-Cárceles, M D; Osuna, E; Luna, A

    2007-10-25

    The determination of the date of death from bone remains is of scientific interest but also has important legal implications. The establishment of the postmortem interval (PMI) is a very complex problem because of the great number of intrinsic factors that may alter the normal course of postmortem change, such as the age, sex, constitution and previous physiological and pathological states of the subject, and external factors. In order to evaluate the utility of X-ray diffraction and the measurement of some components in dating bone remains, a total of 69 long bones from 69 different cadavers (41 males, 28 females) with a mean age of 68 years (S.D.=17.6, range 12-97) were used. The bones were removed from cement tombs of Murcia Cemetery, where they had lain for documented times of between 7 and 54 years (S.D.=11.6, mean time 17.6 years). We have studied potassium, sulphur, nitrogen, urea, total protein, phosphorus, and some X-ray diffraction (XRD) parameters related to the degree of crystallinity of the mineral component in medullar and cortical bone zones to establish which of the two provides the most useful information for calculating the PMI. In the overall analysis of our data, we believe that the use of both XRD and biochemical analyses (especially of urea, potassium and sulphur) particularly in the cortical zone of the bone could be an alternative method for dating osseous remains. PMID:17306944