WorldWideScience

Sample records for incident x-ray diffraction

  1. Grazing Incidence X-ray Scattering and Diffraction

    Indian Academy of Sciences (India)

    IAS Admin

    several materials as a function of angle of incidence, αi with X-rays of wavelength ..... are several advantages of using this formulation for the description of surface ..... print of the surface (as shown at the botton of Figure. 5). A Soller collimator ...

  2. X-ray grazing incidence diffraction from multilayers

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-09-01

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

  3. X-ray radiation damage of organic semiconductor thin films during grazing incidence diffraction experiments

    Energy Technology Data Exchange (ETDEWEB)

    Neuhold, A., E-mail: alfred.neuhold@tugraz.at [Institute of Solid State Physics, Graz University of Technology, Graz (Austria); Novak, J.; Flesch, H.-G.; Moser, A.; Djuric, T. [Institute of Solid State Physics, Graz University of Technology, Graz (Austria); Grodd, L.; Grigorian, S.; Pietsch, U. [Institute of Physics, University Siegen (Germany); Resel, R. [Institute of Solid State Physics, Graz University of Technology, Graz (Austria)

    2012-08-01

    Since modern synchrotrons with highly intense X-ray beams are in use to investigate organic materials, the stability of soft matter materials during beam exposure is a crucial issue. Grazing incidence X-ray diffraction and specular X-ray reflectivity measurements were performed on thin films of organic semiconducting materials, like poly(3-hexylthiophene) (P3HT), sexithiophene and pentacene. These films were irradiated with an average flux density between 10{sup 15} and 10{sup 16} photons/(s mm{sup 2}) and evidenced a different stability in synchrotron X-ray radiation. The semi-crystalline P3HT showed a clear intensity decrease of the 1 0 0 Bragg peak and 0 2 0 Bragg peak compared to the rather stable diffraction features of the molecular crystals sexithiophene and pentacene. The difference in synchrotron X-ray radiation stability is explained by the interaction of the X-ray beam with the individual chemical components in the molecules as well as by the different crystallinities of the materials. Furthermore, the semi-crystalline P3HT film exhibited an increase of film thickness after irradiation and the surface roughness slightly decreased. To summarize, this study shows a strong influence of synchrotron X-ray radiation to specific organic thin films like e.g. P3HT, while others like pentacene and sexithiophene are observed as quite stable.

  4. Surface quality inspection of PbWO4 crystals by grazing incidence X-ray diffraction

    International Nuclear Information System (INIS)

    Mengucci, P.; Di Cristoforo, A.; Lebeau, M.; Majni, G.; Paone, N.; Pietroni, P.; Rinaldi, D.

    2005-01-01

    High-quality scintillating crystals are required for applications in radiographic systems and high-energy physics detectors to achieve the specified optical properties. In order to study the state of the single crystals surface we propose the use of the grazing incidence X-ray diffraction (GID) technique. This technique allows performing a depth profiling of the sample by changing the incidence angle of the X-ray beam with respect to the sample surface. In this work, two samples of a large PbWO 4 (PWO) single crystal exhibiting different surface roughness values have been studied. Results have shown that GID is a suitable technique for surface quality inspection

  5. X-ray diffraction

    International Nuclear Information System (INIS)

    Einstein, J.R.; Wei, C.H.

    1982-01-01

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

  6. X-ray diffraction

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

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

  7. Depth distribution of chemical phase concentration determined by grazing incidence X-ray diffraction

    International Nuclear Information System (INIS)

    Novak, P.; Ballo, P.; Dobrocka, E.; Vallo, M.; Lalinsky, T.

    2013-01-01

    Grazing incidence geometry is widely used in X-ray diffraction analysis of thin films. Penetration depth of radiation can be easily changed by an appropriate selection of the angle of incidence α that enables obtaining information from different depths of the sample. This depth can be decreased up to a nanometer scale by approaching the critical angle α_c for total external reflection. This method therefore provides an efficient tool for the analysis of depth distribution of various structural properties, such as the crystallite size, the amorphous fraction, stress or the concentration of chemical phase. However, absorption of the radiation can be characterized by an average attenuation coefficient μ a special care has to be paid to the last property. Variation of chemical phase concentration with depth usually results in depth dependence on the attenuation coefficient. In this contribution a method for determination of depth distribution of a chemical phase is outlined. The method correctly takes into account the depth variation of the attenuation coefficient. The method is tested on thin oxidized Ir layers. The aim of this paper is a comparison two simple model cases with the experimental results. (authors)

  8. On the determination of stress profiles in expanded austenite by grazing incidence X-ray diffraction and successive layer removal

    DEFF Research Database (Denmark)

    Fernandes, Frederico Augusto Pires; Christiansen, Thomas L.; Winther, Grethe

    2015-01-01

    Surface layers of expanded austenite resulting from nitriding typically exhibit large gradients in residual stress and composition. Evaluation of residual-stress profiles is explored by means of grazing incidence X-ray diffraction (GI-XRD), probing shallow depths, combined with successive layer...... removal. Several factors complicating the stress determination are analysed and discussed: (1) ghost stresses arising from a small variation in the shallow information depths probed with GI-XRD, (2) selection of the grain interaction model used to calculate the X-ray elastic constants for conversion...

  9. On the determination of stress profiles in expanded austenite by grazing incidence X-ray diffraction and successive layer removal

    International Nuclear Information System (INIS)

    Fernandes, Frederico A.P.; Christiansen, Thomas L.; Winther, Grethe; Somers, Marcel A.J.

    2015-01-01

    Surface layers of expanded austenite resulting from nitriding typically exhibit large gradients in residual stress and composition. Evaluation of residual-stress profiles is explored by means of grazing incidence X-ray diffraction (GI-XRD), probing shallow depths, combined with successive layer removal. Several factors complicating the stress determination are analysed and discussed: (1) ghost stresses arising from a small variation in the shallow information depths probed with GI-XRD, (2) selection of the grain interaction model used to calculate the X-ray elastic constants for conversion of lattice strains into residual stress and (3) the composition dependence of these elastic constants

  10. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1{sub 0} ordering in {sup 57}Fe/Pt multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore-452 017 (India); Leitenberger, Wolfram [Institute of Physics, University of Potsdam, 14469 Potsdam (Germany); Pietsch, U [Physics Department, University of Siegen, D-57068 Siegen (Germany)], E-mail: vrreddy@csr.ernet.in, E-mail: varimalla@yahoo.com

    2009-05-06

    In situ high temperature x-ray reflectivity and grazing incidence x-ray diffraction measurements in the energy dispersive mode are used to study the ordered face-centered tetragonal (fct) L 1{sub 0} phase formation in [Fe(19 A)/Pt(25 A)]{sub x 10} multilayers prepared by ion beam sputtering. With the in situ x-ray measurements it is observed that (i) the multilayer structure first transforms to a disordered FePt and subsequently to an ordered fct L 1{sub 0} phase, (ii) the ordered fct L 1{sub 0} FePt peaks start to appear at 320 deg. C annealing, (iii) the activation energy of the interdiffusion is 0.8 eV and (iv) ordered fct FePt grains have preferential out-of-plane texture. The magneto-optical Kerr effect and conversion electron Moessbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 deg. C annealed multilayers. The magnetic data for the 400 {sup 0}C annealed sample indicate that the magnetization is at an angle of {approx}50 deg. from the plane of the film.

  11. Grazing incidence x-ray diffraction at free-standing nanoscale islands: fine structure of diffuse scattering

    International Nuclear Information System (INIS)

    Grigoriev, D; Hanke, M; Schmidbauer, M; Schaefer, P; Konovalov, O; Koehler, R

    2003-01-01

    We have investigated the x-ray intensity distribution around 220 reciprocal lattice point in case of grazing incidence diffraction at SiGe nanoscale free-standing islands grown on Si(001) substrate by LPE. Experiments and computer simulations based on the distorted wave Born approximation utilizing the results of elasticity theory obtained by FEM modelling have been carried out. The data reveal fine structure in the distribution of scattered radiation with well-pronounced maxima and complicated fringe pattern. Explanation of the observed diffraction phenomena in their relation to structure and morphology of the island is given. An optimal island model including its shape, size and Ge spatial distribution was elaborated

  12. Glancing-incidence X-ray diffraction of Ag nanoparticles in gold lustre decoration of Italian Renaissance pottery

    Science.gov (United States)

    Bontempi, E.; Colombi, P.; Depero, L. E.; Cartechini, L.; Presciutti, F.; Brunetti, B. G.; Sgamellotti, A.

    2006-06-01

    Lustre is known as one of the most significant decorative techniques of Medieval and Renaissance pottery in the Mediterranean basin, characterized by brilliant gold and red metallic reflections and iridescence effects. Previous studies by various techniques (SEM-EDS and TEM, UV-VIS, XRF, RBS and EXAFS) demonstrated that lustre consists of a heterogeneous metal-glass composite film, formed by Cu and Ag nanoparticles dispersed within the outer layer of a tin-opacified lead glaze. In the present work the investigation of an original gold lustre sample from Deruta has been carried out by means of glancing-incidence X-ray diffraction techniques (GIXRD). The study was aimed at providing information on structure and depth distribution of Ag nanoparticles. Exploiting the capability of controlling X-ray penetration in the glaze by changing the incidence angle, we used GIXRD measurements to estimate non-destructively thickness and depth of silver particles present in the first layers of the glaze.

  13. Multiple scattering in grazing-incidence X-ray diffraction: impact on lattice-constant determination in thin films

    Energy Technology Data Exchange (ETDEWEB)

    Resel, Roland, E-mail: roland.resel@tugraz.at; Bainschab, Markus; Pichler, Alexander [Graz University of Technology, Graz (Austria); Dingemans, Theo [Delft University of Technology, Delft (Netherlands); Simbrunner, Clemens [Johannes Kepler University, Linz (Austria); University of Bremen, Bremen (Germany); Stangl, Julian [Johannes Kepler University, Linz (Austria); Salzmann, Ingo [Humboldt University, Berlin (Germany)

    2016-04-20

    The use of grazing-incidence X-ray diffraction to determine the crystal structure from thin films requires accurate positions of Bragg peaks. Refraction effects and multiple scattering events have to be corrected or minimized. Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2′:6′,2′′-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films.

  14. X-ray filter for x-ray powder diffraction

    Science.gov (United States)

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

    2018-01-23

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

  15. X-ray diffraction 2 - diffraction principles

    International Nuclear Information System (INIS)

    O'Connor, B.

    1999-01-01

    Full text: The computation of powder diffraction intensities is based on the principle that the powder pattern comprises the summation of the intensity contributions from each of the crystallites (or single crystals) in the material. Therefore, it is of value for powder diffractionists to appreciate the form of the expression for calculating single crystal diffraction pattern intensities. This knowledge is especially important for Rietveld analysis practitioners in terms of the (i) mathematics of the method and (ii) retrieving single crystal structure data from the literature. We consider the integrated intensity from a small single crystal being rotated at velocity ω through the Bragg angle θ for reflection (hkl).... I(hkl) = [l o /ω]. [e 4 /m 2 c 4 ]. [λ 3 δV F(hkl) 2 /υ 2 ].[(1+cos 2 2θ)/2sin2θ] where e, m and c are the usual fundamental constants; λ is the x-ray wavelength, δV is the crystallite volume; F(hkl) is the structure factor; υ is the unit cell volume; and (1+cos 2 θ)/2sin2θ] is the Lorentz-polarisation factor for an unpolarised incident beam. The expression does not include a contribution for extinction. The influence of factors λ, δV, F(hkl) and υ on the intensities should be appreciated by powder diffractionists, especially the structure factor, F(hkl), which is responsible for the fingerprint nature of diffraction patterns, such as the rise and fall of intensity from peak to peak. The structure factor expression represents the summation of the scattered waves from each of the j scattering centres (i e atoms) in the unit cell: F(hkl) Σ f j exp[2πi (h.x j +k.y i +l. z i )] T j . Symbol f is the scattering factor (representing the atom-type scattering efficiency); (x, y, z) are the fractional position coordinates of atom j within the unit cell; and T is the thermal vibration factor for the atom given by: T j = 8π 2 2 > sin 2 θ/λ 2 with 2 > being the mean-square vibration amplitude of the atom (assumed to be isotropic). The

  16. Submicron X-ray diffraction

    International Nuclear Information System (INIS)

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

    2000-01-01

    At the Advanced Light Source in Berkeley the authors have instrumented a beam line that is devoted exclusively to x-ray micro diffraction problems. By micro diffraction they mean those classes of problems in Physics and Materials Science that require x-ray beam sizes in the sub-micron range. The instrument is for instance, capable of probing a sub-micron size volume inside micron sized aluminum metal grains buried under a silicon dioxide insulating layer. The resulting Laue pattern is collected on a large area CCD detector and automatically indexed to yield the grain orientation and deviatoric (distortional) strain tensor of this sub-micron volume. A four-crystal monochromator is then inserted into the beam, which allows monochromatic light to illuminate the same part of the sample. Measurement of diffracted photon energy allows for the determination of d spacings. The combination of white and monochromatic beam measurements allow for the determination of the total strain/stress tensor (6 components) inside each sub-micron sized illuminated volume of the sample

  17. Glancing-incidence X-ray diffraction of Ag nanoparticles in gold lustre decoration of Italian Renaissance pottery

    Energy Technology Data Exchange (ETDEWEB)

    Bontempi, E.; Colombi, P.; Depero, L.E. [Universita di Brescia, Laboratorio di Chimica per le Tecnologie and INSTM, Brescia (Italy); Cartechini, L. [Universita di Perugia, Istituto di Scienze e Tecnologie Molecolari-CNR, Sezione di Perugia, Perugia (Italy); Presciutti, F.; Brunetti, B.G. [Universita di Perugia, INSTM and Centro di Eccellenza SMAArt, Dipartimento di Chimica, Perugia (Italy); Sgamellotti, A. [Universita di Perugia, Istituto di Scienze e Tecnologie Molecolari-CNR, Sezione di Perugia, Perugia (Italy); Universita di Perugia, INSTM and Centro di Eccellenza SMAArt, Dipartimento di Chimica, Perugia (Italy)

    2006-06-15

    Lustre is known as one of the most significant decorative techniques of Medieval and Renaissance pottery in the Mediterranean basin, characterized by brilliant gold and red metallic reflections and iridescence effects. Previous studies by various techniques (SEM-EDS and TEM, UV-VIS, XRF, RBS and EXAFS) demonstrated that lustre consists of a heterogeneous metal-glass composite film, formed by Cu and Ag nanoparticles dispersed within the outer layer of a tin-opacified lead glaze. In the present work the investigation of an original gold lustre sample from Deruta has been carried out by means of glancing-incidence X-ray diffraction techniques (GIXRD). The study was aimed at providing information on structure and depth distribution of Ag nanoparticles. Exploiting the capability of controlling X-ray penetration in the glaze by changing the incidence angle, we used GIXRD measurements to estimate non-destructively thickness and depth of silver particles present in the first layers of the glaze. (orig.)

  18. Glancing-incidence X-ray diffraction of Ag nanoparticles in gold lustre decoration of Italian Renaissance pottery

    International Nuclear Information System (INIS)

    Bontempi, E.; Colombi, P.; Depero, L.E.; Cartechini, L.; Presciutti, F.; Brunetti, B.G.; Sgamellotti, A.

    2006-01-01

    Lustre is known as one of the most significant decorative techniques of Medieval and Renaissance pottery in the Mediterranean basin, characterized by brilliant gold and red metallic reflections and iridescence effects. Previous studies by various techniques (SEM-EDS and TEM, UV-VIS, XRF, RBS and EXAFS) demonstrated that lustre consists of a heterogeneous metal-glass composite film, formed by Cu and Ag nanoparticles dispersed within the outer layer of a tin-opacified lead glaze. In the present work the investigation of an original gold lustre sample from Deruta has been carried out by means of glancing-incidence X-ray diffraction techniques (GIXRD). The study was aimed at providing information on structure and depth distribution of Ag nanoparticles. Exploiting the capability of controlling X-ray penetration in the glaze by changing the incidence angle, we used GIXRD measurements to estimate non-destructively thickness and depth of silver particles present in the first layers of the glaze. (orig.)

  19. Grazing incidence x-ray diffraction analysis of zeolite NaA membranes on porous alumina tubes.

    Science.gov (United States)

    Kyotani, Tomohiro

    2006-07-01

    Zeolite NaA-type membranes hydrothermally synthesized on porous alumina tubes, for dehydration process, were characterized by grazing incidence 2 theta scan X-ray diffraction analysis (GIXRD). The fine structure of the membrane was studied fractionally for surface layer and for materials embedded in the porous alumina tube. The thickness of the surface layer on the porous alumina tube in the membranes used in this study was approximately 2-3 microm as determined from transmission electron microscopy with focused ion beam thin-layer specimen preparation technique (FIB-TEM). To discuss the effects of the membrane surface morphology on the GIXRD measurements, CaA-type membrane prepared by ion exchange from the NaA-type membrane and surface-damaged NaA-type membrane prepared by water leaching were also studied. For the original NaA-type membrane, 2 theta scan GIXRD patterns could be clearly measured at X-ray incidence angles (alpha) ranging from 0.1 to 2.0 deg in increments of 0.1 deg. The surface layers of the 2 - 3 microm on the porous alumina tube correspond to the alpha values up to ca. 0.2 deg. For the CaA-type and the surface-damaged NaA-type membranes, however, diffraction patterns from the surface layer could not be successfully detected and the others were somewhat broad. For all the three samples, diffraction intensities of both zeolite and alumina increased with depth (X-ray incidence angle, alpha) in the porous alumina tube region. The depth profile analysis of the membranes based on the GIXRD first revealed that amount of zeolite crystal embedded in the porous alumina tube is much larger than that in the surface layer. Thus, the 2 theta scan GIXRD is a useful method to study zeolite crystal growth mechanism around (both inside and outside) the porous alumina support during hydrothermal synthesis and to study water permeation behavior in the dehydration process.

  20. X-ray diffraction imaging of material microstructures

    KAUST Repository

    Varga, Laszlo

    2016-10-20

    Various examples are provided for x-ray imaging of the microstructure of materials. In one example, a system for non-destructive material testing includes an x-ray source configured to generate a beam spot on a test item; a grid detector configured to receive x- rays diffracted from the test object; and a computing device configured to determine a microstructure image based at least in part upon a diffraction pattern of the x-rays diffracted from the test object. In another example, a method for determining a microstructure of a material includes illuminating a beam spot on the material with a beam of incident x-rays; detecting, with a grid detector, x-rays diffracted from the material; and determining, by a computing device, a microstructure image based at least in part upon a diffraction pattern of the x-rays diffracted from the material.

  1. Diffractive X-Ray Telescopes

    International Nuclear Information System (INIS)

    Skinner, G.K.; Skinner, G.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 several 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 supermassive 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 atmospheric absorption

  2. Effect of Ar9+ irradiation on Zr-1Nb-1Sn-0.1Fe alloy characterized by Grazing Incidence X-ray diffraction technique

    Science.gov (United States)

    Dutta, Argha; Das, Kalipada; Gayathri, N.; Menon, Ranjini; Nabhiraj, P. Y.; Mukherjee, Paramita

    2018-03-01

    The microstructural parameters such as domain size and microstrain have been estimated from Grazing Incidence X-ray Diffraction (GIXRD) data for Ar9+ irradiated Zr-1Nb-1Sn-0.1Fe sample as a function of dpa (dose). Detail studies using X-ray Diffraction Line Profile Analysis (XRDLPA) from GIXRD data has been carried out to characterize the microstructural parameters like domain size and microstrain. The reorientation of the grains due to effect of irradiation at high dpa (dose) has been qualitatively assessed by the texture parameter P(hkl).

  3. X-ray topography and multiple diffraction

    International Nuclear Information System (INIS)

    Chang, S.-L.

    1983-01-01

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

  4. Measurement of UO2 surface oxidation using grazing-incidence x-ray diffraction: Implications for nuclear forensics

    Science.gov (United States)

    Tracy, Cameron L.; Chen, Chien-Hung; Park, Sulgiye; Davisson, M. Lee; Ewing, Rodney C.

    2018-04-01

    Nuclear forensics involves determination of the origin and history of interdicted nuclear materials based on the detection of signatures associated with their production and trafficking. The surface oxidation undergone by UO2 when exposed to air is a potential signature of its atmospheric exposure during handling and transport. To assess the sensitivity of this oxidation to atmospheric parameters, surface sensitive grazing-incidence x-ray diffraction (GIXRD) measurements were performed on UO2 samples exposed to air of varying relative humidity (34%, 56%, and 95% RH) and temperature (room temperature, 50 °C, and 100 °C). Near-surface unit cell contraction was observed following exposure, indicating oxidation of the surface and accompanying reduction of the uranium cation ionic radii. The extent of unit cell contraction provides a measure of the extent of oxidation, allowing for comparison of the effects of various exposure conditions. No clear influence of relative humidity on the extent of oxidation was observed, with samples exhibiting similar degrees of unit cell contraction at all relative humidities investigated. In contrast, the thickness of the oxidized layers increased substantially with increasing temperature, such that differences on the order of 10 °C yielded readily observable crystallographic signatures of the exposure conditions.

  5. Stress measurements by multi-reflection grazing-incidence X-ray diffraction method (MGIXD) using different radiation wavelengths and different incident angles

    International Nuclear Information System (INIS)

    Marciszko, Marianna; Baczmański, Andrzej; Braham, Chedly; Wróbel, Mirosław; Wroński, Sebastian; Cios, Grzegorz

    2017-01-01

    The presented study introduces the development of the multi-reflection grazing-incidence X-ray diffraction method (MGIXD) for residual stress determination. The proposed new methodology is aimed at obtaining more reliable experimental data and increasing the depth of non-destructive stress determination below the sample surface. To verify proposed method measurements were performed on a classical X-ray diffractometer (Cu Kα radiation) and using synchrotron radiation (three different wavelengths: λ = 1.2527 Å, λ = 1.5419 Å and λ = 1.7512 Å). The Al2017 alloy subjected to three different surface treatments was investigated in this study. The obtained results showed that the proposed development of MGIXD method, in which not only different incident angles but also different wavelengths of X-ray are used, can be successfully applied for residual stress determination, especially when stress gradients are present in the sample.

  6. Molecular-beam epitaxy growth and structural characterization of semiconductor-ferromagnet heterostructures by grazing incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Satapathy, D.K.

    2005-12-19

    The present work is devoted to the growth of the ferromagnetic metal MnAs on the semiconductor GaAs by molecular-beam epitaxy (MBE). The MnAs thin films are deposited on GaAs by molecular-beam epitaxy (MBE). Grazing incidence diffraction (GID) and reflection high-energy electron diffraction (RHEED) are used in situ to investigate the nucleation, evolution of strain, morphology and interfacial structure during the MBE growth. Four stages of the nucleation process during growth of MnAs on GaAs(001) are revealed by RHEED azimuthal scans. GID shows that further growth of MnAs films proceed via the formation of relaxed islands at a nominal thickness of 2.5 ML which increase in size and finally coalesce to form a continuous film. Early on, an ordered array of misfit dislocations forms at the interface releasing the misfit strain even before complete coalescence occurs. The fascinating complex nucleation process of MnAs on GaAs(0 0 1) contains elements of both Volmer-Weber and Stranski-Krastanov growth. A nonuniform strain amounting to 0.66%, along the [1 -1 0] direction and 0.54%, along the [1 1 0] direction is demonstrated from x-ray line profile analysis. A high correlation between the defects is found along the GaAs[1 1 0] direction. An extremely periodic array of misfit dislocations with a period of 4.95{+-}0.05 nm is formed at the interface along the [1 1 0] direction which releases the 7.5% of misfit. The inhomogeneous strain due to the periodic dislocations is confined at the interface within a layer of 1.6 nm thickness. The misfit along the [1 -1 0] direction is released by the formation of a coincidence site lattice. (orig.)

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

    International Nuclear Information System (INIS)

    Cappuccio, G.; Terranova, M.L.

    1996-09-01

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

  8. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

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

  9. Grazing incidence synchrotron X-ray diffraction and Moessbauer spectroscopy analyses of plasma nitrided ASTM F138 stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Danilo Olzon Dionysio de; Ardisson, Jose Domingos, E-mail: dolzon@gmail.com [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Silva, Edilaine Honorio [Studiecentrum voor Kernenergie (Belgium); Olzon-Dionysio, Maristela; Souza, Sylvio Dionysio de; Fabris, Jose Domingos [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil); Martinez, L.G. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2016-07-01

    Full text: systematic investigation of samples of plasma-nitriding austenitic stainless steels ASTM F138 and AISI 316L is reported. The surface treatment of the steels through plasma-nitriding was used to improve further the hardness, wear and corrosion resistance of these stainless steels. The resulting layered crystallographic structure actually corresponds to several phases with close cell parameters, making their identification and quantification a real experimental challenge. The ASTM F138 and AISI 316L stainless steel disks were plasma nitrided for 4 h at 400 deg C in a 80% H{sub 2} -20% N2 atmosphere at 6 torr, using plasma current frequencies between 6 and 100 kHz. Data of Moessbauer (CEMS and CXMS) and grazing incidence synchrotron X-ray diffraction (XRD-SR) were systematically collected. The nitrided layer thickness were not in general influenced by the plasma frequency, except at 12 kHz, which produced a layer thickness of approximately 8.0 mm, being in average 40% thicker than for the other samples. CXMS and CEMS Moessbauer spectra for this 12 kHz-sample show a much more pronounced magnetic resonance lines than for the other samples. The Fe{sub 4}N phase presents a single magnetic hyperfine interaction; the other two (Fe{sub 2-3}N and the expanded austenite) present both paramagnetic and magnetic components, even though their hyperfine parameters may not be safely separated. We also present the results of XRD-SR that were probed at several depths. The data from these techniques may be consistently correlated and this leads to an improved model to explain the structure of the nitrided layers. (author)

  10. Structural stability of naphthyl end-capped oligothiophenes in organic field-effect transistors measured by grazing-incidence X-ray diffraction in operando

    DEFF Research Database (Denmark)

    Huss-Hansen, Mathias K.; Lauritzen, Andreas E.; Bikondoa, Oier

    2017-01-01

    We report on microstructural durability of 5,5′-bis(naphth-2-yl)-2,2′-bithiophene (NaT2) in organic field-effect transistors (OFETs) in operando monitored by grazing-incidence X-ray diffraction (GIXRD). NaT2 maintains its monoclinic bulk motif in operating OFETs with a=20.31±0.06 Å, b=6.00±0.01 Å...

  11. Diffraction enhanced x-ray imaging

    International Nuclear Information System (INIS)

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

    1997-09-01

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

  12. The epitaxial growth and interfacial strain study of VO{sub 2}/MgF{sub 2} (001) films by synchrotron based grazing incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fan, L.L. [Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology, Yancheng 224051 (China); National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029 (China); Chen, S. [National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029 (China); Liu, Q.H. [Science and Technology on Electro-optical Information Security Control Laboratory, Tianjin 300300 (China); Liao, G.M.; Chen, Y.L.; Ren, H. [National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029 (China); Zou, C.W., E-mail: czou@ustc.edu.cn [National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029 (China)

    2016-09-05

    High quality VO{sub 2} films with different thickness were epitaxially grown on MgF{sub 2} (001) substrates by oxide molecular beam epitaxy method. The evolution of interfacial strain was investigated by synchrotron based grazing incidence X-ray diffraction. By adjusting the incidence angles, the penetration depth of X-ray in VO{sub 2} film could be controlled and the thickness-depend lattice distortion in the epitaxial VO{sub 2} film was investigated. Due to the lattice mismatching, the pronounced tensile strain was observed in ultra-thin VO{sub 2} film. As the film thickness increasing, the interfacial strain relaxed gradually and became fully relaxed for thick VO{sub 2} films. Combined with the electric transport measurement, it was revealed that the phase transition temperature of ultra-thin VO{sub 2} film decreased greatly. The effect of interfacial strain induced phase transition modulation and the intrinsic mechanism was systematically discussed. - Highlights: • We prepared high quality VO{sub 2} epitaxial films on MgF{sub 2} (001) substrates by oxide molecular beam epitaxy method. • Synchrotron radiation grazing incidence X-ray diffraction was employed to detect evolution of strain along depth profile. • Based on a classic band structure model, the mechanism of strain controlled phase transition of VO{sub 2} was discussed.

  13. Molecular aggregation states of poly{2-(perfluorooctyl)ethyl acrylate} polymer brush thin film analyzed by grazing incidence X-ray diffraction

    International Nuclear Information System (INIS)

    Yamaguchi, H; Honda, K; Takahara, A; Kobayashi, M; Morita, M; Masunaga, H; Sasaki, S; Takata, M; Sakata, O

    2009-01-01

    Fluoropolymer brush with crystalline side chains was prepared by surface-initiated atom transfer radical polymerization of 2-(perfluorooctyl)ethyl acrylate (FA-C 8 ) from a flat silicon substrate. The crystallization and the molecular aggregation structures of polymer side chain at the outermost surface and internal region in the brush film were characterized by grazing incidence X-ray diffraction (GIXD) measurement using two different incident angles of X-ray. At the air interface of PFA-C 8 brush film, the rod-like R f group was oriented perpendicular to the surface forming a hexagonal packing structure to reduce surface energy. In contrast, the oriented R f groups parallel to the substrate coexisted at the internal region in the brush. This unique depth dependence of crystalline state of the fluoropolymer brush was observed by surface-sensitive GIXD measurement.

  14. Molecular aggregation states of poly{l_brace}2-(perfluorooctyl)ethyl acrylate{r_brace} polymer brush thin film analyzed by grazing incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Yamaguchi, H; Honda, K; Takahara, A [Graduate School of Engineering, Kyushu University, Nishi-ku, Fukuoka 819-0395 (Japan); Kobayashi, M [Institute for Materials Chemistry and Engineering, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 (Japan); Morita, M [Fundamental Research Department, Chemical Division, Daikin Industries, Ltd., 1-1 Nishi Hitotsuya, Settsu-shi, Osaka 566-8585 (Japan); Masunaga, H; Sasaki, S; Takata, M [Japan Synchrotron Research Institute, Mikazuki Sayo, Hyogo 671-5198 (Japan); Sakata, O, E-mail: takahara@cstf.kyushu-u.ac.j [RIKEN Harima Institute, Mikazuki Sayo, Hyogo 671-5198 (Japan)

    2009-08-01

    Fluoropolymer brush with crystalline side chains was prepared by surface-initiated atom transfer radical polymerization of 2-(perfluorooctyl)ethyl acrylate (FA-C{sub 8}) from a flat silicon substrate. The crystallization and the molecular aggregation structures of polymer side chain at the outermost surface and internal region in the brush film were characterized by grazing incidence X-ray diffraction (GIXD) measurement using two different incident angles of X-ray. At the air interface of PFA-C{sub 8} brush film, the rod-like R{sub f} group was oriented perpendicular to the surface forming a hexagonal packing structure to reduce surface energy. In contrast, the oriented R{sub f} groups parallel to the substrate coexisted at the internal region in the brush. This unique depth dependence of crystalline state of the fluoropolymer brush was observed by surface-sensitive GIXD measurement.

  15. Structure of a monolayer of molecular rotors on aqueous subphase from grazing-incidence X-ray diffraction.

    Science.gov (United States)

    Kaleta, Jiří; Wen, Jin; Magnera, Thomas F; Dron, Paul I; Zhu, Chenhui; Michl, Josef

    2018-03-23

    In situ grazing-incidence X-ray scattering shows that a monolayer of artificial rod-shaped dipolar molecular rotors produced on the surface of an aqueous subphase in a Langmuir trough has a structure conducive to a 2D ferroelectric phase. The axes of the rotors stand an average of 0.83 nm apart in a triangular grid, perpendicular to the surface within experimental error. They carry 2,3-dichlorophenylene rotators near rod centers, between two decks of interlocked triptycenes installed axially on the rotor axle. The analysis is based first on simultaneous fitting of observed Bragg rods and second on fitting the reflectivity curve with only three adjustable parameters and the calculated rotor electron density, which also revealed the presence of about seven molecules of water near each rotator. Dependent on preparation conditions, a minor and variable amount of a different crystal phase may also be present in the monolayer.

  16. A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane

    Energy Technology Data Exchange (ETDEWEB)

    Veder, Jean-Pierre [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Nafady, Ayman [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Clarke, Graeme [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Williams, Ross P. [Centre for Materials Research, Department of Imaging and Applied Physics, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); De Marco, Roland, E-mail: r.demarco@curtin.edu.a [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Bond, Alan M. [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia)

    2011-01-01

    An easy to fabricate and versatile cell that can be used with a variety of electrochemical techniques, also meeting the stringent requirement for undertaking cyclic voltammetry under transient conditions in in situ electrocrystallization studies and total external reflection X-ray analysis, has been developed. Application is demonstrated through an in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) characterization of electrocrystallized cadmium (II)-tetracyanoquinodimethane material, Cd(TCNQ){sub 2}, from acetonitrile (0.1 mol dm{sup -3} [NBu{sub 4}][PF{sub 6}]). Importantly, this versatile cell design makes SR-GIXRD suitable for almost any combination of total external reflection X-ray analysis (e.g., GIXRF and GIXRD) and electrochemical perturbation, also allowing its application in acidic, basic, aqueous, non-aqueous, low and high flow pressure conditions. Nevertheless, the cell design separates the functions of transient voltammetry and SR-GIXRD measurements, viz., voltammetry is performed at high flow rates with a substantially distended window to minimize the IR (Ohmic) drop of the electrolyte, while SR-GIXRD is undertaken using stop-flow conditions with a very thin layer of electrolyte to minimize X-ray absorption and scattering by the solution.

  17. Grazing incidence X-ray diffraction study of the tilted phases of Langmuir films: Determination of molecular conformations using simulated annealing

    International Nuclear Information System (INIS)

    Pignat, J.; Daillant, J.; Cantin, S.; Perrot, F.; Konovalov, O.

    2007-01-01

    We have analyzed grazing incidence X-ray diffraction (GIXD) data from condensed phases of Langmuir films of long-chain fatty acids at the air-water using a new method consisting in a careful extraction of the structure factors followed by fitting of molecular parameters using simulated annealing. We show that the information contained in GIXD spectra is enough to obtain near-atomic structural information. In particular, we directly determine the orientation of the chain backbone planes and of the carboxylic headgroups, and we evaluate chain conformation defects

  18. Grazing incidence X-ray diffraction study of the tilted phases of Langmuir films: Determination of molecular conformations using simulated annealing

    Energy Technology Data Exchange (ETDEWEB)

    Pignat, J. [LIONS/Service de Chimie Moleculaire, CEA-Saclay bat. 125, F-91191 Gif-sur-Yvette Cedex (France); LPPI, universite de Cergy-Pontoise, 5 mail Gay-Lussac Neuville/Oise, 95031 Cergy-Pontoise Cedex (France); Daillant, J. [LIONS/Service de Chimie Moleculaire, CEA-Saclay bat. 125, F-91191 Gif-sur-Yvette Cedex (France)]. E-mail: jean.daillant@cea.fr; Cantin, S. [LPPI, universite de Cergy-Pontoise, 5 mail Gay-Lussac Neuville/Oise, 95031 Cergy-Pontoise Cedex (France); Perrot, F. [LPPI, universite de Cergy-Pontoise, 5 mail Gay-Lussac Neuville/Oise, 95031 Cergy-Pontoise Cedex (France); Konovalov, O. [ESRF, 6 rue Jules Horowitz, BP220, 38043 Grenoble Cedex (France)

    2007-05-23

    We have analyzed grazing incidence X-ray diffraction (GIXD) data from condensed phases of Langmuir films of long-chain fatty acids at the air-water using a new method consisting in a careful extraction of the structure factors followed by fitting of molecular parameters using simulated annealing. We show that the information contained in GIXD spectra is enough to obtain near-atomic structural information. In particular, we directly determine the orientation of the chain backbone planes and of the carboxylic headgroups, and we evaluate chain conformation defects.

  19. Surface and interface strains studied by x-ray diffraction

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi; Ichimiya, Ayahiko

    1998-01-01

    The authors have developed a technique of X-ray diffraction in order to measure strain fields near semiconductor surface and interface. The diffraction geometry is using the extremely asymmetric Bragg-case bulk reflection of a small incident angle to the surface and a large angle exiting from the surface. The incident angle of the X-rays is set near critical angle of total reflection by tuning X-ray energy of synchrotron radiation at the Photon Factory, Japan. For thermally grown-silicon oxide/Si(100) interface, the X-ray intensity of the silicon substrate 311 reflection has been measured. From comparison of the full width at half maxima (FWHM) of X-ray rocking curves of various thickness of silicon oxides, it has been revealed that silicon substrate lattice is highly strained in the thin (less than about 5 nm) silicon oxide/silicon system. In order to know the original silicon surface strain, the authors have also performed the same kind of measurements in the ultra-high vacuum chamber. A clean Si(111) 7x7 surface gives sharper X-ray diffraction peak than that of the native oxide/Si(111) system. From these measurements, it is concluded that the thin silicon oxide film itself gives strong strain fields to the silicon substrates, which may be the reason of the existence of the structural transition layer at the silicon oxide/Si interface

  20. Some simple ideas on x-ray reflection and grazing-incidence diffraction from thin surfactant films

    DEFF Research Database (Denmark)

    Kjær, K.

    1994-01-01

    For Langmuir films of long linear amphiphilic molecules at the air-water interface, grazing-incidence diffraction data resolved in terms of both the horizontal and vertical components of the scattering angle can be evaluated to a fair level of detail by means of a slide rule. Specular reflection ...... data require more sophisticated means although some rules of thumb can be formulated.......For Langmuir films of long linear amphiphilic molecules at the air-water interface, grazing-incidence diffraction data resolved in terms of both the horizontal and vertical components of the scattering angle can be evaluated to a fair level of detail by means of a slide rule. Specular reflection...

  1. X-ray diffraction device comprising cooling medium connections provided on the x-ray tube

    NARCIS (Netherlands)

    1996-01-01

    An X-ray diffraction device comprises a water-cooled X-ray tube which exhibits a line focus as well as, after rotation through 90 DEG , a point focus. Contrary to customary X-ray tubes, the cooling water is not supplied via the housing (12) in which the X-ray tube is mounted, but the cooling water

  2. Polarisation resonance in X-ray diffraction

    International Nuclear Information System (INIS)

    Goodman, P.; Paterson, D.; Matheson, S.

    1994-01-01

    The study of crystal structures by means of dynamic X-ray diffraction has placed a challenge to theoreticians to revise the X-ray diffraction theory based on Maxwell's equation. In this paper the feasibility of using 'polarisation resonance' as a tool in the determination of absolute configuration for asymmetric structures is investigated. Two (left- and right-handed), σ + and σ- , circular polarization states for 3-beam conditions are considered. Moreover, extending interaction into the 3 rd. dimension (normal to the beam) opens the possibility of absolute configuration determination of asymmetric structures in 3 dimensions. The computational scheme used is shown in terms of scattering diagrams. 7 refs., 1 tab., 6 figs

  3. Basic of X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-09-01

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

  4. Basic of X-ray diffraction

    International Nuclear Information System (INIS)

    Giacovazzo, C.

    1996-01-01

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

  5. Phase and Texture of Solution-Processed Copper Phthalocyanine Thin Films Investigated by Two-Dimensional Grazing Incidence X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Lulu Deng

    2011-07-01

    Full Text Available The phase and texture of a newly developed solution-processed copper phthalocyanine (CuPc thin film have been investigated by two-dimensional grazing incidence X-ray diffraction. The results show that it has β phase crystalline structure, with crystallinity greater than 80%. The average size of the crystallites is found to be about 24 nm. There are two different arrangements of crystallites, with one dominating the diffraction pattern. Both of them have preferred orientation along the thin film normal. Based on the similarities to the vacuum deposited CuPc thin films, the new solution processing method is verified to offer a good alternative to vacuum process, for the fabrication of low cost small molecule based organic photovoltaics.

  6. Glancing angle synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-09-01

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

  7. X-ray diffraction and chemical bonding

    International Nuclear Information System (INIS)

    Bats, J.W.

    1976-01-01

    Chemical bonds are investigated in sulfamic acid (H 3 N-SO 3 ), sodium sulfonlate dihydrate (H 2 NC 6 H 4 SO 3 Na.2H 2 O), 2,5-dimercaptothiadiazole (HS-C 2 N 2 S-SH), sodium cyanide dihydrate (NaCN.2H 2 O), sodium thiocyanate (NaSCN) and ammonium thiocyanate (NH 4 SCN) by X-ray diffraction, and if necessary completed with neutron diffraction. Crystal structures and electron densities are determined together with bond length and angles. Also the effects of thermal motion are discussed

  8. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Cernik, R.J.

    1996-01-01

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

  9. Evaluation of Poisson's ratio and Young's modulus of nitride films by combining grazing incidence X-ray diffraction and laser curvature techniques

    International Nuclear Information System (INIS)

    Chen, H.-Y.; Chen, J.-H.; Lu, F.-H.

    2007-01-01

    Measurements of Poisson's ratio and the Young's modulus of thin films have been problematic. In this work, evaluation of both Poisson's ratio and Young's modulus is conducted using grazing incidence X-ray diffraction combined with measurement of the induced stress. Poisson's ratio was evaluated from analysis of the X-ray diffraction data to obtain a strain-cos 2 α.sin 2 ψ plot. Moreover, the Young's modulus of the films could be also calculated from that plot as well as from the residual stress, which could be determined by a measurement of stress induced substrate curvature. The ternary nitride TiAlN is used as a model system for the evaluation. The films, prepared by cathodic arc plasma deposition, exhibited a strong (111) preferred orientation and a composition corresponding to Ti 0.6 Al 0.4 N. The measured Poisson's ratio and the Young's modulus of the films were 0.143 ± 0.003 and 310 ± 20 GPa, respectively, which are comparable to those reported in the literature

  10. Si Nanoribbons on Ag(110) Studied by Grazing-Incidence X-Ray Diffraction, Scanning Tunneling Microscopy, and Density-Functional Theory: Evidence of a Pentamer Chain Structure.

    Science.gov (United States)

    Prévot, Geoffroy; Hogan, Conor; Leoni, Thomas; Bernard, Romain; Moyen, Eric; Masson, Laurence

    2016-12-30

    We report a combined grazing incidence x-ray diffraction (GIXD), scanning tunneling microscopy (STM), and density-functional theory (DFT) study which clearly elucidates the atomic structure of the Si nanoribbons grown on the missing-row reconstructed Ag(110) surface. Our study allows us to discriminate between the theoretical models published in the literature, including the most stable atomic configurations and those based on a missing-row reconstructed Ag(110) surface. GIXD measurements unambiguously validate the pentamer model grown on the reconstructed surface, obtained from DFT. This pentamer atomistic model accurately matches the high-resolution STM images of the Si nanoribbons adsorbed on Ag(110). Our study closes the long-debated atomic structure of the Si nanoribbons grown on Ag(110) and definitively excludes a honeycomb structure similar to that of freestanding silicene.

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

    DEFF Research Database (Denmark)

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

    2008-01-01

    Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel to the subst......Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel...... to the substrate. The scattering data is interpreted as a trimodal texture of oriented perylene crystallites, induced by interactions between the perylene molecules and the oriented PTFE substrate. Three families of biaxial orientations are seen, with the axes (h = 1, 2, or 3) parallel to the PTFE alignment......, all having the ab-plane parallel to the substrate. About 92% of the scattered intensity corresponds to a population with highly parallel to (PTFE)....

  12. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    CERN Document Server

    Sasaki, Y C; Adachi, S; Suzuki, Y; Yagi, N

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements.

  13. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    International Nuclear Information System (INIS)

    Sasaki, Y.C.; Okumura, Y.; Adachi, S.; Suzuki, Y.; Yagi, N.

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements

  14. Diffraction anomalous fine structure using X-ray anomalous dispersion

    International Nuclear Information System (INIS)

    Soejima, Yuji; Kuwajima, Shuichiro

    1998-01-01

    A use of X-ray anomalous dispersion effects for structure investigation has recently been developed by using synchrotron radiation. One of the interesting method is the observation of anomalous fine structure which arise on diffraction intensity in energy region of incident X-ray at and higher than absorption edge. The phenomenon is so called Diffraction Anomalous Fine Structure (DAFS). DAFS originates in the same physical process an that of EXAFS: namely photoelectric effect at the corresponding atom and the interaction of photoelectron waves between the atom and neighboring atoms. In contrast with EXAFS, the method is available for only the crystalline materials, but shows effective advantages of the structure investigations by a use of diffraction: one is the site selectivity and the other is space selectivity. In the present study, demonstrations of a use of X-ray anomalous dispersion effect for the superstructure determination will be given for the case of PbZrO 3 , then recent trial investigations of DAFS in particular on the superlattice reflections will be introduced. In addition, we discuss about Forbidden Reflection near Edge Diffraction (FRED) which is more recently investigated as a new method of the structure analysis. (author)

  15. Intensity of diffracted X-rays from biomolecules with radiation damage caused by strong X-ray pulses

    International Nuclear Information System (INIS)

    Kai, Takeshi; Tokuhisa, Atsushi; Moribayashi, Kengo; Fukuda, Yuji; Kono, Hidetoshi; Go, Nobuhiro

    2014-01-01

    In order to realize the coherent X-ray diffractive imaging of single biomolecules, the diffraction intensities, per effective pixel of a single biomolecule with radiation damage, caused by irradiation using a strong coherent X-ray pulse, were examined. A parameter survey was carried out for various experimental conditions, using a developed simulation program that considers the effect of electric field ionization, which was slightly reported on in previous studies. The two simple relationships among the parameters were identified as follows: (1) the diffraction intensity of a biomolecule slightly increases with the incident X-ray energy; and that (2) the diffraction intensity is approximately proportional to the target radius, when the radius is longer than 400 Å, since the upper limit of the incident intensity for damage to the biomolecules marginally changes with respect to the target radius. (author)

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

    International Nuclear Information System (INIS)

    Mayolo, C.M.G. de.

    1991-01-01

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

  17. An X-ray grazing incidence phase multilayer grating

    CERN Document Server

    Chernov, V A; Mytnichenko, S V

    2001-01-01

    An X-ray grazing incidence phase multilayer grating, representing a thin grating placed on a multilayer mirror, is proposed. A high efficiency of grating diffraction can be obtained by the possibility of changing the phase shift of the wave diffracted from the multilayer under the Bragg and total external reflection conditions. A grazing incidence phase multilayer grating consisting of Pt grating stripes on a Ni/C multilayer and optimized for the hard X-ray range was fabricated. Its diffraction properties were studied at photon energies of 7 and 8 keV. The obtained maximum value of the diffraction efficiency of the +1 grating order was 9% at 7 keV and 6.5% at 8 keV. The data obtained are in a rather good accordance with the theory.

  18. Grazing incidence synchrotron X-ray diffraction of marbles consolidated with diammonium hydrogen phosphate treatments: non-destructive probing of buried minerals

    Science.gov (United States)

    Possenti, Elena; Colombo, Chiara; Conti, Claudia; Gigli, Lara; Merlini, Marco; Plaisier, Jasper Rikkert; Realini, Marco; Gatta, G. Diego

    2018-05-01

    Diammonium hydrogen phosphate (DAP)-based consolidating treatments react with carbonatic stones and form calcium phosphates phases, whose composition depends on the availability of free calcium ions. In this work, an innovative non-destructive approach based on grazing incidence X-ray diffraction (GIXRD) with synchrotron radiation (SR) is used to investigate DAP-treated Carrara marble specimens and to study the influence of the substrate composition on the crystallization of calcium phosphate phases. The outcomes indicate that the presence of compositional micro-heterogeneity of Carrara marble favours the formation of specific phases. Dicalcium phosphate dihydrate, a calcium phosphate with a low Ca/P molar ratio, is formed on carbonatic phases with a low Ca amount, such as dolomite grains and Mg-containing veins. Furthermore, this study highlights the potentialities of SR-GIXRD as a powerful non-destructive tool for the diagnostic of Cultural Heritage objects since it allows investigating the conservation history of stone materials and their interaction with the environment.

  19. Temperature-Dependent Change of Packing Structure of Condensed-Phase in a Micro-Phase Separated Langmuir Monolayer Studied by Grazing-Incidence X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Iimura, Ken-ichi [Department of Applied Chemisty, Faculty of Engineering, Utsunomiya University, 7-1-2 Yoto, Utsunomiya 321-8585, Utsunomiya (Japan); Kato, Teiji [Department of Applied Chemisty, Faculty of Engineering, Utsunomiya University, 7-1-2 Yoto, Utsunomiya 321-8585, Utsunomiya (Japan); Brezesinski, Gerald [Max-Planck Instutite of Colloids and Interfaces, Research Campus Golm, D-14476 Potsdam (Germany)

    2007-10-15

    Packing structure of condensed-phase in a binary mixed Langmuir monolayer of behenic acid (C22) and perfluoro-2,5,8-trimethyl-3,6,9-trioxadodecanoic acid (PFPE) on a cadmium acetate aqueous solution was studied by grazing incidence X-ray diffraction (GIXD) as a function of the subphase temperature. The measurements were made during temperature scan at a fixed molecular area to explain the morphological change of the condensed-phase domains due to a thermal treatment reported previously. Analysis of GIXD data implies that the condensed-phase domains are composed of only the C22 molecules perpendicularly oriented and very closely packed in a centered rectangular unit cell with orthorhombic distortion at low temperatures. As the temperature increases the area occupied by molecule increases, and above 25 deg. C the lattice becomes disordered, which would allow morphological transformation of the condensed-phase domains. The process of packing structure change is almost reversible except for non-equilibrium phases observed for the monolayer spread at a low temperature, 5.5 deg. C.

  20. Packing stress reduction in polymer-lipid monolayers at the air-water interface: An X-ray grazing-incidence diffraction and reflectivity study

    Energy Technology Data Exchange (ETDEWEB)

    Kuhl, T.L.; Majewski, J.; Howes, P.B.; Kjaer, K.; Nahmen, A. von; Lee, K.Y.C.; Ocko, B.; Israelachvili, J.N.; Smith, G.S.

    1999-08-25

    Using synchrotron grazing-incidence X-ray diffraction (GIXD) and reflectivity (XR), the authors have determined the in-plane and out-of-plane structure of phospholipid monolayers at the air-water interface as a function of hydrophilic lipid headgroup size. Di-stearoyl-phosphatidyl-ethanolamine (DSPE) lipid monolayers were systematically modified by chemically grafting hydrophilic poly(ethylene glycol) (PEG) chains of MW = 90 g/mol (2 ethylene oxide, EO, units), MW = 350 g/mol (8 EO units), and MW = 750 g/mol (17 EO units) to the lipid headgroups. The monolayers were studied in the solid phase at a surface pressure of 42 mN/m. At these high lipid packing densities, the PEG chains are submerged in the water subphase. The increased packing stresses from these bulky polymer headgroups distort the unit cell and the in-plane packing modes of the monolayers, leading to large out-of-plane alterations and staggering of the lipid molecules. Surprisingly, a change in the molecular packing of the monolayer toward higher packing densities (lower area per molecule) was observed on increasing the PEG MW to 750 g/mol (17 EO units). This rearrangement of the monolayer structure may be due to a conformational change in the PEG chains.

  1. In-situ grazing incidence X-ray diffraction measurements of relaxation in Fe/MgO/Fe epitaxial magnetic tunnel junctions during annealing

    Energy Technology Data Exchange (ETDEWEB)

    Eastwood, D.S. [Department of Physics, Durham University, South Road, Durham DH1 3LE (United Kingdom); Ali, M.; Hickey, B.J. [Department of Physics and Astronomy, University of Leeds, Leeds LS2 1JT (United Kingdom); Tanner, B.K., E-mail: b.k.tanner@dur.ac.uk [Department of Physics, Durham University, South Road, Durham DH1 3LE (United Kingdom)

    2013-12-15

    The relaxation of Fe/MgO/Fe tunnel junctions grown epitaxially on (001) MgO substrates has been measured by in-situ grazing incidence in-plane X-ray diffraction during the thermal annealing cycle. We find that the Fe layers are fully relaxed and that there are no irreversible changes during annealing. The MgO tunnel barrier is initially strained towards the Fe but on annealing, relaxes and expands towards the bulk MgO value. The strain dispersion is reduced in the MgO by about 40% above 480 K post-annealing. There is no significant change in the “twist” mosaic. Our results indicate that the final annealing stage of device fabrication, crucial to attainment of high TMR, induces substantial strain relaxation at the MgO barrier/lower Fe electrode interface. - Highlights: • Lattice relaxation of Fe/MgO/Fe epitaxial magnetic tunnel junctions measured. • In-plane lattice parameter of Fe equal to bulk value; totally relaxed. • MgO barrier initially strained towards the Fe but relaxes on annealing. • Reduction in strain dispersion in the MgO barrier by 40% above about 470 K. • No change in the in-plane “twist” mosaic throughout the annealing cycle.

  2. Crystal and electronic structures of pentacene thin films from grazing-incidence x-ray diffraction and first-principles calculations

    International Nuclear Information System (INIS)

    Nabok, Dmitrii; Puschnig, Peter; Ambrosch-Draxl, Claudia; Werzer, Oliver; Resel, Roland; Smilgies, Detlef-M.

    2007-01-01

    Combined experimental and theoretical investigations on thin films of pentacene are performed in order to determine the structure of the pentacene thin film phase. Grazing incidence x-ray diffraction is used for studying a pentacene thin film with a nominal thickness of 180 nm. The crystal structure is found to exhibit the lattice parameters a=0.592 nm, b=0.754 nm, c=1.563 nm, α=81.5 deg. , β=87.2 deg. , and γ=89.9 deg. . These crystallographic unit cell dimensions are used as the only input parameters for ab initio total-energy calculations within the framework of density functional theory revealing the molecular packing within the crystal structure. Moreover, we calculate the electronic band structure of the thin film phase and compare it to that of the bulk phase. We find the intermolecular bandwidths of the thin film phase to be significantly larger compared to the bulk structure, e.g., the valence bandwidth is twice as large. This remarkable effect is traced back to an enhanced intermolecular π-π overlap due to the upright standing molecules in the thin film phase

  3. In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction-A powerful new technique for the characterization of electrochemical surfaces and interfaces

    Energy Technology Data Exchange (ETDEWEB)

    De Marco, Roland [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)]. E-mail: r.demarco@exchange.curtin.edu.au; Jiang, Z.-T. [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Martizano, Jay [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Lowe, Alex [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Pejcic, Bobby [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Riessen, Arie van [Materials Research Group, Department of Applied Physics, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)

    2006-08-15

    A marriage of electrochemical impedance spectroscopy (EIS) and in situ synchrotron radiation grazing incidence X-ray diffraction (SR-GIXRD) has provided a powerful new technique for the elucidation of the mechanistic chemistry of electrochemical systems. In this study, EIS/SR-GIXRD has been used to investigate the influence of metal ion buffer calibration ligands, along with natural organic ligands in seawater, on the behaviour of the iron chalcogenide glass ion-selective electrode (ISE). The SR-GIXRD data demonstrated that citrate - a previously reported poor iron calibration ligand for the analysis of seawater - induced an instantaneous and total dissolution of crystalline GeSe and Sb{sub 2}Se{sub 3} in the modified surface layer (MSL) of the ISE, while natural organic ligands in seawater and a mixture of ligands in a mimetic seawater ligand system protected the MSL's crystalline inclusions of GeSe and Sb{sub 2}Se{sub 3} from oxidative attack. Expectedly, the EIS data showed that citrate induced a loss in the medium frequency time constant for the MSL of the ISE, while seawater's natural organic ligands and the mimetic ligand system preserved the medium frequency EIS response characteristics of the ISE's MSL. The new EIS/SR-GIXRD technique has provided insights into the suitability of iron calibration ligands for the analysis of iron in seawater.

  4. Temperature-Dependent Change of Packing Structure of Condensed-Phase in a Micro-Phase Separated Langmuir Monolayer Studied by Grazing-Incidence X-ray Diffraction

    International Nuclear Information System (INIS)

    Iimura, Ken-ichi; Kato, Teiji; Brezesinski, Gerald

    2007-01-01

    Packing structure of condensed-phase in a binary mixed Langmuir monolayer of behenic acid (C22) and perfluoro-2,5,8-trimethyl-3,6,9-trioxadodecanoic acid (PFPE) on a cadmium acetate aqueous solution was studied by grazing incidence X-ray diffraction (GIXD) as a function of the subphase temperature. The measurements were made during temperature scan at a fixed molecular area to explain the morphological change of the condensed-phase domains due to a thermal treatment reported previously. Analysis of GIXD data implies that the condensed-phase domains are composed of only the C22 molecules perpendicularly oriented and very closely packed in a centered rectangular unit cell with orthorhombic distortion at low temperatures. As the temperature increases the area occupied by molecule increases, and above 25 deg. C the lattice becomes disordered, which would allow morphological transformation of the condensed-phase domains. The process of packing structure change is almost reversible except for non-equilibrium phases observed for the monolayer spread at a low temperature, 5.5 deg. C

  5. A high resolution position sensitive X-ray MWPC for small angle X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Tappern, G.J.

    1981-02-01

    A small sealed-off delay line readout MWPC X-ray detector has been designed and built for small angle X-ray diffraction applications. Featuring a sensitive area of 100 mm x 25 mm it yields a spatial resolution of 0.13 mm (standard deviation) with a high rate capability and good quantum efficiency for copper K radiation. (author)

  6. 100 years of discovery of X-ray diffraction

    International Nuclear Information System (INIS)

    Zhang Tao

    2012-01-01

    X-ray diffraction was discovered by Max von Laue a hundred years ago. Later, through the work of William H. Bragg and William L. Bragg, an experimental analysis method was developed to solve the structure of molecules at the atomic level. Over the past hundred years, science and technology has been dramatically changed by X-ray diffraction analysis, which has also undergone considerable development. The recent emergence of hard X-ray free electron lasers has provided a new dimension for X-ray diffraction analysis, promising even greater progress in the fields of physics, chemistry and biology. (author)

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

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray...... crystallography and X-ray absorption spectroscopy (XAS) applied to studying different hexameric insulin conformations. (iii) The structures of polymorphs of strontium ranelate and the distribution of strontium in bone tissue. A procedure for fast identification and verification of protein powders using XRPD...... was correction for disordered bulk-solvent, but also correction for background and optimization of unit cell parameters have to be taken into account. A sample holder was designed for collecting powder diffraction data on a standard laboratory X-ray powder diffractometer. The background was reduced by use...

  8. Strain, size and composition of InAs quantum sticks, embedded in InP, determined via X-ray anomalous diffraction and diffraction anomalous fine structure in grazing incidence

    International Nuclear Information System (INIS)

    Letoublon, A.; Favre-Nicolin, V.; Renevier, H.; Proietti, M.G.; Monat, C.; Gendry, M.; Marty, O.; Priester, C.

    2005-01-01

    We report on the study of strain, size and composition of small-size encapsulated semiconductor nanostructures. We show that the partial structure factor of As atoms in InAs stick-like nanostructures (quantum sticks), embedded in InP, can be directly extracted from grazing incidence anomalous X-ray diffraction maps at the As K-edge. We have recovered the average height and strain of the islands and determined their composition. The average height of the quantum sticks (QSs), as deduced from the width of the structure factor profile is 2.54 nm. The InAs out of plane deformation, relative to InP, is equal to 6.1%. Fixed-Q anomalous diffraction spectra, measured at the As K-edge, in grazing incidence provide clear evidence of pure InAs QSs. This is confirmed by the analysis of the diffraction anomalous fine structure (DAFS) that also gives a direct way to recover the strain accomodation inside the quantum sticks. Finite difference method calculations reproduce well the diffraction data. Chemical mixing at interfaces is at most 1 ML. This paper shows that ultimate application of anomalous diffraction and DAFS together with reciprocal space maps is a powerful method to sudy the structural properties of nanostructures

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

    International Nuclear Information System (INIS)

    Seminario, Max; Rocca, Jorge J.; Depine, Ricardo A.; Bach, Benny; Bach, Bernie

    2001-01-01

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

  10. X-ray Microprobe for Fluorescence and Diffraction Analysis

    International Nuclear Information System (INIS)

    Ice, G.E.

    2005-01-01

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

  11. Historical development of synchrotron x-ray diffraction topography

    International Nuclear Information System (INIS)

    Kawado, Seiji

    2011-01-01

    After a short history of X-ray diffraction topography, from the early stage of laboratory X-ray topography to recent synchrotron-radiation applications, is described, the development of science and technology for the synchrotron X-ray topography and its industrial applications are reviewed in more detail. In addition, the recent trend to synchrotron topography research is clarified on the basis of several data obtained from 256 papers which have been published since 2000. (author)

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  13. Interaction between lipid monolayers and poloxamer 188: An X-ray reflectivity and diffraction study

    DEFF Research Database (Denmark)

    Wu, G.H.; Majewski, J.; Ege, C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase ...

  14. Diffractive sub-picosecond manipulation of x-rays

    International Nuclear Information System (INIS)

    Adams, B.

    2004-01-01

    A class of X-ray optical elements for the sub-picosecond manipulation of X-rays is proposed. The design of these elements is based upon a time-dependent dynamical diffraction theory that synthesizes the eikonal theory with the Takagi-Taupin theory. A brief outline of the theory is given

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

    DEFF Research Database (Denmark)

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

    1988-01-01

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

  16. Preparation of specimens for analysis by: X-ray diffraction and X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Banos L, L.

    2004-01-01

    Specimen preparation is one of the most important requirements in the analysis of samples by X-ray Diffraction and X-ray Fluorescence. This statement is especially true for samples containing different types of materials. There are many forms of specimen suitable for X-ray analysis and the type of the sample as received will generally determine the method of pretreatment. It is convenient to refer to the material received for analysis as the sample, and that, which is actually analyzed as the specimen. The powder Diffraction method assumes that the particles in the specimen are ideally random orientation and that there are enough crystallites in the specimen to achieve a representative intensity distribution for these crystallites. X ray Fluorescence is essentially a comparative method of analysis, it is vital that all standards and unknowns be presented to the spectrometer in a reproducible and identical manner. (Author) 3 refs., 6 figs

  17. A differential scanning calorimetric and X-ray diffraction

    Indian Academy of Sciences (India)

    X-ray diffraction analysis of the two groups demonstrated predominance of austenitic ... Discrete crystallographic structure and absence of multiple phases showed ... Division of Orthodontics, Indian Army, 10 Corps Dental Unit, C/O 56 APO, ...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-09-01

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

  19. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

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

    1983-01-01

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

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

    International Nuclear Information System (INIS)

    Rodrigues, S.; Imasava, F.J.

    1988-01-01

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

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

  2. X-ray diffraction analysis of InAs nanowires

    International Nuclear Information System (INIS)

    Davydok, Anton

    2013-01-01

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

  3. CCD-based X-ray detectors for X-ray diffraction studies

    International Nuclear Information System (INIS)

    Ito, K.; Amemiya, Y.

    1999-01-01

    CCD-based X-ray detectors are getting to be used for X-ray diffraction studies especially in the studies where real time (automated) measurements and time-resolved measurements are required. Principles and designs of two typical types of CCD-based detectors are described; one is ths system in which x-ray image intensifiers are coupled to maximize the detective quantum efficiency for time-resolved measurements, and the other is the system in which tapered optical fibers are coupled for the reduction of the image into the CCD, which is optimized for automated measurements for protein crystallography. These CCD-based X-ray detectors have an image distortion and non-uniformity of response to be corrected by software. Correction schemes which we have developed are also described. (author)

  4. X-ray photoelectron spectroscopy, high-resolution X-ray diffraction ...

    Indian Academy of Sciences (India)

    the crystalline quality through full-width at half-maximum values. .... angular divergence of ∆α = 12 arc sec. X-rays generated from the monochromator were diffracted from (0 0 6) LiNbO3 atomic planes with the (+, −, −, +, +) geometry. [8].

  5. Simulating X-ray diffraction of textured films

    DEFF Research Database (Denmark)

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

    2008-01-01

    Computationally efficient simulations of grazing-incidence X-ray diffraction (GIXD) are discussed, with particular attention given to textured thin polycrystalline films on supporting substrates. A computer program has been developed for simulating scattering from thin films exhibiting varying...... degrees of preferred orientation. One emphasized common case is that of a 'fibre' symmetry axis perpendicular to the sample plane, resulting from crystallites having one well defined crystal facet towards the substrate, but no preferred inplane orientation. Peak splitting caused by additional scattering......, the mathematically simplest possible descriptions are sought whenever feasible. The practical use of the program is demonstrated for a selected thin-film example, perylene, which is of relevance for organic electronics....

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

    International Nuclear Information System (INIS)

    1992-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    1992-02-01

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

  8. Crystallized solids characterization by X-ray diffraction

    International Nuclear Information System (INIS)

    Broll, N.

    1996-01-01

    This work deals with the crystallized solids characterization by X-ray diffraction. The powders diffraction principle is described. Then are given the different powders diffraction experimental methods. An X-ray diffraction device is essentially constituted of three parts: the X-rays source, the sample and the detector. The source is usually constituted by an X-rays tube whereas the sample can be fixed on a photographic chamber or put on a goniometer. The different photographic chambers which can be used (Debye-Scherrer, Seeman-Bohlin and Guinier) are described. The powders diffractometer the most used is a Bragg-Brentano focusing diffractometer because it allows to obtain very sharp spectral lines and an important diffracted intensity. The detectors which are the mainly used are the scintillation counters. The most important use in powders diffractometry is the identification of the different phases of a sample. The phases identification consists to compare the unknown sample spectrum at those of standard materials indexed until now. Two methods exist at present. They are explained and their limits in the phases search are given. Another use of the X-ray diffraction is the quantitative analysis. It consists to determine the concentrations of each crystal phases of a sample. The principles of these quantitative methods are given. The lattice parameters of a polycrystal material can be determined from its X-ray pattern too with a very high precision. The way to index powders patterns is given. The residual stresses of materials can also be estimated. The principle of this measured method is explained. It is at last possible to study from an X-ray pattern, the material grain orientations during the different steps of preparation and working. (O.M.). 13 refs., 19 figs., 1 tab

  9. X-ray diffraction topography. Stages and tendencies of development

    International Nuclear Information System (INIS)

    Shul'pina, I.L.

    2000-01-01

    The physical foundation of X-ray diffraction topography, its methods, the achievements in image theory, the stages of evolution were described in this review. It was found that modern topography is well along in development associated with the use of third-generation synchrotron radiation and with its adaptation to advance materials and problems of materials science. Some proposals about prospects for X-ray topography progress in the future have been made [ru

  10. X-ray diffraction microtomography using synchrotron radiation

    CERN Document Server

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

    2001-01-01

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

  11. Three-dimensional x-ray diffraction detection and visualization

    International Nuclear Information System (INIS)

    Allahkarami, Masoud; Hanan, Jay C

    2014-01-01

    A new method of sensing and analyzing three-dimensional (3D) x-ray diffraction (XRD) cones was introduced. Using a two-dimensional area detector, a sequence of frames was collected while moving the detector away from the sample with small equally spaced steps and keeping all other parameters constant. A 3D dataset was created from the subsequent frames. The 3D x-ray diffraction (XRD 3 ) pattern contains far more information than a one-dimensional profile collected with the conventional diffractometer and 2D x-ray diffraction (XRD 2 ). The present work discusses some fundamentals about XRD 3 , such as the data collection method, 3D visualization, diffraction data interpretation and potential applications of XRD 3 . (paper)

  12. High resolution X-ray diffraction studies on unirradiated

    Indian Academy of Sciences (India)

    High-resolution X-ray diffraction technique, employing a three-crystal monochromator–collimator combination is used to study the irradiation induced defects in flux grown Sr-hexaferrite crystals irradiated with 50 MeV Li3+ ion beams at room temperature with a fluence value of 1 × 1014 ions/cm2. The diffraction curves of the ...

  13. X-ray Laue diffraction with allowance for second derivatives of amplitudes in dynamical diffraction equations

    International Nuclear Information System (INIS)

    Balyan, M.K.

    2014-01-01

    Asymmetrical Laue diffraction in a perfect crystal with a plane entrance surface is considered. The second derivatives of amplitudes in the direction, perpendicular to diffraction plane in the dynamical diffraction equations are taken into account. Using the corresponding Green function a general form for the amplitude of diffracted wave in the crystal is derived. The sizes of the source in both directions as well as the source of crystal distance and non-monochromaticity of the radiation incident on the crystal are taken into account. On the basis of obtained expression the coherent properties of the field depending on the sizes of the source and on the width of the spectrum of the incident radiation are analyzed. Taking into account the second derivatives of amplitudes with respect to the direction, perpendicular to the diffraction plane, the time dependent propagation equations for an X-ray pulse in a perfect crystal are given

  14. Coherent X-ray diffraction studies of mesoscopic materials

    International Nuclear Information System (INIS)

    Shabalin, Anatoly

    2015-12-01

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

  15. X-ray powder diffraction data on miscellaneous lanthanide compounds

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Hughes, T.E.

    1978-08-01

    Recent work on neutron absorbing materials has produced various new X-ray diffraction powder patterns of compounds of the lanthanides. Various inconsistencies in previously published data have been noted, and accurate measurements have been made of the lattice parameters of the rare earth oxides Sm 2 0 3 , Eu 2 0 3 , Gd 2 0 3 which have the monoclinic rare earth type B- structure, as well as Eu0. These data are recorded for reference. The optimum conditions for obtaining X-ray powder diffraction data from europium compounds are also noted. (author)

  16. Analytic theory of soft x-ray diffraction by lamellar multilayer gratings

    NARCIS (Netherlands)

    Kozhevnikov, I.V.; van der Meer, R.; Bastiaens, Hubertus M.J.; Boller, Klaus J.; Bijkerk, Frederik

    2011-01-01

    An analytic theory describing soft x-ray diffraction by Lamellar Multilayer Gratings (LMG) has been developed. The theory is derived from a coupled waves approach for LMGs operating in the single-order regime, where an incident plane wave can only excite a single diffraction order. The results from

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

    International Nuclear Information System (INIS)

    Dane V. Morgan

    2006-01-01

    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

  18. Direct methods for surface X-ray diffraction

    International Nuclear Information System (INIS)

    Saldin, D. K.; Harder, R.; Shneerson, V. L.; Vogler, H.; Moritz, W.

    2000-01-01

    We develop of a direct method for surface X-ray diffraction that exploits the holographic feature of a known reference wave from the substrate. A Bayesian analysis of the optimal inference to be made from an incomplete data set suggests a maximum entropy algorithm that balances agreement with the data and other statistical considerations

  19. X-Ray diffraction Investigation of Electrochemically Deposited Copper

    DEFF Research Database (Denmark)

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

    2004-01-01

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

  20. The three dimensional X-ray diffraction technique

    DEFF Research Database (Denmark)

    Juul Jensen, Dorte; Poulsen, Henning Friis

    2012-01-01

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

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

    DEFF Research Database (Denmark)

    Weichel, Steen; Grey, Francois; Rasmussen, Kurt

    2000-01-01

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

  2. Quantitative determination of phases by X-ray diffraction

    International Nuclear Information System (INIS)

    Azevedo, A.L.T.

    1979-01-01

    The internal standard method for the quantitative determination of phases by X-ray diffraction is presented. The method is applicable to multi-phase materials which may be treated as powder. A discussion on sample preparation and some examples follow. (Author) [pt

  3. Residual cold-work determination by X-ray diffraction

    International Nuclear Information System (INIS)

    Pireau, A.; Vanderborck, Y.

    1990-01-01

    The determination of the cold-work level of materials for fast breeder reactors can be made by different techniques. The report compares different methods for an application on austenitic stainless steels and demonstrates that the X-ray diffraction procedure is a reliable technique. A round robin test has been performed between three laboratories; the results are presented and discussed

  4. X-ray diffraction study of pure plutonium under pressure

    Energy Technology Data Exchange (ETDEWEB)

    Faure, Ph. [CEA, Valduc, F-21120 Is-sur-Tille (France)], E-mail: philippe.faure@cea.fr; Genestier, C. [CEA, Valduc, F-21120 Is-sur-Tille (France)

    2009-03-15

    Atomic volume and bulk modulus represent basic cohesion properties of a material and are therefore linked to many other physical properties. However, large discrepancies are found in the literature regarding values for the bulk modulus of pure plutonium ({alpha}-phase). New X-ray diffraction measurements of plutonium in diamond anvil cell are presented and the isothermal bulk modulus is extracted.

  5. The Marshall Grazing Incidence X-ray Spectrometer

    Science.gov (United States)

    Kobayashi, Ken; Winebarger, Amy R.; Savage, Sabrina; Champey, Patrick; Cheimets, Peter N.; Hertz, Edward; Bruccoleri, Alexander R.; Golub, Leon; Ramsey, Brian; Ranganathan, Jaganathan; Marquez, Vanessa; Allured, Ryan; Parker, Theodore; Heilmann, Ralf K.; Schattenburg, Mark L.

    2017-08-01

    The Marshall Grazing Incidence X-ray Spectrometer (MaGIXS) is a NASA sounding rocket instrument designed to obtain spatially resolved soft X-ray spectra of the solar atmosphere in the 6-24 Å (0.5-2.0 keV) range. The instrument consists of a single shell Wolter Type-I telescope, a slit, and a spectrometer comprising a matched pair of grazing incidence parabolic mirrors and a planar varied-line space diffraction grating. The instrument is designed to achieve a 50 mÅ spectral resolution and 5 arcsecond spatial resolution along a +/-4-arcminute long slit, and launch is planned for 2019. We report on the status and our approaches for fabrication and alignment for this novel optical system. The telescope and spectrometer mirrors are replicated nickel shells, and are currently being fabricated at the NASA Marshall Space Flight Center. The diffraction grating is currently under development by the Massachusetts Institute of Technology (MIT); because of the strong line spacing variation across the grating, it will be fabricated through e-beam lithography.

  6. Single photon energy dispersive x-ray diffraction

    International Nuclear Information System (INIS)

    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

    2014-01-01

    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. Single photon energy dispersive x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S. [Department of Physics, Clarendon Laboratory, University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H. [Lawrence Livermore National Laboratory, Livermore, California 94551 (United States); Tang, Henry [Department of Earth and Planetary Science, University of California Berkeley, Berkeley, California 94720 (United States)

    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.

  8. Adjustable Grazing-Incidence X-Ray Optics

    Science.gov (United States)

    O'Dell, Stephen L.; Reid, Paul B.

    2015-01-01

    With its unique subarcsecond imaging performance, NASA's Chandra X-ray Observatory illustrates the importance of fine angular resolution for x-ray astronomy. Indeed, the future of x-ray astronomy relies upon x-ray telescopes with comparable angular resolution but larger aperture areas. Combined with the special requirements of nested grazing-incidence optics, mass, and envelope constraints of space-borne telescopes render such advances technologically and programmatically challenging. The goal of this technology research is to enable the cost-effective fabrication of large-area, lightweight grazing-incidence x-ray optics with subarcsecond resolution. Toward this end, the project is developing active x-ray optics using slumped-glass mirrors with thin-film piezoelectric arrays for correction of intrinsic or mount-induced distortions.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

    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

  10. Raman spectroscopy and X-ray diffraction studies on celestite

    International Nuclear Information System (INIS)

    Chen Yenhua; Yu Shucheng; Huang, Eugene; Lee, P.-L.

    2010-01-01

    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.

  11. Interest of the grazing X ray diffraction to study the evolution of materials under irradiation: behaviour of zirconia under irradiation; Utilisation de la diffraction des rayons X en incidence rasante pour l'etude des solides irradies: application a la zircone

    Energy Technology Data Exchange (ETDEWEB)

    Simeone, D.; Gosset, D.; Bechade, J.L. [CEA Saclay, Dept. des Materiaux pour le Nucleaire DMN, 91 - Gif-sur-Yvette (France)

    2001-07-01

    This document was written to show that grazing X ray diffraction may be a powerful tool to study irradiation damages induced by ion beams in materials. Taking advantage of an asymmetric geometry and a curved detector, it is possible to analyse accurately diffraction diagrams at low angles by taking into account the specific effects induced by the grazing incidence. The interest of grazing incidence is to control the penetration depth of X rays. Such possibility allows to separate effects induced by damages (displacement cascades) and the implantation peak (elastic deformation of the lattice due to the insertion of projectile ions in the matrix). A Rietveld analysis on grazing X ray diagrams shows clearly that displacement cascades induce a phase transition on irradiated zirconia. (authors)

  12. Interest of the grazing X ray diffraction to study the evolution of materials under irradiation: behaviour of zirconia under irradiation; Utilisation de la diffraction des rayons X en incidence rasante pour l'etude des solides irradies: application a la zircone

    Energy Technology Data Exchange (ETDEWEB)

    Simeone, D; Gosset, D; Bechade, J L [CEA Saclay, Dept. des Materiaux pour le Nucleaire DMN, 91 - Gif-sur-Yvette (France)

    2001-07-01

    This document was written to show that grazing X ray diffraction may be a powerful tool to study irradiation damages induced by ion beams in materials. Taking advantage of an asymmetric geometry and a curved detector, it is possible to analyse accurately diffraction diagrams at low angles by taking into account the specific effects induced by the grazing incidence. The interest of grazing incidence is to control the penetration depth of X rays. Such possibility allows to separate effects induced by damages (displacement cascades) and the implantation peak (elastic deformation of the lattice due to the insertion of projectile ions in the matrix). A Rietveld analysis on grazing X ray diagrams shows clearly that displacement cascades induce a phase transition on irradiated zirconia. (authors)

  13. Surface morphology and in-plane-epitaxy of SmBa2Cu3O7-δ films on SrTiO3 (001) substrates studied by STM and grazing incidence x-ray diffraction

    DEFF Research Database (Denmark)

    Jiang, Q.D.; Smilgies, D.M.; Feidenhans'l, R.

    1996-01-01

    The surface morphology and in-plane epitaxy of thin films of SmBa(2)Cu3O(7-delta) (Sm-BCO) grown on SrTiO3 (001) substrates with various thicknesses have been investigated by scanning tunneling microscopy (STM) and grazing incidence x-ray diffraction (GIXRD). As revealed by GIXRD, SmBCO films as ...... films above h(c2), introduction of screw dislocations leads to spiral growth.......The surface morphology and in-plane epitaxy of thin films of SmBa(2)Cu3O(7-delta) (Sm-BCO) grown on SrTiO3 (001) substrates with various thicknesses have been investigated by scanning tunneling microscopy (STM) and grazing incidence x-ray diffraction (GIXRD). As revealed by GIXRD, SmBCO films...... substrate. Three different types of surface morphology were observed by STM with increasing film thickness h: a) 2D growth for hh(c2). With GIXRD, a density modulation is observed in the films with a thickness below h(c2). For thicker...

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    2016-08-15

    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{sup 7} molybdenum Kα photons.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. (paper)

  17. Modern X-ray diffraction. X-ray diffractometry for materials scientists, physicists, and chemicists. 2. rev. and enl. ed.

    International Nuclear Information System (INIS)

    Spiess, Lothar; Teichert, Gerd; Schwarzer, Robert; Behnken, Herfried; Genzel, Christoph

    2009-01-01

    This book offers a comprehensive survey over the applications of X-ray diffractions in fields like materials technique, metallurgy, electrotechniques, mechanical engineering, as well as micro- and nanotechniques. The necessary baic knowledges of X-ray diffraction are mediated foundedly and illustratively. Thereby new techniques and evaluation procedures are presented as well as well known methods

  18. Multiple x-ray diffraction simulation and applications

    International Nuclear Information System (INIS)

    Costa, C.A.B.S. da.

    1989-09-01

    A computer program (MULTX) was implemented for simulation X-ray multiple diffraction diagrams in Renninger geometries. The program uses the X-ray multiple diffraction theory for imperfect crystals. The iterative calculation of the intensities is based on the Taylor series general term, and the primary beam power expansion is given as function of the beam x penetration in the crystal surface. This development allows to consider the simultaneous interaction of the beams involved in the multiple diffraction phenomenon. The simulated diagrams are calculated point-to-point and the tests for the Si and GaAs presented good reproduction of the experimental diagrams for different primary reflections. (L.C.J.A.)

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

    Science.gov (United States)

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

    2009-05-01

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

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

    Science.gov (United States)

    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

    Science.gov (United States)

    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. Extinction correction in white X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Tomiyoshi, S.; Yamada, M.; Watanabe, H.

    1980-01-01

    Extinction effects in white-beam X-ray and neutron diffraction are considered. In white-beam diffraction, a small deviation of the wavelength from the Bragg condition Δlambda is a variable which represents the line profile of the diffraction peaks, so that by using the new parameter Δlambda the theory is converted to one in white-beam diffraction. It is shown that for a convex crystal, primary extinction agrees with the results calculated already for monochromatic diffraction. The same relation is shown to hold in secondary extinction. It is concluded that extinction theory derived for monochromatic diffraction is applicable without any modification in white-beam diffraction. (Auth.)

  3. Studies on strain relaxation of La{sub 0.5}Ba{sub 0.5}MnO{sub 3} film by normal and grazing incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Haiou [Hangzhou Dianzi University, Institute of Materials Physics, Hangzhou (China); Tan, Weishi [Hunan City University, College of Communication and Electronic Engineering, Yiyang (China); Nanjing University of Science and Technology, Key Laboratory of Soft Chemistry and Functional Materials, Department of Applied Physics, Ministry of Education, Nanjing (China); Liu, Hao [Suzhou Institute of Industrial Technology, Department of Electronic and Communication Engineering, Suzhou (China); Cao, Mengxiong; Wang, Xingyu; Ma, Chunlin [Nanjing University of Science and Technology, Key Laboratory of Soft Chemistry and Functional Materials, Department of Applied Physics, Ministry of Education, Nanjing (China); Jia, Quanjie [The Chinese Academy of Sciences, Institute of High Energy Physics, Beijing (China)

    2017-03-15

    Perovskite manganite La{sub 0.5}Ba{sub 0.5}MnO{sub 3} (LBMO) films were deposited on (001)-oriented single-crystal SrTiO{sub 3} (STO) substrates by pulsed laser deposition. High-resolution X-ray diffraction and grazing incidence X-ray diffraction techniques were applied to characterize the crystal structure and lattice strain of LBMO films. The in-plane and out-of-plane growth orientations of LBMO films with respect to substrate surface have been studied. The epitaxial orientation relationship LBMO (001) [100] //STO (001) [100] exists at the LBMO/STO interface. The lattice strain of LBMO film begins to relax with the thickness of LBMO film up to 12 nm. When the thickness is further increased up to 43 nm, the film is in fully strain-relaxed state. Jahn-Teller strain plays an important role in LBMO/STO system. The mechanism for strain relaxation is in accordance with that of tetragonal distortion. (orig.)

  4. X-ray diffraction and measurement of residual stresses

    International Nuclear Information System (INIS)

    Maeder, G.; Lebrun, J.L.; Corcaud, L.

    1977-01-01

    X-ray diffraction technique is a non destructive method for measuring the residual stresses in mechanical parts. This method, called sin 2 PSI method is investigated. It is applied to the measurement of elastic constants in different directions of crystals of Zr alloy (Zircaloy 4) and Ti alloy (TA6V). Stresses in TA6V sheets welded by TIG and electron beam processes are also studied [fr

  5. A structural view of Pd model catalysts : high-pressure surface X-Ray diffraction

    NARCIS (Netherlands)

    Rijn, Richard van

    2012-01-01

    This thesis describes the development of a combined high-pressure/ultrahigh-vacuum flow reactor for the study of model catalysts by means of surface x-ray diffraction and grazing incidence small angle scattering. The system was used to measure a stability diagram for the different oxide phases

  6. X-ray diffraction from single GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Biermanns, Andreas

    2012-11-12

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

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

    International Nuclear Information System (INIS)

    Gulden, Johannes

    2013-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Gulden, Johannes

    2013-03-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-10-15

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

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

    International Nuclear Information System (INIS)

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

    2006-10-01

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

  11. X-ray diffraction and imaging with a coherent beam: application to X-ray optical elements and to crystals exhibiting phase inhomogeneities

    International Nuclear Information System (INIS)

    Masiello, F.

    2011-05-01

    The exceptional properties of synchrotron light sources have been exploited in very different disciplines, from archaeology to chemistry, from material science to biology, from medicine to physics. Among these properties it is important to mention the high brilliance, continuum spectrum, high degree of polarization, time structure, small source size and divergence of the beam, the last resulting in a high transversal coherence of the produced radiation. This high transversal coherence of the synchrotron sources has permitted the development of new techniques, e.g. phase contrast imaging, X-ray photon correlation spectroscopy and coherent X-ray diffraction imaging (CXDI). This thesis work will consist essentially of three parts. In the first part it will be presented the work done as a member of the X-ray Optics Group of ESRF in the characterization of high quality diamond crystals foreseen as X-ray optical elements. The characterization has been done using different complementary X-ray techniques, such as high resolution diffraction, topography, grazing incidence diffraction, reflectivity and measurements of the coherence preservation using the Talbot effect. In the second part, I will show the result obtained in the study of the temperature behaviours of the domain in periodically poled ferroelectrics crystals. This type of measurements, based on Bragg-Fresnel diffraction, are possible only thanks to the high degree of coherence of the beam. In the third part, I will present the results obtained in the characterization of diamonds foreseen for applications other than X-ray optical elements. (author)

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

    Directory of Open Access Journals (Sweden)

    Robert M. Lawrence

    2015-07-01

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

  13. Diffraction enhanced kinetic depth X-ray imaging

    Science.gov (United States)

    Dicken, A.

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

  14. X-ray diffraction imaging of biological cells

    CERN Document Server

    Nakasako, Masayoshi

    2018-01-01

    In this book, the author describes the development of the experimental diffraction setup and structural analysis of non-crystalline particles from material science and biology. Recent advances in X-ray free electron laser (XFEL)-coherent X-ray diffraction imaging (CXDI) experiments allow for the structural analysis of non-crystalline particles to a resolution of 7 nm, and to a resolution of 20 nm for biological materials. Now XFEL-CXDI marks the dawn of a new era in structural analys of non-crystalline particles with dimensions larger than 100 nm, which was quite impossible in the 20th century. To conduct CXDI experiments in both synchrotron and XFEL facilities, the author has developed apparatuses, named KOTOBUKI-1 and TAKASAGO-6 for cryogenic diffraction experiments on frozen-hydrated non-crystalline particles at around 66 K. At the synchrotron facility, cryogenic diffraction experiments dramatically reduce radiation damage of specimen particles and allow tomography CXDI experiments. In addition, in XFEL ex...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-02-15

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

  16. Diamond-anvil cell for radial x-ray diffraction

    International Nuclear Information System (INIS)

    Chesnut, G N; Schiferl, D; Streetman, B D; Anderson, W W

    2006-01-01

    We have designed a new diamond-anvil cell capable of radial x-ray diffraction to pressures of a few hundred GPa. The diffraction geometry allows access to multiple angles of Ψ, which is the angle between each reciprocal lattice vector g(hkl) and the compression axis of the cell. At the 'magic angle', Ψ∼54.7 0 , the effects of deviatoric stresses on the interplanar spacings, d(hkl), are significantly reduced. Because the systematic errors, which are different for each d(hkl), are significantly reduced, the crystal structures and the derived equations of state can be determined reliably. At other values of Ψ, the effects of deviatoric stresses on the diffraction pattern could eventually be used to determine elastic constants

  17. X-ray diffraction measurements in KCl shocked along [100

    International Nuclear Information System (INIS)

    D'Almeida, T.; Gupta, Y.M.

    2000-01-01

    Real time x-ray diffraction measurements were used to examine the polymorphic phase transformation in KCl shocked along the [100] direction. Shock wave continuum data, obtained previously by Hayes, were used to design the experiments and to predict diffraction from KCl shocked to different peak stresses. Here, we present the results obtained below the transition stress: between 1.4 and 2 GPa. Diffraction data obtained were quantitatively related to macroscopic compression. Interplanar spacing measurements revealed isotropic compression of the unit cell in contrast to previously reported results. Above the transition stress, descriptions of the atomic arrangement with respect to shock propagation (not available in the literature) are required for setting up the detection system. Hence, continuum results in combination with various crystallographic considerations were utilized to obtain data above the transition stress

  18. X-ray diffraction of multilayers and superlattices

    International Nuclear Information System (INIS)

    Bartels, W.J.; Hornstra, J.; Lobeek, D.J.W.

    1986-01-01

    Recursion formulae for calculating the reflected amplitude ratio of multilayers and superlattices have been derived from the Takagi-Taupin differential equations, which describe the dynamical diffraction of X-rays in deformed crystals. Calculated rocking curves of complicated layered structures, such as non-ideal superlattices on perfect crystals, are shown to be in good agreement with observed diffraction profiles. The kinematical theory can save computing time only in the case of an ideal superlattice, for which a geometric series can be used, but the reflections must be below 10% so that multiple reflections can be neglected. For a perfect crystal of arbitrary thickness the absorption at the center of the dynamical reflection is found to be proportional to the square root of the reflectivity. Sputter-deposited periodic multilayers of tungsten and carbon can be considered as an artificial crystal, for which dynamical X-ray diffraction calculations give results very similar to those of a macroscopic optical description in terms of the complex index of refraction and Fresnel reflection coefficients. (orig.)

  19. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

    Goebel, H.E.; Snyder, R.L.

    1985-01-01

    The revival of interest in X-ray powder diffraction, being quoted as a metamorphosis from the 'ugly duckling' to a 'beautiful swan', can be attributed to a number of modern developments in instrumentation and evaluation software. They result in faster data collection, improved accuracy and resolution, and better detectability of minor phases. The ease of data evaluation on small computers coupled direct to the instrument allows convenient execution of previously tedious and time-consuming off-line tasks like qualitative and quantitative analysis, characterization of microcrystalline properties, indexing, and lattice-constant refinements, as well as structure refinements or even exploration of new crystal structures. Powder diffraction has also progressed from an isolated analytical laboratory method to an in situ technique for analysing solid-state reactions or for the on-stream control of industrial processes. The paper surveys these developments and their real and potential applications, and tries to emphasize new trends that are regarded as important steps for the further progress of X-ray powder diffraction

  20. X-ray diffraction analysis device with electronic photon counter

    International Nuclear Information System (INIS)

    Fillit, R.Y.; Bruyas, H.; Patay, F.

    1985-01-01

    The means provided to control the movements around the three axes are composed of step-by-step motors related to exits control logic which is connected to the calculation and monitored by a clock. The clock monitors also the calculator so as that the calculator controls, together with the programmable clock and control logic, the coordination of the whole rotation movements, along the three rotation axes, their velocity, their duration and the acquisition of the measured intensities of the diffracted X-ray beam [fr

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

    International Nuclear Information System (INIS)

    Duijn, J.H.

    1988-01-01

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

  2. Accidental exposure with X-ray diffraction equipment

    International Nuclear Information System (INIS)

    Montanez, O.; Blanco, D.

    1991-01-01

    The shutter on one of the windows of an X-ray diffraction apparatus was accidentally left open, exposing the worker to the radiation. The worker was wearing a dosimeter film, which was processed immediately to evaluate the potential risk. It was determined that the exposure rate was 350 Roentgen/minute on the skin surface, with corrections being made for the worker's thin clothing. It was concluded that in spite of the worker receiving a relative high dose, it did not reach the threshold value for producing deterministic effects such as cataracts, erythema, and skin damage

  3. New methods of X-ray diffraction spectrometry. II

    International Nuclear Information System (INIS)

    Soerum, H.; Bremer, J.

    1980-01-01

    The construction principles for a flexible X-ray spectrometer can be equipped either with a single curved crystal or with two curved crystals are described. A few of the theoretical 4+32 possible working modes are selected for a closer investigation and examples of recorded spectra are given. It is shown in the general single-crystal case that for a wavelength close to a cut-off energy the narrow diffraction cone has an elliptic section, as predicted by the theory. The spectrometer is discussed in terms of intensity, resolution and dispersive power. A comparison with other types of spectrometer is made. (Auth.)

  4. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

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

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...... for mobile applications, new materials with high gravimetric and volumetric storage capacity of hydrogen have to be developed. Alkali alanates are promising for hydrogen storage materials. Sodium alanate stores hydrogen reversibly at moderate conditions when catalysed with, e.g. titanium, whereas potassium...

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

    International Nuclear Information System (INIS)

    Als-Nielsen, J.

    1980-12-01

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

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

    International Nuclear Information System (INIS)

    Stern, Stephan

    2013-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Stern, Stephan

    2013-12-15

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

  8. X-ray Diffraction Study of Arsenopyrite at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    D Fan; M Ma; W Zhou; S Wei; Z Chen; H Xie

    2011-12-31

    The high-pressure X-ray diffraction study of a natural arsenopyrite was investigated up to 28.2 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at National Synchrotron Light Source, Brookhaven National Laboratory. The 16:3:1 methanol-ethanol-water mixture was used as a pressure-transmitting medium. Pressures were measured using the ruby-fluorescence method. No phase change has been observed up to 28.2 GPa. The isothermal equation of state (EOS) was determined. The values of K{sub 0}, and K'{sub 0} refined with a third-order Birch-Murnaghan EOS are K{sub 0} = 123(9) GPa, and K'{sub 0} = 5.2(8). Furthermore, we confirm that the linear compressibilities ({beta}) along a, b and c directions of arsenopyrite is elastically isotropic ({beta}{sub a} = 6.82 x 10{sup -4}, {beta}{sub b} = 6.17 x 10{sup -4} and {beta}{sub c} = 6.57 x 10{sup -4} GPa{sup -1}).

  9. Characterization of Brazilian asphalt using X-ray diffraction

    International Nuclear Information System (INIS)

    Cardoso, Edson R.; Pinto, Nivia G.V.; Almeida, Ana P.G.; Braz, Delson; Lopes, Ricardo T.; Barroso, Regina C.; Motta, Laura M.G.

    2007-01-01

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

  10. Quantitative analysis of minerals by X-ray diffraction

    International Nuclear Information System (INIS)

    Pietroluongo, L.R.V.; Veiga, M.M. da

    1982-01-01

    Considerations about the X-ray diffraction technique for quantitative analyses are made; some experiments carried out at CETEM - Centro de Tecnologia Mineral (Rio de Janeiro, Brazil) with synthetic samples and real samples of diatomites (from northeastern region of Brazil) are described. Quartz quantification has been a problem for analytical chemists and is of great importance to the industries which use this raw material. Comments are made about the main factors influencing the intensity of diffracted X-rays, such as: the crystallinity of the mineral phase; the granulometry, the preferential orientation; sample preparation and pressing, the chemical composition of standards and experimental analytical conditions. Several analytical methods used are described: direct measurement of the height or area of a peak resulting from a particular reflection and comparison with a pre-calibrated curve; method of sequential addition of the mineral of interest in the sample and extrapolation of results for ZERO addition; methods of external and internal standards. (C.L.B.) [pt

  11. Advances in thin film diffraction instrumentation by X-ray optics

    International Nuclear Information System (INIS)

    Haase, A.

    1996-01-01

    The structural characterisation of thin films requires a parallel X-ray beam of high intensity. Parallel beam geometry is commonly used in high resolution and single crystal experiments, but also in the field of X-ray diffraction for polycrystalline material (e.g. in phase, texture and stress analysis). For grazing incidence diffraction (GID), the use of small slits on the primary side and of long soller slits with a flat monochromator on the secondary side is standard. New optical elements have been introduced with polychromatic or monochromatic radiation. By means of different applications the results are compared with those of classical beam optics. X-ray fiber optics utilize total external reflection of X-rays on smooth surfaces. Effects of monochromatization are presented. In many fields of application, fiber optics may replace conventional collimators. The use of primary and secondary channel cut crystals can also produce a high parallel monochromatic X-ray beam. A parabolically bent graded multilayer produces a monochromatic parallel beam of high intensity. Compared with classical Bragg-Brentano (focussing) geometry, excellent results have been obtained, especially for samples with an irregular shape. In combination with a channel cut monochromator there is a substantial gain in intensity leading to an increase of the dynamic intensity range of rocking curves

  12. Advances in thin film diffraction instrumentation by X-ray optics

    Energy Technology Data Exchange (ETDEWEB)

    Haase, A [Rich. Seifert and Co., Analytical X-ray Systems, Ahrensburg (Germany)

    1996-09-01

    The structural characterisation of thin films requires a parallel X-ray beam of high intensity. Parallel beam geometry is commonly used in high resolution and single crystal experiments, but also in the field of X-ray diffraction for polycrystalline material (e.g. in phase, texture and stress analysis). For grazing incidence diffraction (GID), the use of small slits on the primary side and of long soller slits with a flat monochromator on the secondary side is standard. New optical elements have been introduced with polychromatic or monochromatic radiation. By means of different applications the results are compared with those of classical beam optics. X-ray fiber optics utilize total external reflection of X-rays on smooth surfaces. Effects of monochromatization are presented. In many fields of application, fiber optics may replace conventional collimators. The use of primary and secondary channel cut crystals can also produce a high parallel monochromatic X-ray beam. A parabolically bent graded multilayer produces a monochromatic parallel beam of high intensity. Compared with classical Bragg-Brentano (focussing) geometry, excellent results have been obtained, especially for samples with an irregular shape. In combination with a channel cut monochromator there is a substantial gain in intensity leading to an increase of the dynamic intensity range of rocking curves.

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

    International Nuclear Information System (INIS)

    Chavez R, A.

    2001-01-01

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

  14. A new theory for X-ray diffraction.

    Science.gov (United States)

    Fewster, Paul F

    2014-05-01

    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.

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  17. Variable-metric diffraction crystals for x-ray optics

    International Nuclear Information System (INIS)

    Smither, R.K.; Fernandez, P.B.

    1992-01-01

    A variable-metric (VM) crystal is one in which the spacing between the crystalline planes changes with position in the crystal. This variation can be either parallel to the crystalline planes or perpendicular to the crystalline planes of interest and can be produced by either introducing a thermal gradient in the crystal or by growing a crystal made of two or more elements and changing the relative percentages of the two elements as the crystal is grown. A series of experiments were performed in the laboratory to demonstrate the principle of the variable-metric crystal and its potential use in synchrotron beam lines. One of the most useful applications of the VM crystal is to increase the number of photons per unit bandwidth in a diffracted beam without losing any of the overall intensity. In a normal synchrotron beam line that uses a two-crystal monochromator, the bandwidth of the diffracted photon beam is determined by the vertical opening angle of the beam which is typically 0.10--0.30 mrad or 20--60 arcsec. When the VM crystal approach is applied, the bandwidth of the beam can be made as narrow as the rocking curve of the diffracting crystal, which is typically 0.005--0.050 mrad or 1--10 arcsec. Thus a very large increase of photons per unit bandwidth (or per unit energy) can be achieved through the use of VM crystals. When the VM principle is used with bent crystals, new kinds of x-ray optical elements can be generated that can focus and defocus x-ray beams much like simple lenses where the focal length of the lens can be changed to match its application. Thus both large magnifications and large demagnifications can be achieved as well as parallel beams with narrow bandwidths

  18. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface, Phase II

    Data.gov (United States)

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

  19. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface, Phase I

    Data.gov (United States)

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

  20. Acemetacin cocrystal structures by powder X-ray diffraction

    Science.gov (United States)

    Bolla, Geetha

    2017-01-01

    Cocrystals of acemetacin drug (ACM) with nicotinamide (NAM), p-aminobenzoic acid (PABA), valerolactam (VLM) and 2-pyridone (2HP) were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD) provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R 3 2(9)R 2 2(8)R 3 2(9) with three different syn amides (VLM, 2HP and caprolactam). The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I) or syn (type II). ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP) surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O⋯H, N⋯H, Cl⋯H and C⋯H interactions. The physicochemical properties of these cocrystals are under study. PMID:28512568

  1. Acemetacin cocrystal structures by powder X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Geetha Bolla

    2017-05-01

    Full Text Available Cocrystals of acemetacin drug (ACM with nicotinamide (NAM, p-aminobenzoic acid (PABA, valerolactam (VLM and 2-pyridone (2HP were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R32(9R22(8R32(9 with three different syn amides (VLM, 2HP and caprolactam. The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I or syn (type II. ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O...H, N...H, Cl...H and C...H interactions. The physicochemical properties of these cocrystals are under study.

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

    International Nuclear Information System (INIS)

    Smith, H.I.

    1988-01-01

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

  3. Secondary extinction in cylindrical and spherical crystals for X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Hu Huachen; Li Zhaohuan; Yang Bin; Shen Caiwan

    2001-01-01

    The distribution of the reflection power ratio for a neutron or x-ray diffracted from a cylindrical crystal immersed in an homogenous incident beam is obtained by the numerical solution of the transfer equations for the first time. The profile well reflects all the physical properties of the absorption and extinction behaviour in the crystals. A systematic investigation of the secondary extinction for cylindrical and spherical crystals was carried out based on these results

  4. Biological imaging by soft X-ray diffraction microscopy

    Science.gov (United States)

    Shapiro, David

    We have developed a microscope for soft x-ray diffraction imaging of dry or frozen hydrated biological specimens. This lensless imaging system does not suffer from the resolution or specimen thickness limitations that other short wavelength microscopes experience. The microscope, currently situated at beamline 9.0.1 of the Advanced Light Source, can collect diffraction data to 12 nm resolution with 750 eV photons and 17 nm resolution with 520 eV photons. The specimen can be rotated with a precision goniometer through an angle of 160 degrees allowing for the collection of nearly complete three-dimensional diffraction data. The microscope is fully computer controlled through a graphical user interface and a scripting language automates the collection of both two-dimensional and three-dimensional data. Diffraction data from a freeze-dried dwarf yeast cell, Saccharomyces cerevisiae carrying the CLN3-1 mutation, was collected to 12 run resolution from 8 specimen orientations spanning a total rotation of 8 degrees. The diffraction data was phased using the difference map algorithm and the reconstructions provide real space images of the cell to 30 nm resolution from each of the orientations. The agreement of the different reconstructions provides confidence in the recovered, and previously unknown, structure and indicates the three dimensionality of the cell. This work represents the first imaging of the natural complex refractive contrast from a whole unstained cell by the diffraction microscopy method and has achieved a resolution superior to lens based x-ray tomographic reconstructions of similar specimens. Studies of the effects of exposure to large radiation doses were also carried out. It was determined that the freeze-dried cell suffers from an initial collapse, which is followed by a uniform, but slow, shrinkage. This structural damage to the cell is not accompanied by a diminished ability to see small features in the specimen. Preliminary measurements on frozen

  5. X-ray diffraction patterns of thermally-reduced graphenes

    International Nuclear Information System (INIS)

    Ju, Hae-Mi; Choi, Sung-Ho; Huh, Seung-Hun

    2010-01-01

    Thermally-reduced graphenes (GPs) from graphene oxides (GOs) in the range of 200 - 800 .deg. C have been investigated by using X-ray diffraction (XRD). The temperature-dependent evolutions of the (002) peaks show that exfoliation of GO sheets occurs, along with wrinkling, at ∼200 .deg. C and that high-quality GPs are produced at ∼ 600 .deg. C (GP 600 ). These phenomena are explained by the vaporization of intercalated water molecules and the effective removal of the oxide groups of GO by thermal annealing, respectively. GP 600 exhibited a clean and sharp (002) peak corresponding to an interlayer distance of 3.392 A, which is close to that of conventional graphene (∼3.4 A). The structure of GP 600 is further discussed.

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

    Science.gov (United States)

    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.

  7. X-ray diffraction study of choline chloride's β form

    International Nuclear Information System (INIS)

    Petrouleas, V.; Lemmon, R.M.; Christensen, A.

    1978-01-01

    The organic salt choline chloride exists in two crystalline polymorphs. One (the α form) is extraordinarily sensitive to ionizing radiation, the other (the β form) is not. The present report describes an x-ray diffraction study of the β form. The structure has been found to be highly disordered face centered cubic. A reasonable least-square refinement of the intensity data has been achieved in the centrosymmetric space group Fm3 or Fm3m by use of a molecular model with restrained bond lengths. The results show that in the β form the electronic density due to the choline cation is closely spaced around the N, so that hydrogen bonding to the chloride is unlikely. Comparison with infrared and NMR data indicates that the disordering is dynamic and can be ascribed to rotations of the choline ion around crystallographic symmetry axes. Possible connections of these results with the radiation stability of the β form are discussed

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

    International Nuclear Information System (INIS)

    Hill, S.L.

    1988-01-01

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

  9. Phosphor Scanner For Imaging X-Ray Diffraction

    Science.gov (United States)

    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.

  10. X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

    Energy Technology Data Exchange (ETDEWEB)

    Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.; Kohn, V. G.; Marchenkova, M. A.; Pisarevskiy, Yu. V.; Prosekov, P. A., E-mail: prosekov@crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2016-05-15

    A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer of the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.

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

    CERN Document Server

    Hambach, D; Schneider, G

    2001-01-01

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

  12. Fundamentals of powder x-ray diffraction practice

    International Nuclear Information System (INIS)

    Raftery, T.

    2002-01-01

    Full text: The goal of powder Xray diffraction is to gain information about a specimen or sample. Key aspects of this goal are 1. the sample selection, preparation and presentation; 2. the data collection process and conditions; 3. the interaction between these and the interpretation of the data. The 'ideal' powder (or polycrystalline) xray diffraction sample is fine grained, randomly orientated, homogenous and representative. There exists standard sample selection and preparation techniques for powders - sometimes however, the required information must be gained by alternate sample selection and preparation techniques. While there are few variables in the data collection process, there are some significant ones such as matching diffractometer resolution and intensity to the data collection goal whether that is phase identity, quantitative analysis or structure refinement, etc. There are also options of optical arrangement (Bragg-Brintano versus parallel beam versus Debye-Scherrer). One important aspect of the collection process is the assessment of the data quality. Powder xray diffraction has many applications from the straight-forward confirmation of phase identity and purity to structural analysis. Some of these applications will be considered and the interaction between the goal of the application and aspects of sample selection. Copyright (2002) Australian X-ray Analytical Association Inc

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

    Energy Technology Data Exchange (ETDEWEB)

    Ichiyanagi, Kouhei; Sasaki, Yuji C. [Department of Advanced Materials Science, Graduate School of Frontier Sciences, The University of Tokyo, 609 Kiban Building 5-1-5 Kashiwanoha, Kahiwashi, Chiba 277-8561 (Japan); Japan Science and Technology Agency, CREST, CREST, Sasaki-Team, 609 Kiban Building, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8561 (Japan); Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Senba, Yasunori; Ohashi, Haruhiko; Ohta, Noboru [Japan Synchrotron Radiation Research Institute, SPring-8, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Hoshisashi, Kentaro; Jae-won, Chang; Tokue, Maki; Matsushita, Yufuku [Department of Advanced Materials Science, Graduate School of Frontier Sciences, The University of Tokyo, 609 Kiban Building 5-1-5 Kashiwanoha, Kahiwashi, Chiba 277-8561 (Japan); Nishijima, Masaki; Inoue, Yoshihisa [Department of Applied Chemistry and Office for University-Industry Collaboration, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan); Yagi, Naoto [Japan Science and Technology Agency, CREST, CREST, Sasaki-Team, 609 Kiban Building, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8561 (Japan); Japan Synchrotron Radiation Research Institute, SPring-8, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

    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.

  14. Effects of oxygen partial pressure and annealing temperature on the residual stress of hafnium oxide thin-films on silicon using synchrotron-based grazing incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Biswas, Debaleen [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064 (India); Sinha, Anil Kumar [ISU, Raja Ramanna Centre for Advanced Technology, Indore 452 013 (India); Homi Bhabha National Institute, BARC, Mumbai 400 094 (India); Chakraborty, Supratic, E-mail: supratic.chakraborty@saha.ac.in [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064 (India)

    2016-10-30

    Highlights: • Residual stress estimation thin hafnium oxide film with thickness of <10 nm. • A mathematical expression is proposed for stress estimation of thin-film using GIXRD. • Residual stress varies with argon content in Ar/O{sub 2} plasma and annealing temperature. • Variation of stress is explained by IL swelling and enhanced structural relaxation. - Abstract: Synchrotron radiation-based grazing incidence X-ray diffraction (GI-XRD) technique is employed here to estimate the residual stress of < 10 nm thin hafnium oxide film deposited on Si (100) substrate at different argon/oxygen ratios using reactive rf sputtering. A decrease in residual stress, tensile in nature, is observed at higher annealing temperature for the samples deposited with increasing argon ratio in the Ar/O{sub 2} plasma. The residual stress of the films deposited at higher p{sub Ar} (Ar:O{sub 2} = 4:1) is also found to be decreased with increasing annealing temperature. But the stress is more or less constant with annealing temperature for the films deposited at lower Ar/O{sub 2} (1:4) ratio. All the above phenomena can be explained on the basis of swelling of the interfacial layer and enhanced structural relaxation in the presence of excess Hf in hafnium oxide film during deposition.

  15. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

    Science.gov (United States)

    Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  16. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

    Science.gov (United States)

    Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

  17. Extended X-ray absorption fine structure and X-ray diffraction studies on supported Ni catalysts

    International Nuclear Information System (INIS)

    Aldea, N.; Marginean, P.; Yaning, Xie; Tiandou, Hu; Tao, Liu; Wu, Zhongua; ZhenYa, Dai

    1999-01-01

    In the first part of this paper, we present a study based on EXAFS spectroscopy. This method can yield structural information about the local environment around a specific atomic constituent in the amorphous materials, the location and chemical state of any catalytic atom on any support or point defect structures, in alloys and composites. EXAFS is a specific technique of the scattering of X-ray on materials. The present study is aimed toward elucidation of the local structure of Ni atoms and their interaction with oxide support. The second goal of the paper consists in X-ray diffraction on the same samples. X-ray diffraction method that is capable to determine average particle size, microstrains, probability of faults as well as particle size distribution function of supported Ni catalysts is presented. The method is based on the Fourier analysis of a single X-Ray diffraction profile. The results obtained on supported nickel catalysts, which are used in H/D isotopic exchange reactions are reported. The global structure is obtained with a new fitting method based on the Generalised Fermi Function facilities for approximation and Fourier transform of the experimental X-Ray line profiles. Both types of measurements were performed on Beijing Synchrotron Radiation Facilities (BSRF). (authors)

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

    International Nuclear Information System (INIS)

    Montemont, G.; Monnet, O.; Stanchina, S.; Verger, L.; Kosciesza, D.; Schlomka, J.P.

    2013-01-01

    We present the development of a CZT-based detection module dedicated to X-ray diffraction imaging. This kind of application requires a good energy and spatial resolution in order to resolve Bragg peaks. In a first part, we present the detector configuration used and dimensioning constraints. As the input energy range is comprised between 20 and 150 keV, we use 5 mm thick high resistivity CZT crystals. The 660 mm 2 detection area is segmented on both sides into 192 anodes and 12 cathodes. Signals from both sides are read jointly in order to perform multi parametric event corrections (depth of interaction, charge sharing, induction sharing). In order to be integrated easily inside an X-ray imaging system, the system has been conceived to be completely autonomous: it is powered by a single 12 V supply and is interfaced with the external system by Ethernet for communication and RS485 for synchronization. In a second part, we describe the system readout architecture and then the implementation of the data processing. An FPGA circuit embeds a digital processing chain that carries out readout ASIC interfacing and advanced multi parametric data corrections. Gain, offset but also depth of interaction and charge sharing are corrected on the flow. Incoming events from different channels are clustered together by comparing their location and time of occurrence. The FPGA also embeds a processor running an operating system that controls the system, carries out all calibrations, automated tests and acquisitions. Eventually, we show the results obtained and demonstrate the relative influence of depth of interaction and charge sharing. Homogeneity of detector behavior is also discussed and the reproducibility of the performance between modules is presented. The average energy resolution at 25 C is 2.4 % FWHM at 122 keV and 3.8 % FWHM at 60 keV and the average efficiency is 73 %. (authors)

  19. IL 12: Femtosecond x-ray powder diffraction

    International Nuclear Information System (INIS)

    Woerner, M.; Zamponi, F.; Rothhardt, P.; Ansari, Z.; Dreyer, J.; Freyer, B.; Premont-Schwarz, M.; Elsaesser, T.

    2010-01-01

    A chemical reaction generates new compounds out of one or more initial species. On a molecular level, the spatial arrangement of electrons and nuclei changes. While the structure of the initial and the product molecules can be measured routinely, the transient structures and molecular motions during a reaction have remained unknown in most cases. This knowledge, however, is a key element for the exact understanding of the reaction. The ultimate dream is a 'reaction microscope' which allows for an in situ imaging of the molecules during a reaction. We report on the first femtosecond x-ray powder diffraction experiment in which we directly map the transient electronic charge density in the unit cell of a crystalline solid with 30 pico-meter spatial and 100 femtosecond temporal resolution. X-ray diffraction from polycrystalline powder samples, the Debye Scherrer diffraction technique, is a standard method for determining equilibrium structures. The intensity of the Debye Scherrer rings is determined by the respective x-ray structure factor which represents the Fourier transform of the spatial electron density. In our experiments, the transient intensity and angular positions of up to 20 Debye Scherrer reactions from a polycrystalline powder are measured and unravel for the first time a concerted electron and proton transfer in hydrogen-bonded ionic (NH 4 ) 2 SO 4 crystals. Photoexcitation of ammonium sulfate induces a sub-100 fs electron transfer from the sulfate groups into a highly conned electron channel along the z-axis of the unit cell. The latter geometry is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps derived from the diffraction data display a periodic modulation of the channels charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A deeper insight into the underlying microscopic

  20. Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

    International Nuclear Information System (INIS)

    Voronov, D.L.; Warwick, T.; Gullikson, E. M.; Salmassi, F.; Padmore, H. A.

    2016-01-01

    High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs via numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4"t"h or 5"t"h order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.

  1. X-ray diffraction using the time structure of the SRS

    International Nuclear Information System (INIS)

    Tanner, B.K.

    1983-01-01

    The subject is discussed under the headings: introduction (advances in the techniques of X-ray topography; comparison with transmission electron microscopy); stroboscopic X-ray topography; stroboscopic X-ray topography of travelling surface acoustic waves; possible general diffraction experiments. (U.K.)

  2. X-ray diffraction studies of NbTe 2 single crystal

    Indian Academy of Sciences (India)

    The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size ...

  3. Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

    Energy Technology Data Exchange (ETDEWEB)

    Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil; Liu, Zunping; Lang, Keenan; Huang, Xianrong; Wieczorek, Michael; Kasman, Elina; Hammonds, John; Macrander, Albert; Assoufid, Lahsen [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2016-07-27

    We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity and spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.

  4. High-Resolution Detector For X-Ray Diffraction

    Science.gov (United States)

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

    1988-01-01

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

  5. Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

    Science.gov (United States)

    Tang, M X; Zhang, Y Y; E, J C; Luo, S N

    2018-05-01

    Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

  6. Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

    Energy Technology Data Exchange (ETDEWEB)

    Tang, M. X.; Zhang, Y. Y.; E, J. C.; Luo, S. N.

    2018-04-24

    Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

  7. Performances for confocal X-ray diffraction technology based on polycapillary slightly focusing X-ray optics

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hehe; Liu, Zhiguo [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Sun, Tianxi, E-mail: stxbeijing@163.com [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Peng, Song [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Ma, Yongzhong [Center for Disease Control and Prevention of Beijing, Beijing 100013 (China); Sun, Weiyuan; Li, Yude; Lin, Xiaoyan; Zhao, Weigang; Zhao, Guangcui; Luo, Ping; Pan, Qiuli; Ding, Xunliang [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

    2013-09-21

    The confocal X-ray diffraction (XRD) technology based on a polycapillary slightly focusing X-ray lens (PSFXRL) in excitation channel and a polycapillary parallel X-ray lens (PPXRL) with a long input focal distance in detection channel was developed. The output focal spot of the PSFXRL and the input focal spot of the PPXRL were adjusted in confocal configuration, and only the X-rays from the volume overlapped by these foci could be accordingly detected. This confocal configuration was helpful in decreasing background. The convergence of the beam focused by the PSFXRL and divergence of the beam which could be collected by the PPXRL with a long input focal distance were both about 9 mrad at 8 keV. This was helpful in improving the resolution of lattice spacing of this confocal XRD technology. The gain in power density of such PSFXRL and PPXRL was about 120 and 7 at 11 keV, respectively, which was helpful in using the low power source to perform XRD analysis efficiently. The performances of this confocal XRD technology were provided, and some common plastics were analyzed. The experimental results demonstrated that the confocal diffraction technology base on polycapillary slightly focusing X-ray optics had wide potential applications.

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

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Flesher, A.C.; Bryant, C.J.; Lincoln, A.D.; Tucker, P.A.; Swanton, S.W.

    1986-08-01

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

  9. Electrochemically adsorbed Pb on Ag (111) studied with grazing- incidence x-ray scattering

    International Nuclear Information System (INIS)

    Kortright, J.B.; Ross, P.N.; Melroy, O.R.; Toney, M.F.; Borges, G.L.; Samant, M.G.

    1989-04-01

    Grazing-incidence x-ray scattering studies of the evolution of electrochemically deposited layers of lead on silver (111) as a function of applied electrochemical potential are presented. Measurements were made with the adsorbed layers in contact with solution in a specially designed sample cell. The observed lead structures are a function of the applied potential and range from an incommensurate monolayer, resulting from underpotential deposition, to randomly oriented polycrystalline bulk lead, resulting from lower deposition potentials. These early experiments demonstrate the ability of in situ x-ray diffraction measurements to determine structures associated with electrochemical deposition. 6 refs., 4 figs

  10. X-ray diffraction imaging of material microstructures

    KAUST Repository

    Varga, Laszlo; Varga, Bonbien; Calo, Victor

    2016-01-01

    Various examples are provided for x-ray imaging of the microstructure of materials. In one example, a system for non-destructive material testing includes an x-ray source configured to generate a beam spot on a test item; a grid detector configured

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

    International Nuclear Information System (INIS)

    Salih, Suad Z.Elabdeen

    1997-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Allan

    1970-12-15

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

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

    International Nuclear Information System (INIS)

    Brown, Allan

    1970-12-01

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

  14. Federated repositories of X-ray diffraction images.

    Science.gov (United States)

    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.

  15. X-ray topography under conditions of monochromatic spherical wave diffraction

    International Nuclear Information System (INIS)

    Aristov, V.V.; Polovinkina, V.I.; Ibhikawa, Tetsuya; Kiduta, Seishi.

    1981-01-01

    An X-ray topographic scheme was developed in which there is a large distance between the X-ray source and the specimen. A monochromatic X-ray beam with an angular divergence 6 x 10 - 5 rad obtained by double successive diffraction in the (n 1 , +n 2 ) setting was used. This scheme enables diffraction focusing of a weakly absorbed wave field onto the exit surface of the crystal to be performed. Topographs of a wedge-shaped silicon crystal were obtained. Interference effects such as focusing, anomalous and ordinary Pendelloesung effects peculiar to X-ray spherical wave diffraction were observed in the topographs with high resolution. (author)

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

    DEFF Research Database (Denmark)

    Ludwig, Wolfgang; King, A.; Herbig, M.

    2010-01-01

    The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using...... propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray...

  17. Modifications to 8x8 dynamical theory: Polarizations redefined according to x-ray diffraction convention

    International Nuclear Information System (INIS)

    Macrander, A.T.; Blasdell, R.C.

    1993-09-01

    Dynamical x-ray diffraction theory can be cast in matrix form. In recent years, an 8x8 matrix theory was developed that treated asymmetric reflections from strained crystals. The polarization of the incident, specularly reflected, reflected diffracted, transmitted diffracted, and transmitted electromagnetic wave fields were all defined as s or p. That is, polarizations were defined with respect to the plane containing the incident beam direction and the surface normal. The authors present modifications of the theory to treat σ and π polarizations for Bragg diffraction from asymmetric planes, that is, for polarizations defined with respect to the plane containing the incident beam direction and the reciprocal lattice vector for Bragg diffraction. They present results of this theory for unstrained crystals in the inclined geometry. In this geometry the incident beam wavevector, the reciprocal lattice vector, and the surface normal are not coplanar. The inclined crystal geometry appears promising for use in a high-heat-load monochromator for undulator radiation at the Advanced Photon Source. As expected, they find a weak π-polarization component in the diffracted beam when the polarization of the incident beam is pure σ

  18. Development of glancing-incidence and glancing-take-off X-ray fluorescence apparatus for surface and thin-film analyses

    International Nuclear Information System (INIS)

    Tsuji, Kouichi; Wagatsuma, Kazuaki; Yamada, Takashi; Utaka, Tadashi

    1997-01-01

    We have studied X-ray fluorescence analysis under glancing incidence and glancing take-off conditions. Recently, we have developed a third apparatus for detecting glancing-incidence and take-off X-ray fluorescence, which makes it possible to measure the incident-angle dependence, the take-off-angle dependence. X-ray reflectivity, and X-ray diffraction. Primarily, we have measured the take-off angular dependence of X-ray fluorescence using this apparatus. Glancing take-off X-ray fluorescence has some advantages in comparison with glancing-incidence X-ray fluorescence. The surface density and the absolute angles were determined by analysing the take-off angle dependence of the fluorescent X-rays emitted from identical atoms with the aid of the reciprocity theorem. (Author)

  19. Liquid ammonia: Molecular correlation functions from x-ray diffraction

    International Nuclear Information System (INIS)

    Narten, A.H.

    1977-01-01

    For nearly spherical molecules the x-ray scattering from liquids yields structure and correlation functions for molecular centers. The distribution of electron density in an ammonia molecular is very nearly spherical, and orientational correlation between molecules in the liquid is not ''seen'' by x rays. Structure and correlation functions for molecular centers (nitrogen atoms) are derived from x-ray data on liquid NH 3 at 4 degreeC and tabulated. They provide a sensitive test for future work on a molecular theory of liquid ammonia

  20. Modelling the X-ray powder diffraction of nitrogen-expanded austenite using the Debye formula

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

    Stress-free and homogeneous samples of nitrogen-expanded austenite, a defect-rich f.c.c. structure with a high interstitial nitrogen occupancy (between 0.36 and 0.61), have been studied using X-ray powder diffraction and Debye simulations. The simulations confirm the presence of deformation...... to be indistinguishable to X-ray powder diffraction....

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

    Science.gov (United States)

    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…

  2. Qualitative analysis of powder x-ray diffraction data

    International Nuclear Information System (INIS)

    Raftery, T.

    1999-01-01

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

  3. Determination of global and local residual stresses in SOFC by X-ray diffraction

    International Nuclear Information System (INIS)

    Villanova, Julie; Sicardy, Olivier; Fortunier, Roland; Micha, Jean-Sebastien; Bleuet, Pierre

    2010-01-01

    Solid Oxide Fuel Cell (SOFC) is a high-performance electrochemical device for energy conversion. A single cell is composed of five layers made of different ceramic materials: anode support, anode functional layer, electrolyte, cathode functional layer and cathode. The mechanical integrity of the cell is a major issue during its lifetime, especially for the electrolyte layer. Damage of the cells is mainly due to the high operating temperature, the 'redox' behaviour of the anode and the brittleness of the involved materials. Since residual stresses are known to play a significant role in the damage evolution, it is important to determine them. For this purpose, residual stresses in an anode-supported planar SOFC were measured by X-ray diffraction. Firstly, macroscopic stresses in each phase of each layer were studied using the sin 2 ψ method on a laboratory X-ray goniometer at room temperature. This technique enables the calculation of residual stress of the material from the measurement of the crystal lattice deformation. The electrolyte has been found under bi-axial compressive stress of -920 MPa. Secondly, X-ray measurements controlling depth penetration were made in the electrolyte using grazing incidence method. The results show that the stress is not homogenous in the layer. The first five micrometers of the electrolyte have been found less constrained (-750 MPa) than the complete layer, suggesting a gradient of deformation in the electrolyte from the interface with the Anode Functional Layer to the free surface. Finally, local stress measurements were made on the electrolyte layer by X-ray synchrotron radiation that allows high accuracy measurement on the (sub-) micrometer scale. Polychromatic and monochromatic beams are used to determine the complete strain tensor from grain to grain in the electrolyte. First results confirm the macroscopic stress trend of the electrolyte. These X-ray techniques at different scales will contribute to a better understanding

  4. X-ray diffraction studies of the structure and orientations of thiophene and fluorenone based molecule

    International Nuclear Information System (INIS)

    Porzio, William; Pasini, Mariacecilia; Destri, Silvia; Giovanella, Umberto; Fontaine, Philippe

    2006-01-01

    The crystal structure of a conjugated molecule containing thiophene and fluorenone residues has been determined from powder X-ray diffraction (XRD). Thin films ( -5 Pa) onto oxidized silicon substrates, are oriented along with different crystallographic directions. A comparison of XRD in both Grazing Incidence and Bragg-Brentano geometries allowed to perform a quantitative analysis of the various orientations. This approach is generally applicable in the case of multi-oriented films. The results fully account for the poor performance of this molecule in p-type field effect transistor devices

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

    DEFF Research Database (Denmark)

    Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2008-01-01

    We derive the basic theoretical formulation for X-ray diffraction with pulsed fields, using a fully quantized description of light and matter. Relevant time scales are discussed for coherent as well as incoherent X-ray pulses, and we provide expressions to be used for calculation...... of the experimental diffraction signal for both types of X-ray sources. We present a simple analysis of time-resolved X-ray scattering for direct bond breaking in diatomic molecules. This essentially analytical approach highlights the relation between the signal and the time-dependent quantum distribution...

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

    DEFF Research Database (Denmark)

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

    2009-01-01

    Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes....... A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape...

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

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Flesher, A.C.; Tucker, P.A.; Swanton, S.W.

    1987-01-01

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

  8. The phase problem and perspectives of surface X-ray diffraction

    International Nuclear Information System (INIS)

    Tajiri, Hiroo; Takahashi, Toshio

    2009-01-01

    The emergence of synchrotron radiation sources has accelerated the application of diffraction techniques to surface sciences. Surface X-ray diffraction has become the state-of-the-art technique for determining ordered structures of atoms on crystal surfaces. We introduce surface X-ray diffraction briefly from the historical point of view and describe the concept that not only determine constellation of surface atoms but also view surface atoms as image. The progress in experimental and theoretical studies of surface X-ray diffraction including crystallographic direct methods is reviewed. (author)

  9. Phase transitions in diglyceride monolayers studied by computer simulations, pressure-area isotherms and x-ray diffraction

    DEFF Research Database (Denmark)

    Peters, Günther H.J.; Toxværd, S.; Larsen, N.B.

    1994-01-01

    1,2-sn-diglyceride monolayers exhibit unique and complex phase transitions as a function of surface pressure. The dynamical response of the layer on expanding the film has been investigated by computer simulations, (π-A) isotherms and grazing-incidence X-ray diffraction. Good agreement is found b...

  10. Three-dimensional visualization of a human chromosome using coherent x-ray diffraction

    International Nuclear Information System (INIS)

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

    2010-01-01

    We succeeded in observing a human chromosome in two- and three-dimensions using x-ray diffraction microscopy. X-ray diffraction microscopy is a lens-less imaging technique utilizing coherent x-ray diffraction, and can overcome various limitations in conventional lens-based x-ray microscopy. Biological applications of the method have been limited to 2D observation, and 3D observation has been long waited. We found that the reconstructed chromosome images contain high-density axial structure, which has not been observed under unstained or unlabeled conditions. The result experimentally demonstrates the effectiveness of x-ray diffraction microscopy in observing internal structures of unstained biological samples with high image contrast. (author)

  11. Single shot diffraction of picosecond 8.7-keV x-ray pulses

    Directory of Open Access Journals (Sweden)

    F. H. O’Shea

    2012-02-01

    Full Text Available We demonstrate multiphoton, single shot diffraction images of x rays produced by inverse Compton scattering a high-power CO_{2} laser from a relativistic electron beam, creating a pulse of 8.7 keV x rays. The tightly focused, relatively high peak brightness electron beam and high photon density from the 2 J CO_{2} laser yielded 6×10^{7} x-ray photons over the full opening angle in a single shot. Single shot x-ray diffraction is performed by passing the x rays though a vertical slit and on to a flat silicon (111 crystal. 10^{2} diffracted photons were detected. The spectrum of the detected x rays is compared to simulation. The diffraction and detection of 10^{2} x rays is a key step to a more efficient time resolved diagnostic in which the number of observed x rays might reach 10^{4}; enabling a unique, flexible x-ray source as a sub-ps resolution diagnostic for studying the evolution of chemical reactions, lattice deformation and melting, and magnetism.

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

    International Nuclear Information System (INIS)

    Srinivasan, C.; Balasingh, C.; Singh, A.K.

    1979-07-01

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

  13. Detectors for X-ray diffraction and scattering: a user's overview

    International Nuclear Information System (INIS)

    Bruegemann, Lutz; Gerndt, E.K.E.

    2004-01-01

    An overview of the applications of X-ray detectors to material research is given. Four experimental techniques and their specific detector requirements are described. Detector types are classified and critical parameters described in the framework of X-ray diffraction and X-ray scattering experiments. The article aims at building a bridge between detector end-users and detector developers. It gives limits of critical detector parameters, like angular resolution, energy resolution, dynamic range, and active area

  14. Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

    International Nuclear Information System (INIS)

    Tanaka, M; Katsuya, Y; Matsushita, Y

    2013-01-01

    The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe 2 O 4 and Fe 3 O 4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe 2+ /Fe 3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

  15. Design of a normal incidence multilayer imaging X-ray microscope

    Science.gov (United States)

    Shealy, David L.; Gabardi, David R.; Hoover, Richard B.; Walker, Arthur B. C., Jr.; Lindblom, Joakim F.

    Normal incidence multilayer Cassegrain X-ray telescopes were flown on the Stanford/MSFC Rocket X-ray Spectroheliograph. These instruments produced high spatial resolution images of the sun and conclusively demonstrated that doubly reflecting multilayer X-ray optical systems are feasible. The images indicated that aplanatic imaging soft X-ray/EUV microscopes should be achievable using multilayer optics technology. A doubly reflecting normal incidence multilayer imaging X-ray microscope based on the Schwarzschild configuration has been designed. The design of the microscope and the results of the optical system ray trace analysis are discussed. High resolution aplanatic imaging X-ray microscopes using normal incidence multilayer X-ray mirrors should have many important applications in advanced X-ray astronomical instrumentation, X-ray lithography, biological, biomedical, metallurgical, and laser fusion research.

  16. Partially coherent X-ray wavefront propagation simulations including grazing-incidence focusing optics.

    Science.gov (United States)

    Canestrari, Niccolo; Chubar, Oleg; Reininger, Ruben

    2014-09-01

    X-ray beamlines in modern synchrotron radiation sources make extensive use of grazing-incidence reflective optics, in particular Kirkpatrick-Baez elliptical mirror systems. These systems can focus the incoming X-rays down to nanometer-scale spot sizes while maintaining relatively large acceptance apertures and high flux in the focused radiation spots. In low-emittance storage rings and in free-electron lasers such systems are used with partially or even nearly fully coherent X-ray beams and often target diffraction-limited resolution. Therefore, their accurate simulation and modeling has to be performed within the framework of wave optics. Here the implementation and benchmarking of a wave-optics method for the simulation of grazing-incidence mirrors based on the local stationary-phase approximation or, in other words, the local propagation of the radiation electric field along geometrical rays, is described. The proposed method is CPU-efficient and fully compatible with the numerical methods of Fourier optics. It has been implemented in the Synchrotron Radiation Workshop (SRW) computer code and extensively tested against the geometrical ray-tracing code SHADOW. The test simulations have been performed for cases without and with diffraction at mirror apertures, including cases where the grazing-incidence mirrors can be hardly approximated by ideal lenses. Good agreement between the SRW and SHADOW simulation results is observed in the cases without diffraction. The differences between the simulation results obtained by the two codes in diffraction-dominated cases for illumination with fully or partially coherent radiation are analyzed and interpreted. The application of the new method for the simulation of wavefront propagation through a high-resolution X-ray microspectroscopy beamline at the National Synchrotron Light Source II (Brookhaven National Laboratory, USA) is demonstrated.

  17. [X-ray diffraction experiments with condenser matter

    International Nuclear Information System (INIS)

    Coppens, P.

    1990-01-01

    This report discusses research on the following topics: high-T c 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

  18. Structural Investigations of Nanowires Using X-Ray Diffraction

    DEFF Research Database (Denmark)

    Stankevic, Tomas

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

  19. X-ray powder diffraction in forensic practice

    Czech Academy of Sciences Publication Activity Database

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

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

  20. Refractive x-ray lens for high pressure diffraction

    International Nuclear Information System (INIS)

    Ohishi, Yasuo

    2001-01-01

    A stacked compound refractive x-ray lens was designed to produce a efficiently focused (φ 2 and a peak gain of 12, is well matched to these requirements. It is composed of many plastic chips made by molding, which is allowing many identical chips to be made precisely. Other advantages of this lens include high throughput, simple energy tunability and easy installation. (author)

  1. X-ray microscopy using grazing-incidence reflections optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1983-01-01

    The role of Kirkpatrick-Baez microscopes as the workhorse of the x-ray imaging devices is discussed. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  2. X-ray microscopy using grazing-incidence reflection optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1981-01-01

    The Kirkpatrick-Baez microscopes are described along with their role as the workhorse of the x-ray imaging devices. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  3. Physical methods for studying minerals and solid materials: X-ray, electron and neutron diffraction; scanning and transmission electron microscopy; X-ray, electron and ion spectrometry

    International Nuclear Information System (INIS)

    Eberhart, J.-P.

    1976-01-01

    The following topics are discussed: theoretical aspects of radiation-matter interactions; production and measurement of radiations (X rays, electrons, neutrons); applications of radiation interactions to the study of crystalline materials. The following techniques are presented: X-ray and neutron diffraction, electron microscopy, electron diffraction, X-ray fluorescence analysis, electron probe microanalysis, surface analysis by electron emission spectrometry (ESCA and Auger electrons), scanning electron microscopy, secondary ion emission analysis [fr

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

    Directory of Open Access Journals (Sweden)

    Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

    2009-01-01

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

  5. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    International Nuclear Information System (INIS)

    Chen Xing; Chu Wangsheng; Cai Quan; Xia Dingguo; Wu Zhonghua; Wu Ziyu

    2006-01-01

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L 2,3 edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced

  6. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    Energy Technology Data Exchange (ETDEWEB)

    Chen Xing [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Chu Wangsheng [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); University of Science and Technology of China, Hefei, 230036 (China); Cai Quan [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Xia Dingguo [College of Environmental and Energy Engineering, Beijing University of Technology, 100022 Beijing (China); Wu Zhonghua [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Wu Ziyu [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China) and National Center for Nanoscience and Technology (China)]. E-mail: wuzy@ihep.ac.cn

    2006-11-15

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L{sub 2,3} edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced.

  7. Degradation of periodic multilayers as seen by small-angle x-ray scattering and x-ray diffraction

    CERN Document Server

    Rafaja, D; Simek, D; Zdeborova, L; Valvoda, V

    2002-01-01

    The capabilities of small-angle x-ray scattering (SAXS) and wide-angle x-ray diffraction (XRD) to recognize structural changes in periodic multilayers were compared on Fe/Au multilayers with different degrees of structural degradation. Experimental results have shown that both methods are equally sensitive to the multilayer degradation, i.e., to the occurrence of non-continuous interfaces, to short-circuits in the multilayer structure and to the multilayer precipitation. XRD yielded additional information on the multilayer crystallinity, whilst SAXS could better recognize fragments of a long-range periodicity (remnants of the original multilayer structure). Changes in the multilayer structure were initiated by successive annealing at 200 and 300 deg. C. Experimental data were complemented by numerical simulations performed using a combination of optical theory and the distorted wave Born approximation for SAXS or the kinematical Born approximation for XRD.

  8. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Unknown

    X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and ... The layered structure compound, NbTe2, is one of the typical materials which lead to charge .... financial assistance to carry out this work. References. Brown B E 1966 Acta ...

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

    International Nuclear Information System (INIS)

    Souza, A.M. de; Carmo, L.C.S. do; Pereira, V.J.E.; Soares, E.A.

    1984-01-01

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

  10. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F.

    2012-01-01

    -Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms

  11. High-energy X-ray diffraction studies of disordered materials

    International Nuclear Information System (INIS)

    Kohara, Shinji; Suzuya, Kentaro

    2003-01-01

    With the arrival of the latest generation of synchrotron sources and the introduction of advanced insertion devices (wigglers and undulators), the high-energy (E≥50 keV) X-ray diffraction technique has become feasible, leading to new approaches in the quantitative study of the structure of disordered materials. High-energy X-ray diffraction has several advantages: higher resolution in real space due to a wide range of scattering vector Q, smaller correction terms (especially the absorption correction), reduction of truncation errors, the feasibility of running under extreme environments, including high-temperatures and high-pressures, and the ability to make direct comparisons between X-ray and neutron diffraction data. Recently, high-energy X-ray diffraction data have been combined with neutron diffraction data from a pulsed source to provide more detailed and reliable structural information than that hitherto available

  12. Characterization of sintered samples of La/Sr/Cu/O by X-ray diffraction, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS)

    International Nuclear Information System (INIS)

    Gonzalez, C.O. de; Polla, Griselda; Manghi, Estela

    1987-01-01

    Samples of La/Sr/Cu/O were sinterized by solid state reaction starting from a nominal composition of La 1 .8, Sr 0 .2, CuO 4 . They presented superconductive properties with T c = 40.9 K (onset) and δ T c = 17 K. Two phases were observed by X-ray diffraction and the more abundant was the tetragonal phase. The mean grain size was 1-5 μm. The X-ray photoelectron spectroscopy measurements were carried out using Mg kα (1486.6 eV) as incident radiation. Sample temperature was varied between -180 deg C and 420 deg C, approximately. The temperature variation produces a change in the atomic concentration of the surface components. Deconvolutions of the O 1s peaks show three components with binding energies (B.E.). The decomposition of Cu 2p 3 /2 peaks presents two components corresponding to Cu + and Cu 2+ . (Author) [es

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

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  14. Preferred orientation determination using line source x-ray diffraction

    International Nuclear Information System (INIS)

    Kimmel, G.; Shmarjahu, D.

    1977-10-01

    A texture goniometer has been attached to a diffractometer connected to a line-focus x-ray source. Reasonable results are obtained for the texture of rolled sheets and the test procedure is given. To illustrate the test procedure, the determination of preferred orientation in cold-rolled copper is described, as compared with random powder of sintered copper. Improvements of the measurements are proposed

  15. Quantitative determination of alpha-quartz in airborne dust samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz In airborne respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube Is employed. NiO is used as Internal standard In order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (Author) 17 refs

  16. Quantitative determination of alpha-quartz in airbone dust samples by X-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz in airbone respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube is employec. NiO is used as internal standard in order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (auth.) [es

  17. Reflectivity and diffraction of X rays applied to organic thin films

    International Nuclear Information System (INIS)

    Rieutord, Francois

    1987-01-01

    This research thesis reports the study of organic thin films by using X-ray-based technologies, and more particularly X-ray reflectivity. After some recalls on X ray diffraction, and on the fabrication of Langmuir-Blodgett films, the author shows how, by combining three X-ray-based techniques, it is possible to study a volume structure of a thin film. He describes the technique of measurement by X- ray reflexivity, its experimental implementation, and methods for result interpretation. In the next part, the author reports the study of peculiar interference effects which are noticed in reflexivity on Langmuir-Blodgett films, and then describes the nature of these films by correlating results of X ray reflexivity with direct observations performed by electronic microscopy on replica [fr

  18. Metrology and Alignment of Light Weight Grazing Incidence X-Ray Mirrors

    Science.gov (United States)

    Zhang, William; Content, David; Petre, Robert; Saha, Timo

    2000-01-01

    Metrology and alignment of light weight X-ray optics have been a challenge for two reasons: (1) that the intrinsic mirror quality and distortions caused by handling can not be easily separated, and (2) the diffraction limits of the visible light become a severe problem at the order of one arc-minute. Traditional methods of using a normal incident pencil or small parallel beam which monitors a tiny fraction of the mirror in question at a given time can not adequately monitor those distortions. We are developing a normal incidence setup that monitors a large fraction, if not the whole, of the mirror at any given time. It will allow us to align thin X-ray mirrors to-an accuracy of a few arc seconds or to a limit dominated by the mirror intrinsic quality.

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

    International Nuclear Information System (INIS)

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

    1998-06-01

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

  20. X-ray nanoprobes and diffraction-limited storage rings: opportunities and challenges of fluorescence tomography of biological specimens

    Energy Technology Data Exchange (ETDEWEB)

    Jonge, Martin D. de, E-mail: martin.dejonge@synchrotron.org.au [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia); Ryan, Christopher G. [CSIRO Earth Science and Research Engineering, Clayton, Victoria 3168 (Australia); Jacobsen, Chris J. [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Department of Physics, Chemistry of Life Processes Institute, Northwestern University, 2170 Campus Drive, Evanston, IL 60208 (United States); Chemistry of Life Processes Institute, Northwestern University, 2170 Campus Drive, Evanston, IL 60208 (United States)

    2014-08-27

    Nanoscale X-ray scanning microscopes, or X-ray nanoprobes, will benefit greatly from diffraction-limited storage rings. Here the requirements for nanoscale fluorescence tomography are explored to gain insight into the scientific opportunities and technical challenges that such sources offer. X-ray nanoprobes require coherent illumination to achieve optic-limited resolution, and so will benefit directly from diffraction-limited storage rings. Here, the example of high-resolution X-ray fluorescence tomography is focused on as one of the most voracious demanders of coherent photons, since the detected signal is only a small fraction of the incident flux. Alternative schemes are considered for beam delivery, sample scanning and detectors. One must consider as well the steps before and after the X-ray experiment: sample preparation and examination conditions, and analysis complexity due to minimum dose requirements and self-absorption. By understanding the requirements and opportunities for nanoscale fluorescence tomography, one gains insight into the R&D challenges in optics and instrumentation needed to fully exploit the source advances that diffraction-limited storage rings offer.

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

    International Nuclear Information System (INIS)

    Andreeva, N. S.

    2006-01-01

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

  2. Quantitative method of X-ray diffraction phase analysis of building materials

    International Nuclear Information System (INIS)

    Czuba, J.; Dziedzic, A.

    1978-01-01

    Quantitative method of X-ray diffraction phase analysis of building materials, with use of internal standard, has been presented. The errors committed by determining the content of particular phases have been also given. (author)

  3. Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

    Science.gov (United States)

    Chung, Frank H

    2017-05-01

    For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

  4. Structural investigation of GaInP nanowires using X-ray diffraction

    DEFF Research Database (Denmark)

    Kriegner, D.; Persson, Johan Mikael; Etzelstorfer, T.

    2013-01-01

    In this work the structure of ternary GaxIn1−xP nanowires is investigated with respect to the chemical composition and homogeneity. The nanowires were grown by metal–organic vapor-phase epitaxy. For the investigation of ensemble fluctuations on several lateral length scales, X-ray diffraction...... gradients along the sample by recording diffraction patterns at different positions. In addition, compositional variations were found also within single nanowires in X-ray energy dispersive spectroscopy measurements....

  5. Study of the solid solution formation in mixed oxides by X-ray diffraction

    International Nuclear Information System (INIS)

    Riella, H.G.

    1984-01-01

    A method to determine the plutonium distribution in mixed oxides - UO 2 /PuO 2 is described. The distribution function and the medium size of crystallite are obtained from the X-ray diffraction profile. Through the deconvolution by Fourier analysis, the X-ray diffraction profile is obtained without the influence of the difractrometer. Some experimental results for different samples of UO 2 -PuO 2 discussed. (Author) [pt

  6. On the evaluation of X-ray diffraction experiments by the regularization method

    Energy Technology Data Exchange (ETDEWEB)

    Trubin, V.A.; Szasz, A. (Lab. of Surface and Interface Physics, Eoetvoes Univ., Budapest (Hungary))

    1991-05-16

    The characteristic property of diffractometers as the presence of occasional and systematic errors in measured patterns requires such an evaluation which is as informative as possible. This circumstance gives rise to the problem of optimal planning of the experiment. The X-ray diffraction optimization problem with application of the regularization method is studied. The proposal permits to determine more accurately the unknown true characteristics of the X-ray diffraction experiment. (orig.).

  7. On the evaluation of X-ray diffraction experiments by the regularization method

    International Nuclear Information System (INIS)

    Trubin, V.A.; Szasz, A.

    1991-01-01

    The characteristic property of diffractometers as the presence of occasional and systematic errors in measured patterns requires such an evaluation which is as informative as possible. This circumstance gives rise to the problem of optimal planning of the experiment. The X-ray diffraction optimization problem with application of the regularization method is studied. The proposal permits to determine more accurately the unknown true characteristics of the X-ray diffraction experiment. (orig.)

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

    International Nuclear Information System (INIS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-01-01

    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. (orig.)

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

    Science.gov (United States)

    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.

  10. Device for high-temperature X-ray diffraction analysis. Ustrojstvo dlya vysokotemperaturnogo rentgenostrukturnogo analiza

    Energy Technology Data Exchange (ETDEWEB)

    Epifanov, V G; Zavilinskij, A V; Pet' kov, V V; Polenur, A V

    1975-01-07

    Device for high-temperature X-ray diffraction analysis, containing a vacuum chamber with a window for X-ray transit, in which sample- and standard-holders, heater, thermal shields and means for standard and sample temperature measurement are located, is proposed. In order to increase the working temperature level and the structural change detection accuracy the heater is located between the sample- and standard-holders. The standard-holder is linked with the mechanism of control of its position in relation to the heater. The device is intended for investigating phase transformations by differential thermal analysis method with the simultaneous diffraction pattern detection using X-ray diffractometry method.

  11. Neutron and X-ray diffraction from modulated structures

    International Nuclear Information System (INIS)

    Harris, P.

    1994-07-01

    This thesis describes X-ray and neutron scattering experiments performed on two examples of modulated structures. After an introduction to the subject of modulated structures, the thesis is divided in three parts. A single crystal elastic neutron scattering experiment between 4.2 and 115 Κ has been performed and four-circle X-ray data have been collected at 8 Κ for the monoclinic low-temperature phase of the layered perovskite PAMC. The results from the neutron scattering experiment indicate that magnetoelastic effects influence the ordering of the crystal. The X-ray experiments have made it possible to determine the crystal structure in the low-temperature phase. The superspace group is P2 1 /b(β-30)Os, with β = 1/3. A small-angle neutron scattering experiment has been performed on the magnetic structure of manganese silicide. When a magnetic field is applied, the modulation vectors turn towards the field direction, showing domain growth and diverging peak widths as they approach the field direction. Phase 'A' is established to have the modulation vectors directed perpendicular to the field direction. Cooling in zero field shows increasing peak widths at low temperatures, indicating a lock-in transition below the lowest reached temperature. To be able to analyse the data of the magnetic order in MnSi, and analytical calculation of the three dimensional resolution function for a small-angle neutron scattering spectrometer has been performed. The calculation is done by application of a combination of phase space analysis and Gaussian approximations for the neutron distribution as well as for the transmission functions of the different apertures. A finite mosaic spread of the crystal and finite correlation widths of the Bragg reflections have been included in the cross section. (au) (3 tabs., 48 ills., 100 refs.)

  12. X-Ray Diffraction and Reflectivity Validation of the Depletion Attraction in the Competitive Adsorption of Lung Surfactant and Albumin

    DEFF Research Database (Denmark)

    Stenger, Patric C.; Wu, Guohui; Miller, Chad E.

    2009-01-01

    as on a pristine interface, but with a more compact lattice corresponding to a small increase in the surface pressure. These results confirm that albumin adsorption creates a physical barrier that inhibits LS adsorption, and that PEG in the subphase generates a depletion attraction between the LS aggregates...... to subsequent LS adsorption that can be overcome by the depletion attraction induced by polyethylene glycol (PEG) in solution. A combination of grazing incidence x-ray diffraction (GIXD), x-ray reflectivity (XR), and pressure-area isotherms provides molecular-resolution information on the location...

  13. Residual stress analysis on materials with steep stress gradient by using X-ray incidence at higher angles

    International Nuclear Information System (INIS)

    Ohya, Shin-ichi; Yoshioka, Yasuo; Maeno, Shigeki

    1996-01-01

    X-ray stress measurements for isotropic polycrystalline are materials are usually carried out by the sin 2 ψ method under the assumption of no stress gradient in X-ray penetration depth. When a steep stress gradient exists in the vicinity of surface layer, however, non-linear sin 2 ψ relation is observed and the sin 2 ψ method cannot be applied on such cases. Although several X-ray stress analyzers have been developed for materials with steep stress gradient in the surface layer, it is desirable to use diffraction data at higher incident angles of ψ 0 as possible as close on 90 degrees in order to determine the both values of surface stress and stress gradient with high accuracy. In the present study, an X-ray stress analyzer based on Ω geometry was fabricated to enable X-ray incidence at higher angle of ψ 0 . The X-ray detector was positioned on -η side against X-ray incident beam. Both of the residual surface stress and stress gradient were determined by use of the COSψ method on shot-peened steel and silicon nitride specimens. This prototype stress analyzer was found effective to perform a biaxial or triaxial stress analysis. (author)

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

    International Nuclear Information System (INIS)

    Shtypulyak, N.I.; Yakimov, I.I.; Litvintsev, V.V.

    1989-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Katharina Fucke

    2010-07-01

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

  16. Background removal in X-ray fiber diffraction patterns

    International Nuclear Information System (INIS)

    Millane, R.P.; Arnott, S.

    1985-01-01

    Background can be a major source of error in measurement of diffracted intensities in fiber diffraction patterns. Errors can be large when poorly oriented less-crystalline specimens give diffraction patterns with little uncontaminated background. A method for estimating and removing a general global background in such cases is described and illustrated with an example. (orig.)

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

    Science.gov (United States)

    Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

    2007-06-26

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

  18. Correction of X-ray diffraction profiles in linear-type PSPC by position factor

    International Nuclear Information System (INIS)

    Takahashi, Toshio

    1992-01-01

    PSPC (Position Sensitive Proportional Counter) makes it possible to obtain one-dimentional diffraction profiles without mechanical scanning. In a linear-type PSPC, the obtained profiles need correcting, because the position factor influences the intensity of the diffracted X-ray beam and the counting rate at each position on PSPC. The distances from the specimen are not the same at the center and at the edge of the detector, and the intensity decreases at the edge because of radiation and absorption. The counting rate varies with the incident angle of the diffracted beam at each position on PSPC. The position factor f i at channel i of the multichannel-analyser is given by f i = cos 4 α i ·exp{-μR(1/cosα i -1)} where R is the distance between the specimen and the center of PSPC, μ is the linear absorption coefficient and α i is the incident angle of the diffracted beam at channel i. The background profiles of silica gel powder were measured with CrKα and CuKα. The parameters of the model function were fitted to the profiles by the non-linear least squares method. The agreement between these parameters and the calculated values shows that the position factor can correct the measured profiles properly. (author)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2016-06-01

    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.

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

    Science.gov (United States)

    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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    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{211} and Fe{310} plane families

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

    International Nuclear Information System (INIS)

    Bilello, J.C.

    1983-01-01

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

  4. Soft X-ray images of the solar corona using normal incidence optics

    Science.gov (United States)

    Bruner, M. E.; Haisch, B. M.; Brown, W. A.; Acton, L. W.; Underwood, J. H.

    1988-01-01

    A solar coronal loop system has been photographed in soft X-rays using a normal incidence telescope based on multilayer mirror technology. The telescope consisted of a spherical objective mirror of 4 cm aperture and 1 m focal length, a film cassette, and a focal plane shutter. A metallized thin plastic film filter was used to exclude visible light. The objective mirror was covered with a multilayer coating consisting of alternating layers of tungsten and carbon whose combined thicknesses satisfied the Bragg diffraction condition for 44 A radiation. The image was recorded during a rocket flight on October 25, 1985 and was dominated by emission lines arising from the Si XII spectrum. The rocket also carried a high resolution soft X-ray spectrograph that confirmed the presence of Si XII line radiation in the source. This image represents the first successful use of multilayer technology for astrophysical observations.

  5. X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

    Science.gov (United States)

    Girardin, E; Millet, P; Lodini, A

    2000-02-01

    To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

  6. Determination of electronic and atomic properties of surface, bulk and buried interfaces: Simultaneous combination of hard X-ray photoelectron spectroscopy and X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Rubio-Zuazo, J., E-mail: rubio@esrf.fr [SpLine, Spanish CRG BM25 Beamline at the ESRF, ESRF, B.P. 220, F-38043 Grenoble (France); Instituto de Ciencia de Materiales de Madrid, ICMM, CSIC, Cantoblanco, E-28049 Madrid (Spain); Castro, G.R. [SpLine, Spanish CRG BM25 Beamline at the ESRF, ESRF, B.P. 220, F-38043 Grenoble (France); Instituto de Ciencia de Materiales de Madrid, ICMM, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2013-10-15

    Highlights: •We have developed a novel and exceptional tool for non-destructive characterization of bulk and buried interfaces that combine XRD and HAXPES. •We studied the correlation between the atomic, electronic and transport properties of oxygen deficient manganite thin films. •The diffraction data showed a cooperative tilt of the MnO{sub 6} block along the out-of-plane direction. •We shown the absence of the conventional basal plane rotation for the oxygen deficient samples. -- Abstract: Hard X-ray photoelectron spectroscopy (HAXPES) is a powerful novel emerging technique for bulk compositional, chemical and electronic properties determination in a non-destructive way. It benefits from the exceptionally large escape depth of high kinetic energy photoelectrons enabling the study of bulk and buried interfaces up to several tens of nanometres depth. Its advantage over conventional XPS is based on the long mean free path of high kinetic energetic photoelectrons. Using the advantage of tuneable X-ray radiation provided by synchrotron sources the photoelectron kinetic energy, i.e. the information depth can be changed and consequently electronic and compositional depth profiles can be obtained. The combination of HAXPES with an atomic structure sensitive technique, as X-ray diffraction, opens a new research field with great potential for many systems in which their electronic properties are intimately linked to their crystallographic structure. At SpLine, the Spanish CRG Beamline at the European Synchrotron Radiation Facility (ESRF) we have developed a novel and exceptional set-up that combine grazing incidence X-ray diffraction (GIXRD) and HAXPES. Both techniques can be operated simultaneously on the same sample and using the same excitation source. The set-up includes a heavy 2S+3D diffractometer and UHV chamber equipped with an electrostatic analyzer. The UHV chamber has also MBE evaporation sources, an ion gun, a LEED optic, a sample heating and cooling

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

    Science.gov (United States)

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

    2003-01-01

    Application of in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2 to 30 nrn diameter in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (nanoparticles of different grain size.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-11

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

  9. Comparative study of macrotexture analysis using X-ray diffraction and electron backscattered diffraction techniques

    International Nuclear Information System (INIS)

    Serna, Marilene Morelli

    2002-01-01

    The macrotexture is one of the main characteristics in metallic materials, which the physical properties depend on the crystallographic direction. The analysis of the macrotexture to middles of the decade of 80 was just accomplished by the techniques of Xray diffraction and neutrons diffraction. The possibility of the analysis of the macrotexture using, the technique of electron backscattering diffraction in the scanning electronic microscope, that allowed to correlate the measure of the orientation with its location in the micro structure, was a very welcome tool in the area of engineering of materials. In this work it was studied the theoretical aspects of the two techniques and it was used of both techniques for the analysis of the macrotexture of aluminum sheets 1050 and 3003 with intensity, measured through the texture index 'J', from 2.00 to 5.00. The results obtained by the two techniques were shown reasonably similar, being considered that the statistics of the data obtained by the technique of electron backscatter diffraction is much inferior to the obtained by the X-ray diffraction. (author)

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

    International Nuclear Information System (INIS)

    Freyer, Benjamin

    2013-01-01

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

  11. X-ray diffraction and molecular-dynamics studies: Structural analysis of phases in diglyceride monolayers

    DEFF Research Database (Denmark)

    Peters, Günther H.J.; Larsen, Niels Bent; Bjørnholm, T.

    1998-01-01

    We report a detailed structural analysis of the phases of 1,2-sn-dipalmitoylglycerol Langmuir monolayers at room temperature. Pressure-induced transitions have been investigated by combination of molecular-dynamics simulations and grazing-incidence x-ray diffraction (XRD). The diglyceride film...... undergoes two phase transitions occurring at 38.3 and 39.8 Angstrom(2)/molecule. Simulation indicates that the first transition involves a reorientation of the headgroups while simulation and XRD show that in the second transition the order parameter is the tilt angle of the alkyl chains. A methodology......; At the lowest pressure the tilt angle reaches approximate to 14 degrees in a direction close to a nearest neighbor direction. Both arrangements of the alkyl chains are confirmed by XRD. For higher order and fractional order Bragg peaks, simulations predict higher intensities than observed with XRD. This may...

  12. Microbeam high-resolution diffraction and x-ray standing wave methods applied to semiconductor structures

    International Nuclear Information System (INIS)

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

    2004-01-01

    A new approach to conditioning x-ray microbeams for high angular resolution x-ray diffraction and scattering techniques is introduced. We combined focusing optics (one-bounce imaging capillary) and post-focusing collimating optics (miniature Si(004) channel-cut crystal) to generate an x-ray microbeam with a size of 10 μm and ultimate angular resolution of 14 μrad. The microbeam was used to analyse the strain in sub-micron thick InGaAsP epitaxial layers grown on an InP(100) substrate by the selective area growth technique in narrow openings between the oxide stripes. For the structures for which the diffraction peaks from the substrate and the film overlap, the x-ray standing wave technique was applied for precise measurements of the strain with a Δd/d resolution of better than 10 -4 . (rapid communication)

  13. Three-Dimensional X-Ray Diffraction Technique for Metals Science

    DEFF Research Database (Denmark)

    Zhang, Yubin; Fan, Guohua

    2017-01-01

    The three-dimensional X-ray diffraction (3DXRD) is a new, advanced technique for materials characterization. This technique utilizes high-energy synchrotron X-rays to characterize the 3D crystallographic structure and strain/stress state of bulk materials. As the measurement is non......-destructive, the microstructural evolution as a function of time can be followed, i.e. it allows 4D (x, y, z characterizations, t). The high brilliance of synchrotron X-rays ensures that diffraction signals from volumes of micrometer scale can be quickly detected and distinguished from the background noise, i.e. its spatial...... implemented in several large synchrotron facilities, e.g. the Advanced Photon Source (APS) in USA and the Spring-8 in Japan. Another family of 3DXRD technique that utilizes white beam synchrotron X-rays has also been developed in parallel in cooperation between Oak Ridge National Laboratory and APS...

  14. New tubes and techniques for flash X-ray diffraction and high contrast radiography

    International Nuclear Information System (INIS)

    Charbonnier, F.M.; Barbour, J.P.; Brewster, J.L.

    High energy electrons are particularly efficient in producing characteristic X-rays and soft polychromatic. A line of wide spectrum beryllium window flash X-ray tubes, ranging from 150 to 600kV, has been developed to exploit this property. Laue and Debye Scherrer flash X-ray diffraction patterns have been obtained using a single 30 ns pulse exposure. X-ray diffraction tests obtained are shown. Extremely high contrast flash radiography of small, low density objects has been obtained using industrial film without screen. Alternatively, particularly at high voltages and for subjects which include a broad range of materials and thicknesses, special film techniques can be used to produce extremely wide latitudes. Equipment, techniques and results are discussed

  15. Determination of the structure factors of a LiF powder sample by the energy dispersive x-ray diffraction

    International Nuclear Information System (INIS)

    Uno, R.; Ahtee, A.; Paakkari, T.

    1977-01-01

    The structure factors of a LiF powder sample were determined by energy dispersive x-ray diffraction in the range 9 to 25 keV, with the use of a Si(Li) solid state detector, following the method applied on GaP. Since the absorption coefficient of LiF is small at high energy, a fraction of the incident x-rays penetrates through the sample and does not contribute to the diffraction. This effect was taken into account in the determination of the structure factors. Then the structure factors generally agree, within the limit of 5 % error, with those obtained by the usual angle dispersive method, if the penetrated part of the incident beam is less than 40 %. (author)

  16. Development of low temperature and high magnetic field X-ray diffraction facility

    Energy Technology Data Exchange (ETDEWEB)

    Shahee, Aga; Sharma, Shivani; Singh, K.; Lalla, N. P., E-mail: nplallaiuc82@gmail.com; Chaddah, P. [UGC-DAE Consortium for Scientific Research, University campus, Khandwa Road, Indore-452001 (India)

    2015-06-24

    The current progress of materials science regarding multifunctional materials (MFM) has put forward the challenges to understand the microscopic origin of their properties. Most of such MFMs have magneto-elastic correlations. To investigate the underlying mechanism it is therefore essential to investigate the structural properties in the presence of magnetic field. Keeping this in view low temperature and high magnetic field (LTHM) powder x-ray diffraction (XRD), a unique state-of-art facility in the country has been developed at CSR Indore. This setup works on symmetric Bragg Brentano geometry using a parallel incident x-ray beam from a rotating anode source working at 17 kW. Using this one can do structural studies at non-ambient conditions i.e. at low- temperatures (2-300 K) and high magnetic field (+8 to −8 T). The available scattering angle ranges from 5° to 115° 2θ with a resolution better than 0.1°. The proper functioning of the setup has been checked using Si sample. The effect of magnetic field on the structural properties has been demonstrated on Pr{sub 0.5}Sr{sub 0.5}MnO{sub 3} sample. Clear effect of field induced phase transition has been observed. Moreover, the effect of zero field cooled and field cooled conditions is also observed.

  17. Three-dimensional structure determination protocol for noncrystalline biomolecules using x-ray free-electron laser diffraction imaging.

    Science.gov (United States)

    Oroguchi, Tomotaka; Nakasako, Masayoshi

    2013-02-01

    Coherent and intense x-ray pulses generated by x-ray free-electron laser (XFEL) sources are paving the way for structural determination of noncrystalline biomolecules. However, due to the small scattering cross section of electrons for x rays, the available incident x-ray intensity of XFEL sources, which is currently in the range of 10(12)-10(13) photons/μm(2)/pulse, is lower than that necessary to perform single-molecule diffraction experiments for noncrystalline biomolecules even with the molecular masses of megadalton and submicrometer dimensions. Here, we propose an experimental protocol and analysis method for visualizing the structure of those biomolecules by the combined application of coherent x-ray diffraction imaging and three-dimensional reconstruction methods. To compensate the small scattering cross section of biomolecules, in our protocol, a thin vitreous ice plate containing several hundred biomolecules/μm(2) is used as sample, a setup similar to that utilized by single-molecule cryoelectron microscopy. The scattering cross section of such an ice plate is far larger than that of a single particle. The images of biomolecules contained within irradiated areas are then retrieved from each diffraction pattern, and finally provide the three-dimensional electron density model. A realistic atomic simulation using large-scale computations proposed that the three-dimensional structure determination of the 50S ribosomal subunit embedded in a vitreous ice plate is possible at a resolution of 0.8 nm when an x-ray beam of 10(16) photons/500×500 nm(2)/pulse is available.

  18. Information extracting and processing with diffraction enhanced imaging of X-ray

    International Nuclear Information System (INIS)

    Chen Bo; Chinese Academy of Science, Beijing; Chen Chunchong; Jiang Fan; Chen Jie; Ming Hai; Shu Hang; Zhu Peiping; Wang Junyue; Yuan Qingxi; Wu Ziyu

    2006-01-01

    X-ray imaging at high energies has been used for many years in many fields. Conventional X-ray imaging is based on the different absorption within a sample. It is difficult to distinguish different tissues of a biological sample because of their small difference in absorption. The authors use the diffraction enhanced imaging (DEI) method. The authors took images of absorption, extinction, scattering and refractivity. In the end, the authors presented pictures of high resolution with all these information combined. (authors)

  19. Dynamical x-ray diffraction studies of interfacial strain in superlattices grown by molecular beam epitaxy

    International Nuclear Information System (INIS)

    Vandenberg, J.M.; Chu, S.N.G.; Hamm, R.A.; Panish, M.B.; Ritter, D.; Mancrander, A.T.

    1992-01-01

    This paper reports on dynamical X-ray diffraction studies that have been carried out for lattice-matched InGaAs/InP superlattices grown by modified molecular beam epitaxy (MBE) techniques. The (400) X-ray satellite pattern, which is predominantly affected by the strain modulation, was analyzed. The strain and thickness of the actual layers including the presence of strained interfacial regions were determined

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-05-21

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

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

    International Nuclear Information System (INIS)

    Ancharov, A.I.; Potapov, S.S.; Moiseenko, T.N.; Feofilov, I.V.; Nizovskii, A.I.

    2007-01-01

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

  2. Ultrafast Structural Dynamics in InSb Probed by Time-Resolved X-Ray Diffraction

    International Nuclear Information System (INIS)

    Chin, A.H.; Shank, C.V.; Chin, A.H.; Schoenlein, R.W.; Shank, C.V.; Glover, T.E.; Leemans, W.P.; Balling, P.

    1999-01-01

    Ultrafast structural dynamics in laser-perturbed InSb are studied using time-resolved x-ray diffraction with a novel femtosecond x-ray source. We report the first observation of a delay in the onset of lattice expansion, which we attribute to energy relaxation processes and lattice strain propagation. In addition, we observe direct indications of ultrafast disordering on a subpicosecond time scale. copyright 1999 The American Physical Society

  3. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation

    Czech Academy of Sciences Publication Activity Database

    Hrdý, Jaromír; Mikulík, P.; Oberta, Peter

    2011-01-01

    Roč. 18, č. 2 (2011), s. 299-301 ISSN 0909-0495 R&D Projects: GA MPO FR-TI1/412 Institutional research plan: CEZ:AV0Z10100522 Keywords : diffractive-refractive optics * x-ray synchrotron radiation monochromator * x-ray crystal monochromator * harmonics separation Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.726, year: 2011

  4. Nano-fabrication of diffractive optics for soft X-ray and atom beam focusing

    International Nuclear Information System (INIS)

    Rehbein, S.

    2002-01-01

    Nano-structuring processes are described for manufacturing diffractive optics for the condenser-monochromator 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 free-standing nickel zone plates for helium atom beam focusing experiments is presented. (author)

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

    International Nuclear Information System (INIS)

    Mai Zhenhong

    2012-01-01

    In April 1912, Friedrich, Knipping and Laue discovered X-ray diffraction in a CuSO 4 crystal. Later, Laue derived the famous Laue equations which explain the diffraction phenomenon. For this, Laue was awarded a Nobel Prize for Physics in 1914. In 1912 W. H. Bragg and W. L. Bragg received news of Laue 's discovery, and from X-ray diffraction experiments in a ZnS crystal they derived the famous Bragg equation. For this work, father and son were together awarded the Nobel Prize for Physics in 1915, To commemorate the 100th anniversary of the discovery of X-ray diffraction, this article reviews the important contributions of the early pioneers and their historic impact on science and technology worldwide. (author)

  6. Size effect in X-ray and electron diffraction patterns from hydroxyapatite particles

    International Nuclear Information System (INIS)

    Suvorova, E.I.; Buffat, P.-A.

    2001-01-01

    High-resolution transmission electron microscopy (HRTEM), electron microdiffraction, and X-ray diffraction were used to study hydroxyapatite specimens with particle sizes from a few nanometers to several hundreds of nanometers. Diffuse scattering (without clear reflections in transmission diffraction patterns) or strongly broadened peaks in X-ray diffraction patterns are characteristic for agglomerated hydroxyapatite nanocrystals. However, HRTEM and microdiffraction showed that this cannot be considered as an indication of the amorphous state of the matter but rather as the demonstration of size effect and the morphological and structural features of hydroxyapatite nanocrystals

  7. Mechanical characterisation of surface layers by x-ray diffraction -application to tribology

    International Nuclear Information System (INIS)

    Farrahi, G.H.

    1996-01-01

    The results presented in this paper show that X-ray diffraction can be employed for the characterisation of surface layer damage through residual stresses and work hardening by some tribological actions such as fretting and dry sliding. X-ray diffraction technique can also be employed for a rapid and non-destructive measurement of hardness of hardened steel. The diffraction profile analysis can offer a good indication about the materials characteristics and the microstructural evolution caused by heat treatment or by mechanical loading

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

    Indian Academy of Sciences (India)

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

  9. In-situ X-ray diffraction : a useful tool to investigate hydride-formation reactions

    NARCIS (Netherlands)

    Notten, P.H.L.; Daams, J.L.C.; Veirman, de A.E.M.; Staals, A.A.

    1994-01-01

    A high-pressure X-ray diffraction (XRD) cell has been designed which allowed us to study simultaneously hydrogen absorption/desorption isotherms and XRD powder diffraction patterns on (de)hydrided intermetallic compounds. The hydride formation reaction was investigated in the case of LaNi5 under

  10. Small angle X ray diffraction investigation of twinned opal_like structures

    NARCIS (Netherlands)

    Samusev, A.K.; Sinev, I.S.; Samusev, K.B.; Rybin, M.V.; Mistonov, A.A.; Grigoryeva, N.A.; Grigoriev, S.V.; Petukhov, A.V.; Byelov, D.; Trofimova, E.Y.; Kurdyukov, D.A.; Golubev, V.G.; Limonov, M.F.

    2012-01-01

    Small angle X ray diffraction from synthetic opal films has been investigated as a function of the orientation of the sample. All the observed (hkl) diffraction reflections have been interpreted. The reconstruct tion of the reciprocal lattice of the studied opal films has been carried out. The

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

    DEFF Research Database (Denmark)

    Foss, M.; Feidenhans'l, R.; Nielsen, M.

    1993-01-01

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

  12. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction

    International Nuclear Information System (INIS)

    Fernandes, P.

    2007-04-01

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B 2 liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B 2 phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  14. X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

    Science.gov (United States)

    Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

    2017-05-01

    Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

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

    International Nuclear Information System (INIS)

    Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

    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] or Twaron[reg

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

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I. M. [Institut Laue-Langevin (ILL); Urban, Volker S [ORNL; Gardner, K. H. [DuPont Experimental Station; Forsyth, V. T. [Institut Laue Langevin and Keele University

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

    Science.gov (United States)

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

    2005-08-01

    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® or Twaron®.

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

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I.M. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France); Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom); Urban, V. [Oak Ridge National Laboratory, P.O. Box 2008, Oak Ridge, TN 37831-6100 (United States); Gardner, K.H. [Department of Materials Science and Engineering University of Delaware, Newark, DE 19719 (United States); Forsyth, V.T. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France) and Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom)]. E-mail: tforsyth@ill.fr

    2005-08-15

    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] or Twaron[reg].

  20. Computed tomography of x-ray index of refraction using the diffraction enhanced imaging method

    International Nuclear Information System (INIS)

    Dilmanian, F.A.; Ren, B.; Wu, X.Y.; Orion, I.; Zhong, Z.; Thomlinson, W.C.; Chapman, L.D.

    2000-01-01

    Diffraction enhanced imaging (DEI) is a new, synchrotron-based, x-ray radiography method that uses monochromatic, fan-shaped beams, with an analyser crystal positioned between the subject and the detector. The analyser allows the detection of only those x-rays transmitted by the subject that fall into the acceptance angle (central part of the rocking curve) of the monochromator/analyser system. As shown by Chapman et al , in addition to the x-ray attenuation, the method provides information on the out-of-plane angular deviation of x-rays. New images result in which the image contrast depends on the x-ray index of refraction and on the yield of small-angle scattering, respectively. We implemented DEI in the tomography mode at the National Synchrotron Light Source using 22 keV x-rays, and imaged a cylindrical acrylic phantom that included oil-filled, slanted channels. The resulting 'refraction CT image' shows the pure image of the out-of-plane gradient of the x-ray index of refraction. No image artefacts were present, indicating that the CT projection data were a consistent set. The 'refraction CT image' signal is linear with the gradient of the refractive index, and its value is equal to that expected. The method, at the energy used or higher, has the potential for use in clinical radiography and in industry. (author)

  1. Growth of ω inclusions in Ti alloys: An X-ray diffraction study

    International Nuclear Information System (INIS)

    Šmilauerová, J.; Harcuba, P.; Pospíšil, J.; Matěj, Z.; Holý, V.

    2013-01-01

    We investigated the size and crystal structure of nanometer-sized ω inclusions in single crystals of β-Ti alloys by X-ray diffraction pole-figure measurements and reciprocal space mapping. We studied the topotactical relation of the β and ω crystal lattices, and from the positions and shapes of the diffraction maxima of the ω lattice determined the mean size of the ω inclusions and the misfit of the inclusion lattice with respect to the host lattice, as well as their changes during ageing. The lattice of the ω inclusions exhibits a large positive misfit already before ageing and the misfit is subsequently reduced during the ageing process. Using the theories of elasticity and X-ray scattering we simulated diffuse X-ray scattering around the β diffraction maxima and demonstrated that the diffuse scattering is caused mainly by local elastic strains in the β host phase around the ω inclusions

  2. Determination of the strain hardening rate of metals and alloys by X ray diffraction

    International Nuclear Information System (INIS)

    Cadalbert, Robert

    1977-01-01

    This report for engineering graduation is based on the study of X ray diffraction line profile which varies with the plastic strain rate of the metal. After some generalities of strain hardening (consequence of a plastic deformation on the structure of a polycrystalline metal, means to study a strain hardened structure, use of X ray diffraction to analyse the strain hardened crystalline structure), the author reports the strain hardening rate measurement by using X ray diffraction. Several aspects are addressed: principles, experimental technique, apparatus, automation and programming of the measurement cycle, method sensitivity and precision. In the next part, the author reports applications: measurement of the strain hardening rate in different materials (tubes with hexagonal profile, cylindrical tubes in austenitic steel), and study of the evolution of strain hardening with temperature [fr

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-31

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

  4. Submicron x-ray diffraction and its applications to problems in materials and environmental science

    Science.gov (United States)

    Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Spolenak, R.; Valek, B. C.; Meier Chang, N.; Manceau, A.; Patel, J. R.

    2002-03-01

    The availability of high brilliance third generation synchrotron sources together with progress in achromatic focusing optics allows us 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 Advanced Light Source, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

    Patel, J. R.

    2002-08-16

    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. Submicron X-ray diffraction and its applications to problems in materials and environmental science

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, N.; Celestre, R.S.; MacDowell, A.A.; Padmore, H.A.; Spolenak, R.; Valek, B.C.; Meier Chang, N.; Manceau, A.; Patel, J.R.

    2002-03-26

    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.

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

    International Nuclear Information System (INIS)

    Sun, Cheng-Jun; Brewe, Dale L.; Heald, Steve M.; Zhang, Bangmin; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.

    2014-01-01

    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 0.67 Sr 0.33 MnO 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Shymanovich, U.

    2007-11-13

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

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

    International Nuclear Information System (INIS)

    Shymanovich, U.

    2007-01-01

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

  10. Control of synchrotron x-ray diffraction by means of standing acoustic waves

    International Nuclear Information System (INIS)

    Zolotoyabko, E.; Quintana, J.P.

    2004-01-01

    Synchrotron x-ray diffraction measurements in quartz crystals of different thickness excited by standing acoustic waves were carried out at the Advanced Photon Source of Argonne National Laboratory. We demonstrated the ability to significantly modify the quartz rocking curves for 20-25 keV x rays by changing the shear wave parameters in the frequency range between 15 and 105 MHz. Dynamic deformation introduced into the crystal lattice by acoustic waves resulted in a remarkable broadening of the rocking curves. The broadening effect strongly depends on the strength of the ultrasound, which can be easily regulated by changing the acoustic amplitude or frequency near the resonance. The maximum rocking curve broadening reached 17 times, which corresponds to the wavelength band, Δλ/λ=4x10 -3 , when used as a monochromator or analyzer for 20-25 keV x rays. The initial rocking curve shape is restored by sweeping the acoustic frequency within a 50-100 kHz range near the resonance. The tunable broadening effect allows effective manipulation of x-ray intensities in time domain. Time-resolved x-ray diffraction measurements under a 19.6 MHz acoustic wave excitation were performed by synchronizing the acoustic wave and x-ray burst periodicity. We used the fact that twice per period the standing wave produces a zero net deformation across the crystal thickness. By introducing an oscillating delay to the acoustic excitation, we were able to effectively change the phase of the acoustic wave relative to the x-ray burst periodicity. The x-ray diffraction intensity was strongly affected by tuning the timing of the x-ray arrivals to the minimum or maximum acoustic deformation. A deep modulation of x rays was observed in a wide frequency range between 0.1 Hz and 1 MHz, which certifies that acoustically excited quartz crystals can potentially be used as slow and fast x-ray modulators with high duty cycle

  11. X-ray diffraction patterns of metal aurocyanides

    International Nuclear Information System (INIS)

    Selig, W.S.; Smith, G.S.; Harding, K.K.; Summers, L.J.

    1989-06-01

    Aurocyanides of the following metal cations have been prepared: Ag, Hg(II), Ga, Fe(III), Tl(I), Bi, Pb, Mn(II), Ni, Zn, Cu(II), Cd, In, and Co(II). Most of the aurocyanides are of the type M[Au(CN) 2 ] x where M is the metal cation and x its valence. However, under some conditions mixed aurocyanides containing K may be formed, such as KCo[Au(CN) 2 ] 3 . Only Ag and Hg(II) form aurocyanides which are sufficiently insoluble for the potentiometric determination of the aurocyanide anion. The diffraction patterns of the various aurocyanides are reported. 12 refs., 16 tabs

  12. X-ray diffraction microscopy based on refractive optics

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis; Jakobsen, A. C.; Simons, Hugh

    2017-01-01

    A formalism is presented for dark‐field X‐ray microscopy using refractive optics. The new technique can produce three‐dimensional maps of lattice orientation and axial strain within millimetre‐sized sampling volumes and is particularly suited to in situ studies of materials at hard X‐ray energies....... An objective lens in the diffracted beam magnifies the image and acts as a very efficient filter in reciprocal space, enabling the imaging of individual domains of interest with a resolution of 100 nm. Analytical expressions for optical parameters such as numerical aperture, vignetting, and the resolution...

  13. Coherent x-ray diffraction imaging of paint pigment particles by scanning a phase plate modulator

    International Nuclear Information System (INIS)

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

    2011-01-01

    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.

  14. Correlation between protein sequence similarity and x-ray diffraction quality in the protein data bank.

    Science.gov (United States)

    Lu, Hui-Meng; Yin, Da-Chuan; Ye, Ya-Jing; Luo, Hui-Min; Geng, Li-Qiang; Li, Hai-Sheng; Guo, Wei-Hong; Shang, Peng

    2009-01-01

    As the most widely utilized technique to determine the 3-dimensional structure of protein molecules, X-ray crystallography can provide structure of the highest resolution among the developed techniques. The resolution obtained via X-ray crystallography is known to be influenced by many factors, such as the crystal quality, diffraction techniques, and X-ray sources, etc. In this paper, the authors found that the protein sequence could also be one of the factors. We extracted information of the resolution and the sequence of proteins from the Protein Data Bank (PDB), classified the proteins into different clusters according to the sequence similarity, and statistically analyzed the relationship between the sequence similarity and the best resolution obtained. The results showed that there was a pronounced correlation between the sequence similarity and the obtained resolution. These results indicate that protein structure itself is one variable that may affect resolution when X-ray crystallography is used.

  15. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

    Science.gov (United States)

    Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

    2011-03-01

    A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

  16. Long wave-length x-ray diffraction crystal and method of manufacturing same

    International Nuclear Information System (INIS)

    Zingaro, W.P.; Sicignano, A.

    1980-01-01

    An x-ray diffraction crystal of the Langemuir-Blodgett type capable of detecting radiation having a wavelength greater than 50 Arystroms and a method of making such a crystal are described. The crystal consists of a pair of alternate monolayers, one a heavy metal soap, and one a light metal soap. Selecting cation pairs with a significant difference in atomic number and dispersing power, such as Pb and Be, Mg, or Ca, increases the effective interplanar distance since the Pb planes cause the predominant x-ray diffraction. (LL)

  17. An introduction to three-dimensional X-ray diffraction microscopy

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis

    2012-01-01

    Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly...... penetrating hard X-rays from a synchrotron source and the application of tomographic reconstruction algorithms for the analysis of the diffraction data. In favourable cases, the position, morphology, phase and crystallographic orientation can be derived for up to 1000 elements simultaneously. For each grain...

  18. X-ray diffraction investigation of spin reorientation in SmFe2

    International Nuclear Information System (INIS)

    Gaviko, V.S.; Korolyov, A.V.; Mushnikov, N.V.

    1996-01-01

    Spontaneous magnetoelastic crystal lattice distortions in the spin reorientation region of high magnetostrictive SmFe 2 have been investigated by X-ray diffraction in the temperature range 80-300 K. Comparison of experimental shapes of X-ray diffraction lines with calculated shapes shows that, in the region of the spin reorientation transition, a mixture of left angle 110 right angle and left angle 111 right angle phases rather than the angular left angle uuw right angle -type phase is realized. The temperature dependence of the relative volume content of left angle 110 right angle and left angle 111 right angle phases is determined using least-squares fitting. (orig.)

  19. X-ray diffraction studies of chitosan acetate-based polymer electrolytes

    International Nuclear Information System (INIS)

    Osman, Z.; Ibrahim, Z.A.; Abdul Kariem Arof

    2002-01-01

    Chitosan is the product when partially deacetylated chitin dissolves in dilute acetic acid. This paper presents the x-ray diffraction patterns of chitosan acetate, plasticised chitosan acetate and plasticised-salted chitosan acetate films. The results show that the chitosan acetate based polymer electrolyte films are not completely amorphous but it is partially crystalline. X-ray diffraction study also confirms the occurrence of the complexation between chitosan and the salt and the interaction between salt and plasticizer. The salt-chitosan interaction is clearly justified by infrared spectroscopy. (Author)

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

    International Nuclear Information System (INIS)

    Azevedo, A.L.T. de

    1980-01-01

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

  1. Introducing the ARL X'Tra x-ray diffraction system

    International Nuclear Information System (INIS)

    Harris, L.

    2002-01-01

    Full text: The ARL X'Tra is a state-of-the-art solution for powder X-ray diffraction in a large range of applications such as pharmaceuticals and biosciences, chemicals, earth sciences, semi-conductors, metallurgy and ceramics. The X'Tra offers the latest technology in key diffraction components to produce a high performance instrument at an affordable price. This presentation examines some of the hardware and performance features of this instrument. Copyright (2002) Australian X-ray Analytical Association Inc

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

    International Nuclear Information System (INIS)

    Waddill, G.D.; Tobin, J.G.

    1994-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Matthias Frank

    2014-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Alexeyev, V.I., E-mail: vial@x4u.lebedev.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Eliseyev, A.N., E-mail: elisseev@pluton.lpi.troitsk.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Irribarra, E., E-mail: esteban.irribarra@epn.edu.ec [Escuela Politécnica Nacional, Ladrón de Guevara E11-253, Quito (Ecuador); Kishin, I.A., E-mail: ivan.kishin@mail.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Kubankin, A.S., E-mail: kubankin@bsu.edu.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Nazhmudinov, R.M., E-mail: fizeg@bk.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation)

    2016-08-19

    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. - Highlights: • Parametric X-ray radiation below the low energy threshold for diffraction of free X-rays. • Experimental separation of the contributions from different radiation mechanisms. • PXR from relativistic electrons in mosaic crystals and textured polycrystlas.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ghammraoui, B., E-mail: bahaa.ghammraoui@cea.fr [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Tabary, J. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Pouget, S. [CEA-INAC Sciences de la matieres, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Paulus, C.; Moulin, V.; Verger, L. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Duvauchelle, Ph. [CNDRI-Insa Lyon, Universite de Lyon, F-69621, Villeurbanne Cedex (France)

    2012-02-01

    Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

  6. Two new tensile devices for X-ray diffraction experiments

    International Nuclear Information System (INIS)

    Freri, N.; Tintori, A.; Depero, L.E.; Sangaletti, L.; Cernuschi, F.; Ghia, S.

    1995-12-01

    Two tensile devices were designed to be used with parallel beam and parafocusing-geometry diffractometers. In the first case the device was designed to be attached to a strainflex diffractometer by Rigaku Inc., dedicated to stress analysis and commonly used in metallurgical industry. Since the sample does not move during the measurement, the tensile device can be kept fixed on the experimental table. The device design takes into account the steric hindrance by moving parts of diffractometer. The maximun load that can be applied to the sample is 60.000 N. An attachement to a Siemens D5000 diffractometer with Eulerian cradle has also benn designed for applying a load up tp 6000 N to a sample in the parafocusing-geometry. The installation does not require a re-alignment of the diffractometer. In both cases strain gages were applied to both sides of the specimen for the simultaneous determination of the macroscopic strains. Experiments based on the use of these devices are planned to determine the crystallographic elastic constants and study the influence of the microstructure on the mechanical behaviour of residual stresses in the zone of almost static stresses as well as the influence of residual stresses on uniaxially loaded samples. In addition, by using these devices, it is possible to measure the unstressed d-0 spacings providing useful information in the neutron diffraction study fo stress fields in steel samples

  7. Two new tensile devices for X-ray diffraction experiments

    Energy Technology Data Exchange (ETDEWEB)

    Freri, N.; Tintori, A.; Depero, L.E.; Sangaletti, L. [Brescia Univ. (Italy); Cernuschi, F.; Ghia, S. [Ente Nazionale per l`Energia Elettrica, Milan (Italy)

    1995-12-01

    Two tensile devices were designed to be used with parallel beam and parafocusing-geometry diffractometers. In thefirst case the device was designed to be attached to a strainflex diffractometer by Rigaku Inc., dedicated to stress analysis and commonly used in metallurgical industry. Since the sample does not move during the measurement, the tensile device can be kept fixed on the experimental table. The device design takes into account the steric hindrance by moving parts of diffractometer. The maximun load that can be applied to the sample is 60.000 N. An attachement to a Siemens D5000 diffractometer with Eulerian cradle has also benn designed for applying a load up tp 6000 N to a sample in the parafocusing-geometry. The installation does not require a re-alignment of the diffractometer. In both cases strain gages were applied to both sides of the specimen for the simultaneous determination of the macroscopic strains. Experiments based on the use of these devices are planned to determine the crystallographic elastic constants and study the influence of the microstructure on the mechanical behaviour of residual stresses in the zone of almost static stresses as well as the influence of residual stresses on uniaxially loaded samples. In addition, by using these devices, it is possible to measure the unstressed d-0 spacings providing useful information in the neutron diffraction study fo stress fields in steel samples.

  8. Coded diffraction system in X-ray crystallography using a boolean phase coded aperture approximation

    Science.gov (United States)

    Pinilla, Samuel; Poveda, Juan; Arguello, Henry

    2018-03-01

    Phase retrieval is a problem present in many applications such as optics, astronomical imaging, computational biology and X-ray crystallography. Recent work has shown that the phase can be better recovered when the acquisition architecture includes a coded aperture, which modulates the signal before diffraction, such that the underlying signal is recovered from coded diffraction patterns. Moreover, this type of modulation effect, before the diffraction operation, can be obtained using a phase coded aperture, just after the sample under study. However, a practical implementation of a phase coded aperture in an X-ray application is not feasible, because it is computationally modeled as a matrix with complex entries which requires changing the phase of the diffracted beams. In fact, changing the phase implies finding a material that allows to deviate the direction of an X-ray beam, which can considerably increase the implementation costs. Hence, this paper describes a low cost coded X-ray diffraction system based on block-unblock coded apertures that enables phase reconstruction. The proposed system approximates the phase coded aperture with a block-unblock coded aperture by using the detour-phase method. Moreover, the SAXS/WAXS X-ray crystallography software was used to simulate the diffraction patterns of a real crystal structure called Rhombic Dodecahedron. Additionally, several simulations were carried out to analyze the performance of block-unblock approximations in recovering the phase, using the simulated diffraction patterns. Furthermore, the quality of the reconstructions was measured in terms of the Peak Signal to Noise Ratio (PSNR). Results show that the performance of the block-unblock phase coded apertures approximation decreases at most 12.5% compared with the phase coded apertures. Moreover, the quality of the reconstructions using the boolean approximations is up to 2.5 dB of PSNR less with respect to the phase coded aperture reconstructions.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  10. Soft x-ray resonant magnetic powder diffraction on PrNiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Staub, U [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); GarcIa-Fernandez, M [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Mulders, A M [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth WA 6845 (Australia); Bodenthin, Y [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); MartInez-Lope, M J [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain); Alonso, J A [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2007-03-07

    We report on the first soft x-ray resonant powder diffraction experiments performed at the Ni L{sub 2,3} edges of PrNiO{sub 3}. The temperature, polarization and energy dependence of the (1/2 0 1/2) reflection indicates a magnetic origin for the signal. This experiment demonstrates that x-ray resonant magnetic powder diffraction can be relatively easily performed in the soft x-ray regime due to the very large enhancement factors at the absorption edges. Such experiments allow us to extract important information on the electronic states of the d shell. Similar results can be anticipated from orbital reflections measured in a powder. (fast track communication)

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

    Science.gov (United States)

    2013-01-01

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

  12. X-ray diffraction on nanoparticles chromium and nickel oxides obtained by gelatin using synchrotron radiation

    International Nuclear Information System (INIS)

    Menezes, Alan Silva de; Medeiros, Angela Maria de Lemos; Miranda, Marcus Aurelio Ribeiro; Almeida, Juliana Marcela Abraao; Remedios, Claudio Marcio Rocha; Silva, Lindomar R.D. da; Gouveia, S.T.; Sasaki, Jose Marcos; Jardim, P.M.

    2003-01-01

    Full text: Cr 2 O 3 nanoparticles has many applications like green pigments, wear resistance, and coating materials for thermal protection. Several methods to produce chromium oxide nanoparticles have already been studied, gas condensation, laser induced pyrolysis, microwave plasma, sol-gel and gamma radiation methods. Many applications for this kind of material can be provide concerning the particle size. For instance, particle size approximately of 200 nm are preferable as pigment due to its opacity and below 50 nm can be used as transparent pigment. In this work we have demonstrated that chromium and nickel oxide nanoparticles can be prepared by gelatin method. X-Ray diffraction (XRD) show that mean particle size for chromium oxide of 15-150 nm and nickel oxide of 90 nm were obtained for several temperature of sintering. The X-Ray powder diffraction pattern were performed using Synchrotron Radiation X-Ray source at XRD1 beamline in National Laboratory of Light Synchrotron (LNLS). (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-06-29

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

  14. X-ray diffraction patterns of single crystals implanted with high-energy light ions

    International Nuclear Information System (INIS)

    Wieteska, K.

    1998-01-01

    X-ray diffraction patterns of silicon and gallium arsenide single crystals implanted with high-energy protons and α-particles were studied. A various models of lattice parameter changes were analysed. The agreement between the simulation and experiment proves that the lattice parameter depth-distribution can be assumed to be proportional to vacancy distribution obtained by Monte-Carlo method and from the Biersack-Ziegler theory. Most of the X-ray experiments were performed using synchrotron source of X-ray radiation in particular in the case of back-reflection and transmission section topographic methods. The new method of direct determination of the implanted ion ranges was proposed using synchrotron radiation back-reflection section topography. A number of new interference phenomena was revealed and explained. These interferences are important in the applications of diffraction theory in studying of the real structure of implanted layers. (author)

  15. Residual stress estimation of ceramic thin films by X-ray diffraction and indentation techniques

    Energy Technology Data Exchange (ETDEWEB)

    Atar, Erdem; Sarioglu, Cevat; Demirler, Ugur; Sabri Kayali, E.; Cimenoglu, Huseyin

    2003-05-15

    The residual stresses in ceramic thin films obtained by the indentation method have been found to be three times higher than those of the X-ray diffraction method. This discrepancy can be eliminated by setting the geometrical factor for the Vickers pyramid indenter to 1 in the relevant equation of the indentation method.

  16. Residual stress estimation of ceramic thin films by X-ray diffraction and indentation techniques

    International Nuclear Information System (INIS)

    Atar, Erdem; Sarioglu, Cevat; Demirler, Ugur; Sabri Kayali, E.; Cimenoglu, Huseyin

    2003-01-01

    The residual stresses in ceramic thin films obtained by the indentation method have been found to be three times higher than those of the X-ray diffraction method. This discrepancy can be eliminated by setting the geometrical factor for the Vickers pyramid indenter to 1 in the relevant equation of the indentation method

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

    International Nuclear Information System (INIS)

    Yoo, Keun Bong; Kim, Jae Hoon

    2009-01-01

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

  18. Small angles X-ray diffraction and Mössbauer characterization of ...

    Indian Academy of Sciences (India)

    Abstract. The effect of thermal annealing on the structure and magnetic properties of crystalline Tb/Fe multilayers has been studied using conversion electron Mössbauer spectrometry and small-angle X-ray diffraction. The growth of Tb–Fe amorphous alloy from the interface is observed with increasing annealing ...

  19. Quantitative phase analysis of uranium carbide from x-ray diffraction data using the Rietveld method

    International Nuclear Information System (INIS)

    Singh Mudher, K.D.; Krishnan, K.

    2003-01-01

    Quantitative phase analysis of a uranium carbide sample was carried out from the x-ray diffraction data by Rietveld profile fitting method. The method does not require the addition of any reference material. The percentage of UC, UC 2 and UO 2 phases in the sample were determined. (author)

  20. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    International Nuclear Information System (INIS)

    Barbosa, Caroline M.; Azeredo, Soraia R.; Lopes, Ricardo T.; Souza, Sheila M.F.M de

    2013-01-01

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (I rel ). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

  1. Mössbauer effect studies and X-ray diffraction analysis of cobalt ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 26; Issue 5. Mössbauer effect studies and X-ray diffraction analysis of cobalt ferrite prepared in powder form by thermal decomposition method. M D Joseph Sebastian B Rudraswamy M C Radhakrishna Ramani. Magnetic Materials Volume 26 Issue 5 August 2003 pp ...

  2. High-pressure X-ray diffraction of L-ALANINE crystal

    DEFF Research Database (Denmark)

    Olsen, J.S.; Gerward, Leif; Souza, A.G.

    2006-01-01

    L-ALANINE has been studied by X-ray diffraction at ambient temperature and pressure up to 10.3 GPa. The material is found to transform to a tetragonal structure between 2 and 3 GPa. and to a monoclinic structure between 8 and 10 GPa. The experimental bulk modulus is 25(5) GPa for the orthorhombic...

  3. Small angles X-ray diffraction and Mössbauer characterization of ...

    Indian Academy of Sciences (India)

    The effect of thermal annealing on the structure and magnetic properties of crystalline Tb/Fe multilayers has been studied using conversion electron Mössbauer spectrometry and small-angle X-ray diffraction. The growth of Tb–Fe amorphous alloy from the interface is observed with increasing annealing temperature.

  4. A greedy method for reconstructing polycrystals from three-dimensional X-ray diffraction data

    DEFF Research Database (Denmark)

    Kulshreshth, Arun Kumar; Alpers, Andreas; Herman, Gabor T.

    2009-01-01

    An iterative search method is proposed for obtaining orientation maps inside polycrystals from three-dimensional X-ray diffraction (3DXRD) data. In each step, detector pixel intensities are calculated by a forward model based on the current estimate of the orientation map. The pixel at which...

  5. Non-destructive characterization of recrystallization kinetics using three-dimensional X-ray diffraction microscopy

    DEFF Research Database (Denmark)

    Lauridsen, E.M.; Schmidt, Søren; Fæster Nielsen, Søren

    2006-01-01

    Three-dimensional X-ray diffraction (3DXRD) is used to characterize the nucleation and early growth of individual bulk nuclei in situ during recrystallization of 92% cold-rolled copper. It is found that some cube nuclei, but not all, have a significantly faster initial growth than the average...

  6. Determining grain resolved stresses in polycrystalline materials using three-dimensional X-ray diffraction

    DEFF Research Database (Denmark)

    Oddershede, Jette; Schmidt, Søren; Poulsen, Henning Friis

    2010-01-01

    An algorithm is presented for characterization of the grain resolved (type II) stress states in a polycrystalline sample based on monochromatic X-ray diffraction data. The algorithm is a robust 12-parameter-per-grain fit of the centre-of-mass grain positions, orientations and stress tensors...

  7. Simultaneous X-ray diffraction from multiple single crystals of macromolecules

    DEFF Research Database (Denmark)

    Paithankar, Karthik S.; Sørensen, Henning Osholm; Wright, Jonathan P.

    2011-01-01

    The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedure...

  8. Simultaneous resonant x-ray diffraction measurement of polarization inversion and lattice strain in polycrystalline ferroelectrics

    DEFF Research Database (Denmark)

    Gorfman, S.; Simons, Hugh; Iamsasri, T.

    2016-01-01

    and strain in ferroelectrics is an ongoing challenge that so far has obscured its fundamental behaviour. By utilizing small intensity differences between Friedel pairs due to resonant scattering, we demonstrate a time-resolved X-ray diffraction technique for directly and simultaneously measuring both lattice...

  9. Caracterization of the crystalline phases by X-Ray diffraction in electrode coatings

    International Nuclear Information System (INIS)

    Neves, M.C.G.P.; Souza Caillaux, Z. de

    1981-01-01

    Some electrodes and their respective coatings were studied in order to verify their compatibility with their utilization in the welding of base metals appropriate for the equipment of sugar and alcohol plants. The carried out studies include the characterization, by X-ray diffraction, of crystaline phases, existent in electrodes coatings. (Author) [pt

  10. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Barbosa, Caroline M., E-mail: carolmattosb@yahoo.com.br [Instituto de Arqueologia Brasileira (IAB), Belford Roxo, RJ (Brazil); Azeredo, Soraia R.; Lopes, Ricardo T., E-mail: soraia@lin.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/LIN/UFRJ), Rio de Janeiro, RJ (Brazil). Laboratorio de Instrumentacao Nuclear; Souza, Sheila M.F.M de, E-mail: sferraz@ensp.fiocruz.br [Fundacao Oswaldo Cruz (ENSP/FIOCRUZ), Rio de Janeiro, RJ (Brazil). Escola Nacional de Saude Publica Sergio Arouca

    2013-07-01

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (I{sub rel}). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

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

    DEFF Research Database (Denmark)

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

    1988-01-01

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

  12. A three-dimensional X-ray diffraction microscope for deformation studies of polycrystals

    DEFF Research Database (Denmark)

    Fæster Nielsen, Søren; Lauridsen, E.M.; Juul Jensen, D.

    2001-01-01

    -dimensional X-ray diffraction (3DXRD) microscope installed at the European Synchrotron Radiation Facility in Grenoble provides a fast and non-destructive technique for mapping the embedded grains within thick samples in three dimensions. All essential features like the position, volume, orientation, stress...

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

    Science.gov (United States)

    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 ...

  14. Hut clusters on Ge(001) surfaces studied by STM and synchrotron X-ray diffraction

    DEFF Research Database (Denmark)

    Nielsen, M.; Smilgies, D.-M.; Feidenhans'l, R.

    1996-01-01

    Nanoscale hut clusters formed on Ge(001) surfaces by depositing one monolayer of indium and annealing at temperatures between 350 and 500 degrees C were studied by scanning tunnelling microscopy and synchrotron X-ray diffraction. It was found that the hut clusters form regular arrays over...

  15. Moessbauer spectroscopy, X-ray diffraction and infrared studies of prehistoric materials from Minas Gerais

    International Nuclear Information System (INIS)

    Jesus Filho, M.F. de; Costa, G.M. da; Prous, A.

    1988-01-01

    Eight samples of pigmented materials from an archaelogical site in Santana do Riacho (Minas Gerais, Brazil) were studied by X-ray diffraction, infrared and Moessbauer spectroscopy. These three techniques and the results of chemical analysis allowed the approximated composition of each sample to be proposed. No trace of organic material was found in any sample. (author)

  16. Crystallization Kinetics of Nanocrystalline Materials by Combined X-ray Diffraction and Differential Scanning Calorimetry Experiments

    Czech Academy of Sciences Publication Activity Database

    Gil-González, E.; Perejón, A.; Sánchez-Jiménez, P. E.; Medina-Carrasco, S.; Kupčík, Jaroslav; Šubrt, Jan; Criado, J. M.; Pérez-Maqueda, L. A.

    2018-01-01

    Roč. 18, č. 5 (2018), s. 3107-3116 ISSN 1528-7483 Institutional support: RVO:61388980 Keywords : nanocrysalline alloys * combined X ray diffraction * crystallization kinetics Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 4.055, year: 2016

  17. Evaluated Plan Stress Of Weld In Pressure Tube Using X Ray Diffraction Technique

    International Nuclear Information System (INIS)

    Phan Trong Phuc; Nguyen Duc Thanh; Luu Anh Tuyen

    2011-01-01

    X ray diffraction is a fundamental technique measuring stress, this technique has determined crystal strain in materials, from that determined stress in materials. This paper presents study of evaluating plane stress of weld in pressure tube, using modern XRD apparatus: X Pert Pro. (author)

  18. Revealing stacking sequences in inverse opals by microradian X-ray diffraction

    NARCIS (Netherlands)

    Sinitskii, A.; Abramova, V.; Grigorieva, N.; Grigoriev, S.; Snigirev, A.; Byelov, D.; Petukhov, A.V.

    2010-01-01

    We present the results of the structural analysis of inverse opal photonic crystals by microradian X-ray diffraction. Inverse opals based on different oxide materials (TiO2, SiO2 and Fe2O3) were fabricated by templating polystyrene colloidal crystal films grown by the vertical deposition technique.

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

    OpenAIRE

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

    2010-01-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported.

  20. X-ray diffraction studies of sucrose and sucrose irradiated with γ-radiation

    International Nuclear Information System (INIS)

    Prasad, Mahendra

    1981-01-01

    In order to understand and solve numerous problems related to sugar quality and its storage life, X-ray diffraction studies of sucrose and sucrose irradiated with γ-radiation have been made. It is observed that the interplanar spacing 'd' in irradiated sucrose is reduced indicating the partial damage of sucrose lattice. (author)

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

    DEFF Research Database (Denmark)

    Stern, Stephan; Holmegaard, Lotte; Filsinger, Frank

    2014-01-01

    We give a detailed account of the theoretical analysis and the experimental results of an x-ray-diffraction experiment on quantum-state selected and strongly laser-aligned gas-phase ensembles of the prototypical large asymmetric rotor molecule 2,5-diiodobenzonitrile, performed at the Linac Cohere...

  2. Electron Paramagnetic Resonance and X-ray Diffraction of Boron- and Phosphorus-Doped Nanodiamonds

    Science.gov (United States)

    Binh, Nguyen Thi Thanh; Dolmatov, V. Yu.; Lapchuk, N. M.; Shymanski, V. I.

    2017-11-01

    Powders of boron- and phosphorus-doped detonation nanodiamonds and sintered pellets of non-doped nanodiamond powders were studied using electron paramagnetic resonance and x-ray diffraction. Doping of detonation nanodiamond crystals with boron and phosphorus was demonstrated to be possible. These methods could be used to diagnose diamond nanocrystals doped during shock-wave synthesis.

  3. New imaging technique based on diffraction of a focused x-ray beam

    Energy Technology Data Exchange (ETDEWEB)

    Kazimirov, A [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853 (United States); Kohn, V G [Russian Research Center ' Kurchatov Institute, 123182 Moscow (Russian Federation); Cai, Z-H [Advanced Photon Source, 9700 S. Cass Avenue, Argonne, IL 60439 (United States)], E-mail: ayk7@cornell.edu

    2009-01-07

    We present first experimental results from a new diffraction depth-sensitive imaging technique. It is based on the diffraction of a focused x-ray beam from a crystalline sample and recording the intensity pattern on a high-resolution CCD detector positioned at a focal plane. Structural non-uniformity inside the sample results in a region of enhanced intensity in the diffraction pattern. The technique was applied to study silicon-on-insulator thin layers of various thicknesses which revealed a complex strain profile within the layers. A circular Fresnel zone plate was used as a focusing optic. Incoherent diffuse scattering spreads out of the diffraction plane and results in intensity recorded outside of the focal spot providing a new approach to separately register x-rays scattered coherently and incoherently from the sample. (fast track communication)

  4. Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry.

    Science.gov (United States)

    Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

    2017-04-01

    X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La 3 Ga 5 SiO 14 ) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space-time modulation of an X-ray beam.

  5. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

    Energy Technology Data Exchange (ETDEWEB)

    Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031 (China); Huang, J. W.; Zeng, X. L.; Li, Y.; E, J. C.; Huang, J. Y. [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Sun, T.; Fezzaa, K. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Wang, Z. [Physics Division P-25, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

    2016-05-15

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.

  6. X-ray diffraction studies of Pompeian wall paintings using synchrotron radiation and dedicated laboratory made systems

    International Nuclear Information System (INIS)

    Duran, A.; Castaing, J.; Walter, P.

    2010-01-01

    The full identification of artwork materials requires not only elemental analysis but also structural information of the compounds as provided by X-ray diffraction (XRD). This is easily done when taking samples (or micro-samples) from artworks. However, there is an increasing interest in performing non-destructive studies that require adapted XRD systems. Comparative study of synchrotron high-resolution X-ray powder diffraction (SR-HRPD) and laboratory non-destructive systems (portable XRD and micro-XRD) is the main objective of this work. There are no qualitative differences among the three systems as for detected phases in the Pompeian wall paintings that were studied, except in the case of minority phases which only were detected by SR-HRPD. The identified pigments were goethite, hematite, cinnabar, glauconite, Pompeian blue, together with calcite, dolomite and aragonite. Synchrotron XRD diagrams show better resolution than the others. In general, the peak widths in the diagrams obtained with the portable XRD system are similar to those obtained by micro-diffraction equipment. Factors such as residual divergence of X-ray sources, incidence angle and slit or collimator size are discussed in relation with the quality of XRD diagrams. (orig.)

  7. Characterization of breast tissue using energy-dispersive X-ray diffraction computed tomography

    International Nuclear Information System (INIS)

    Pani, S.; Cook, E.J.; Horrocks, J.A.; Jones, J.L.; Speller, R.D.

    2010-01-01

    A method for sample characterization using energy-dispersive X-ray diffraction computed tomography (EDXRDCT) is presented. The procedures for extracting diffraction patterns from the data and the corrections applied are discussed. The procedures were applied to the characterization of breast tissue samples, 6 mm in diameter. Comparison with histological sections of the samples confirmed the possibility of grouping the patterns into five families, corresponding to adipose tissue, fibrosis, poorly differentiated cancer, well differentiated cancer and benign tumour.

  8. Ultrafast coherent diffractive imaging of nanoparticles using X-ray free-electron laser radiation

    International Nuclear Information System (INIS)

    Kassemeyer, Stephan

    2014-01-01

    Coherent diffractive imaging with X-ray free-electron lasers (X-FEL) promises high-resolution structure determination of single microscopic particles without the need for crystallization. The diffraction signal of small samples can be very weak, a difficulty that can not be countered by merely increasing the number of photons because the sample would be damaged by a high absorbed radiation dose. Traditional X-ray crystallography avoids this problem by bringing many sample particles into a periodic arrangement, which amplifies the individual signals while distributing the absorbed dose. Depending on the sample, however, crystallization can be very difficult or even impossible. This thesis presents algorithms for a new imaging approach using X-FEL radiation that works with single, non-crystalline sample particles. X-FELs can deliver X-rays with a peak brilliance many orders of magnitude higher than conventional X-ray sources, compensating for their weak interaction cross sections. At the same time, FELs can produce ultra-short pulses down to a few femtoseconds. In this way it is possible to perform ultra-fast imaging, essentially ''freezing'' the atomic positions in time and terminating the imaging process before the sample is destroyed by the absorbed radiation. This thesis primarily focuses on the three-dimensional reconstruction of single (and not necessarily crystalline) particles using coherent diffractive imaging at X-FELs: in order to extract three-dimensional information from scattering data, two-dimensional diffraction patterns from many different viewing angles must be combined. Therefore, the diffraction signal of many identical sample copies in random orientations is measured. The main result of this work is a globally optimal algorithm that can recover the sample orientations solely based on the diffraction signal, enabling three-dimensional imaging for arbitrary samples. The problem of finding three-dimensional orientations is

  9. Phases quantification in titanium oxides by means of X-ray diffraction

    International Nuclear Information System (INIS)

    Macias B, L.R.; Garcia C, R.M.; Ita T, A. de; Chavez R, A.

    2001-01-01

    In this work two phases of titanium oxides are quantified which belong to the same crystalline system and by means of a computer program named Quanto created by the first author, contains the information for calculating the absorption coefficients, it can be quantified phases having one of the pure phases and the problem samples. In order to perform this work different mixtures of different titanium oxides were prepared measuring by means of the X-ray diffraction technique in the Siemens X-ray diffractometer of ININ which were processed with the Peakfit package and also they were evaluated by means of the computer program with the necessary information finding acceptable results. (Author)

  10. X-Ray diffraction studies of silicon implanted with high energy ions

    International Nuclear Information System (INIS)

    Wieteska, K.; Wierzchowski, W.; Graeff, W.

    1998-01-01

    The character of lattice deformation in silicon implanted with high energy alpha-particles and protons was studied using a number of X-ray methods. The experiments included double-crystal spectrometer method as well as single crystal section and projection topography realised both with conventional and synchrotron X-ray sources. All observed diffraction patterns were reasonably explainable assuming the lattice parameter distribution proportional to the vacancy-interstitial distribution coming from the Biersack-ziegler theory. The theoretical rocking curves and distribution in back-reflection double-crystal and section topographs well corresponding to the experimental results were calculated using numerical integration of the takagi-taupin equations

  11. Quantitative X-ray diffraction analysis of alumina, silicon carbide and zirconium carbide in ceramic composites

    International Nuclear Information System (INIS)

    Veiga, Sonia M.B.; Bressiani, Jose Carlos; Veiga, Marcello M.; Chaklader, Asoke C.D.

    1995-01-01

    The x-ray diffraction technique has been successfully applied to determine the phases formed in a carbo thermal synthesis of ceramic composites (Al 2 O 3 -Si C and Al 2 O 3 -Si C-Zr C) using kaolinite, cyanite and zircon as precursors. The powder method using fluorite as internal standard has shown reliable results to estimate accurately phases in composites (relative error as low as 5%). In addition, quantitative X-ray analysis allows an indirect evaluation of Si O (gas) losses from the system during the carbo thermal reaction. (author)

  12. Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

    International Nuclear Information System (INIS)

    Roberts, G.A.; Stewart, K.D.

    2004-01-01

    The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

  13. Preliminary study of determination of UO2 grain size using X-ray diffraction method

    International Nuclear Information System (INIS)

    Mulyana, T.; Sambodo, G. D.; Juanda, D.; Fatchatul, B.

    1998-01-01

    The determination of UO 2 grain size has accomplished using x-ray diffraction method. The UO 2 powder is obtained from sol-gel process. A copper target as radiation source in the x-ray diffractometer was used in this experiment with CμKα characteristic wavelength 1.54433 Angstrom. The result indicate that the UO 2 mean grain size on presintered (temperature 800 o C) has the value 456.8500 Angstrom and the UO 2 mean grain size on sintered (temperature 1700 o C) has value 651.4934 Angstrom

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

    International Nuclear Information System (INIS)

    Milch, J.

    1976-02-01

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

  15. X-ray diffraction in laser-irradiated epsomite crystals grown in presence of borax

    International Nuclear Information System (INIS)

    Zaitseva, E.V.; Portnov, V.N.; Faddeev, M.A.; Chuprunov, E.V.

    1997-01-01

    Relative changes in the intensities ΔI/I of the (220) and (440) X-ray diffraction reflection during laser irradiation of epsomite (MgSO 2 ·7H 2 O) crystals grown from an aqueous solution in the presence of borax (Na 2 B 4 O 7 ·10H 2 O) were measured using the CoK α , CuK α , MoK α radiations. The intensities measured depend on the real crystal structure dependent on the borax content in the solution. The dependence of ΔI/I is studied as a function of borax in the solution and X-ray-radiation wavelength

  16. Investigation of surface residual stress profile on martensitic stainless steel weldment with X-ray diffraction

    Directory of Open Access Journals (Sweden)

    I.I. Ahmed

    2018-04-01

    Full Text Available The development of residual stresses during fabrication is inevitable and often neglected with dire consequences during the service life of the fabricated components. In this work, the surface residual stress profile following the martensitic stainless steel (MSS pipe welding was investigated with X-ray diffraction technique. The results revealed the presence of residual stresses equilibrated across the weldment zones. Tensile residual stress observed in weld metal was balanced by compressive residual stresses in the parent material on the opposing sides of weld metal. Keywords: Residual stress, Weld, Stainless steel, X-ray, HAZ

  17. Qualitative and quantitative determination of sediments phases in Chillon River by x-ray diffraction

    International Nuclear Information System (INIS)

    Miramira Tipula, Biviano; Zeballos Velasquez, Elvira; Chui Betancur, Heber; Valencia Salazar, Edilberto; Huaypar Vasquez, Yesena; Olivera de Lescano, Paula

    2008-01-01

    With this paper, we pretend to contribute with the recovery of Chillon River from a characterization of sediments. The objectives are the identification of pollution places along the bed of the Chillon River, from the Canta Province to Lima Province (Comas) and the determination of the preponderant factors of pollution. The qualitative and semi-quantitative determination of the sediments components have been carried out using the x-ray diffraction and x-ray fluorescence techniques, both of them will allow us to identify the pollute elements, for example the lead level in the Chillon River. (author)

  18. A sample holder for in-house X-ray powder diffraction studies of protein powders

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

    2011-01-01

    A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin....

  19. Fluence thresholds for grazing incidence hard x-ray mirrors

    Czech Academy of Sciences Publication Activity Database

    Aquila, A.; Sobierajski, R.; Ozkan, C.; Hájková, Věra; Burian, Tomáš; Chalupský, Jaromír; Juha, Libor; Störmer, M.; Bajt, S.; Klepka, M.T.; Dlužewski, P.; Morawiec, K.; Ohashi, H.; Koyama, T.; Tono, K.; Inubushi, Y.; Yabashi, M.; Sinn, H.; Tschentscher, T.; Mancuso, A.P.; Gaudin, J.

    2015-01-01

    Roč. 106, č. 24 (2015), "241905-1"-"241905-5" ISSN 0003-6951 R&D Projects: GA ČR(CZ) GA14-29772S Grant - others:AVČR(CZ) M100101221 Institutional support: RVO:68378271 Keywords : XFEL * Free Electron Laser * damage threshold * X-ray optics Subject RIV: BH - Optics , Masers, Lasers Impact factor: 3.142, year: 2015

  20. X-ray grazing incidence study of inhomogeneous strain relaxation in Si/SiGe wires

    International Nuclear Information System (INIS)

    Hesse, A.; Zhuang, Y.; Holy, V.; Stangl, J.; Zerlauth, S.; Schaeffler, F.; Bauer, G.; Darowski, N.; Pietsch, U.

    2003-01-01

    The elastic strain relaxation in a series of dry-etched periodic multilayer Si/SiGe wire samples with different etching depths was investigated systematically by means of grazing incidence diffraction (GID). The samples were patterned by holographic lithography and reactive ion etching from a Si/SiGe superlattice grown by molecular beam epitaxy. Scanning electron microscopy and atomic force microscopy were employed to obtain information on the shape of the wires. The inhomogeneous strain distribution in the etched wires and in the non-etched part of the multilayers was derived by means of finite element calculations which were used as an input for simulations of the scattered X-ray intensities in depth dependent GID. The theoretical calculations for the scattered intensities are based on distorted-wave Born approximation. The unperturbed scattering potential was chosen with a reduced optical density corresponding to the ratio of wire width and wire period, in order to reflect the main interaction between the incident X-rays and the patterned samples. The calculations are in good agreement with the experimental data demonstrating the variation of strain relaxation with depth

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

    DEFF Research Database (Denmark)

    King, A.; Herbig, M.; Ludwig, W.

    2010-01-01

    Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting new possibilities for mapping 3D grain shapes and crystallographic orientations in different classes of polycrystalline materials. X-ray diffraction contrast tomography (DCT) is a monochromatic beam...... imaging technique combining the principles of X-ray micro-tomography and three-dimensional X-ray diffraction microscopy (3DXRD). DCT provides simultaneous access to 3D grain shape, crystallographic orientation and attenuation coefficient distribution at the micrometer length scale. The microtexture...

  2. Moessbauer spectroscopy and X-ray diffraction study of 304 L stainless steel thin films

    International Nuclear Information System (INIS)

    Boubeker, B.; Eymery, J.P.; Goudeau, P.; Sayouty, E.H.

    1994-01-01

    304 L stainless steel films (SS) were elaborated using an ion-beam sputtering technique. The target material was a sheet of commercial grade 304 L SS. The starting material was first analysed by both conversion electron Moessbauer spectroscopy (CEMS) and X-ray diffraction. The nonmagnetic state and f.c.c. structure of this material were confirmed. The films were deposited on various substrates with thicknesses in the 175-800 nm range. The films are found to have both b.c.c. structure and ferromagnetic character. X-ray diffraction technique was also used in order to determine the residual stresses developed during the deposition process. The second stage of the work is devoted to the evolution of the film structure as a function of annealing treatments. So isochronal and isothermal kinetics at temperatures higher than 913 K have allowed to follow the alpha --> gamma phase transformation using X-ray diffraction and CEMS technique.The X-ray diffractograms reveal the existence of both b.c.c. and f.c.c. phases. Similar results can be deduced from Moessbauer spectra due to the single line coming from the non-magnetic phase and the sextet coming from the ferromagnetic phase. In addition the CEMS spectra reveal that the ferromagnetic component is split into two parts which indicates the existence of two iron sites. 1 fig., 4 refs.(author)

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Science.gov (United States)

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

    2013-09-01

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

  5. Rapid, low dose X-ray diffractive imaging of the malaria parasite Plasmodium falciparum

    International Nuclear Information System (INIS)

    Jones, Michael W.M.; Dearnley, Megan K.; Riessen, Grant A. van; Abbey, Brian; Putkunz, Corey T.; Junker, Mark D.; Vine, David J.; McNulty, Ian; Nugent, Keith A.; Peele, Andrew G.; Tilley, Leann

    2014-01-01

    Phase-diverse X-ray coherent diffractive imaging (CDI) provides a route to high sensitivity and spatial resolution with moderate radiation dose. It also provides a robust solution to the well-known phase-problem, making on-line image reconstruction feasible. Here we apply phase-diverse CDI to a cellular sample, obtaining images of an erythrocyte infected by the sexual stage of the malaria parasite, Plasmodium falciparum, with a radiation dose significantly lower than the lowest dose previously reported for cellular imaging using CDI. The high sensitivity and resolution allow key biological features to be identified within intact cells, providing complementary information to optical and electron microscopy. This high throughput method could be used for fast tomographic imaging, or to generate multiple replicates in two-dimensions of hydrated biological systems without freezing or fixing. This work demonstrates that phase-diverse CDI is a valuable complementary imaging method for the biological sciences and ready for immediate application. - Highlights: • Phase-diverse coherent X-ray diffraction microscopy provides high-resolution and high-contrast images of intact biological samples. • Rapid nanoscale resolution imaging is demonstrated at orders of magnitude lower dose than previously possible. • Phase-diverse coherent X-ray diffraction microscopy is a robust technique for rapid, quantitative, and correlative X-ray phase imaging

  6. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

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

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1986-01-01

    A method is described of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where mless than or equal ton, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K/sub j/=(X/sub j//X/sub l/)(I/sub l//I/sub j/) for each mineral (j=2...n) in the group of known minerals (j=2...n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; identifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X/sub j//X/sub l/ for each mineral (j=2...m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I/sub j/ of each mineral in the test sample to the measured highest integrated intensity peak I/sub l/ of the reference mineral in the test sample, and from the previously determined standard coefficients, X/sub j//X/sub l/=K/sub j/(I/sub j//I/sub l/

  8. Rapid, low dose X-ray diffractive imaging of the malaria parasite Plasmodium falciparum

    Energy Technology Data Exchange (ETDEWEB)

    Jones, Michael W.M., E-mail: michael.jones@latrobe.edu.au [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Dearnley, Megan K. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Biochemistry and Molecular Biology, Bio21 Institute, The University of Melbourne, Victoria 3010 (Australia); Riessen, Grant A. van [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Abbey, Brian [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Melbourne Centre for Nanofabrication, Victoria 3168 (Australia); Putkunz, Corey T. [ARC Centre of Excellence for Coherent X-Ray Science, School of Physics, The University of Melbourne, Victoria 3010 (Australia); Junker, Mark D. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Vine, David J. [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); McNulty, Ian [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); Centre for Nanoscale Materials, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Nugent, Keith A. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Peele, Andrew G. [ARC Centre of Excellence for Coherent X-Ray Science, Department of Physics, La Trobe University, Victoria 3086 (Australia); Australian Synchrotron, 800 Blackburn Road, Clayton 3168 (Australia); Tilley, Leann [ARC Centre of Excellence for Coherent X-Ray Science, Department of Biochemistry and Molecular Biology, Bio21 Institute, The University of Melbourne, Victoria 3010 (Australia)

    2014-08-01

    Phase-diverse X-ray coherent diffractive imaging (CDI) provides a route to high sensitivity and spatial resolution with moderate radiation dose. It also provides a robust solution to the well-known phase-problem, making on-line image reconstruction feasible. Here we apply phase-diverse CDI to a cellular sample, obtaining images of an erythrocyte infected by the sexual stage of the malaria parasite, Plasmodium falciparum, with a radiation dose significantly lower than the lowest dose previously reported for cellular imaging using CDI. The high sensitivity and resolution allow key biological features to be identified within intact cells, providing complementary information to optical and electron microscopy. This high throughput method could be used for fast tomographic imaging, or to generate multiple replicates in two-dimensions of hydrated biological systems without freezing or fixing. This work demonstrates that phase-diverse CDI is a valuable complementary imaging method for the biological sciences and ready for immediate application. - Highlights: • Phase-diverse coherent X-ray diffraction microscopy provides high-resolution and high-contrast images of intact biological samples. • Rapid nanoscale resolution imaging is demonstrated at orders of magnitude lower dose than previously possible. • Phase-diverse coherent X-ray diffraction microscopy is a robust technique for rapid, quantitative, and correlative X-ray phase imaging.

  9. X-ray diffraction characteristics of curved monochromators for sychrotron radiation

    International Nuclear Information System (INIS)

    Boeuf, A.; Rustichelli, F.; Mazkedian, S.; Puliti, P.; Melone, S.

    1978-01-01

    A theoretical study is presented concerning the diffraction characteristics of curved monochromators for X-ray synchrotron radiation used at the laboratories of Hamburg, Orsay and Stanford. The investigation was performed by extending to the X-ray case a simple model recently developed and fruitfully employed to describe the neutron diffraction properties of curved monochromators. Several diffraction patterns were obtained corresponding to different monochromator materials (Ge, Si) used by the different laboratories, for different reflecting planes (111), (220), asymmetry angles, X-ray wave-lengths (Mo Kα, Cu Kα, Cr Kα) and curvature radii. The results are discussed in physical terms and their implications on the design of curved monochromators for synchrotron radiation are presented. In particular, the study shows that all the monochromators used in the different laboratories should behave practically as perfect crystals and therefore should have a very low integrated reflectivity corresponding to an optimized wavelength passband Δlambda/lambda approximately 10 -4 . The gain that can be obtained by increasing the curvature, by introducing a gradient in the lattice spacing or by any other kind of imperfection is quite limited and much lower than the desirable value. The adopted model can help in obtaining a possible moderate gain in intensity by also taking into consideration other parameters, such as crystal material, reflecting plane, asymmetry of the reflection and X-ray wavelength. (Auth.)

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

    Science.gov (United States)

    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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  12. Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

    Science.gov (United States)

    Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

    2013-01-01

    Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

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

    Science.gov (United States)

    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

    2016-04-01

    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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Berenguer de la Cuesta, Felisa; Bean, Richard J; Bozec, Laurent; Robinson, Ian K [London Centre for Nanotechnology (LCN), University College London (UCL), London WC1H 0AH (United Kingdom); McCallion, Catriona; Wallace, Kris [Department of Physics and Astronomy, University College London (UCL), London WC1E 6BT (United Kingdom); Hiller, Jen C; Terrill, Nicholas J, E-mail: f.berenguer@ucl.ac.u [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom)

    2010-10-01

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

  16. Femtosecond x-ray photoelectron diffraction on gas-phase dibromobenzene molecules

    International Nuclear Information System (INIS)

    Rolles, D; Boll, R; Epp, S W; Erk, B; Foucar, L; Hömke, A; Adolph, M; Gorkhover, T; Aquila, A; Chapman, H N; Coppola, N; Delmas, T; Gumprecht, L; Holmegaard, L; Bostedt, C; Bozek, J D; Coffee, R; Decleva, P; Filsinger, F; Johnsson, P

    2014-01-01

    We present time-resolved femtosecond photoelectron momentum images and angular distributions of dissociating, laser-aligned 1,4-dibromobenzene (C 6 H 4 Br 2 ) molecules measured in a near-infrared pump, soft-x-ray probe experiment performed at an x-ray free-electron laser. The observed alignment dependence of the bromine 2p photoelectron angular distributions is compared to density functional theory calculations and interpreted in terms of photoelectron diffraction. While no clear time-dependent effects are observed in the angular distribution of the Br(2p) photoelectrons, other, low-energy electrons show a pronounced dependence on the time delay between the near-infrared laser and the x-ray pulse. (paper)

  17. Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

    Science.gov (United States)

    Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

    2004-11-01

    The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

  18. Nondestructive strain depth profiling with high energy X-ray diffraction: System capabilities and limitations

    Science.gov (United States)

    Zhang, Zhan; Wendt, Scott; Cosentino, Nicholas; Bond, Leonard J.

    2018-04-01

    Limited by photon energy, and penetration capability, traditional X-ray diffraction (XRD) strain measurements are only capable of achieving a few microns depth due to the use of copper (Cu Kα1) or molybdenum (Mo Kα1) characteristic radiation. For deeper strain depth profiling, destructive methods are commonly necessary to access layers of interest by removing material. To investigate deeper depth profiles nondestructively, a laboratory bench-top high-energy X-ray diffraction (HEXRD) system was previously developed. This HEXRD method uses an industrial 320 kVp X-Ray tube and the Kα1 characteristic peak of tungsten, to produces a higher intensity X-ray beam which enables depth profiling measurement of lattice strain. An aluminum sample was investigated with deformation/load provided using a bending rig. It was shown that the HEXRD method is capable of strain depth profiling to 2.5 mm. The method was validated using an aluminum sample where both the HEXRD method and the traditional X-ray diffraction method gave data compared with that obtained using destructive etching layer removal, performed by a commercial provider. The results demonstrate comparable accuracy up to 0.8 mm depth. Nevertheless, higher attenuation capabilities in heavier metals limit the applications in other materials. Simulations predict that HEXRD works for steel and nickel in material up to 200 µm, but experiment results indicate that the HEXRD strain profile is not practical for steel and nickel material, and the measured diffraction signals are undetectable when compared to the noise.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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

  20. Strain fields in crystalline solids: prediction and measurement of X- ray diffraction patterns and electron diffraction contrast images

    NARCIS (Netherlands)

    Bor, Teunis Cornelis

    2000-01-01

    Lattice imperfections, such as dislocations and misfitting particles, shift and/or broaden X-ray diffraction (XRD) line profiles. Most of the present analysis methods of the shift and broadening of XRD line profiles do not provide the characteristics of lattice imperfections. The main part of this

  1. Slow scan sit detector for x-ray diffraction studies using synchrotron radiation

    International Nuclear Information System (INIS)

    Milch, J.R.

    1978-01-01

    A TV-type x-ray detector using a SIT vidicon has been used for biological diffraction studies at the EMBL outstation at DESY, Hamburg, Germany. The detector converts the two-dimensional diffraction pattern to a charge pattern on the vidicon target, which is read out in the slow-scan mode. This detector has high DOE, no count-rate limit, and is simple and inexpensive to construct. Radiation from the storage ring DORIS was used to study the structure of live muscle at various phases of contraction. Typically the count-rate on the detector was 10 6 x-rays/sec and a total exposure of a few seconds was needed to record the weak diffraction from muscle. This compares with usual exposure times of several hours using a rotating anode generator and film

  2. Characterization of nanophase materials by x-ray diffraction and computer simulation

    International Nuclear Information System (INIS)

    Eastman, J.A.; Thompson, L.J.

    1989-06-01

    X-ray diffraction experiments on nanophase Pd have been performed with the primary goal of determining the nature of grain boundary structures in nanophase materials. A kinematical diffraction analysis has been developed to interpret x-ray θ--2θ data by comparing actual scans with scans produced by computer simulation. This simulation program has been used to explore the effects on diffracted intensity of a variety of microstructural and grain boundary structural parameters such as void concentration, grain size, grain boundary width, and changes in interplanar spacing and density in grain boundary regions. It has been found that a reasonable match to experimental data is produced by at least two model structures; in one, the material contains randomly positioned voids or vacancies, while in the other, the interplanar spacings in grain boundary regions are varied with respect to the spacings found in the grain interiors. 7 refs., 4 figs

  3. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  4. Contained x-ray diffraction goniometer for examination of radioactive materials

    International Nuclear Information System (INIS)

    Smith, P.K.; Osgood, B.C.; Blaser, D.E.; Howell, R.E.; Stuhler, H.; Stauver, J.

    1987-11-01

    Radioactive materials are being characterized for chemical form and certain physical properties with an x-ray diffraction goniometer customized for containment in a shielded alpha glovebox. A Siemens D500 goniometer was customized by Siemens to locate the associated electronics and x-ray generator outside the glovebox to minimize corrosion and facilitate maintenance. A graphite monochromator is used with a shielded scintillation detector to separate diffracted x-radiation from nuclear radiation. The diffraction system is computer automated for data acquisition and reduction. The facility is designed to handle primarily alpha- and beta-emitting samples with moderate neutron and gamma radiation. Samples containing plutonium, enriched uranium, and other transuranic elements are analyzed in support of site nuclear operations and development programs on nuclear waste, chemical separations, reactor fuels, and product forms

  5. Femtosecond X-ray diffraction from an aerosolized beam of protein nanocrystals.

    Science.gov (United States)

    Awel, Salah; Kirian, Richard A; Wiedorn, Max O; Beyerlein, Kenneth R; Roth, Nils; Horke, Daniel A; Oberthür, Dominik; Knoska, Juraj; Mariani, Valerio; Morgan, Andrew; Adriano, Luigi; Tolstikova, Alexandra; Xavier, P Lourdu; Yefanov, Oleksandr; Aquila, Andrew; Barty, Anton; Roy-Chowdhury, Shatabdi; Hunter, Mark S; James, Daniel; Robinson, Joseph S; Weierstall, Uwe; Rode, Andrei V; Bajt, Saša; Küpper, Jochen; Chapman, Henry N

    2018-02-01

    High-resolution Bragg diffraction from aerosolized single granulovirus nanocrystals using an X-ray free-electron laser is demonstrated. The outer dimensions of the in-vacuum aerosol injector components are identical to conventional liquid-microjet nozzles used in serial diffraction experiments, which allows the injector to be utilized with standard mountings. As compared with liquid-jet injection, the X-ray scattering background is reduced by several orders of magnitude by the use of helium carrier gas rather than liquid. Such reduction is required for diffraction measurements of small macromolecular nanocrystals and single particles. High particle speeds are achieved, making the approach suitable for use at upcoming high-repetition-rate facilities.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Pravica, Michael; Bai, Ligang; Bhattacharya, Neelanjan (UNLV)

    2012-03-15

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

  8. Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Xian-Rong; Gog, Thomas; Kim, Jungho; Kasman, Elina; Said, Ayman H.; Casa, Diego M.; Wieczorek, Michael; Hönnicke, Marcelo G.; Assoufid, Lahsen

    2018-02-01

    Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h1h2h3L} and {h2h1h3L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystals therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.

  9. Non-Destructive Quantification of Plastic Deformation in Steel: Employing X-Ray Diffraction Peak Broadening Analysis

    Science.gov (United States)

    2013-09-01

    justifier l’élaboration d’une nouvelle analyse des pics de DRX dans les installations de RDDC Atlantique. Résultats : Plusieurs auteurs se sont penchés...2 3 X-Ray Diffraction Theory ...3 X-Ray Diffraction Theory The manifestation of desirable physical and chemical material properties may be readily discerned through investigation

  10. JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

    Science.gov (United States)

    Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

    2006-01-01

    X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

  11. Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

    Science.gov (United States)

    Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

    2017-11-01

    The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

  12. Characteristics of X-ray photons in tilted incident laser-produced plasma

    International Nuclear Information System (INIS)

    Wang Ruirong; Chen Weimin; Xie Dongzhu

    2008-01-01

    Characteristics of X-ray and spout direction of heat plasma flow were studied on Shenguang-II laser facility. Using of pinhole X-ray camera, X-ray photons from the plasma of aluminum (Al) irradiated by 1.053 μm laser, was measured and analysed. It is observed that the spatial distribution of X-ray photons in Al plasma for tilted irradiation is symmetic at the center of the target. The spout direction of heat plasma flow is inferred by the distribution contour of X-ray photons. the experimental results show that the spout direction of heat plasma flow is normal to target plane and the output intensity of X-ray photons does not increase significantly for tilted laser incidence. Uniformity of laser energy deposition is improved by superposing tilted incident and laser perpendicularly incident laser. At the same time, it is found that the conversion efficiency from the tilted incident laser energy to X-ray photons of laser-produced plasma is decreased. (authors)

  13. A Monte Carlo error simulation applied to calibration-free X-ray diffraction phase analysis

    International Nuclear Information System (INIS)

    Braun, G.E.

    1986-01-01

    Quantitative phase analysis of a system of n phases can be effected without the need for calibration standards provided at least n different mixtures of these phases are available. A series of linear equations relating diffracted X-ray intensities, weight fractions and quantitation factors coupled with mass balance relationships can be solved for the unknown weight fractions and factors. Uncertainties associated with the measured X-ray intensities, owing to counting of random X-ray quanta, are used to estimate the errors in the calculated parameters utilizing a Monte Carlo simulation. The Monte Carlo approach can be generalized and applied to any quantitative X-ray diffraction phase analysis method. Two examples utilizing mixtures of CaCO 3 , Fe 2 O 3 and CaF 2 with an α-SiO 2 (quartz) internal standard illustrate the quantitative method and corresponding error analysis. One example is well conditioned; the other is poorly conditioned and, therefore, very sensitive to errors in the measured intensities. (orig.)

  14. Complete k-space visualization of x-ray photoelectron diffraction

    International Nuclear Information System (INIS)

    Denlinger, J.D.; Lawrence Berkeley Lab., CA; Rotenberg, E.; Lawrence Berkeley Lab., CA; Kevan, S.D.; Tonner, B.P.

    1996-01-01

    A highly detailed x-ray photoelectron diffraction data set has been acquired for crystalline Cu(001). The data set for bulk Cu 3p emission encompasses a large k-space volume (k = 3--10 angstrom -1 ) with sufficient energy and angular sampling to monitor the continuous variation of diffraction intensities. The evolution of back-scattered intensity oscillations is visualized by energy and angular slices of this volume data set. Large diffraction data sets such as this will provide rigorous experimental tests of real-space reconstruction algorithms and multiple-scattering simulations

  15. Influence of beam divergence on form-factor in X-ray diffraction radiation

    International Nuclear Information System (INIS)

    Sergeeva, D.Yu.; Tishchenko, A.A.; Strikhanov, M.N.

    2015-01-01

    Diffraction radiation from divergent beam is considered in terms of radiation in UV and X-ray range. Scedastic form of Gaussian distribution of the particle in the bunch, i.e. Gaussian distribution with changing dispersion has been used, which is more adequate for description of divergent beams than often used Gaussian distribution with constant dispersion. Both coherent and incoherent form-factors are taken into account. The conical diffraction effect in diffraction radiation is proved to make essential contribution in spectral-angular characteristics of radiation from a divergent beam

  16. Identification of inversion domains in KTiOPO{sub 4}via resonant X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fabrizi, Federica, E-mail: federica.fabrizi@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, OX11 0DE (United Kingdom); Thomas, Pamela A. [Department of Physics, University of Warwick, Coventry, CV4 7AL (United Kingdom); Nisbet, Gareth; Collins, Stephen P. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, OX11 0DE (United Kingdom)

    2015-05-14

    The identification and high-resolution mapping of the absolute crystallographic structure in multi-domain ferroelectric KTiOPO{sub 4} is achieved through a novel synchrotron X-ray diffraction method. On a single Bragg reflection, the intensity ratio in resonant diffraction below and above the Ti absorption K edge demonstrates a domain contrast up to a factor of ∼270, thus implementing a non-contact, non-destructive imaging technique with micrometre spatial resolution, applicable to samples of arbitrarily large dimensions. A novel method is presented for the identification of the absolute crystallographic structure in multi-domain polar materials such as ferroelectric KTiOPO{sub 4}. Resonant (or ‘anomalous’) X-ray diffraction spectra collected across the absorption K edge of Ti (4.966 keV) on a single Bragg reflection demonstrate a huge intensity ratio above and below the edge, providing a polar domain contrast of ∼270. This allows one to map the spatial domain distribution in a periodically inverted sample, with a resolution of ∼1 µm achieved with a microfocused beam. This non-contact, non-destructive technique is well suited for samples of large dimensions (in contrast with traditional resonant X-ray methods based on diffraction from Friedel pairs), and its potential is particularly relevant in the context of physical phenomena connected with an absence of inversion symmetry, which require characterization of the underlying absolute atomic structure (such as in the case of magnetoelectric coupling and multiferroics)

  17. Influence of preferred orientation of minerals in the mineralogical identification process by X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Amanda Luzia da; Oliveira, Arno H. de [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear; Fernandes, Maria Lourdes Souza, E-mail: lourdesfernandes@ufmg.b [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Inst. de GeoCiencias. Centro de Pesquisa Professor Manoel Teixeira da Costa

    2011-07-01

    The X-ray diffraction corresponds to one of the main techniques for characterization of microstructures in crystalline materials, widely used in the identification of minerals in samples of geological materials. Some minerals have a property called preferred orientation which corresponds to the orientation tendency of the crystals of ground minerals to orient themselves in certain directions according to a preferred crystallographic plane. This property affects the analysis by X-ray diffraction and this fact can generates erroneous results in the characterization. The purpose of this study is to identify the negative influence of the preferred orientation of a mineral in the generation of diffraction patterns obtained in the X-ray diffraction analysis. For this, a sample of muscovite, a mineral of mica group, was prepared by two different methods: the frontal method and the back loading method. In the analysis using the frontal method there was displacement of the XRD pattern in the abscissa axis, where it was observed changes in interplanar distance and angle 2{theta} values, which are essential information for characterization and identification of a mineral. In the analysis using the back loading method, the generated XRD pattern showed no displacement in the axis of abscissas and showed interplanar distance and angle 2{theta} values closer to the real values for the muscovite. The results showed that one can only make improvements to the process of sample preparation minimizing the effect of preferred orientation in the analysis. There is no need to change conditions of diffractometer measurements. (author)

  18. Influence of preferred orientation of minerals in the mineralogical identification process by X-ray diffraction

    International Nuclear Information System (INIS)

    Silva, Amanda Luzia da; Oliveira, Arno H. de; Fernandes, Maria Lourdes Souza

    2011-01-01

    The X-ray diffraction corresponds to one of the main techniques for characterization of microstructures in crystalline materials, widely used in the identification of minerals in samples of geological materials. Some minerals have a property called preferred orientation which corresponds to the orientation tendency of the crystals of ground minerals to orient themselves in certain directions according to a preferred crystallographic plane. This property affects the analysis by X-ray diffraction and this fact can generates erroneous results in the characterization. The purpose of this study is to identify the negative influence of the preferred orientation of a mineral in the generation of diffraction patterns obtained in the X-ray diffraction analysis. For this, a sample of muscovite, a mineral of mica group, was prepared by two different methods: the frontal method and the back loading method. In the analysis using the frontal method there was displacement of the XRD pattern in the abscissa axis, where it was observed changes in interplanar distance and angle 2θ values, which are essential information for characterization and identification of a mineral. In the analysis using the back loading method, the generated XRD pattern showed no displacement in the axis of abscissas and showed interplanar distance and angle 2θ values closer to the real values for the muscovite. The results showed that one can only make improvements to the process of sample preparation minimizing the effect of preferred orientation in the analysis. There is no need to change conditions of diffractometer measurements. (author)

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Yanagisawa, Yasuhide [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Chatake, Toshiyuki [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Chiba-Kamoshida, Kaori [National Institute of Advanced Industrial Science and Technology (AIST), Umezono 1-1-1, Tsukuba, Ibaraki 305-8568 (Japan); Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki [Kurashiki University of Science and Arts, Nishinoura 2640, Tsurajima-cho, Kurashiki, Okayama 712-8505 (Japan); Yasuda, Ichiro [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Morimoto, Yukio [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan)

    2010-12-01

    Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported. 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{sub 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.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  3. The structural analysis of zinc borate glass by laboratory EXAFS and X-ray diffraction measurements

    International Nuclear Information System (INIS)

    Kajinami, Akihiko; Harada, Yasushi; Inoue, Shinsuke; Deki, Shigehito; Umesaki, Norimasa

    1999-01-01

    The structure of zinc borate glass has been investigated by laboratory EXAFS and X-ray diffraction measurement as preliminary investigations for the detailed study in SPring-8. The zinc borate glass was prepared in the range from 40 to 65 mol% of zinc oxide content. The X-ray diffraction was measured by horizontal θ-θ goniometer with 60 kV and 300 mA output of Mo target. The EXAFS of zinc borate glass was measured by laboratory EXAFS system with 20 kV, 100 mA output of Mo target for the K absorption edge of zinc atom. From the X-ray diffraction and the EXAFS measurements, it is found that the zinc ion is surrounded by four oxygen atoms and formed a tetrahedral structure whose (Zn-O) distance is about 2 A and that the structure is unchanged with the zinc oxide content. The diffraction data show that the neighboring structure of boron atom transforms from BO 4 tetrahedra to BO 3 tetragonal planar structure with increasing of the zinc oxide content. (author)

  4. Near-surface density profiling of Fe ion irradiated Si (100) using extremely asymmetric x-ray diffraction by variation of the wavelength

    Energy Technology Data Exchange (ETDEWEB)

    Khanbabaee, B., E-mail: khanbabaee@physik.uni-siegen.de; Pietsch, U. [Solid State Physics, University of Siegen, D-57068 Siegen (Germany); Facsko, S. [Helmholtz-Zentrum Dresden-Rossendorf, 01314 Dresden (Germany); Doyle, S. [Synchrotron Light Source ANKA, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen (Germany)

    2014-10-20

    In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradiated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5 nm, the extremely asymmetrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0°. The density variation was extracted from the deviations from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.

  5. Theoretical study of the properties of X-ray diffraction moiré fringes. I

    International Nuclear Information System (INIS)

    Yoshimura, Jun-ichi

    2015-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Gabbasov, Raul, E-mail: gabbasov-raul@yandex.ru [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Polikarpov, Michael; Cherepanov, Valery [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Chuev, Michael; Mischenko, Iliya; Lomov, Andrey [Institute of Physics and Technology, Russian Academy of Sciences, Moscow (Russian Federation); Wang, Andrew [Ocean NanoTech. Springdale, AR (United States); Panchenko, Vladislav [National Research Center “Kurchatov Institute”, Moscow (Russian Federation)

    2015-04-15

    Water soluble magnetite iron oxide nanoparticles with oleic polymer coating and average diameters in the range of 5–25 nm, previously determined by TEM, were characterized using Mössbauer, magnetization and X-ray diffraction measurements. Comparative analysis of the results demonstrated a large diversity of magnetic relaxation regimes. Analysis showed the presence of an additional impurity component in the 25 nm nanoparticles, with principally different magnetic nature at the magnetite core. In some cases, X-ray diffraction measurements were unable to estimate the size of the magnetic core and Mössbauer data were necessary for the correct interpretation of the experimental results. - Highlights: • KV parameter, obtained from Mössbauer spectra can be used for nanoparticle size characterization. • Mössbauer spectra of 10–25 nm nanoparticles can be effectively described by ferromagnetic model. • Surface impurities can cause incorrect nanoparticle size determination.

  7. X-ray diffraction study of phase transitions in iron(II) trisnioximate hexadecylboronate clathrochelate complex

    International Nuclear Information System (INIS)

    Vorontsov, I.I.; Antipin, M.Yu.; Dubovik, I.I.; Papkov, V.S.; Potekhin, K.A.; Voloshin, Ya.Z.; Stash, A.I.; Belsky, V.K.

    2001-01-01

    Crystals of the iron(II) nioximate hexadecylboronate clathrochelate complex-FeNx 3 (BHd ) 2 [tris(μ-1,2-cyclohexanedionedioximato-O:O ' )di-n-hexadecyldiborato(2-) - N,'''N''',N''',N''',N''',N ' ]iron(II) - are investigated by differential scanning calorimetry and X-ray diffraction. Two structural phase transitions are revealed at T cr1 = 290(3) K and T cr2 = 190(3) K. The crystal structures of phases I, II, and III are determined by X-ray diffraction analysis at 303, 243, and 153 K, respectively. It is demonstrated that the I ↔ II phase transition is due to a change in the system of translations, and the II ↔ III phase transition is accompanied only by a jumpwise change in the unit cell parameters. The possible mechanisms of phase transitions are discussed in terms of geometry and molecular packing of FeNx 3 (BHd) 2 in all three phases

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

    Energy Technology Data Exchange (ETDEWEB)

    Kiyota, Eduardo [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Sousa, Sylvia Morais de [Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Santos, Marcelo Leite dos; Costa Lima, Aline da [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Menossi, Marcelo [Departamento de Genética e Evolução, Instituto de Biologia, Universidade Estadual de Campinas, Campinas-SP (Brazil); Yunes, José Andrés [Laboratório de Biologia Molecular, Centro Infantil Boldrini, Campinas-SP (Brazil); Aparicio, Ricardo, E-mail: aparicio@iqm.unicamp.br [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil)

    2007-11-01

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

  9. X-ray diffraction, Raman and photoacoustic studies of InSb nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Ersching, K., E-mail: kleb85@hotmail.com [Departamento de Fisica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Campos, C.E.M.; Lima, J.C. de; Grandi, T.A. [Departamento de Fisica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Souza, S.M. [Departamento de Engenharia Mecanica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, 13 565-905 Sao Carlos, SP (Brazil)

    2010-08-01

    Zinc blend InSb nanocrystals were generated by mechanical alloying and X-ray diffraction, Raman spectroscopy and photoacoustic absorption spectroscopy techniques were used to study its structural, optical and thermal properties. Annealed nanocrystals were also studied. Residual amorphous and minority crystalline (Sb and In{sub 2}O{sub 3}) phases were also observed for mechanical alloyed and thermal annealed samples, respectively. The structural parameters, phase fractions, average crystallite sizes and microstrains of all crystalline phases found in the samples were obtained from Rietveld analyses of their X-ray diffraction patterns. Raman results for both as-milled and annealed samples show the Raman active LO and TO modes of the zinc blend InSb phase and Sb-rich regions. The photoacoustic results of both samples were satisfactorily explained by thermal bending heat transfer mechanism and an increase on effective thermal diffusivity coefficient was observed after annealing.

  10. X-ray diffraction investigation of self-annealing in nanocrystalline copper electrodeposits

    DEFF Research Database (Denmark)

    Pantleon, Karen; Somers, Marcel A. J.

    2006-01-01

    X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multip...... twinning during self-annealing. The kinetics of self-annealing depends on the layer thickness as well as on the orientation and/or the size of the as-deposited crystallites. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.......X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multiple...

  11. Atomic structure of large angle grain boundaries determined by quantitative X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Fitzsimmons, M.R.; Sass, S.L.

    1988-01-01

    Quantitative X-ray diffraction techniques have been used to determine the atomic structure of the Σ = 5 and 13 [001] twist boundaries in Au with a resolution of 0.09 Angstrom or better. The reciprocal lattices of these boundaries were mapped out using synchrotron radiation. The atomic structures were obtained by testing model structures against the intensity observations with a chi square analysis. The boundary structure were modeled using polyhedra, including octahedra, special configurations of tetrahedra and Archimedian anti-prisms, interwoven together by the boundary symmetry. The results of this work point to the possibility of obtaining general rules for grain boundary structure based on X-ray diffraction observations that give the atomic positions with high resolution

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    DEFF Research Database (Denmark)

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

    1998-01-01

    within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

  14. Quantitative strain analysis of surfaces and interfaces using extremely asymmetric x-ray diffraction

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi

    2010-01-01

    Strain can reduce carrier mobility and the reliability of electronic devices and affect the growth mode of thin films and the stability of nanometer-scale crystals. To control lattice strain, a technique for measuring the minute lattice strain at surfaces and interfaces is needed. Recently, an extremely asymmetric x-ray diffraction method has been developed for this purpose. By employing Darwin's dynamical x-ray diffraction theory, quantitative evaluation of strain at surfaces and interfaces becomes possible. In this paper, we review our quantitative strain analysis studies on native SiO 2 /Si interfaces, reconstructed Si surfaces, Ni/Si(111)-H interfaces, sputtered III-V compound semiconductor surfaces, high-k/Si interfaces, and Au ion-implanted Si. (topical review)

  15. Applications of the Warren-Averbach method of X-ray diffraction line profile analysis

    International Nuclear Information System (INIS)

    Ichikawa, Rodrigo Uchida

    2013-01-01

    The objective of this work was to develop and implement a methodology of X-ray Line Profile Analysis (XLPA) for the study and determination of the mean crystallite sizes and microstrains in materials. A computer program was developed to speed up the treatment of diffraction peaks and perform the deconvolution utilizing the Stokes method to correct the instrumental contribution in the X-ray diffraction measurements. The XLPA methods used were the Scherrer, Williamson-Hall and Single-Line methods, which can be called real space methods, and the Fourier space method of Warren-Averbach. Furthermore, considering a mathematical modelling it was possible to calculate the crystallite size distribution, considering the log-normal distribution and spherical crystallites. It was possible to demonstrate the proposed theory can provide reliable results evaluating a dispersion parameter. The methodologies described above were applied in two distinct materials: in the alloy Zircaloy-4 and in ZnO. (author)

  16. Thermogravimetric and x-ray diffraction analyses of Luna-24 regolith samples

    International Nuclear Information System (INIS)

    Deshpande, V.V.; Dharwadkar, S.R.; Jakkal, V.S.

    1979-01-01

    Two samples of Luna-24 were analysed by X-ray diffraction and thermogravimetric (TG) techniques. The sample 24123.12 shows a weight loss of nearly 0.85 percent between 23O-440deg C and followed by 1.16 percent weight gain from 500 to 800deg C. The sample 23190.13 showed only a weight gain of about 1.5 percent from 5O0deg C to 900deg C. X-ray diffraction analyses show the presence of olivine, plagioclase, pigeonite, enstatite, and native iron in both the virgin samples. The heated samples, however, show that only the native iron got oxidized to iron oxide. The other constituents remain unaltered. (auth.)

  17. Correlated microradiography, X-ray microbeam diffraction and electron probe microanalysis of calcifications in an odontoma

    International Nuclear Information System (INIS)

    Aoba, T.; Yoshioka, C.; Yagi, T.

    1980-01-01

    Using microradiography, X-ray microbeam diffraction and electron probe microanalysis, a correlated morphologic and crystallographic study was performed on dysplastic enamel in a compound odontoma. The tumor was found in the lateral incisor-canine region of the left mandible of a 36-year-old woman. A conspicuous feature was the presence of hypomineralized areas, which were situated in the proximity of enamel surface and distinctly demarcated from the adjacent enamel. X-ray microbeam diffraction and electron microanalysis showed that these lesions have a lower crystallinity and a higher concentration of magnesium as compared with the adjacent enamel. In addition, the present study revealed the presence of two other types of calcifications: 1) calcified structures within the fissure or on the enamel surface, which include lacunae of varying size and which resemble a form of coronal cementum, and 2) spherical calcifications which may be an epithelial product. (author)

  18. Determination of diffusion profiles in thin film couples by means of X-ray-diffraction

    International Nuclear Information System (INIS)

    Wagendristel, A.

    1975-01-01

    An X-ray method for the determination of concentration profiles in thin film diffusion couples is presented. This method is based on the theory of Fourier analysis of X-ray diffraction profiles which is generalized to polycrystalline samples showing non-uniform lattice parameter. A Fourier synthesis of the concentration spectrum is possible when the influences of the particle size and the strain in the sample as well as the instrumental function are eliminated from the measured diffraction profile. This can be done by means of reference profiles obtained from layers of the diffusion components. Absorption of the radiation in the sample is negligible when diffusion couples of symmetrical sandwich structure are used. The method is tested experimentally in the system Au-Cu. (orig.) [de

  19. Investigation of mosaicity of epitaxic multilayers by the statistical theory of X-ray dynamical diffraction

    International Nuclear Information System (INIS)

    Li Ming; Mai Zhenhong; Li Jianhua; Li Chaorong; Cui Shufan

    1995-01-01

    Based on the statistical theory of X-ray dynamical diffraction for thin films, the mosaicity of three types of semiconductor epitaxic layers has been investigated by analyzing their rocking curves by the X-ray double-crystal diffraction method. It is shown that the statistical theory can provide quantitative information on the mosaicity of the epitaxic layers such as the mean size and the mean disorientation of mosaic blocks in the layers. Some misunderstandings in interpreting experimental data are cleared up by taking into account the effect of diffuse scattering. It is emphasized that attempts to obtain structural parameters of specimens from their rocking curves by means of the Takagi-Taupin equations for coherent fields only are not strictly correct since diffuse scattering causes additional changes in the tails of the rocking curves. (orig.)

  20. Detectors for X-ray diffraction and scattering: current technology and future challenges

    International Nuclear Information System (INIS)

    Bahr, D.; Brugemann, L.; Gerndt, E.

    2003-01-01

    Full text: Detectors are crucial devices determining the quality, the reliability and the throughput of x-ray diffraction (XRD) and scattering investigations. This is of utmost importance in an industrial environment where in many cases untrained personnel or even without human intervention the experiments and data evaluations are running. The currently used technology of 0-dimensional to 2-dim XRD detectors is presented using selected examples. The application specific requirements on e.g. energy range and resolution, count rate limit, background and dynamic range, and size versus price are discussed. Due to the fact that x-ray diffraction investigations are becoming increasingly attractive in science, research and industry the advance in detector technology is pushed beyond existing limits. The discussion of the resultant market opportunities versus the cost of ownership and market entrance barrier is the final section of the presentation

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    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 1 2 1 2 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

  2. Diamond Thermal Expansion Measurement Using Transmitted X-ray Back-diffraction.

    OpenAIRE

    Giles, Carlos; Adriano, Cris; Lubambo, Adriana Freire; Cusatis, Cesar; Mazzaro, Irineu; Hönnicke, Marcelo Goncalves

    2015-01-01

    The linear thermal expansion coefficient of diamond has been measured using forward-diffracted profiles in X-ray backscattering. This experimental technique is presented as an alternative way of measuring thermal expansion coefficients of solids in the high-resolution Bragg backscattering geometry without the intrinsic difficulty of detecting the reflected beam. The temperature dependence of the lattice parameter is obtained from the high sensitivity of the transmitted profiles to the Bragg a...

  3. Calculated powder x-ray diffraction data for three tantalum tungstates

    International Nuclear Information System (INIS)

    Holcombe, C.E. Jr.

    1976-11-01

    A study was made of computer-simulated powder x-ray diffraction data for Ta 22 W 4 O 67 , Ta 2 WO 8 , and Ta 16 W 18 O 94 --the three compounds in the Ta 2 O 5 --WO 3 system from 27 to 69 mole percent WO 3 . The crystal structures of Ta 2 WO 8 and one form of Ta 16 W 18 O 94 (Type B) were deduced from reported data. 8 tables

  4. X-ray diffraction (XRD) characterization of microstrain in some iron and uranium alloys

    International Nuclear Information System (INIS)

    Kimmel, G.; Dayan, D.; Frank, G.A.; Landau, A.

    1996-01-01

    The high linear attenuation coefficient of steel, uranium and uranium based alloys is associated with the small penetration depth of X-rays with the usual wavelength used for diffraction. Nevertheless, by using the proper surface preparation technique, it is possible of obtaining surfaces with bulk properties (free of residual mechanical microstrain). Taking advantage of the feasibility to obtain well prepared surfaces, extensive work has been conducted in studying XRD line broadening effects from flat polycrystalline samples of steel, uranium and uranium alloys

  5. Qualitative mineralogical characterization of the sinter by X-ray diffraction

    International Nuclear Information System (INIS)

    Greca, M.C.; Pietroluongo, L.R.V.; Baliza, S.V.; Costa Pereira, E.A. da

    1987-01-01

    This paper aims the qualitative mineralogical characterization of sinters and raw materials employed on its fabrication, via X-ray diffraction technique. Thus, sample with constant coke breeze content and variable contents of sand, limestone, dunite and dolomite were prepared to obtain current sinter compositions, with variable basicity. The tests were performed at the research of the following institutions: Companhia Siderurgica Nacional, Centro de Tecnologia Mineral and Instituto Nacional de Tecnologia. (author) [pt

  6. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    International Nuclear Information System (INIS)

    Conconi, M.S.; Gauna, M.R.; Serra, M.F.; Suarez, G.; Aglietti, E.F.; Rendtorff, N.M.

    2014-01-01

    The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

  7. Time and space domain separation of pulsed X-ray beams diffracted from vibrating crystals

    Energy Technology Data Exchange (ETDEWEB)

    Nosik, V. L., E-mail: v-nosik@yandex.ru, E-mail: nosik@ns.crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation)

    2016-11-15

    It is known that a set of additional reflections (satellites) may arise on rocking curves in the case of X-ray diffraction in the Bragg geometry from crystals where high-frequency ultrasonic vibrations are excited. It is shown that, under certain conditions, the pulse wave fields of the satellites and main reflection may be intersected in space (playing the role of pump and probe beams) and in time (forming interference superlattices).

  8. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    Energy Technology Data Exchange (ETDEWEB)

    Conconi, M.S.; Gauna, M.R.; Serra, M.F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC), Buenos Aires (Argentina); Suarez, G.; Aglietti, E.F.; Rendtorff, N.M., E-mail: rendtorff@cetmic.unlp.edu.ar [Universidad Nacional de La Plata (UNLP), Buenos Aires (Argentina). Fac. de Ciencias Exactas. Dept. de Quimica

    2014-10-15

    The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

  9. Measurement and Interpretation of Diffuse Scattering in X-Ray Diffraction for Macromolecular Crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Wall, Michael E. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-10-16

    X-ray diffraction from macromolecular crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering reflects the mean electron density in the unit cells of the crystal. The diffuse scattering arises from correlations in the variations of electron density that may occur from one unit cell to another, and therefore contains information about collective motions in proteins.

  10. Sample cell for in-field X-ray diffraction experiments

    Directory of Open Access Journals (Sweden)

    Viktor Höglin

    2015-01-01

    Full Text Available A sample cell making it possible to perform synchrotron radiation X-ray powder diffraction experiments in a magnetic field of 0.35 T has been constructed. The device is an add-on to an existing sample cell and contains a strong permanent magnet of NdFeB-type. Experiments have shown that the setup is working satisfactory making it possible to perform in-field measurements.

  11. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    Directory of Open Access Journals (Sweden)

    M. S. Conconi

    2014-12-01

    Full Text Available The firing transformations of traditional (clay based ceramics are of technological and archeological interest, and are usually reported qualitatively or semiquantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite, the low crystalline (metakaolinite and/or spinel type pre-mullite and glassy phases evolution of a triaxial (clay-quartz-feldspar ceramic fired in a wide temperature range between 900 and 1300 ºC. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 ºC spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and

  12. GaN quantum dot polarity determination by X-ray photoelectron diffraction

    Czech Academy of Sciences Publication Activity Database

    Romanyuk, Olexandr; Bartoš, Igor; Brault, J.; De Mierry, P.; Paskova, T.; Jiříček, Petr

    2016-01-01

    Roč. 389, Dec (2016), s. 1156-1160 ISSN 0169-4332 R&D Projects: GA ČR GA15-01687S; GA MŠk LM2015088 Institutional support: RVO:68378271 Keywords : GaN * semipolar GaN * quantum dots * X-ray photoelectron diffraction * surface polarity Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.387, year: 2016

  13. Drug design based on x-ray diffraction and steered molecular dynamics

    Czech Academy of Sciences Publication Activity Database

    Hašek, Jindřich; Skálová, Tereza; Dohnálek, Jan; Dušková, Jarmila; Petroková, Hana; Vondráčková, Eva; Zimmermann, K.

    2005-01-01

    Roč. 12, č. 3 (2005), s. 208-210 ISSN 1211-5894. [VUFB Conference on Modern Methods in Synthesis and Analysis of Active Pharmaceutical Substances /5./. Praha, 23.11.2005-24.11.2005] R&D Projects: GA AV ČR KJB4050312 Institutional research plan: CEZ:AV0Z40500505 Keywords : drug design * X-ray diffraction * steered molecular dynamics Subject RIV: CF - Physical ; Theoretical Chemistry

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

    International Nuclear Information System (INIS)

    Leung, P.L.; Yang, B.

    1999-01-01

    The thermal activation characteristics (TACs) of the sensitivity of the '110 deg. 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

  15. X-ray diffraction study of pentachlorides of 5-7 group heavy transition metals

    International Nuclear Information System (INIS)

    Drobot, D.V.; Pisarev, E.A.

    1984-01-01

    The X-ray diffraction study of niobiume tantalum, molybdenum, tungsten and rhenium pentachlorides is performed. It is shown that all MCl 5 (M=Nb, Ta, Mo, W and Re) are crystallized in the NbCl 5 structural type and with the exception of TaCl 5 have some polymorphous modifications. The parameters of pentachloride lattices are determined and the frequencies reference in the IR spectrum of tungsten pentachoride is performed

  16. Structural transformation of compressed solid Ar: An x-ray diffraction study to 114 GPa

    International Nuclear Information System (INIS)

    Errandonea, D.; Boehler, R.; Japel, S.; Mezouar, M.; Benedetti, L. R.

    2006-01-01

    Room temperature angle-dispersive x-ray diffraction measurements on solid Ar up to 114 GPa reveal evidence of a structural phase transformation after stress relaxation by laser heating. Beyond 49.6 GPa, Ar exhibits the coexistence of fcc and hcp phases with an increasing hcp/fcc ratio, similar to the observation made recently on krypton and xenon. From the present results, we estimate the fcc-to-hcp transition to be completed at 300 GPa

  17. Qualitative characterization by x-ray diffraction from soils: mineralogy conditions to benefit the environment

    International Nuclear Information System (INIS)

    Fujiyama, Bruna Sayuri; Tavares, Mauricio de Moraes

    2010-01-01

    Four samples were collected from four soil profiles located in the Rural Federal University of Amazonia. These, were analyzed parameters such as color, texture, consistency, granulometry, porosity and water absorption. We identified the following soil types: Distrofic Yellow Latosoil; Lateritic Concretionary; distrofic Low Humic Gley. The work was to continue the qualitative analysis by X-rays diffraction, identifying the mineralogical composition of each sample. Explaining the mineralogical conditions that affect or benefit the environment. (author)

  18. Quantitative analysis of calcined fertilizers by X-ray diffraction patterns

    International Nuclear Information System (INIS)

    Cekinski, E.

    1987-01-01

    An X-ray diffraction pattern method for quantitative analyses of phosphate fertilizers obtained by calcination of a misture of Anitapolis phosphate concentrate and sodium carbonate is described. The method consists in plotting a calibration curve, using spinel (MgAl 2 O 4 ) as internal standard, of the phases that were formed by calcination, sintetized in laboratory. The tests conducted in order to avail the method accuracy showed good correlation between the obtained data and the real values. (author) [pt

  19. High-pressure powder x-ray diffraction experiments on Zn at low temperature

    CERN Document Server

    Takemura, K; Fujihisa, H; Kikegawa, T

    2002-01-01

    High-pressure powder x-ray diffraction experiments have been performed on Zn with a He-pressure medium at low temperature. When the sample was compressed in the He medium at low temperature, large nonhydrostaticity developed, yielding erroneous lattice parameters. On the other hand, when the pressure was changed at high temperatures, good hydrostaticity was maintained. No anomaly in the volume dependence of the c/a axial ratio has been found.

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

    Energy Technology Data Exchange (ETDEWEB)

    Leung, P.L.; Yang, B. E-mail: yangbr@bnu.edu.cn

    1999-09-01

    The thermal activation characteristics (TACs) of the sensitivity of the '110 deg. 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.

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

    Science.gov (United States)

    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.

  2. Influence of the crystal-surface unevenness on the angular spread of an x-ray diffracted beam

    International Nuclear Information System (INIS)

    Hrda, JaromIra; Potlovskiy, Kirill; Hrdy, JaromIr; Slechtova, Venceslava

    2005-01-01

    One of the factors influencing the focus size in diffractive-refractive optics is the quality of diffracting surface. If the surface is uneven, as it is when the silicon crystal surface is only etched, then the diffraction at each point of the surface is a combination of an asymmetric and inclined diffraction (general asymmetric diffraction). This somewhat deviates and spreads the diffracted beam. The integration over the surface hit by an incident beam gives the angular spread of the diffracted beam. It is shown theoretically that in some cases (highly asymmetric, highly inclined cut) the etched surface may create the spread of the diffracted beam such that it causes a significant broadening of the focus. In this case a mechanical-chemical polishing is necessary. This has been verified by us earlier in a preliminary experiment with synchrotron radiation. In this work the new experiment with the same crystals is performed using double crystal (+, -) arrangement and a laboratory x-ray source (CuKα radiation). We compared two samples; one of them is mechanically-chemically (MC) polished and thus the diffracting surface is almost perfect; the other is only etched. This experiment allows a better comparison of the result with the theory. The difference between the measured rocking curve widths for the etched and MC polished crystals (10'') roughly agrees with theory (7''), which supports the correctness of the theoretical approach

  3. Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

    Science.gov (United States)

    Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

    2016-11-01

    The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc

  4. Application of in-plane x-ray diffraction technique for residual stress measurement of TiN film/WC-Co alloy

    International Nuclear Information System (INIS)

    Takago, Shigeki; Yasui, Haruyuki; Awazu, Kaoru; Sasaki, Toshihiko; Hirose, Yukio; Sakurai, Kenji

    2006-01-01

    An in-plane X-ray diffraction technique was used to measure the residual stress of a CVD (chemical vapor deposition) TiN-coated WC-Co alloy. We could obtain the diffraction pattern from a thin film layer, eliminating that of the substrate. In the case of a conventional X-ray diffractometer, the X-ray penetration depth is about few μm. However, for a grazing incidence beam it is only 0.2μm. Depth profiles of residual stress in TiN film layer were evaluated by the present method and the conventional sin 2 ψ technique. We concluded that the in-plane diffraction technique enables us to determine the residual stress in a DVD-TiN film having an oriented texture. It was found that the residual tensile stress generated a mismatch of the coefficient of thermal expansion between the film and the substrate. (author)

  5. Application of in-plane x-ray diffraction technique for residual stress measurement of TiN film/WC-Co alloy

    Energy Technology Data Exchange (ETDEWEB)

    Takago, Shigeki; Yasui, Haruyuki; Awazu, Kaoru [Industrial Research Inst. of Ishikawa, Kanazawa, Ishikawa (Japan); Sasaki, Toshihiko; Hirose, Yukio [Kanazawa Univ., Dept. of Materials Science and Engineering, Kanazawa, Ishikawa (Japan); Sakurai, Kenji [National Inst. for Materials Science, Tsukuba, Ibaraki (Japan)

    2006-06-15

    An in-plane X-ray diffraction technique was used to measure the residual stress of a CVD (chemical vapor deposition) TiN-coated WC-Co alloy. We could obtain the diffraction pattern from a thin film layer, eliminating that of the substrate. In the case of a conventional X-ray diffractometer, the X-ray penetration depth is about few {mu}m. However, for a grazing incidence beam it is only 0.2{mu}m. Depth profiles of residual stress in TiN film layer were evaluated by the present method and the conventional sin{sup 2}{psi} technique. We concluded that the in-plane diffraction technique enables us to determine the residual stress in a DVD-TiN film having an oriented texture. It was found that the residual tensile stress generated a mismatch of the coefficient of thermal expansion between the film and the substrate. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Ludwig, W., E-mail: ludwig@esrf.fr [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); King, A. [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); School of Materials, University of Manchester, Manchester, M13 9PL (United Kingdom); Reischig, P. [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); Herbig, M. [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); Lauridsen, E.M.; Schmidt, S. [Riso National Laboratory for Sustainable Energy, Technical University of Denmark, P.O. Box 49, DK-4000 Roskilde (Denmark); Proudhon, H.; Forest, S. [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Cloetens, P.; Roscoat, S. Rolland du [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); Buffiere, J.Y. [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); Marrow, T.J. [School of Materials, University of Manchester, Manchester, M13 9PL (United Kingdom); Poulsen, H.F. [Riso National Laboratory for Sustainable Energy, Technical University of Denmark, P.O. Box 49, DK-4000 Roskilde (Denmark)

    2009-10-25

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

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

    International Nuclear Information System (INIS)

    Ludwig, W.; King, A.; Reischig, P.; Herbig, M.; Lauridsen, E.M.; Schmidt, S.; Proudhon, H.; Forest, S.; Cloetens, P.; Roscoat, S. Rolland du; Buffiere, J.Y.; Marrow, T.J.; Poulsen, H.F.

    2009-01-01

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

  8. Residual stress characterization of welds using x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Pineault, J.A.; Brauss, M.E.

    1996-01-01

    Neglect of residual stresses created during processes lead to stress corrosion cracking, distortion, fatigue cracking, premature failures in components, and instances of over design. Automated residual stress mapping and truly portable equipment have now made the characterization of residual stresses using x-ray diffraction (XRI) practical. The nondestructive nature of the x-ray diffraction technique has made the tile residual stress characterization of welds a useful tool for process optimization and failure analysis, particularly since components can be measured before and after welding and post welding processes. This paper illustrates the importance of residual stress characterization in welds and presents examples where x-ray diffraction techniques were applied in the characterization of various kinds of welds. arc welds, TIG welds, resistance welds, laser welds and electron beam welds. Numerous techniques are available to help manage potentially harmfull residual stresses created during the welding process thus, the effects of a few example post weld processes such as grinding, heat treating and shot peening are also addressed

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

    Energy Technology Data Exchange (ETDEWEB)

    Lambert, P. K.; Hustedt, C. J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C. [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Vecchio, K. S. [Department of NanoEngineering, University of California San Diego, La Jolla, California 92093 (United States); Huskins, E. L. [Oak Ridge Institute for Science and Education, Oak Ridge, Tennessee 37830 (United States); US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, Maryland 21005 (United States); Casem, D. T. [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, Maryland 21005 (United States); Gruner, S. M. [Department of Physics, Cornell University, Ithaca, New York 14853 (United States); Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853 (United States); Kavli Institute at Cornell for Nanoscale Science, Cornell University, Ithaca, New York 14853 (United States); Tate, M. W.; Philipp, H. T.; Purohit, P.; Weiss, J. T. [Department of Physics, Cornell University, Ithaca, New York 14853 (United States); Woll, A. R. [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853 (United States); Kannan, V.; Ramesh, K. T. [Department of Mechanical Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Kenesei, P.; Okasinski, J. S.; Almer, J. [X-ray Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    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.

  10. AUSPEX: a graphical tool for X-ray diffraction data analysis.

    Science.gov (United States)

    Thorn, Andrea; Parkhurst, James; Emsley, Paul; Nicholls, Robert A; Vollmar, Melanie; Evans, Gwyndaf; Murshudov, Garib N

    2017-09-01

    In this paper, AUSPEX, a new software tool for experimental X-ray data analysis, is presented. Exploring the behaviour of diffraction intensities and the associated estimated uncertainties facilitates the discovery of underlying problems and can help users to improve their data acquisition and processing in order to obtain better structural models. The program enables users to inspect the distribution of observed intensities (or amplitudes) against resolution as well as the associated estimated uncertainties (sigmas). It is demonstrated how AUSPEX can be used to visually and automatically detect ice-ring artefacts in integrated X-ray diffraction data. Such artefacts can hamper structure determination, but may be difficult to identify from the raw diffraction images produced by modern pixel detectors. The analysis suggests that a significant portion of the data sets deposited in the PDB contain ice-ring artefacts. Furthermore, it is demonstrated how other problems in experimental X-ray data caused, for example, by scaling and data-conversion procedures can be detected by AUSPEX.

  11. EPR and X-ray diffraction investigation of some Greek marbles and limestones

    International Nuclear Information System (INIS)

    Duliu, Octavian; Grecu, Maria Nicoleta; Cristea, Corina

    2009-01-01

    Twelve different marble and limestone samples collected from well-known Greek quarries have been investigated by X-ray diffraction and electron paramagnetic resonance (EPR). X-ray diffraction spectra permitted to determine both major (calcite and dolomite) and minor (quartz or magnesite) mineralogical components. EPR has been used to investigate the same samples unirradiated and after 10 kGy gamma-ray irradiation. The unirradiated samples display typical EPR spectra of Mn 2+ in calcite and dolomite as well as a superposition of these while some samples displayed EPR free radicals signals of centers (low field signal) and centers (high field signal). From X-ray diffraction and EPR spectra it was possible to extract numerical values of several numerical parameters such as dolomite to calcite ratio, EPR intensity parameter, and low field to high field EPR signals intensity ratio. These values as well as the correlation coefficients between the digital functions that described the low field Mn 2+ ions EPR line have been used as entry data for cluster analysis to quantify the resemblance and differences between analyzed samples. (authors)

  12. A X-ray diffraction analysis on graphene layers of Assam coal

    Energy Technology Data Exchange (ETDEWEB)

    Saikia, B.K.; Boruah, R.K.; Gogoi, P.K. [CSIR, Jorhat (India)

    2009-01-15

    The so-called turbostatic structure of carbons in coal with randomly oriented stacking of the lamellae (graphene) produces intense peaks, which are the dominant features in its X-ray diffraction profiles. The diffractogram may be conveniently divided into two regions of reciprocal space, the medium S region (1 < S < 3 {angstrom}) and a high S region (S > 3 {angstrom}) where S = 4 {pi} {lambda} {sup -1}sin{theta}. To better understand the molecular level structure of high sulphur Assam coal, two coal samples (Tirap-1 and Tirap-2) from Tirap colliery of Makum coalfield, Assam (India) has been interpreted in this study by using the X-ray diffraction profiles. Random layered (graphene) structural parameters of these coals were determined by using X-ray diffraction technique, which showed that the L{sub a} and L{sub c} are 64.99 angstrom and 22.63 angstrom for Tirap-2 and 55.54 angstrom and 23.80 angstrom for that of Tirap-1 coals respectively. The position of {gamma} band was found to be at 4.34 {angstrom} and 4.13 angstrom for Tirap-2 and Tirap-1 coals respectively. The number of layers and average number of carbon atoms (N) per aromatic graphene were found to be 21 and 8 for both the coal samples. Proximate, ultimate and ash analysis of the two coal samples were also carried out in this investigation.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

  14. Individual GaAs nanorods imaged by coherent X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Pietsch, Ullrich; Biermanns, Andreas; Davydok, Anton [Universitaet Siegen (Germany); Paetzelt, Hendrik [Universitaet Leipzig (Germany); IOM Leipzig (Germany); Diaz, Ana; Metzger, Hartmut [ID01 Beamline, ESRF (France); Gottschalch, Volker [Universitaet Leipzig (Germany)

    2010-07-01

    Semiconductor nanorods are of particular interest for new semiconductor devices because the nanorod approach can be used to form heterostructures of materials with a large lattice mismatch and to define nanorod arrays with tailored inter-rod distance. However, all applications require objects with uniform physical properties based on uniform morphology. Complementary to electron microscopy techniques, destruction free X-ray diffraction techniques can be used to determine structural and morphological details. Using scanning X-ray diffraction microscopy with a spot size of 220 x 600 nm{sup 2} we were able to inspect individual GaAs nanorods grown by seed-free MOVPE through circular openings in a SiN{sub x} mask in a periodic array with 3 {mu}m spacing on GaAs[111]B. The focussed X-ray beam allows the determination of the strain state of individual rods and in combination with coherent diffraction imaging, we were able to characterize also morphological details. Rods grown at different positions in the array show significant differences in shape, size and strain state.

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

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Wu, M.; Loisel, G. P. [Sandia National Laboratories, Albuquerque, New Mexico 87123 (United States)

    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.

  16. Computer simulation tools for X-ray analysis scattering and diffraction methods

    CERN Document Server

    Morelhão, Sérgio Luiz

    2016-01-01

    The main goal of this book is to break down the huge barrier of difficulties faced by beginners from many fields (Engineering, Physics, Chemistry, Biology, Medicine, Material Science, etc.) in using X-rays as an analytical tool in their research. Besides fundamental concepts, MatLab routines are provided, showing how to test and implement the concepts. The major difficult in analyzing materials by X-ray techniques is that it strongly depends on simulation software. This book teaches the users on how to construct a library of routines to simulate scattering and diffraction by almost any kind of samples. It provides to a young student the knowledge that would take more than 20 years to acquire by working on X-rays and relying on the available textbooks. In this book, fundamental concepts in applied X-ray physics are demonstrated through available computer simulation tools. Using MatLab, more than eighty routines are developed for solving the proposed exercises, most of which can be directly used in experimental...

  17. Ultrafast lattice dynamics in photoexcited nanostructures. Femtosecond X-ray diffraction with optimized evaluation schemes

    International Nuclear Information System (INIS)

    Schick, Daniel

    2013-01-01

    Within the course of this thesis, I have investigated the complex interplay between electron and lattice dynamics in nanostructures of perovskite oxides. Femtosecond hard X-ray pulses were utilized to probe the evolution of atomic rearrangement directly, which is driven by ultrafast optical excitation of electrons. The physics of complex materials with a large number of degrees of freedom can be interpreted once the exact fingerprint of ultrafast lattice dynamics in time-resolved X-ray diffraction experiments for a simple model system is well known. The motion of atoms in a crystal can be probed directly and in real-time by femtosecond pulses of hard X-ray radiation in a pump-probe scheme. In order to provide such ultrashort X-ray pulses, I have built up a laser-driven plasma X-ray source. The setup was extended by a stable goniometer, a two-dimensional X-ray detector and a cryogen-free cryostat. The data acquisition routines of the diffractometer for these ultrafast X-ray diffraction experiments were further improved in terms of signal-to-noise ratio and angular resolution. The implementation of a high-speed reciprocal-space mapping technique allowed for a two-dimensional structural analysis with femtosecond temporal resolution. I have studied the ultrafast lattice dynamics, namely the excitation and propagation of coherent phonons, in photoexcited thin films and superlattice structures of the metallic perovskite SrRuO 3 . Due to the quasi-instantaneous coupling of the lattice to the optically excited electrons in this material a spatially and temporally well-defined thermal stress profile is generated in SrRuO 3 . This enables understanding the effect of the resulting coherent lattice dynamics in time-resolved X-ray diffraction data in great detail, e.g. the appearance of a transient Bragg peak splitting in both thin films and superlattice structures of SrRuO 3 . In addition, a comprehensive simulation toolbox to calculate the ultrafast lattice dynamics and the

  18. X-ray diffraction and X-ray absorption of strained CoO and MnO thin films

    NARCIS (Netherlands)

    Csiszár, Szilárd Istvan; Tjeng, L.H

    2005-01-01

    The aim of this project was to study the influence of epitaxial strain on the electronic and magnetic structure of transition metal oxide layers. In the first part of the thesis the discovery of characteristic diffuse X-ray scattering patterns is reported. They are caused by the misfit dislocations,

  19. Structural study on Ni nanowires in an anodic alumina membrane by using in situ heating extended x-ray absorption fine structure and x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Cai Quan; Chen Xing; Chen Zhongjun; Wang Wei; Mo Guang; Wu Zhonghua; Zhang Junxi; Zhang Lide; Pan Wei

    2008-01-01

    Polycrystalline Ni nanowires have been prepared by electrochemical deposition in an anodic alumina membrane template with a nanopore size of about 60 nm. In situ heating extended x-ray absorption fine structure and x-ray diffraction techniques are used to probe the atomic structures. The nanowires are identified as being mixtures of nanocrystallites and amorphous phase. The nanocrystallites have the same thermal expansion coefficient, of 1.7 x 10 -5 K -1 , as Ni bulk; however, the amorphous phase has a much larger thermal expansion coefficient of 3.5 x 10 -5 K -1 . Details of the Ni nanowire structures are discussed in this paper

  20. Effects of proton irradiation on structure of NdFeB permanent magnets studied by X-ray diffraction and X-ray absorption fine structure

    International Nuclear Information System (INIS)

    Yang, L.; Zhen, L.; Xu, C.Y.; Sun, X.Y.; Shao, W.Z.

    2011-01-01

    The effects of proton irradiation on the structure of NdFeB permanent magnet were investigated by X-ray diffraction and X-ray absorption fine structure (XAFS). The results reveal that proton irradiation has no effect on the long-range structure, but significantly affects the atomic local structure of the NdFeB magnet. The alignment degree of the magnet decreases and the internal stress of the lattice increases after proton irradiation. XAFS results show that the coordination number of Fe-Nd in the first neighboring coordination shell of the Fe atoms decreases and the disorder degree increases.

  1. Effects of proton irradiation on structure of NdFeB permanent magnets studied by X-ray diffraction and X-ray absorption fine structure

    Energy Technology Data Exchange (ETDEWEB)

    Yang, L. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zhen, L., E-mail: lzhen@hit.edu.c [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Xu, C.Y.; Sun, X.Y.; Shao, W.Z. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2011-01-15

    The effects of proton irradiation on the structure of NdFeB permanent magnet were investigated by X-ray diffraction and X-ray absorption fine structure (XAFS). The results reveal that proton irradiation has no effect on the long-range structure, but significantly affects the atomic local structure of the NdFeB magnet. The alignment degree of the magnet decreases and the internal stress of the lattice increases after proton irradiation. XAFS results show that the coordination number of Fe-Nd in the first neighboring coordination shell of the Fe atoms decreases and the disorder degree increases.

  2. Real-time observation of epitaxial crystal growth in gaseous environment using x-ray diffraction and x-ray reflectometry

    International Nuclear Information System (INIS)

    Kawamura, Tomoaki; Bhunia, Satyaban; Watanabe, Yoshio; Fujikawa, Seiji

    2008-01-01

    We made the x-ray diffractometer combined with the MOCVD growth system for the real-time observation of epitaxial growth in gaseous environment, and investigated the growth mechanism of InP crystals. Changes of the (-5/2 O) Bragg diffraction during the growth revealed that the growth starts immediately after the In source has been supplied and gradually stopped, owing to the migrating In atoms on the surface. Additionally, one can easily determine the growth modes, including 3-dimensional mode, layer-by-layer mode, and step-flow mode, by observing the change of x-ray reflectivity with various growth conditions. (author)

  3. X-ray diffraction without sample preparation: Proof-of-principle experiments

    International Nuclear Information System (INIS)

    Hansford, Graeme M.

    2013-01-01

    The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

  4. Optimization of an X-ray diffraction imaging system for medical and security applications

    International Nuclear Information System (INIS)

    Marticke, Fanny

    2016-01-01

    X-ray diffraction imaging is a powerful noninvasive technique to identify or characterize different materials. Compared to traditional techniques using X-ray transmission, it allows to extract more material characteristic information, such as the Bragg peak positions for crystalline materials as well as the molecular form factor for amorphous materials. The potential of this technique has been recognized by many researchers and numerous applications such as luggage inspection, nondestructive testing, drug detection and biological tissue characterization have been proposed. The method of energy dispersive X-ray diffraction (EDXRD) is particularly suited for this type of applications as it allows the use of a conventional X-ray tube, the acquisition of the whole spectrum at the same time and parallelized architectures to inspect an entire object in a reasonable time. The purpose of the present work is to optimize the whole material characterization chain. Optimization comprises two aspects: optimization of the acquisition system and of data processing. The last one concerns especially the correction of diffraction pattern degraded by acquisition process. Reconstruction methods are proposed and validated on simulated and experimental spectra. System optimization is realized using figures of merit such as detective quantum efficiency (DQE), contrast to noise ratio (CNR) and receiver operating characteristic (ROC) curves.The first chosen application is XRD based breast imaging which aims to distinguish cancerous tissues from healthy tissues. Two non-multiplexed collimation configurations combining EDXRD and ADXRD are proposed after optimization procedure. A simulation study of the whole system and a breast phantom was realized to determine the required dose to detect a 4 mm carcinoma nodule. The second application concerns detection of illicit materials during security check. The possible benefit of a multiplexed collimation system was examined. (author) [fr

  5. Computer simulations of X-ray six-beam diffraction in a perfect silicon crystal. I

    Czech Academy of Sciences Publication Activity Database

    Kohn, V.G.; Khikhlukha, Danila

    2016-01-01

    Roč. 72, May (2016), s. 349-356 ISSN 2053-2733 R&D Projects: GA MŠk EF15_008/0000162; GA MŠk ED1.1.00/02.0061 Grant - others:ELI Beamlines(XE) CZ.02.1.01/0.0/0.0/15_008/0000162; ELI Beamlines(XE) CZ.1.05/1.1.00/02.0061 Institutional support: RVO:68378271 Keywords : X-ray diffraction * silicon crystal * six-beam diffraction * section topography * computer simulations Subject RIV: BL - Plasma and Gas Discharge Physics OBOR OECD: Fluids and plasma physics (including surface physics) Impact factor: 5.725, year: 2016

  6. A new device for X-ray Diffraction analyses of irradiated materials

    International Nuclear Information System (INIS)

    Valot, Christophe; Blay, Thierry; Caillot, Laurent; Ferroud-Plattet, Marie Pierre

    2008-01-01

    A new X-Ray Diffraction (XRD) equipment is being implemented in the LECA (Cea - Cadarache) hot laboratory. The device will be dedicated to structural characterization on irradiated fuels, as PWR fuels, transmutation targets and innovative fuels. The paper will present the specific design that was decided in order to reduce the number of components in contaminated volume and to make servicing easier. The analytical performances of this new equipment will be illustrated on some model samples: -) micro-diffraction capabilities will be detailed on heterogeneous material; -) strain and stress analyses on fresh uranium oxide pellets. (authors)

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

    International Nuclear Information System (INIS)

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

    2006-01-01

    Crystals adequate for X-ray diffraction analysis have been prepared from L. interrogans ferredoxin-NADP + reductase. Ferredoxin-NADP + 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Alessandro S.; Ferrarezi, Thiago [Instituto de Física de São Carlos, Universidade de São Paulo, Av. Trabalhador Saocarlense 400, São Carlos, SP, 13560-970 (Brazil); Catalano-Dupuy, Daniela L.; Ceccarelli, Eduardo A. [Facultad de Ciencias Bioquímicas y Farmacéuticas, Molecular Biology Division, Instituto de Biología Molecular y Celular de Rosario (IBR), CONICET, Universidad Nacional de Rosario, Suipacha 531, S2002LRK Rosario (Argentina); Polikarpov, Igor, E-mail: ipolikarpov@if.sc.usp.br [Instituto de Física de São Carlos, Universidade de São Paulo, Av. Trabalhador Saocarlense 400, São Carlos, SP, 13560-970 (Brazil)

    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.

  9. Use of overlapped reflection for determining the retained austenite by X-ray diffraction

    International Nuclear Information System (INIS)

    Garin, J.L.; Gonzalez, C.F.

    1988-01-01

    Retainec austenite in high-carbon steels has been determined by means of new computation techniques applied to the processing of X-ray diffraction data. Instead of using the traditional procedure based on the weak (200) reflections of martensite and austenite, intensity measurements of the overlapped (110) peak of martensite and (111) peak of austenite were performed. The separation of the peaks was based on a Pearson VII function, which is capable of describing all diffraction profiles. The accuracy of integrated intensities was then improved with the beneficial effects of higher precision in the calculation of the amount of retained austenite. (author) [pt

  10. Real Structure and Resudal Stresses in Advanced Welds Determined by X-ray and Neutron Diffraction

    Czech Academy of Sciences Publication Activity Database

    Trojan, K.; Hervoches, Charles; Ganev, N.; Mikula, Pavol; Čapek, J.

    2017-01-01

    Roč. 9, SEP (2017), s. 32-38 E-ISSN 2336-5382 R&D Projects: GA MŠk LM2015056; GA ČR GB14-36566G Institutional support: RVO:61389005 Keywords : laser and MAG welding * residual stresses * X-ray diffraction * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) https://ojs.cvut.cz/ojs/index.php/APP/article/view/4401/4298

  11. New analytical method for asbestos determination in Syrian soils using X-ray diffraction

    International Nuclear Information System (INIS)

    Kassem, M.

    2009-07-01

    In this work, a standard samples have been prepared by mixing a definite quantity of soil with calculated concentration of asbestos; 1, 2, 4, 8, 10, 20, 40, 60, 80, 100% wt . The samples have been analyzed by x-ray powder diffraction using the same parameters ; 2θ between 5-90, detector step= 0.5 /30 sec. The diffraction peaks intensities have been chosen such a manner than no superposition with those of the soil. confidence levels has been used as accuracy method for error calculation of the peaks positions. (author)

  12. Hard X-ray nanoimaging method using local diffraction from metal wire

    Energy Technology Data Exchange (ETDEWEB)

    Takano, Hidekazu, E-mail: htakano@sci.u-hyogo.ac.jp; Konishi, Shigeki; Shimomura, Sho; Azuma, Hiroaki; Tsusaka, Yoshiyuki; Kagoshima, Yasushi [Center for Novel Material Science under Multi-Extreme Conditions, Graduate School of Material Science, University of Hyogo, Kamigori, Hyogo 678-1297 (Japan)

    2014-01-13

    A simple hard X-ray imaging method achieving a high spatial resolution is proposed. Images are obtained by scanning a metal wire through the wave field to be measured and rotating the sample to collect data for back projection calculations; the local diffraction occurring at the edges of the metal wire operates as a narrow line probe. In-line holograms of a test sample were obtained with a spatial resolution of better than 100 nm. The potential high spatial resolution of this method is shown by calculations using diffraction theory.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

    Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it's main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-12-01

    Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it`s main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

  15. X-ray fluorescence analysis of thin films at glancing-incident and -takeoff angles

    International Nuclear Information System (INIS)

    Tsuji, K.; Sato, S.; Hirokawa, K.

    1995-01-01

    We have developed a new analytical method, Glancing-Incidence and -Takeoff X-Ray Fluorescence (GIT-XRF) method for the first time. Here, we present an idea for a thin-film analysis and a surface analysis by the GIT-XRF method. In this method, the dependence of the fluorescent x-ray intensity on takeoff angle is measured at various incident angles of the primary x-ray. Compared with a total reflection x-ray fluorescence method, the GIT-XRF method allows a detailed thin-film analysis, because the thin film is cross-checked by many experimental curves. Moreover, a surface-sensitive analysis is also possible by the GIT-XRF method. (author)

  16. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Directory of Open Access Journals (Sweden)

    Hongjia Zhang

    2018-03-01

    Full Text Available High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short. As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation.

  17. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Science.gov (United States)

    Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

    2018-01-01

    High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kohn, V. G., E-mail: kohnvict@yandex.ru [National Research Centre “Kurchatov Institute” (Russian Federation); Smirnova, I. A. [Russian Academy of Sciences, Institute of Solid State Physics (Russian Federation)

    2016-07-15

    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 MoK{sub 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.

  20. Room temperature femtosecond X-ray diffraction of photosystem II microcrystals

    Science.gov (United States)

    Kern, Jan; Alonso-Mori, Roberto; Hellmich, Julia; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Sellberg, Jonas; Lassalle-Kaiser, Benedikt; Gildea, Richard J.; Glatzel, Pieter; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; McQueen, Trevor A.; DiFiore, Dörte; Fry, Alan R.; Messerschmidt, Marc; Miahnahri, Alan; Schafer, Donald W.; Seibert, M. Marvin; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Messinger, Johannes; Sauter, Nicholas K.; Zouni, Athina; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K.

    2012-01-01

    Most of the dioxygen on earth is generated by the oxidation of water by photosystem II (PS II) using light from the sun. This light-driven, four-photon reaction is catalyzed by the Mn4CaO5 cluster located at the lumenal side of PS II. Various X-ray studies have been carried out at cryogenic temperatures to understand the intermediate steps involved in the water oxidation mechanism. However, the necessity for collecting data at room temperature, especially for studying the transient steps during the O–O bond formation, requires the development of new methodologies. In this paper we report room temperature X-ray diffraction data of PS II microcrystals obtained using ultrashort (< 50 fs) 9 keV X-ray pulses from a hard X-ray free electron laser, namely the Linac Coherent Light Source. The results presented here demonstrate that the ”probe before destroy” approach using an X-ray free electron laser works even for the highly-sensitive Mn4CaO5 cluster in PS II at room temperature. We show that these data are comparable to those obtained in synchrotron radiation studies as seen by the similarities in the overall structure of the helices, the protein subunits and the location of the various cofactors. This work is, therefore, an important step toward future studies for resolving the structure of the Mn4CaO5 cluster without any damage at room temperature, and of the reaction intermediates of PS II during O–O bond formation. PMID:22665786