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Sample records for insitu x-ray diffraction

  1. X-Ray Diffraction and Fluorescence Measurements for In-situ Planetary Instruments

    Science.gov (United States)

    Hansford, G.; Hill, K. S.; Vernon, D.; Ambrosi, R. M.; Bridges, J.; Hutchinson, I.

    2010-12-01

    The X-Ray Diffraction (XRD) instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA EXOMARS missions and will provide the first demonstrations of an XRF/XRD instrument’s capabilities in-situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-Ray Diffraction instrument, Mars XRD. The ExoMars X-ray diffraction instrument incorporates an 55-Fe radioisotope source and three fixed-position CCDs to simultaneously acquire an X-Ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition [1]. The CCDs cover an angular range from 6 to 65-deg enabling the analysis of silicates, from clays, or other phyllosilicates characterised by varying d-spacings, to oxides, and carbonates or evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an 55-Fe source and X-ray sensitive CCD [1]. The XRD/XRD test system consists of a single CCD on a motorised arm, an 55-Fe X-ray source, source collimator and a sample table which approximately replicate the reflection geometry of the XRD instrument. It was used to test geological reference standard materials and Martian analogues. Incidence angle and CCD angles on both the diffraction and fluorescence results were evaluated. A key area of interest is the effect of sample roughness on the XRD/XRF results. We present results from testing pressed powder pellet samples of varying surface roughness, and a comparison with model results [2]. So far we have found that increased roughness causes a reduced intensity at lower take-off angles. Several methods for measuring surface roughness of the samples have been used including an Alicona Infinite

  2. X-ray induced chemical reaction revealed by in-situ X-ray diffraction and scanning X-ray microscopy in 15 nm resolution (Conference Presentation)

    Science.gov (United States)

    Ge, Mingyuan; Liu, Wenjun; Bock, David; De Andrade, Vincent; Yan, Hanfei; Huang, Xiaojing; Marschilok, Amy; Takeuchi, Esther; Xin, Huolin; Chu, Yong S.

    2016-09-01

    The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever increasing source brightness, which have significantly advanced ex-situ and in-situ research for energy materials, such as lithium-ion batteries. However, the strong beam-matter interaction arisen from the high beam flux can significantly modify the material structure. The parasitic beam-induced effect inevitably interferes with the intrinsic material property, which brings difficulties in interpreting experimental results, and therefore requires comprehensive evaluation. Here we present a quantitative in-situ study of the beam-effect on one electrode material Ag2VO2PO4 using four different X-ray probes with different radiation dose rate. The material system we reported exhibits interesting and reversible radiation-induced thermal and chemical reactions, which was further evaluated under electron microscopy to illustrate the underlying mechanism. The work we presented here will provide a guideline in using synchrotron X-rays to distinguish the materials' intrinsic behavior from extrinsic structure changed induced by X-rays, especially in the case of in-situ and operando study where the materials are under external field of either temperature or electric field.

  3. Uranium oxidation kinetics monitored by in-situ X-ray diffraction

    Science.gov (United States)

    Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

    2017-03-01

    The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

  4. X-Ray Diffraction.

    Science.gov (United States)

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

    1980-01-01

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

  5. X-Ray Diffraction.

    Science.gov (United States)

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

    1980-01-01

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

  6. Diffraction imaging for in-situ characterization of double-crystal x-ray monochromators

    CERN Document Server

    Stoupin, Stanislav; Heald, Steve M; Brewe, Dale; Meron, Mati

    2015-01-01

    Imaging of the Bragg reflected x-ray beam is proposed and validated as an in-situ method for characterization of performance of double-crystal monochromators under the heat load of intense synchrotron radiation. A sequence of images is collected at different angular positions on the reflectivity curve of the second crystal and analyzed. The method provides rapid evaluation of the wavefront of the exit beam, which relates to local misorientation of the crystal planes along the beam footprint on the thermally distorted first crystal. The measured misorientation can be directly compared to results of finite element analysis. The imaging method offers an additional insight on the local intrinsic crystal quality over the footprint of the incident x-ray beam.

  7. Titanium boride equation of state determined by in-situ X-ray diffraction

    OpenAIRE

    Shigeaki Ono; Takumi Kikegawa

    2016-01-01

    The equation of state (EOS) of titanium boride, TiB2, was investigated by in situ X-ray diffraction in a diamond anvil cell and multianvil high-pressure apparatus. The pressure-volume-temperature (P-V-T) data were collected at up to 111 GPa and room temperature for the diamond-anvil cell experiments and at up to 15 GPa and 1300 K for the multianvil experiments. No phase transition was observed through the entire range of experimental conditions. The pressure-volume data at room temperature we...

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

    Science.gov (United States)

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

    2016-06-01

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

  9. Titanium boride equation of state determined by in-situ X-ray diffraction.

    Science.gov (United States)

    Ono, Shigeaki; Kikegawa, Takumi

    2016-12-01

    The equation of state (EOS) of titanium boride, TiB2, was investigated by in situ X-ray diffraction in a diamond anvil cell and multianvil high-pressure apparatus. The pressure-volume-temperature (P-V-T) data were collected at up to 111 GPa and room temperature for the diamond-anvil cell experiments and at up to 15 GPa and 1300 K for the multianvil experiments. No phase transition was observed through the entire range of experimental conditions. The pressure-volume data at room temperature were fitted using a Vinet EOS to obtain the isothermal bulk modulus, BT0 = 256.7 GPa, and its pressure derivative, B' T0 = 3.83. When fitting a thermal EOS using the P-V-T data for the multianvil experiments, we find that [Formula: see text] = 0.095 (GPa/K) and α 0 = 2.49 × 10(-5) K(-1).

  10. Characterization of beryllium deformation using in-situ x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Magnuson, Eric Alan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Donald William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Clausen, Bjorn [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Sisneros, Thomas A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Park, Jun-Sang [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-08-24

    Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advanced Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.

  11. Titanium boride equation of state determined by in-situ X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Shigeaki Ono

    2016-12-01

    Full Text Available The equation of state (EOS of titanium boride, TiB2, was investigated by in situ X-ray diffraction in a diamond anvil cell and multianvil high-pressure apparatus. The pressure-volume-temperature (P-V-T data were collected at up to 111 GPa and room temperature for the diamond-anvil cell experiments and at up to 15 GPa and 1300 K for the multianvil experiments. No phase transition was observed through the entire range of experimental conditions. The pressure-volume data at room temperature were fitted using a Vinet EOS to obtain the isothermal bulk modulus, BT0 = 256.7 GPa, and its pressure derivative, B’T0 = 3.83. When fitting a thermal EOS using the P-V-T data for the multianvil experiments, we find that (∂BT/∂TV = 0.095 (GPa/K and α0 = 2.49 × 10−5 K−1.

  12. In-situ synchrotron wide-angle X-ray diffraction as a rapid method for cocrystal/salt screening.

    Science.gov (United States)

    Dong, Pin; Lin, Ling; Li, Yongcheng; Huang, Zhengwei; Lang, Tianqun; Wu, Chuanbin; Lu, Ming

    2015-12-30

    The purpose of this work was to explore in-situ synchrotron wide-angle X-ray diffraction (WAXD) as a rapid and accurate tool to screen and monitor the formation of cocrystal/salts during heating. The active pharmaceutical ingredients (caffeine, carbamazepine and lamotrigine) were respectively mixed with the coformer (saccharin), and then heated by the hot stage. Real-time process monitoring was performed using synchrotron WAXD to assess cocrystal formation and subsequently compared to differential scanning calorimetry (DSC) measurements. The effect of heating rates and cocrystal growth behavior were investigated. Synchrotron WAXD was fast and sensitive to detect cocrystal formation with the appearance of characteristic diffraction rings, even at the heating rate of 30°C/min, while DSC curves showed overlapped peaks. Unlike the indirect characterization of DSC on endo/exothermic peaks, synchrotron WAXD can directly and qualitatively determine cocrystal by diffraction peaks. The diffraction intensity-temperature curves and the corresponding first-derivative curves clearly exhibited the growth behavior of cocrystal upon heating, providing useful information to optimize the process temperature of hot melt extrusion to continuously manufacture cocrystal. The study suggests that in-situ synchrotron WAXD could provide a one-step process to screen cocrystal at high efficiency and reveal the details of cocrystal/salts growth behavior.

  13. Crystallization in Fe- and Co-Based Amorphous Alloys Studied by In-Situ X-Ray Diffraction

    Science.gov (United States)

    Zhang, L. J.; Yu, P. F.; Cheng, H.; Zhang, M. D.; Liu, D. J.; Zhou, Z.; Jin, Q.; Liaw, P. K.; Li, G.; Liu, R. P.

    2016-12-01

    The amorphous alloys, Fe80Si20, Fe78Si9B13, and Fe4Co67Mo1.5Si16.5B11, were prepared by the spinning method in pure argon. The crystallization behaviors of the three amorphous alloys were researched by in-situ X-ray diffraction (XRD), and the crystallization activation energy was calculated, based on the results of differential scanning calorimetry. The crystallization mechanism of the Fe- and Co-based alloys was analyzed, based on the experimental data. The transformation kinetics was described in terms of Johnson-Mehl-Avrami kinetics, except that the Avrami exponent of the Fe78Si9B13 amorphous alloy annealed at 753 K (480 °C) was 4.12; the obtained values for the overall Avrami exponents of the other three amorphous alloys were below 1, as usually found for the Fe-Si amorphous alloys.

  14. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Energy Technology Data Exchange (ETDEWEB)

    Sarma, Abhisakh; Sanyal, Milan K., E-mail: milank.sanyal@saha.ac.in [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064 (India)

    2014-09-15

    In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 10{sup 7}. This value remain almost constant over a frequency range from 1Hz to 10{sup 6} Hz even at 80 K temperature.

  15. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Directory of Open Access Journals (Sweden)

    Abhisakh Sarma

    2014-09-01

    Full Text Available In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 107. This value remain almost constant over a frequency range from 1Hz to 106 Hz even at 80 K temperature.

  16. X-Ray Diffraction Apparatus

    Science.gov (United States)

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

    1996-01-01

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

  17. In-situ Characterization of Water-Gas Shift Catalysts using Time-Resolved X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, J.; Hanson, J; Wen, W; Wang, X; Brito, J; Martnez-Arias, A; Fernandez-Garca, M

    2009-01-01

    Time-resolved X-ray diffraction (XRD) has emerged as a powerful technique for studying the behavior of heterogeneous catalysts (metal oxides, sulfides, carbides, phosphides, zeolites, etc.) in-situ during reaction conditions. The technique can identify the active phase of a heterogeneous catalyst and how its structure changes after interacting with the reactants and products (80 K < T < 1200 K; P < 50 atm). In this article, we review a series of recent works that use in-situ time-resolved XRD for studying the water-gas shift reaction (WGS, CO + H2O ? H2 + CO2) over several mixed-metal oxides: CuMoO4, NiMoO4, Ce1-xCuxO2-d and CuFe2O4. Under reaction conditions the oxides undergo partial reduction. Neutral Cu0 (i.e. no Cu1+ or Cu2+ cations) and Ni0 are the active species in the catalysts, but interactions with the oxide support are necessary in order to obtain high catalytic activity. These studies illustrate the important role played by O vacancies in the mechanism for the WGS. In the case of Ce1-xCuxO2-d, Rietveld refinement shows expansions/contractions in the oxide lattice which track steps within the WGS process: CO(gas) + O(oxi) ? CO2(gas) + O(vac); H2O(gas) + O(vac) ? O(oxi) + H2(gas).

  18. In-situ and operando characterization of batteries with energy-dispersive synchrotron x-ray diffraction

    Science.gov (United States)

    Paxton, William Arthur

    Batteries play a pivotal role in the low-carbon society that is required to thwart the effects of climate change. Alternative low-carbon energy sources, such as wind and solar, are often intermittent and unreliable. Batteries are able capture their energy and deliver it later when it is needed. The implementation of battery systems in grid-level and transportation sectors is essential for efficient use of alternative energy sources. Scientists and engineers need better tools to analyze and measure the performance characteristics of batteries. One of the main hindrances in the progress of battery research is that the constituent electrode materials are inaccessible once an electrochemical cell is constructed. This leaves the researcher with a limited number of available feedback mechanisms to assess the cell's performance, e.g., current, voltage, and impedance. These data are limited in their ability to reveal the more-localized smaller-scale structural mechanisms on which the batteries' performance is so dependent. Energy-dispersive x-ray diffraction (EDXRD) is one of the few techniques that can internally probe a sealed battery. By analyzing the structural behavior of battery electrodes, one is able to gain insight to the physical properties on which the battery's performance is dependent. In this dissertation, EDXRD with ultrahigh energy synchrotron radiation is used to probe the electrodes of manufactured primary and secondary lithium batteries under in-situ and operando conditions. The technique is then applied to solve specific challenges facing lithium ion batteries. Diffraction spectra are collected from within a battery at 40 micrometer resolution. Peak-fitting is used to quantitatively estimate the abundance of lithiated and non-lithiated phases. Through mapping the distribution of phases within, structural changes are linked to the battery's galvanic response. A three-dimensional spatial analysis of lithium iron phosphate batteries suggests that evolution

  19. In-situ High-energy X-ray Diffraction Study of the Local Structure of Supercooled Liquid Si

    Science.gov (United States)

    Lee, G. W.; Kim, T. H.; Sieve, B.; Gangopadhyay, A. K.; Hyers, R. W.; Rathz, T. J.; Rogers, J. R.; Robinson, D. S.; Kelton, K. F.; Goldman, A. I.

    2005-01-01

    While changes in the coordination number for liquid silicon upon supercooling, signaling an underlying liquid-liquid phase transition, have been predicted, x-ray and neutron measurements have produced conflicting reports. In particular some studies have found an increase in the first shell coordination as temperature decreases in the supercooled regime, while others have reported increases in the coordination number with decreasing temperature. Employing the technique of electrostatic levitation coupled with high energy x-ray diffraction (125 keV), and rapid data acquisition (100ms collection times) using an area detector, we have obtained high quality structural data more deeply into the supercooled regime than has been possible before. No change in coordination number is observed in this temperature region, calling into question previous experimental claims of structural evidence for the existence of a liquid-liquid phase transition.

  20. Chromium Reaction Mechanisms for Speciation using Synchrotron in-Situ High-Temperature X-ray Diffraction.

    Science.gov (United States)

    Low, Fiona; Kimpton, Justin; Wilson, Siobhan A; Zhang, Lian

    2015-07-07

    We use in situ high-temperature X-ray diffraction (HT-XRD), ex-situ XRD and synchrotron X-ray absorption near edge structure spectroscopy (XANES) to derive fundamental insights into mechanisms of chromium oxidation during combustion of solid fuels. To mimic the real combustion environment, mixtures of pure eskolaite (Cr(3+)2O3), lime (CaO) and/or kaolinite [Al2Si2O5(OH)4] have been annealed at 600-1200 °C in air versus 1% O2 diluted by N2. Our results confirm for the first time that (1) the optimum temperature for Cr(6+) formation is 800 °C for the coexistence of lime and eskolaite; (2) upon addition of kaolinite into oxide mixture, the temperature required to produce chromatite shifts to 1000 °C with a remarkable reduction in the fraction of Cr(6+). Beyond 1000 °C, transient phases are formed that bear Cr in intermediate valence states, which convert to different species other than Cr(6+) in the cooling stage; (3) of significance to Cr mobility from the waste products generated by combustion, chromatite formed at >1000 °C has a glassy disposition that prevents its water-based leaching; and (4) Increasing temperature facilitates the migration of eskolaite particles into bulk lime and enhances the extent to which Cr(3+) is oxidized, thereby completing the oxidation of Cr(3+) to Cr(6+) within 10 min.

  1. Diffractive X-Ray Telescopes

    Science.gov (United States)

    Skinner, Gerald K.

    2010-01-01

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

  2. Diffractive X-ray Telescopes

    CERN Document Server

    Skinner, Gerald K

    2010-01-01

    Diffractive X-ray telescopes using zone plates, phase Fresnel lenses, or related optical elements have the potential to provide astronomers with true imaging capability with resolution 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 space- time in the immediate vicinity of the super-massive black holes in the center of active galaxies What then is precluding their immediate adoption? Extremely long focal lengths, very limited bandwidth, and difficulty stabilizing the image are the main problems. The history, and status of the development of such lenses is reviewed here and the prospects for managing the challenges that they present are discussed.

  3. Advanced Techniques for In-Situ Monitoring of Phase Transformations During Welding Using Synchrotron-Based X-Ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Elmer, J W; Palmer, T A; Zhang, W; DebRoy, T

    2005-06-05

    Understanding the evolution of microstructure in welds is an important goal of welding research because of the strong correlation between weld microstructure and weld properties. To achieve this goal it is important to develop a quantitative measure of phase transformations encountered during welding in order to ultimately develop methods for predicting weld microstructures from the characteristics of the welding process. To aid in this effort, synchrotron radiation methods have been developed at Lawrence Livermore National Laboratory (LLNL) for direct observation of microstructure evolution during welding. Using intense, highly collimated synchrotron radiation, the atomic structure of the weld heat affected and fusion zones can be probed in real time. Two synchrotron-based techniques, known as spatially resolved (SRXRD) and time resolved (TRXRD) x-ray diffraction, have been developed for these investigations. These techniques have now been used to investigate welding induced phase transformations in titanium alloys, low alloy steels, and stainless steel alloys. This paper will provide a brief overview of these methods and will discuss microstructural evolution during the welding of low carbon (AISI 1005) and medium carbon (AISI 1045) steels where the different levels of carbon influence the evolution of microstructures during welding.

  4. Predicting Fracture Toughness of TRIP 800 using Phase Properties Characterized by In-Situ High Energy X-Ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Soulami, Ayoub; Choi, Kyoo Sil; Liu, Wenning N.; Sun, Xin; Khaleel, Mohammad A.; Ren, Yang; Wang, Yan-Dong

    2010-05-01

    TRansformation Induced Plasticity (TRIP) steel is a typical representative of 1st generation advanced high strength steel (AHSS) which exhibits a combination of high strength and excellent ductility due to its multiphase microstructure. In this paper, we study the crack propagation behavior and fracture resistance of a TRIP 800 steel using a microstructure-based finite element method with the various phase properties characterized by in-situ high energy Xray diffraction (HEXRD) technique. Uniaxial tensile tests on the notched TRIP 800 sheet specimens were also conducted, and the experimentally measured tensile properties and R-curves (Resistance curves) were used to calibrate the modeling parameters and to validate the overall modeling results. The comparison between the simulated and experimentally measured results suggests that the micromechanics based modeling procedure can well capture the overall complex crack propagation behaviors and the fracture resistance of TRIP steels. The methodology adopted here may be used to estimate the fracture resistance of various multiphase materials.

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

    Science.gov (United States)

    Eastwood, D. S.; Ali, M.; Hickey, B. J.; Tanner, B. K.

    2013-12-01

    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.

  6. Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

    Science.gov (United States)

    Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.; Almer, Jonathan D.

    2016-04-01

    High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c δ hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the α-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 °C. The f.c.c δ was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region and region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 °C.

  7. Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.; Almer, Jonathan D.

    2016-04-01

    High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c delta hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the alpha-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 degrees C. The f.c.c delta was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region and region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 degrees C.

  8. Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Jun-li; Han, Xiaochun [Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL (United States); Heuser, Brent J., E-mail: bheuser@illinois.edu [Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL (United States); Almer, Jonathan D. [Advanced Photon Source, Argonne National Laboratory, Argonne, IL (United States)

    2016-04-01

    High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c δ hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the α-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 °C. The f.c.c δ was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region and region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 °C.

  9. Using in-situ synchrotron x-ray diffraction to investigate phase transformation and lattice relaxation of a three-way piezo-phototronic soft material

    Science.gov (United States)

    Ko, Wen-Ching; Hsu, Yu-Hsiang; Weng, Shih-Chang; Chang, Chung-Kai; Lee, Ming-Tao; Chuang, Wei-Tsung; Thong, Hao-Cheng; Ali, Muhammad; Huang, E.-Wen

    2017-07-01

    A poly(vinylidene fluoride-co-trifluoro-ethylene) piezoelectric polymer is blended with nano particles of titanium oxide phthalocyanine to bridge photoconductive and piezoelectric effects. In this study, a system is examined by in situ synchrotron x-ray to test a three-way piezo-phototronic soft-material design. The sample is heated for in situ phase transformation characterization. The semi-crystalline poly (vinylidene fluoride-co-trifluoro-ethylene) polymer gradually transforms to an amorphous structure. A complementary piezoelectric experiment before and after the heating experiment shows that the piezoelectric performance is proportional to the phase ratio. Secondly, the system is examined to test its phototronic effect. Piezoelectric responses are measured by controlling the light illumination. The positive and negative controls of light illumination which validate this newly-designed system can be modulated by a three-way piezo-phototronic effect. In-situ synchrotron x-ray diffraction experiments are employed to measure the microstructure evolution as a function of applied voltage up to 800 V. We then turned off both the light and the applied voltage to examine the kinetic behavior of the system. There is orientation-dependent anisotropic relaxation. We compared the lattice-strain evolutions. Piezo-phototronic creep is found in the (110), but not the (310) planes.

  10. In-situ high-energy X-ray diffraction investigation on stress-induced martensitic transformation in Ti-Nb binary alloys

    Energy Technology Data Exchange (ETDEWEB)

    Chang, L. L.; Wang, Y. D.; Ren, Y.

    2016-01-10

    Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated prior to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.

  11. X-ray diffraction: instrumentation and applications.

    Science.gov (United States)

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

    2015-01-01

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

  12. X-Ray Diffractive Optics

    Science.gov (United States)

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

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

  13. 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

  14. In-situ Curvature Monitoring and X-Ray Diffraction Study of InGaAsP/InGaP Quantum Wells

    Energy Technology Data Exchange (ETDEWEB)

    Steiner, Myles A [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Geisz, John F [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Kuciauskas, Darius [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Dippo, Patricia C [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Jain, Nikhil [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Sayed, Islam E. M. [North Carolina State University; Colter, Peter C. [North Carolina State University

    2017-06-02

    The use of InGaAsP/InGaP quantum well structures is a promising approach for subcells in next generation multi-junction devices due to their tunable bandgap (1.50-1.80 eV) and for being aluminum-free. Despite these potentials, the accumulation of stress during the growth of these structures and high background doping in the quantum well region have previously limited the maximum number of quantum wells and barriers that can be included in the intrinsic region and the sub-bandgap external quantum efficiency to less than 30.0%. In this paper, we report on the use of in-situ curvature monitoring by multi-beam optical stress (MOS) sensor measurements during the growth of this quantum well structure to monitor the stress evolution in these thin films. A series of In0.32Ga0.68AsP/In0.49Ga0.51P quantum wells with various arsine to phosphine ratios have been analyzed by in-situ curvature monitoring and X-ray diffraction (XRD) to obtain nearly strain-free lattice matched structures. Sharp interfaces, as indicated by the XRD fringes, have been achieved by using triethyl-gallium and trimethyl-gallium as gallium precursors in InGaAsP and InGaP, respectively, with constant flows of trimethyl-indium and phosphine through the entire quantum well structure. The effect of the substrate miscut on quantum well growth was compared and analyzed using XRD, photoluminescence and time resolved photoluminescence. A 100 period quantum well device was successfully grown with minimal stress and approximately flat in-situ curvature.

  15. In-situ observation of zinc electrodeposition on iron single crystal using synchrotron radiation x-ray diffraction

    CERN Document Server

    Kurosaki, M; Kawasaki, K

    2002-01-01

    Continuous in-situ observations of changes in crystal orientation during zinc electrodeposition were performed using novel electrolysis cell that secure uniform current distribution through thin electrolyte layer. It has been clarified that electrodeposition can be separated into the two regions. First one is epitaxial deposition region in which orientations of deposited zinc and substrate keep following relations; Fe(100)//Zn(10 centre dot 1) Fe(110)//Zn(00 centre dot 2), Fe(111)//Zn(00 centre dot 2). This region continued until the thickness of the deposit became about 0.5 mu m. Second one is bulk deposition region, in which the overpotential settled by electrolysis conditions determines the crystal orientation. Low overpotential leads to promoting Zn(00 centre dot 2) deposition, and higher overpotential Zn(10 centre dot 1) and Zn(11 centre dot 0). Influences of the current density changes on the crystal orientation were also clarified. The use of an adsorbing organic additive influences both on the epitaxi...

  16. The application of in-situ 3D X-ray diffraction in annealing experiments: First interpretation of substructure development in deformed NaCl

    DEFF Research Database (Denmark)

    Borthwick, Verity; Schmidt, Søren; Piazolo, Sandra;

    2012-01-01

    In-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to nondestructively document and subsequently analyse the development of substructures during heating, without the influence...... of surface effects. A sample of deformed single crystal halite was heated to between 260-400 °. Before and after heating a volume of 500 by 500 by 300 μm was mapped using a planar beam, which was translated over the sample volume at intervals of 5-10 μm in the vertical dimension. In the following we present...... partially reconstructed orientation maps over one layer before and after heating for 240min at 260 °. Additional small syn-heating "maps" over a constrained sample rotation of 12-30°. The purpose of this was to illuminate a few reflections from 1 or 2 subgrains and follow their evolution during heating...

  17. In-situ X-ray diffraction studies of time and thickness dependence of crystallization of amorphous TiO{sub 2} thin films and stress evolution

    Energy Technology Data Exchange (ETDEWEB)

    Kuzel, R., E-mail: kuzel@karlov.mff.cuni.c [Department of Condensed Matter Physics, Faculty of Mathematics and Physics, Charles University in Prague, 121 16 Praha 2 (Czech Republic); Nichtova, L.; Matej, Z. [Department of Condensed Matter Physics, Faculty of Mathematics and Physics, Charles University in Prague, 121 16 Praha 2 (Czech Republic); Musil, J. [Department of Physics, Faculty of Applied Sciences, University of West Bohemia in Pilsen, Pilsen (Czech Republic)

    2010-12-30

    Remarkable properties of titanium dioxide films such as hydrophilicity or photocatalytic activity depend largely on their phase composition, microstructure and in particular on the crystallinity. By in-situ X-ray diffraction studies of isochronal and isothermal annealing of amorphous films with different thickness at different temperatures it was found that the crystallization process can be quite well described by the Johnson-Mehl-Avrami-Kolmogorov formula modified by the introduction of crystallization onset. This and other parameters of the formula strongly depend on the film thickness. For thickness below about 500 nm the crystallization is very slow. Simultaneously, the appearance and increase of tensile stresses with the annealing time were observed and these stresses were confirmed by detailed studies by both total pattern fitting and sin{sup 2{psi}} method on post-annealed samples. The stresses rapidly increase with decreasing thickness of the films. It seems that there is a strong correlation between the stresses and crystallization onset and/or crystallization rate. Tensile stresses that are generated during crystallization further inhibit crystallization and cause significant thickness dependence of the crystallization. The temperature and time dependence of microstructure of crystallized amorphous films differ significantly from those obtained for as-deposited nanocrystalline films or nanocrystalline powders. During annealing, quite large crystallites are formed quickly with the preferred orientation (001) that is suppressed with the proceeding time.

  18. Advanced Micromechanical Model for Transformation-Induced Plasticity Steels with Application of In-Situ High-Energy X-Ray Diffraction Method

    Science.gov (United States)

    Choi, K. S.; Liu, W. N.; Sun, X.; Khaleel, M. A.; Ren, Y.; Wang, Y. D.

    2008-12-01

    Compared to other advanced high-strength steels, transformation-induced plasticity (TRIP) steels exhibit better ductility at a given strength level and can be used to produce complicated automotive parts. This enhanced formability comes from the transformation of retained austenite to martensite during plastic deformation. In this study, as a first step in predicting optimum processing parameters in TRIP steel productions, a micromechanical finite element model is developed based on the actual microstructure of a TRIP 800 steel. The method uses a microstructure-based representative volume element (RVE) to capture the complex deformation behavior of TRIP steels. The mechanical properties of the constituent phases of the TRIP 800 steel and the fitting parameters describing the martensite transformation kinetics are determined using the synchrotron-based in-situ high-energy X-ray diffraction (HEXRD) experiments performed under a uniaxial tensile deformation. The experimental results suggest that the HEXRD technique provides a powerful tool for characterizing the phase transformation behavior and the microstress developed due to the phase-to-phase interaction of TRIP steels during deformation. The computational results suggest that the response of the RVE well represents the overall macroscopic behavior of the TRIP 800 steel under deformation. The methodology described in this study may be extended for studying the effects of the various processing parameters on the macroscopic behaviors of TRIP steels.

  19. In-situ energy dispersive x-ray diffraction study of the growth of CuO nanowires by annealing method

    Energy Technology Data Exchange (ETDEWEB)

    Srivastava, Himanshu; Ganguli, Tapas; Deb, S. K. [Indus Synchrotrons Utilization Division, Raja Ramanna Centre for Advanced technology, Indore-452013 (India); Sant, Tushar; Poswal, H. K.; Sharma, Surinder M. [High Pressure and Synchrotron Radiation Physics Division, Bhabha Atomic Research Centre, Mumbai (India)

    2013-10-14

    The in-situ growth of CuO nanowires was studied by Energy Dispersive X-ray Diffraction (EDXRD) to observe the mechanism of growth. The study was carried out for comparison at two temperatures—at 500 °C, the optimum temperature of the nanowires growth, and at 300 °C just below the temperature range of the growth. The in situ observation revealed the successive oxidation of Cu foil to Cu{sub 2}O layer and finally to CuO layer. Further analysis showed the presence of a compressive stress in CuO layer due to interface at CuO and Cu{sub 2}O layers. The compressive stress was found to increase with the growth of the nanowires at 500 °C while it relaxed with the growth of CuO layer at 300 °C. The present results do not support the existing model of stress relaxation induced growth of nanowires. Based on the detailed Transmission Electron Microscope, Scanning Electron Microscope, and EDXRD results, a microstructure based growth model has been suggested.

  20. In-situ high-pressure X-ray diffraction on the Zn{sub 6}Sc 1/1 periodic cubic approximant to a quasicrystal

    Energy Technology Data Exchange (ETDEWEB)

    Yamada, Tsunetomo; Boissieu, Marc de [Tokyo University of Science, Noda (Japan). Dept. of Materials Science and Technology; Grenoble-INP, CNRS, UJF, St Martin d' Heres (France). Sciences et Ingeenierie des Materiaux et Procees; Garbarino, Gaston [European Synchrotron Radiation Facility (ESRF), Grenoble (France); Takakura, Hiroyuki [Hokkaido Univ., Sapporo (Japan). Div. of Applied Physics; Pay Gomez, Cesar [Uppsala Univ. (Sweden). Dept. of Chemistry; Tamura, Ryuji [Tokyo University of Science, Noda (Japan). Dept. of Materials Science and Technology

    2014-04-01

    The Zn{sub 6}Sc 1/1 cubic approximant to a quasicrystal has been studied in-situ at high pressures by single-crystal X-ray diffraction. This phase can be described as a bcc packing of Tsai-type icosahedral clusters whose center is occupied by a disordered Zn{sub 4} tetrahedron. At ambient pressure the Zn{sub 6}Sc undergoes a structural phase transition at 159 K to a monoclinic superstructure in which the Zn{sub 4} tetrahedra are orientationally ordered along the direction of the high-temperature bcc phase. In the pressure range up to 35 GPa, two new superstructures have been observed. The second phase corresponds to a four-fold pseudo cubic superstructure, i.e. a very large unit cell with a lattice parameter of about 5.5 nm. The resulting pressure-temperature phase diagram is different from that of Cd{sub 6}Yb, which was reported by Watanuki et al. (2006). (orig.)

  1. X-Ray Diffraction Analysis Program

    Science.gov (United States)

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

    1986-01-01

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

  2. Single Particle X-ray Diffractive Imaging

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-01

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

  3. Crystallization kinetics of Fe-B based amorphous alloys studied in-situ using X-rays diffraction and differential scanning calorimetry

    Directory of Open Access Journals (Sweden)

    Santos D.R. dos

    2001-01-01

    Full Text Available The crystallization processes for the amorphous metallic alloys Fe74B17Si2Ni4Mo3 and Fe86B6Zr7Cu1 (at. % were investigated using X-rays diffraction measurements performed in-situ during Joule-heating, with simultaneous monitoring of the electrical resistance. We determined the main structural transitions and crystalline phases formed during heating, and correlated these results to the observed resistance variations. As the annealing current is increased, the resistance shows an initial decrease due to stress relaxation, followed by a drop to a minimum value due to massive nucleation and growth of alpha-Fe nanocrystals. Further annealing causes the formation of small fractions of Fe-B, B2Zr or ZrO2, while the resistance increases due to temperature enhancement. In situ XRD measurements allowed the identification of metastable phases, as the gamma-Fe phase which occurs at high temperatures. The exothermal peaks observed in the differential scanning calorimetry (DSC for each alloy corroborate the results. We also have performed DSC measurements with several heating rates, which allowed the determination of the Avrami exponent and crystallization activation energy for each alloy. The obtained activation energies (362 and 301 kJ/mol for Fe-B-Zr-Cu; 323 kJ/mol for Fe-B-Si-Ni-Mo are comparable to reported values for amorphous iron alloys, while the Avrami exponent values (n = 1.0 or n = 1.2 are consistent with diffusion controlled crystallization processes with nucleation rates close to zero.

  4. The Dynamical Theory of X Ray Diffraction

    Science.gov (United States)

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

    1974-01-01

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

  5. [X-ray diffraction spectrum of heroin].

    Science.gov (United States)

    Hu, X; Kan, J; Yuan, B

    1999-06-01

    In this paper, practical measured X-ray diffraction spectra of heroin and opium are given and the parameters of each diffraction peak of the heroin are listed. The heroin belongs to orthorhombic crystal system; the basic vectors of the primitive cell are: a = 8.003, b = 14.373, c = 16.092 x 10(-10) m. As compared with the standard spectra of pure heroin and sucrose, the main doped additive checked by us, is sugar affirmatively.

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

    Science.gov (United States)

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

    2016-08-09

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

  7. Application of in-situ nano-scanning calorimetry and X-ray diffraction to characterize Ni–Ti–Hf high-temperature shape memory alloys

    Energy Technology Data Exchange (ETDEWEB)

    McCluskey, Patrick J., E-mail: mccluske@ge.com [GE Global Research, One Research Circle, Niskayuna, NY 12309 (United States); Xiao, Kechao [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States); Gregoire, John M. [Joint Center for Artificial Photosynthesis, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Dale, Darren [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Vlassak, Joost J. [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States)

    2015-03-10

    Combinatorial nanocalorimetry and synchrotron X-ray diffraction were combined to study the martensite–austenite (M–A) phase transformation behavior of Ni–Ti–Hf shape memory alloys. A thin-film library of Ni–Ti–Hf samples with a range of compositions was deposited on a parallel nano-scanning calorimeter device using sputter deposition. Crystallization of each amorphous as-deposited sample by local heating at approximately 10{sup 4} K/s produced a nanoscale grain structure of austenite and martensite. Individual samples were then cycled through the M–A transformation, while the transformation enthalpy was measured by nanocalorimetry and the low- and high-temperature phase compositions were determined by X-ray diffraction. The techniques enable correlation of the observed behavior during thermal cycling with the thermodynamic and structural properties of the samples.

  8. 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.

  9. The behavior of single-crystal silicon to dynamic loading using in-situ X-ray diffraction and phase contrast imaging

    Science.gov (United States)

    Lee, Hae Ja; Xing, Zhou; Galtier, Eric; Arnold, Brice; Granados, Eduardo; Brown, Shaughnessy B.; Tavella, Franz; McBride, Emma; Fry, Alan; Nagler, Bob; Schropp, Andreas; Seiboth, Frank; Samberg, Dirk; Schroer, Christian; Gleason, Arianna E.; Higginbotham, Andrew

    Hydrostatic and uniaxial compression studies have revealed that crystalline silicon undergoes phase transitions from a cubic diamond structure to a variety of phases including orthorhombic Imma phase, body-centered tetragonal phase, and a hexagonal primitive phase. The dynamic response of silicon at high pressure, however, is not well understood. Phase contrast imaging has proven to be a powerful tool for probing density changes caused by the shock propagation into a material. In order to characterize the elastic and phase transitions, we image shock waves in Si with high spatial resolution using the LCLS X-ray free electron laser and Matter in Extreme Conditions instrument. In this study, the long pulse optical laser with pseudo-flat top shape creates high pressures up to 60 GPa. We measure the crystal structure by observing X-ray diffraction orthogonal to the shock propagation direction over a range of pressures. We describe the capability of simultaneously performing phase contrast imaging and in situ X-ray diffraction during shock loading and discuss the dynamic response of Si in high-pressure phases Use of the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515. The MEC instrument is supported by.

  10. 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.

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

    DEFF Research Database (Denmark)

    2012-01-01

    Source: US2012008736A An X-ray diffraction contrast tomography system (DCT) comprising a laboratory X-ray source (2), a staging device (5) rotating a polycrystalline material sample in the direct path of the X-ray beam, a first X-ray detector (6) detecting the direct X-ray beam being transmitted...... through the crystalline material sample, a second X-ray detector (7) positioned between the staging device and the first X-ray detector for detecting diffracted X-ray beams, and a processing device (15) for analysing detected values. The crystallographic grain orientation of the individual grain...

  12. In-Situ Chemical Dynamics and Phase Mapping Under Steep Thermal Gradients Using Time-Resolved and Spatially Resolved X-Ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wong, J.; Larson, E.M.; Holt, J.B.; Ressler, T.; Elmer, J.W.

    1999-09-17

    Time-resolved and spatially-resolved diffraction techniques have been developed recently to perform materials dynamics study in-situ extending into the time and spatial domain in high temperature processes. The applications of these methods to investigate the chemical dynamics of solid combustion reactions and to map phases and their transformation in fusion welds are exemplified in this paper.

  13. Building X-ray Diffraction Calibration Software

    Energy Technology Data Exchange (ETDEWEB)

    Lande, Joshua; /Marlboro Coll.

    2007-10-31

    X-ray diffraction is a technique used to analyze the structure of crystals. It records the interference pattern created when x-rays travel through a crystal. Three dimensional structure can be inferred from these two dimensional diffraction patterns. Before the patterns can be analyzed, diffraction data must be precisely calibrated. Calibration is used to determine the experimental parameters of the particular experiment. This is done by fitting the experimental parameters to the diffraction pattern of a well understood crystal. Fit2D is a software package commonly used to do this calibration but it leaves much to be desired. In particular, it does not give very much control over the calibration of the data, requires a significant amount of manual input, does not allow for the calibration of highly tilted geometries, does not properly explain the assumptions that it is making, and cannot be modified. We build code to do this calibration while at the same time overcoming the limitations of Fit2D. This paper describes the development of the calibration software and the assumptions that are made in doing the calibration.

  14. Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ high energy X-ray diffraction and X-ray absorption near edge spectroscopy

    Science.gov (United States)

    Ma, Tianyuan; Xu, Gui-Liang; Zeng, Xiaoqiao; Li, Yan; Ren, Yang; Sun, Chengjun; Heald, Steve M.; Jorne, Jacob; Amine, Khalil; Chen, Zonghai

    2017-02-01

    In situ high energy X-ray diffraction (HEXRD) and in situ X-ray absorption near edge spectroscopy (XANES) were carried out to understand the solid state synthesis of NaxMnO2, with particular interest on the synthesis of P2 type Na2/3MnO2. It was found that there were multi intermediate phases formed before NaMnO2 appeared at about 600 °C. And the final product after cooling process is a combination of O‧3 NaMnO2 with P2 Na2/3MnO2. A P2 type Na2/3MnO2 was synthesized at reduced temperature (600 °C). The influence of Na2CO3 impurity on the electrochemical performance of P2 Na2/3MnO2 was thoroughly investigated in our work. It was found that the content of Na2CO3 can be reduced by optimizing Na2CO3/MnCO3 ratio during the solid state reaction or other post treatment such as washing with water. We expected our results could provide a good guide for future development of high performance cathode materials for sodium-ion batteries.

  15. Direct Observation of Phase Transformations in Austenitic Stainless Steel Welds Using In-situ Spatially Resolved and Time-resolved X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Elmer, J.; Wong, J.; Ressler, T.

    1999-09-23

    Spatially resolved x-ray diffraction (SRXRD) and time resolved x-ray diffraction (TRXRD) were used to investigate real time solid state phase transformations and solidification in AISI type 304 stainless steel gas tungsten arc (GTA) welds. These experiments were conducted at Stanford Synchrotron Radiation Laboratory (SSRL) using a high flux beam line. Spatially resolved observations of {gamma} {leftrightarrow} {delta} solid state phase transformations were performed in the heat affected zone (HAZ) of moving welds and time-resolved observations of the solidification sequence were performed in the fusion zone (FZ) of stationary welds after the arc had been terminated. Results of the moving weld experiments showed that the kinetics of the {gamma}{yields}{delta} phase transformation on heating in the HAZ were sufficiently rapid to transform a narrow region surrounding the liquid weld pool to the {delta} ferrite phase. Results of the stationary weld experiments showed, for the first time, that solidification can occur directly to the {delta} ferrite phase, which persisted as a single phase for 0.5s. Upon solidification to {delta}, the {delta} {yields} {gamma} phase transformation followed and completed in 0.2s as the weld cooled further to room temperature.

  16. X-ray diffraction with novel geometry

    Energy Technology Data Exchange (ETDEWEB)

    Prokopiou, Danae [Department of Engineering and Applied Science Cranfield University, Shrivenham Campus, Swindon (United Kingdom); Rogers, Keith, E-mail: k.d.rogers@cranfield.ac.uk [Department of Engineering and Applied Science Cranfield University, Shrivenham Campus, Swindon (United Kingdom); Evans, Paul; Godber, Simon [Imaging Science Group, School of Science and Technology, Nottingham Trent University Clifton Campus, Nottingham (United Kingdom); Shackel, James [Department of Engineering and Applied Science Cranfield University, Shrivenham Campus, Swindon (United Kingdom); Dicken, Anthony [Imaging Science Group, School of Science and Technology, Nottingham Trent University Clifton Campus, Nottingham (United Kingdom)

    2014-01-21

    An innovative geometry for high efficiency harvesting of diffracted X-rays is explored. Further to previous work where planar samples were fixed normal to the primary axis, this work extends focal construct geometry (FCG), to samples randomly oriented with respect to the incident beam. The effect of independent sample rotation around two axes upon the scattering distributions was investigated in analytical, simulation and empirical manners. It was found that, although the profile of Bragg maxima were modified when the sample was rotated, high intensity diffraction data was still acquired. Modelling produced a good match to the empirical data and it was shown that the distortions caused by sample rotation were not severe and predictable even when sample rotations were large. The implications for this are discussed.

  17. Hydration forces between aligned DNA helices undergoing B to A conformational change: In-situ X-ray fiber diffraction studies in a humidity and temperature controlled environment.

    Science.gov (United States)

    Case, Ryan; Schollmeyer, Hauke; Kohl, Phillip; Sirota, Eric B; Pynn, Roger; Ewert, Kai E; Safinya, Cyrus R; Li, Youli

    2017-07-19

    Hydration forces between DNA molecules in the A- and B-Form were studied using a newly developed technique enabling simultaneous in situ control of temperature and relative humidity. X-ray diffraction data were collected from oriented calf-thymus DNA fibers in the relative humidity range of 98%-70%, during which DNA undergoes the B- to A-form transition. Coexistence of both forms was observed over a finite humidity range at the transition. The change in DNA separation in response to variation in humidity, i.e. change of chemical potential, led to the derivation of a force-distance curve with a characteristic exponential decay constant of∼2Å for both A- and B-DNA. While previous osmotic stress measurements had yielded similar force-decay constants, they were limited to B-DNA with a surface separation (wall-to-wall distance) typically>5Å. The current investigation confirms that the hydration force remains dominant even in the dry A-DNA state and at surface separation down to∼1.5Å, within the first hydration shell. It is shown that the observed chemical potential difference between the A and B states could be attributed to the water layer inside the major and minor grooves of the A-DNA double helices, which can partially interpenetrate each other in the tightly packed A phase. The humidity-controlled X-ray diffraction method described here can be employed to perform direct force measurements on a broad range of biological structures such as membranes and filamentous protein networks. Copyright © 2017. Published by Elsevier Inc.

  18. 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.

  19. In-situ X-ray diffraction analysis of the recrystallization process in Cu{sub 2}ZnSnS{sub 4} nanoparticles synthesised by hot-injection

    Energy Technology Data Exchange (ETDEWEB)

    Brandl, Marco [Chair for Crystallography and Structural Physics, Friedrich-Alexander-Universität Erlangen-Nürnberg, Staudtstr. 3, 91058 Erlangen (Germany); Ahmad, Rameez; Distaso, Monica [Institute of Particle Technology, Friedrich-Alexander-Universität Erlangen-Nürnberg, Cauerstr. 4, 91058 Erlangen (Germany); Azimi, Hamed; Hou, Yi [Institute of Materials for Electronics and Energy Technology (I-MEET), Friedrich-Alexander-Universität Erlangen-Nürnberg, Martensstr. 7, 91058 Erlangen (Germany); Peukert, Wolfgang [Institute of Particle Technology, Friedrich-Alexander-Universität Erlangen-Nürnberg, Cauerstr. 4, 91058 Erlangen (Germany); Brabec, Christoph J. [Institute of Materials for Electronics and Energy Technology (I-MEET), Friedrich-Alexander-Universität Erlangen-Nürnberg, Martensstr. 7, 91058 Erlangen (Germany); Hock, Rainer [Chair for Crystallography and Structural Physics, Friedrich-Alexander-Universität Erlangen-Nürnberg, Staudtstr. 3, 91058 Erlangen (Germany)

    2015-05-01

    Kesterite Cu{sub 2}ZnSnS{sub 4} (CZTS) is a promising material for thin film solar cell applications. The biggest advantages of this compound lie in the abundance and non-toxicity of the contained elements. Low temperature hot injection synthesis can provide an economic way to produce CZTS nanoparticles for application in solution processed solar cells. Powder X-ray diffraction (PXRD) measurements on the as-synthesised particles suggest that the crystal structure is cubic and can be best described as sphalerite-like. This means that the cations in the CZTS are statistically distributed on the cation sites of the crystal lattice rather than well-ordered like in the tetragonal kesterite structure. An in-situ PXRD measurement while annealing the particles up to 550 °C revealed a recrystallization process that transforms the structure from cubic to tetragonal meaning an ordering of the cations. - Highlights: • Cu{sub 2}ZnSnS{sub 4} (CZTS) nanoparticles crystallise in an apparent cubic structure. • In-situ X-ray diffraction reveals a phase transition to the tetragonal crystal system. • Post annealing measurements show a well ordered tetragonal CZTS.

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

    Science.gov (United States)

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

    2016-07-08

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

  1. Surface mechanical property and residual stress of peened nickel-aluminum bronze determined by in-situ X-ray diffraction

    Science.gov (United States)

    Wang, Chengxi; Jiang, Chuanhai; Zhao, Yuantao; Chen, Ming; Ji, Vincent

    2017-10-01

    As one of the most important surface strengthening method, shot peening is widely used to improve the fatigue and stress corrosion crack resistance of components by introducing the refined microstructure and compressive residual stress in the surface layer. However, the mechanical properties of this thin layer are different from the base metal and are difficult to be characterized by conventional techniques. In this work, a micro uniaxial tensile tester equipped with in-situ X-ray stress analyzer was employed to make it achievable on a nickel-aluminum bronze with shot peening treatment. According to the equivalent stress-strain relationship based on Von Mises stress criterion, the Young's modulus and yield strength of the peened layer were calculated. The results showed that the Young's modulus was the same as the bulk material, and the yield strength corresponding to the permanent plastic strain of 0.2% was increased by 21% after SP. But the fractographic analysis showed that the fracture feature of the surface layer was likely to transform from the dimple to the cleavage, indicating the improved strength might be attained at the expense of ductility. The monotonic and cyclic loading were also performed via the same combined set-up. In addition, the specific relaxation behavior of compressive residual stress was quantified by linear logarithm relationship between residual stress and cycle numbers. It was found that the compressive residual stress mainly relaxed in the first few cycles, and then reached steady state with further cycles. The relaxation rate and the stable value were chiefly depended on the stress amplitude and number of cycles. The retained residual stress kept in compressive under all given applied stress levels, suggesting that the shot peening could introduce a more stable surface layer of compressive residual stress other than the elevated strength of nickel-aluminum bronze alloy.

  2. X-Ray-Diffraction Tests Of Irradiated Electronic Devices: II

    Science.gov (United States)

    Shaw, David C.; Lowry, Lynn E.; Barnes, Charles E.

    1993-01-01

    Report describes research on use of x-ray diffraction to measure stresses in metal conductors of complementary metal oxide/semiconductor (CMOS) integrated circuits exposed to ionizing radiation. Expanding upon report summarized in "X-Ray-Diffraction Tests Of Irradiated Electronic Devices: I" (NPO-18803), presenting data further suggesting relationship between electrical performances of circuits and stresses and strains in metal conductors.

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

    DEFF Research Database (Denmark)

    Abdolvand, Hamidreza; Majkut, Marta; Oddershede, Jette

    2015-01-01

    ) microscopy. In-situ uniaxial straining was carried out at seven steps up to 2.7% in the macroscopic direction that favors twin formation, while center-of-mass position, crystallographic orientation, elastic strain, stress, and relative volume of each grain were measured. This information was used......High anisotropy in the elastic and plastic properties of hexagonal close-packed (hcp) structured metals not only results in drastic stress variation across grain boundaries, but also heterogeneous distributions within grains. Understanding the mechanism of load sharing between different grains...... becomes more complicated when deformation twinning plays a significant role in accommodating an externally applied load. In this paper, a comprehensive study of stress development in a coarse grained strongly textured hcp polycrystal Zircaloy-2, is given using three-dimensional X-ray diffraction (3DXRD...

  4. In-situ X-ray diffraction studies of the phase transformations and structural states of B2, R and B19′ phases in Ti{sub 49.5}Ni{sub 50.5} alloy

    Energy Technology Data Exchange (ETDEWEB)

    Ostapenko, Marina G., E-mail: artifakt@ispms.tsc.ru [Institute of Strength Physics and Materials Science SB RAS, Tomsk, 634055 (Russian Federation); National Research Tomsk Polytechnic University, Tomsk, 634050 (Russian Federation); Meisner, Ludmila L., E-mail: llm@ispms.tsc.ru [Institute of Strength Physics and Materials Science SB RAS, Tomsk, 634055 (Russian Federation); National Research Tomsk State University, Tomsk, 634050 (Russian Federation); Lotkov, Aleksandr I., E-mail: lotkov@ispms.tsc.ru; Gudimova, Ekaterina Y., E-mail: egu@ispms.tsc.ru [Institute of Strength Physics and Materials Science SB RAS, Tomsk, 634055 (Russian Federation); Zakharova, Margarita A., E-mail: tibiboreth@gmail.com [National Research Tomsk Polytechnic University, Tomsk, 634050 (Russian Federation)

    2015-10-27

    The martensitic transformation, Debye–Waller factor, mean-square atomic displacements and the coefficient of thermal expansion on cooling of the Ti{sub 49.5}Ni{sub 50.5} shape memory alloy were examined using in-situ X-ray diffraction. It was revealed B2→R (T{sub R} ≡ T = 273 ± 10 K) along with B2→B19’ (M{sub s} ≡ T = 273 ± 10 K) transitions occur. It was found that Debye–Waller factor and mean-square displacement of B2 phase undergo significant increase as functions of temperature when phase transition B2→R and B2→B19’ take place. The analysis of the thermal expansion coefficient of the B2 phase indicates that the value of a increases almost linearly while cooling.

  5. In-situ X-ray diffraction study on MlNi3.75 Co0.75 Mn0.3 Al0.2 during electrochemical hydriding-dehydriding process

    Institute of Scientific and Technical Information of China (English)

    袁志庆; 吕光烈; 顾建明; 屠小燕; 王新喜

    2004-01-01

    Phase transformations and lattice expansions of M1Ni3.75 Co0.75 Mn0.3 Al0.2 during the electrochemical hydriding-dehydriding process were investigated using in-situ X-ray diffraction. An intermediate hydride γ phase between the hydrogen solid solution a phase and fully hydrided β phase can be observed during the cycling. The formation of γ phase is related to the diffusion of hydrogen in the crystal grains. The lower the charge rate is, the higher the content of γ phase is. The phase transformations during the hydriding-dehydriding process can be described as α(→←)α+γ+β(→←)β(→←)γ+α(→←)α. The lattice expansion from a toβ is discrete, while that from γ to β is continuous. The formation of γ phase can reduce the discrete lattice expansion from a toβ by 30 %.

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

    OpenAIRE

    Lane, D W.; Nyombi, A.; Shackel, J.

    2014-01-01

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

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

    DEFF Research Database (Denmark)

    2012-01-01

    Source: US2012008736A An X-ray diffraction contrast tomography system (DCT) comprising a laboratory X-ray source (2), a staging device (5) rotating a polycrystalline material sample in the direct path of the X-ray beam, a first X-ray detector (6) detecting the direct X-ray beam being transmitted ...... in the polycrystalline sample is determined based on the two-dimensional position of extinction spots and the associated angular position of the sample for a set of extinction spots pertaining to the individual grain....

  8. 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 developed and tested on micro-crystals of lysozyme and insulin. Different protein crystal forms were identified by comparing experimental powder diffraction patternswith patterns calculated from PDB coordinates. The key factor to bring the calculated patterns in agreement with the observed patterns...

  9. 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...

  10. 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.

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  12. An X-ray diffraction study of titanium oxidation

    Science.gov (United States)

    Wiedemann, K. E.; Unnam, J.

    1984-01-01

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

  13. 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....

  14. 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....

  15. 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....

  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 pro...

  17. 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...

  18. X-ray diffraction comparator - new possibilities.

    Science.gov (United States)

    Brytov, I A; Dmitriev, G D; Ivanov, V N; Klevtsov, S A

    1997-01-01

    We have studied the possibilities to determine precisely the lattice constants of quartz using an X-ray diffractometer-comparator. This device has double-crystal optical scheme, continuously swinging crystal-monochromator and an original angular reference system. The measurement strategy uses the difference in angular positions of two different Bragg planes relative the third one. On assumption that the wavelength of the used radiation is known with accuracy of ± 1.2,ppm, the accuracy of determined lattice constants is estimated in ± 5×10-5Å. The described measurement strategy proves to be efficient in measuring the changes of the lattice constants with temperature and in precision testing of a quartz single-crystal homogeneity. We discuss also the features of other instruments for the automatic sorting of quartz blanks in groups by the cut angle, which use the same monochromator pendulum system.

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

    Directory of Open Access Journals (Sweden)

    G. Cheung

    2016-08-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

  1. Enhancement of coherent X-ray diffraction from nanocrystals by introduction of X-ray optics.

    Science.gov (United States)

    Robinson, Ian; Pfeiffer, Franz; Vartanyants, Ivan; Sun, Yugang; Xia, Younan

    2003-09-22

    Coherent X-ray Diffraction is applied to investigate the structure of individual nanocrystalline silver particles in the 100nm size range. In order to enhance the available signal, Kirkpatrick-Baez focusing optics have been introduced in the 34-ID-C beamline at APS. Concerns about the preservation of coherence under these circumstances are addressed through experiment and by calculations.

  2. 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.

  3. Glancing angle x-ray diffraction : A different approach

    NARCIS (Netherlands)

    Brussel, B.A. van; Hosson, J.Th.M. De

    1994-01-01

    This letter describes a novel technique of diffracted beam glancing angle x-ray diffraction by which depth profiles of stresses and transformed phases in structures like implanted materials can be determined. An important feature is that this method may be applied successfully in a standard powder d

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-26

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

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

    Science.gov (United States)

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

    2016-09-01

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

  6. Coherent X-ray diffraction studies of mesoscopic materials

    Energy Technology Data Exchange (ETDEWEB)

    Shabalin, Anatoly

    2015-12-15

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

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

    Science.gov (United States)

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

    1999-01-01

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

  8. In-situ investigations of magnetron sputtering processes with laboratory X-ray equipment

    Energy Technology Data Exchange (ETDEWEB)

    Ringpfeil, Clemens [Fachbereich C-Physik, Bergische Universitaet Wuppertal, Gaussstr. 20, D-42097 Wuppertal (Germany)]. E-mail: Clemens@physik.uni-wuppertal.de; Luetzenkirchen-Hecht, Dirk [Fachbereich C-Physik, Bergische Universitaet Wuppertal, Gaussstr. 20, D-42097 Wuppertal (Germany); Frahm, Ronald [Fachbereich C-Physik, Bergische Universitaet Wuppertal, Gaussstr. 20, D-42097 Wuppertal (Germany)

    2007-05-23

    An Fe-Al duplex film was prepared on a Si(111)-wafer by sputter deposition in a vacuum chamber with two integrated small magnetron sources. The chamber allows the in-situ investigation of such sputtering processes using grazing incidence X-ray reflectivity, X-ray scattering measurements and X-ray diffraction. We will present details of the new cell and present the first results obtained using reflectivity measurements of the Fe-Al thin films. Here we will focus on the detailed evaluation of the specular reflectivity data of the iron films only, which clearly indicates the presence of an iron oxide, the density and roughness of which were determined and their changes with the film thickness were discussed in the framework of thin film growth models.

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

    Institute of Scientific and Technical Information of China (English)

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

    2004-01-01

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

  10. X-Ray-Diffraction Tests Of Irradiated Electronic Devices: I

    Science.gov (United States)

    Shaw, David C.; Lowry, Lynn E.; Barnes, Charles E.

    1993-01-01

    X-ray-diffraction tests performed on aluminum conductors in commercial HI1-507A complementary metal oxide/semiconductor (CMOS) integrated-circuit analog multiplexers, both before and after circuits exposed to ionizing radiation from Co(60) source, and after postirradiation annealing at ambient and elevated temperatures. Tests in addition to electrical tests performed to determine effects of irradiation and of postirradiation annealing on electrical operating characteristics of circuits. Investigators sought to determine whether relationship between effects of irradiation on devices and physical stresses within devices. X-ray diffraction potentially useful for nondestructive measurement of stresses.

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

    Science.gov (United States)

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

    1997-07-01

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

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

    Science.gov (United States)

    Authier, André

    2012-01-01

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

  13. Dynamic X-ray diffraction sampling for protein crystal positioning.

    Science.gov (United States)

    Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

    2017-01-01

    A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by

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

    Science.gov (United States)

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

    2015-11-01

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

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

    Science.gov (United States)

    Johnson, Neil E.

    2001-01-01

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

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

    Science.gov (United States)

    Johnson, Neil E.

    2001-01-01

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

  17. 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...

  18. A Practical Method of Simulating X-Ray Diffraction

    Science.gov (United States)

    Brisse, F.; Sundararajan, P. R.

    1975-01-01

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

  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. Computer Simulation and X-ray Diffraction of Nanocrystals

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

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

  2. A Practical Method of Simulating X-Ray Diffraction

    Science.gov (United States)

    Brisse, F.; Sundararajan, P. R.

    1975-01-01

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

  3. Computing Composition/Depth Profiles From X-Ray Diffraction

    Science.gov (United States)

    Wiedemann, K. E.; Unnam, J.

    1986-01-01

    Diffraction-intensity bands deconvolved relatively quickly. TIBAC constructs composition/depth profiles from X-ray diffraction-intensity bands. Intensity band extremely sensitive to shape of composition/depth profile. TIBAC incorporates straightforward transformation of intensity band that retains accuracy of earlier simulation models, but is several orders of magnitude faster in total computational time. TIBAC written in FORTRAN 77 for batch execution.

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

    DEFF Research Database (Denmark)

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

    1995-01-01

    The use of hard X-rays (60-300 keV) for diffraction studies of disordered materials has several advantages: higher resolution in direct space, smaller correction terms, removal of truncation effects, the possibility for operating in extreme environments and for direct comparison between X-ray.......3(3)degrees with a rms value of 4.2(3)degrees. For the Si-O-Si bond angle, several types of distribution V(alpha) = V-1(alpha) sin(alpha) were investigated. Best fits were obtained for rather broad distributions with V having its maximum at 147 degrees and V-1 at 180 degrees....

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-08-15

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

  6. 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.

  7. 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.

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

    CERN Document Server

    McBride, L

    2000-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    刘景

    2016-01-01

    This article summarizes the developments of experimental techniques for high pressure x-ray diffraction (XRD) in diamond anvil cells (DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, time-resolved diffraction with dynamic DAC and development of modulated heating techniques are briefl y introduced. The current status of the high pressure beamline at BSRF (Beijing Synchrotron Radiation Facility) and some results are also presented.

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

    CERN Document Server

    Ito, M

    2002-01-01

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

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

    Science.gov (United States)

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

    2016-08-01

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

  12. 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.

  13. Spatiotemporal Response of Crystals in X-ray Bragg Diffraction

    CERN Document Server

    Shvyd'ko, Yuri

    2012-01-01

    The spatiotemporal response of crystals in x-ray Bragg diffraction resulting from excitation by an ultra-short, laterally confined x-ray pulse is studied theoretically. The theory presents an extension of the analysis in symmetric reflection geometry [1] to the generic case, which includes Bragg diffraction both in reflection (Bragg) and transmission (Laue) asymmetric scattering geometries. The spatiotemporal response is presented as a product of a crystal-intrinsic plane wave spatiotemporal response function and an envelope function defined by the crystal-independent transverse profile of the incident beam and the scattering geometry. The diffracted wavefields exhibit amplitude modulation perpendicular to the propagation direction due to both angular dispersion and the dispersion due to Bragg's law. The characteristic measure of the spatiotemporal response is expressed in terms of a few parameters: the extinction length, crystal thickness, Bragg angle, asymmetry angle, and the speed of light. Applications to...

  14. Incoherent Diffractive Imaging via Intensity Correlations of Hard X Rays

    Science.gov (United States)

    Classen, Anton; Ayyer, Kartik; Chapman, Henry N.; Röhlsberger, Ralf; von Zanthier, Joachim

    2017-08-01

    Established x-ray diffraction methods allow for high-resolution structure determination of crystals, crystallized protein structures, or even single molecules. While these techniques rely on coherent scattering, incoherent processes like fluorescence emission—often the predominant scattering mechanism—are generally considered detrimental for imaging applications. Here, we show that intensity correlations of incoherently scattered x-ray radiation can be used to image the full 3D arrangement of the scattering atoms with significantly higher resolution compared to conventional coherent diffraction imaging and crystallography, including additional three-dimensional information in Fourier space for a single sample orientation. We present a number of properties of incoherent diffractive imaging that are conceptually superior to those of coherent methods.

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

    Science.gov (United States)

    Liao, Keliang; Hong, Youli; Sheng, Weifan

    2014-10-01

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

  16. Locating and Visualizing Crystals for X-Ray Diffraction Experiments.

    Science.gov (United States)

    Becker, Michael; Kissick, David J; Ogata, Craig M

    2017-01-01

    Macromolecular crystallography has advanced from using macroscopic crystals, which might be >1 mm on a side, to crystals that are essentially invisible to the naked eye, or even under a standard laboratory microscope. As crystallography requires recognizing crystals when they are produced, and then placing them in an X-ray, electron, or neutron beam, this provides challenges, particularly in the case of advanced X-ray sources, where beams have very small cross sections and crystals may be vanishingly small. Methods for visualizing crystals are reviewed here, and examples of different types of cases are presented, including: standard crystals, crystals grown in mesophase, in situ crystallography, and crystals grown for X-ray Free Electron Laser or Micro Electron Diffraction experiments. As most techniques have limitations, it is desirable to have a range of complementary techniques available to identify and locate crystals. Ideally, a given technique should not cause sample damage, but sometimes it is necessary to use techniques where damage can only be minimized. For extreme circumstances, the act of probing location may be coincident with collecting X-ray diffraction data. Future challenges and directions are also discussed.

  17. X-ray diffraction and the beginnings of X-ray crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Juretschke, H.J. [Polytechnic Univ., Brooklyn, NY (United States)

    1995-12-31

    A retelling of the discovery of X-ray diffraction in Munich in 1912, and an overview of its rapidity spreading applications to crystal structure determination. The early work by Laue`s group and by approaches and different instrumentation, soon set two basic patterns of investigations in this field, with Ewald offering a grand theoretical framework for encompassing both. Some of the successes, problems, and interplays of these trends are reviewed, also as reflected in the stimulation and response by other early participants in structural research, as well as by the interruptions caused by the first World War.

  18. New-corrected functions of X-ray powder diffraction

    Institute of Scientific and Technical Information of China (English)

    ZHANG QingLi; LIU WenPeng; DING LiHua; JIANG HaiHe; YIN ShaoTang

    2009-01-01

    X-ray powder diffraction is an indispensable technique to study material structure,phase transition and so on.It is necessary for high quality diffraction data to get high-precision diffraction angle.This work proposed four corrected functions of X-ray powder diffraction angle.Two methods,linearization method and modified Levenberg-Marquardt iteration method,are given to solve the function parameters,and the modified Levenberg-Marquardt method has fast convergent speed and stable solution.Two methods can give closed parameters,including those of Lu,Liu,and Chu functions and polynomial.New-corrected functions were used to fit the diffraction angle error of the tetragonal rutile polycrystalline TiO_2 mixed with Gd_(0.45)Y_(2.55)Sc_2Ga_3O_(12) as a standard sample,and the computation result indicates that these functions can characterize the diffraction error very well.In some cases,the new-corrected functions can describe the diffraction angle error better than the reported corrected functions.At the same time,the lattice parameter of Gd_(0.45)Y_(2.55)Sc_2Ga_3O_(12) was computed with two methods.When the corrected function parameters and lattice parameters were solved by the least square method,the interaction of the function parameters and lattice parameters would result in great error.However,when the X-ray diffraction angles were corrected by corrected functions using a standard sample,the authentic lattice parameters can be obtained by the least square fitting.

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

    Science.gov (United States)

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

    2016-03-14

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

  20. 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)....

  1. Structured illumination for tomographic X-ray diffraction imaging.

    Science.gov (United States)

    Greenberg, Joel A; Hassan, Mehadi; Krishnamurthy, Kalyani; Brady, David

    2014-02-21

    Tomographic imaging of the molecular structure of an object is important for a variety of applications, ranging from medical and industrial radiography to security screening. X-ray diffraction imaging is the preeminent technique for performing molecular analysis of large volumes. Here we propose and demonstrate a new measurement architecture to improve the source and detector efficiency for diffraction imaging. In comparison with previous techniques, our approach reduces the required overall scan time by 1-2 orders of magnitude, which makes possible real-time scanning of a broad range of materials over a large volume using a table-top setup. This method, which relies on structuring spatially the illumination incident on an object moving relative to the X-ray source, is compatible with existing systems and has the potential to significantly enhance performance in an array of areas, such as medical diagnostic imaging and explosives detection.

  2. 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

  3. MAX200x: In-situ X-ray Measurements at High Pressure and High Temperatures.

    Science.gov (United States)

    Lathe, C.; Mueller, H. J.; Wehber, M.; Lauterjung, J.; Schilling, F. R.

    2009-05-01

    Twenty years ago geoscientists from all over the world launched in-situ X-ray diffraction experiments under extreme pressure and temperature conditions at synchrotron beamlines. One of the first apparatus was installed at HASYLAB, MAX80, a single-stage multi-anvil system. MAX80 allows in-situ diffraction studies in conjunction with the simultaneous measurement of elastic properties up to 12 GPa and 1600 K. This very successful experiment, unique in Europe, is operated by Helmholtz Centre Potsdam and is used by more than twenty groups from different countries every year. Experiments for both, applied and basic research are conducted, ranging from life-sciences, chemistry, physics, over material sciences to geosciences. Today new materials and the use of high brilliant synchrotron sources allow constructing double-stage multi-anvil systems for X-ray diffraction to reach much higher pressures. The newly designed high-flux hard wiggler (HARWI-II) beamline is an ideal X-ray source for this kind of experiments. As only the uppermost few kilometres of the Earth (less than 0.1% of its radius) are accessible for direct observations (e.g. deep drilling), sophisticated techniques are required to observe and to understand the processes in the deep interior of our planet. In-situ studies are an excellent tool to investigate ongoing geodynamic processes within the laboratory. One of the fundamental regions to study geodynamic processes seems to be the so-called transition zone, the boundary between upper and lower Earth's mantle between 410 and 670 km depth. Mineral reactions, phase transitions, as wheel as fluid rock interaction in this area might have the potential to strongly influence and control the dynamic motions within our whole planet. Around 25 GPa and 2 000 K are required to simulate these processes in the laboratory. The new MAX200x will be an excellent tool for these ambitious experiments.

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

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza Cuevas, Ariadna, E-mail: ariadna@mail.or [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba); Perez Gravie, Homero, E-mail: homero.perezgravie@mail.co [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba)

    2011-03-21

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

  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...... from the totally substrate-reflected beam ( two-beam approximation) and refraction effects are also included in the program, together with the geometrical intensity corrections associated with GIXD measurements. To achieve 'user friendliness' for scientists less familiar with diffraction......, 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. 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

  7. 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.

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

    Science.gov (United States)

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

    2012-01-01

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

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

    Science.gov (United States)

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

    2012-01-01

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

  10. X-ray diffraction of protein crystal grown in a nano-liter scale droplet in a microchannel and evaluation of its applicability.

    Science.gov (United States)

    Maeki, Masatoshi; Yoshizuka, Saori; Yamaguchi, Hiroshi; Kawamoto, Masahide; Yamashita, Kenichi; Nakamura, Hiroyuki; Miyazaki, Masaya; Maeda, Hideaki

    2012-01-01

    We describe the technical aspects of the in-situ X-ray diffraction of a protein crystal prepared by a nanodroplet-based crystallization method. We were able to obtain diffraction patterns from a crystal grown in a capillary without any manipulation. Especially in our experimental approach, the crystals that moved to the nanodroplet interface were fixed strongly enough to carry out X-ray diffraction measurements that could be attributed to the high surface tension of the nanodroplet. The crystal was damaged by an indirect action of the X-rays because our in-situ X-ray diffraction measurement was carried out in the liquid phase without freezing the crystal; however, the obtained several diffraction patterns were of sufficiently fine quality for the crystal structure factors to be generated. We consider the technical examination presented in this paper to represent a seamless coupling of crystallization to X-ray analysis.

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

    Science.gov (United States)

    Jing, Liu

    2016-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Freund, A.K.; Munkholm, A.; Brennan, S. [Stanford Synchrotron Radiation Lab., CA (United States)

    1996-12-31

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

  13. Microbeam x-ray diffraction analysis of dental calculus.

    Science.gov (United States)

    Kani, T; Kani, M; Moriwaki, Y; Doi, Y

    1983-02-01

    The crystalline components of human dental calculus were investigated using microbeam x-ray diffraction analysis. Hydroxyapatite and octacalcium phosphate were most frequently found in that portion having porous and zonal structure. In the portion of the homogeneous illustration showing high calcification, whitlockite is a main component. Brushite was unexpectedly rare, and no calcite was detected in any portion of human dental calculus. The mechanism of the formation of dental calculus being considered in this paper is that octacalcium phosphate or brushite is formed during the initial stage of calcification of dental plaque, and is gradually hydrolyzed and transformed into hydroxyapatite and/or whitlockite.

  14. Ultrafast X-Ray Diffraction of Heterogeneous Solid Hydrogen

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-08-19

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

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

    Indian Academy of Sciences (India)

    Digamber G Porob; T N Guru Row

    2001-10-01

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

  16. 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...... the formation of a regular array of screw dislocations. This satellite reflection first appears at an annealing temperature of 800 degrees C, and increases abruptly up to temperatures of 1000 degrees C. We propose that this transition occurs when there is sufficient mobility for the reorganization of atomic...

  17. Anomalous X-ray Diffraction Studies for Photovoltaic Applications

    Energy Technology Data Exchange (ETDEWEB)

    2011-06-22

    Anomalous X-ray Diffraction (AXRD) has become a useful technique in characterizing bulk and nanomaterials as it provides specific information about the crystal structure of materials. In this project we present the results of AXRD applied to materials for photovoltaic applications: ZnO loaded with Ga and ZnCo{sub 2}O{sub 4} spinel. The X-ray diffraction data collected for various energies were plotted in Origin software. The peaks were fitted using different functions including Pseudo Voigt, Gaussian, and Lorentzian. This fitting provided the integrated intensity data (peaks area values), which when plotted as a function of X-ray energies determined the material structure. For the first analyzed sample, Ga was not incorporated into the ZnO crystal structure. For the ZnCo{sub 2}O{sub 4} spinel Co was found in one or both tetrahedral and octahedral sites. The use of anomalous X-ray diffraction (AXRD) provides element and site specific information for the crystal structure of a material. This technique lets us correlate the structure to the electronic properties of the materials as it allows us to probe precise locations of cations in the spinel structure. What makes it possible is that in AXRD the diffraction pattern is measured at a number of energies near an X-ray absorption edge of an element of interest. The atomic scattering strength of an element varies near its absorption edge and hence the total intensity of the diffraction peak changes by changing the X-ray energy. Thus AXRD provides element specific structural information. This method can be applied to both crystalline and liquid materials. One of the advantages of AXRD in crystallography experiments is its sensitivity to neighboring elements in the periodic tables. This method is also sensitive to specific crystallographic phases and to a specific site in a phase. The main use of AXRD in this study is for transparent conductors (TCs) analysis. TCs are considered to be important materials because of their

  18. Ultrafast molecular processes mapped by femtosecond x-ray diffraction

    Science.gov (United States)

    Elsaesser, Thomas

    2012-02-01

    X-ray diffraction with a femtosecond time resolution allows for mapping photoinduced structural dynamics on the length scale of a chemical bond and in the time domain of atomic and molecular motion. In a pump-probe approach, a femtosecond excitation pulse induces structural changes which are probed by diffracting a femtosecond hard x-ray pulse from the excited sample. The transient angular positions and intensities of diffraction peaks give insight into the momentary atomic or molecular positions and into the distribution of electronic charge density. The simultaneous measurement of changes on different diffraction peaks is essential for determining atom positions and charge density maps with high accuracy. Recent progress in the generation of ultrashort hard x-ray pulses (Cu Kα, wavelength λ=0.154 nm) in laser-driven plasma sources has led to the implementation of the powder diffraction and the rotating crystal method with a time resolution of 100 fs. In this contribution, we report new results from powder diffraction studies of molecular materials. A first series of experiments gives evidence of a so far unknown concerted transfer of electrons and protons in ammonium sulfate [(NH4)2SO4], a centrosymmetric structure. Charge transfer from the sulfate groups results in the sub-100 fs generation of a confined electron channel along the c-axis of the unit cell which is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps display a periodic modulation of the channel's charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A second study addresses atomic rearrangements and charge dislocations in the non-centrosymmetric potassium dihydrogen phosphate [KH2PO4, KDP]. Photoexcitation generates coherent low-frequency motions along the LO and TO phonon coordinates, leaving the average atomic positions unchanged

  19. 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}).

  20. X-ray diffraction study of arsenopyrite at high pressure

    Science.gov (United States)

    Fan, D. W.; Ma, M. N.; Zhou, W. G.; Wei, S. Y.; Chen, Z. Q.; Xie, H. S.

    2011-02-01

    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 0, and K' 0 refined with a third-order Birch-Murnaghan EOS are K 0 = 123(9) GPa, and K' 0 = 5.2(8). Furthermore, we confirm that the linear compressibilities (β) along a, b and c directions of arsenopyrite is elastically isotropic (β a = 6.82 × 10-4, β b = 6.17 × 10-4 and β c = 6.57 × 10-4 GPa-1).

  1. Characterization of Brazilian asphalt using X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cardoso, Edson R.; Pinto, Nivia G.V.; Almeida, Ana P.G.; Braz, Delson; Lopes, Ricardo T. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE). Lab. de Instrumentacao Nuclear], E-mail: ecardoso@lin.ufrj.br; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica], E-mail: cely@uerj.br; Motta, Laura M.G. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE). Lab. de Geotecnia], E-mail: laura@coc.ufrj.br

    2007-07-01

    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 {theta}-2{theta} 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)

  2. X-ray diffraction of III-nitrides

    Energy Technology Data Exchange (ETDEWEB)

    Moram, M A; Vickers, M E [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke St., Cambridge, CB2 3QZ (United Kingdom)], E-mail: mam65@cam.ac.uk

    2009-03-15

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

  3. X-ray diffraction of III-nitrides

    Science.gov (United States)

    Moram, M A; Vickers, M E

    2009-03-01

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

  4. X-ray diffraction study of Be to megabar pressure

    CERN Document Server

    Nakano, K; Kawamura, H

    2002-01-01

    Powder x-ray diffraction experiments on a low-Z element, Be, were performed at pressures up to 171 GPa using the synchrotron radiation source at SPring-8. All profiles were assigned to the hcp structure of the ambient phase, and the theoretically predicted hcp-bcc phase transition was not observed. The previously proposed hcp-hexagonal phase transition around 14.5 GPa was also not confirmed. The equation of state of hcp-Be was determined by a least mean squares fitting to the Birch-Murnaghan equation from these diffraction data. Calculated values of K sub 0 and K sub 0 ' were 97.2 +- 2.5 GPa and 3.61 +- 0.07, respectively.

  5. X-ray diffraction studies of dynamically compressed diamond

    Energy Technology Data Exchange (ETDEWEB)

    Eggert, J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2010-06-10

    We propose a series of experiments to use X-ray diffraction (XRD) to study material properties using the NIF. XRD is the best way to determine the structure, lattice deformation, and texture of materials. Advances in synchrotron XRD facilities in the past two decades have revolutionized the study of materials at static high pressure in diamond anvil cells (DACs) up to about 3 Mbar. The National Ignition Facility (NIF) has the potential to do the same for dynamic materials studies at high-pressure. Members of our scientific team have pioneered XRD on many smaller laser facilities around the world. Our results suggest that diffraction on solids approaching 100 Mbar may be possible on the NIF, providing access to new regime for matter at extreme conditions.

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

    Science.gov (United States)

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

    2000-01-01

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

  7. In-situ Scanning Transmission X-Ray Microscopy of Catalytic Solids and Related Nanomaterials

    NARCIS (Netherlands)

    de Groot, F.M.F.; de Smit, E.; van Schooneveld, M.M.; Aramburo, L.R.; Weckhuysen, B.M.

    2013-01-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the e

  8. In-situ scanning transmission X-ray microscopy of catalytic materials under reaction conditions

    NARCIS (Netherlands)

    de Smit, E.; Creemer, J.F.; Zandbergen, H.W.; Weckhuysen, B.M.; de Groot, F.M.F.

    2009-01-01

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-11

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

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

    OpenAIRE

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

    2011-01-01

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

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

    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...

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

    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,...

  13. The first X-ray diffraction measurements on Mars

    Directory of Open Access Journals (Sweden)

    David Bish

    2014-11-01

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

  14. In situ X-ray diffraction during pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Vonk, Vedran [Max-Planck-Institute for Metals Research, Stuttgart (Germany); Huijben, Mark [University of California, Berkeley (United States); Driessen, Kurt; Rijnders, Guus; Blank, Dave; Harkema, Sybolt [University of Twente, Enschede (Netherlands); Graafsma, Heinz [Deutsches Elektronen- Synchrotron, Hamburg (Germany)

    2007-07-01

    The use of in situ X-ray diffraction for the study of thin film growth enables in a straightforward way to derive the atomic structure, because the kinematical scattering approximation holds. Here we present the results of studying the heteroepitaxial growth by Pulsed Laser Deposition of complex oxides such as the High-T c superconductor YBa{sub 2}Cu{sub 3}O{sub 7-x} and the insulator LaAlO{sub 3} on SrTiO{sub 3}(001) substrates. A special sample chamber has been constructed to be used with synchrotron X-rays. Detailed pictures of the growth kinetics and of the atomic interface structure at deposition conditions result from fitting quantitatively both the intensity growth oscillations and the crystal truncation rods. The growth of the complex oxide thin films presented here is characterized by substantial interlayer-mass transport and large deviations from the bulk room-temperature atomic structure. The results show the effects of the interplay between formation and diffusion energies on the processes of nucleation and kinetics during heteroepitaxial growth.

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

    Science.gov (United States)

    Sutter, John P.

    2011-09-01

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

  16. Phase retrieval methods for surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Saldin, D.K.; Harder, R.J.; Shneerson, V.L. [Department of Physics, University of Wisconsin-Milwaukee, Milwaukee, WI (United States); Moritz, W. [Institute of Crystallography and Applied Mineralogy, University of Munich, Munich (Germany)

    2001-11-26

    We develop an iterative input-output feedback method for the phasing of surface x-ray diffraction (SXRD) amplitudes that relies on successive operations in real and reciprocal space. We demonstrate its use for the recovery of the real and positive electron density of a surface unit cell from simulated SXRD intensities. We have successfully recovered the entire surface electron density in a case where the two-dimensional surface unit cell is the same as that of the bulk and also in one where the surface unit cell is four times larger than that of the bulk. We show that the exponential modelling algorithm for structure completion derived earlier from maximum entropy theory may be regarded as a special case of an input-output phasing algorithm with a particular form of object-domain operations. (author)

  17. 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.

  18. Parts per Million Powder X-ray Diffraction.

    Science.gov (United States)

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

    2015-11-01

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

  19. Liquid structure of pure iron by X-ray diffraction

    Institute of Scientific and Technical Information of China (English)

    Jun Luo; Qijie Zhai; Pei Zhao; Xubo Qin

    2004-01-01

    The liquid structure of pure iron at 1540, 1560 and 1580℃ was studied by X-ray diffraction. The results show that near the melting point there is a medium-range order structure that fades away with the increasing temperature. The average nearest distance of atoms is almost independent of the melts temperature, but the average coordination number, the atom cluster size and the atom number in an atom cluster all decrease with the increasing temperature of the melt. Near the melting point there area lot of atom clusters in the pure iron melt. The atom cluster of pure iron has the body-centered cubic lattices, which are kept from the solid state. And the body-centered cubic lattices connect into network by occupying a same edge. The atoms in the surrounding of the atom clusters are arranged disorderly.

  20. 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.

  1. In-situ X-ray diffraction study of stress-induced phase transition of (1 − x)BaZr{sub 0.2}Ti{sub 0.8}O{sub 3}–xBa{sub 0.7}Ca{sub 0.3}TiO{sub 3} in polymer matrix composite

    Energy Technology Data Exchange (ETDEWEB)

    Wang, W., E-mail: spacexuanwu@163.com [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Li, W.L. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); National Key Laboratory of Science and Technology on Precision Heat Processing of Metals, Harbin Institute of Technology, Harbin 150001 (China); Feng, Y.; Hou, Y.F.; Xu, D.; Wang, M. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Fei, W.D., E-mail: wdfei@hit.edu.cn [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2014-08-01

    Phase transitions of (1 − x)BaZr{sub 0.2}Ti{sub 0.8}O{sub 3}–xBa{sub 0.7}Ca{sub 0.3}TiO{sub 3} (BZT–xBCT) powders under tensile stress were investigated using in-situ X-ray diffraction (XRD). Uniaxial stress was applied to the designed BZT–xBCT/polyimide composite films during XRD. Under stress, the rhombohedral (R) phase was found to transform into a tetragonal (T) phase, while the [001] direction of the T phase tends to be parallel to the tensile direction. T → R phase transition was not observed in the films upon tensile stress loading, implying that R → T phase transitions may be the decisive factor for the huge piezoelectric response of the BZT–xBCT system. - Highlights: • The in-situ X-ray diffraction was studied on BZT–xBCT during tensile process. • Stress-induced phase transition of BZT–xBCT was observed during tensile process. • R → T phase transition may be the decisive factor for the huge d{sub 33} of BZT–xBCT.

  2. 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

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

    Science.gov (United States)

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

    2004-01-01

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

  4. Ultrafast Time Resolved X-ray Diffraction Studies of Laser Heated Metals and Semiconductors

    Science.gov (United States)

    Chen, Peilin; Tomov, I. V.; Rentzepis, P. M.

    1998-03-01

    Time resolved hard x-ray diffraction has been employed to study the dynamics of lattice structure deformation. When laser pulse energy is deposited in a material it generates a non uniform transient temperature distribution, which alters the lattice structure of the crystal. The deformed crystal lattice will change the angle of diffraction for a monochromatic x-ray beam. We report picosecond and nanosecond time resolved x-ray diffraction measurements of the lattice temperature distribution, transient structure and stress, in Pt (111) and GaAs (111) crystals, caused by pulsed UV laser irradiation. An ArF excimer laser operated at 300 Hz was used, both, to drive an x-ray diode with copper anode and heat the crystal. Bragg diffracted x-ray radiation was recorded by a direct imaging x-ray CCD. Changes in the diffraction patterns induced by a few millijouls pulse energy were observed at different time delays between the laser heating pulse and the x-ray probing pulse. A kinematical model for time resolved x-ray diffraction was used to analyze the experimental data. Good agreement between the measured and calculated scattered x-ray intensities profiles was achieved, indicating that detailed time resolved x-ray diffraction measurements can be made with nanosecond and picosecond resolution for small temperature changes. Our system can detect changes in the lattice spacing of about 10-3 A.

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

    Science.gov (United States)

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

    2013-12-01

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

  6. Comparative studies of the phase evolution in M-doped LixMn1.5Ni0.5O4 (M = Co, Al, Cu and Mg) by in-situ X-ray diffraction

    Science.gov (United States)

    Zhu, W.; Liu, D.; Trottier, J.; Gagnon, C.; Guerfi, A.; Julien, C. M.; Mauger, A.; Zaghib, K.

    2014-10-01

    A series of metal-doped LiMn1.5Ni0.5O4 (metal = Co, Al, Cu and Mg) positive electrode materials for lithium ion batteries were synthesized and their structural changes during the galvanostatic charge/discharge process at C/24 rate were investigated by using in situ X-ray diffraction (XRD) measurements. The phase diagram shows that similar series of first-order phase transitions with two regions of two-phase coexistence are observed during intercalation/de-intercalation of lithium among all the doped cathode materials. However, minor differences of the phase evolution and the electrochemical properties point to the different roles of the dopant ions. The phase diagram is analyzed and discussed, together with the differences among different results reported in the literature to distinguish between general intrinsic properties of spinel and sample-dependent properties due to the degree of cation ordering, out-of-equilibrium effects, electro-negativity and radii of the dopant ions. Among the metal-substituted samples, we argue that the Co-doping is the most promising approach with improved electrochemical property.

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

    OpenAIRE

    F. H. O’Shea; O. Williams; Andonian, G.; Barber, S; Sakai, Y.; Rosenzweig, J. B.; Pogorelsky, I.; Fedurin, M.; K. Kusche; Yakimenko, V.

    2012-01-01

    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 ...

  8. 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.

  9. X-ray Spectroscopy and Diffraction at HPCAT - An Integrated High Pressure Synchrotron Facility

    Science.gov (United States)

    Mao, H.; Hemley, R. J.; Hausermann, D.; Hu, M.; Meng, Y.; Somayazulu, M.

    2002-05-01

    High Pressure Collaborative Access Team (HPCAT) is a new facility dedicated for high-pressure research using the high-energy synchrotron beams at the Advanced Photon Source for in-situ investigations of crystallographic, elastic, rheologic, electronic, and magnetic properties of solids, liquids, and amorphous materials at high P and simultaneous high T or cryogenic T. The HPCAT high-brilliance undulator beamline is optimized for a full range of high-pressure x-ray spectroscopy. For instance, nuclear resonant inelastic scattering measures phonon densities of state of Fe-containing samples that yield valuable information on acoustic wave velocity, elasticity, elastic anisotropy, and thermodynamic quantities (vibrational energy, heat capacity, entropy, Debye temperature, and Gr\\x81neisen parameter) of materials at high pressures. Nuclear resonant x-ray forward scattering measures M”ssbauer spectra in the time domain that yield information on magnetism, site occupancy, oxidation states, and the Lamb-M”ssbauer coefficient of Fe. Resonant inelastic x-ray scattering measures element-specific electronic transitions. The medium-resolution (10-100 meV) non-resonant x-ray inelastic scattering measures electronic energies and dispersions that yield information on plasmons, excitons, electronic band structures, and chemical bondings, and high-resolution (<10 meV) inelastic scattering measures phonon dispersions that yield information on acoustic wave velocity and elasticity as a function of crystallographic orientation. X-ray emission spectroscopy yields information on valence electrons and spin states of d-electrons. A diamond branch monochromator diverts a full-intensity undulator monochromatic beam at energies up to 35 keV for full-time x-ray diffraction studies of crystallography, phase transitions, and equations of state in a side station without affecting the simultaneous operation of the main undualtor beamline. The HPCAT bending-magnet beamline is divided into two

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

    Directory of Open Access Journals (Sweden)

    Muakthong, D.

    2005-01-01

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

  11. 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.

  12. In-situ scanning transmission X-ray microscopy of catalytic materials under reaction conditions

    OpenAIRE

    E. Smit; Creemer, J.F.; Zandbergen, H. W.; Weckhuysen, B. M.; Groot, F.M.F. de

    2009-01-01

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant reaction conditions, and provide detailed information on the morphology and composition of the catalyst material. The nanometer resolution combined with powerful chemical speciation by XAS and the...

  13. High-pressure investigations on Piplia Kalan eucrite meteorite using in-situ X-ray diffraction and 57Fe Mössbauer spectroscopic technique up to 16 GPa

    Directory of Open Access Journals (Sweden)

    Usha Chandra

    2016-03-01

    Full Text Available We report here high-pressure investigations on Piplia Kalan eucrite–a member of HED (Howardite–Eucrite–Diogenite family from asteroid 4-Vesta based on synchrotron X-ray diffraction (up to 16 GPa and 57Fe Mössbauer spectroscopy (up to 8 GPa. Dominant with anorthite-rich plagioclase, pigeonite-rich pyroxene and clino-ferrosilite, the sample displayed various phase transitions attaining amorphous character at 16 GPa. These phase transitions of individual components could be explained simultaneously through variations in high-pressure XRD patterns and the Mössbauer parameters. Most prominent P21/c to C2/c transition of pigeonite and ferrosilite was exhibited both as sudden variation in Mössbauer parameters and population inversion of Fe2+ in M1 and M2 sites between 2.9 and 3.8 GPa and variation in intensity profile in XRD patterns at 3.56 GPa. Anorthite seemed to respond more to such impact than other components in the sample. Complete amorphization in anorthite which occurred at lower pressure of ∼12 GPa implied residual stress experienced due to shock impact. The presence of high pressure (monoclinic phase of pigeonite and ferrosilite at ambient condition in this eucrite sample confirmed earlier suggestions of an early shock event. This report is an attempt to emphasize the role of anorthite in the determination of the residual stress due to impact process in the parent body thus to understand the behavioral differences amongst HED members.

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

    Science.gov (United States)

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

    2013-06-01

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

  15. Study of texture effect on elastic properties of Au thin films by x-ray diffraction and Brillouin light scattering

    Energy Technology Data Exchange (ETDEWEB)

    Faurie, D [LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse (France); Djemia, P [LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse (France); Renault, P-O [LMP, UMR 6630 CNRS, Universite de Poitiers, 86962 Futuroscope (France); Roussigne, Y [LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse (France); Cherif, S M [LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse (France); Bourhis, E Le [LMP, UMR 6630 CNRS, Universite de Poitiers, 86962 Futuroscope (France); Goudeau, Ph [LMP, UMR 6630 CNRS, Universite de Poitiers, 86962 Futuroscope (France)

    2007-12-15

    We have shown a strong texture effect on elastic properties of gold thin films deposited by physical vapour deposition. Elastic properties of non-textured and {l_brace}111{r_brace} fiber textured gold thin films were investigated by x-ray diffraction combined with in-situ tensile testing and Brillouin light scattering. These static and dynamic methods allowed characterizing the local and macroscopic elastic behavior of gold films.

  16. Austenite nucleation and growth observed on the level of individual grains by three-dimensional X-ray diffraction microscopy

    OpenAIRE

    Savran, V.I.; Offerman, S. E.; Sietsma, J.

    2010-01-01

    Austenite nucleation and growth is studied during continuous heating using three-dimensional X-ray diffraction (3-D XRD) microscopy at the European Synchrotron Radiation Facility (ESRF) (Grenoble, France). Unique in-situ observations of austenite nucleation and growth kinetics were made for two commercial medium-carbon low-alloy steels (0.21 and 0.35 wt pct carbon with an initial microstructure of ferrite and pearlite). The measured austenite volume fraction as a function of temperature shows...

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

    NARCIS (Netherlands)

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

    1999-01-01

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

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

    Science.gov (United States)

    Blanchard, Frank N.

    1980-01-01

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

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

    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…

  20. 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…

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

    Science.gov (United States)

    Blanchard, Frank N.

    1980-01-01

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

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

    Science.gov (United States)

    Fujisaki, Kazuhiro; Tadano, Shigeru

    2010-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Garg, Alka B. [High Pressure and Synchrotron Radiation Physics Division, Bhabha Atomic Research Centre, Mumbai 400085, Maharashtra (India); Errandonea, D., E-mail: daniel.errandonea@uv.es [Departamento de Física Aplicada—ICMUV, MALTA Consolider Team, Universidad de Valencia, Edificio de Investigación, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain)

    2015-03-15

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

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

    Science.gov (United States)

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

    2013-09-01

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

  5. X-RAY DIFFRACTION STUDY OF A PANCHAVAKTRA RAS

    Directory of Open Access Journals (Sweden)

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

    2012-06-01

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

  6. The rotating-crystal method in femtosecond X-ray diffraction.

    Science.gov (United States)

    Freyer, B; Stingl, J; Zamponi, F; Woerner, M; Elsaesser, T

    2011-08-01

    We report the first implementation of the rotating-crystal method in femtosecond X-ray diffraction. Applying a pump-probe scheme with 100 fs hard X-ray probe pulses from a laser-driven plasma source, the novel technique is demonstrated by mapping structural dynamics of a photoexcited bismuth crystal via changes of the diffracted intensity on a multitude of Bragg reflections. The method is compared to femtosecond powder diffraction and to Bragg diffraction from a crystal with stationary orientation.

  7. Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

    Science.gov (United States)

    Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

    2004-01-01

    X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

  8. 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...

  9. In-situ scanning transmission X-ray microscopy of catalytic solids and related nanomaterials.

    Science.gov (United States)

    de Groot, Frank M F; de Smit, Emiel; van Schooneveld, Matti M; Aramburo, Luis R; Weckhuysen, Bert M

    2010-04-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the experimental boundary conditions that determine the potential applications for in-situ XAS and in-situ STXM studies are discussed. Nanoscale chemical imaging of catalysts under working conditions is outlined using cobalt and iron Fischer-Tropsch catalysts as showcases. In the discussion, we critically compare STXM-XAS and STEM-EELS (scanning transmission electron microscopy-electron energy loss spectroscopy) measurements and indicate some future directions of in-situ nanoscale imaging of catalytic solids and related nanomaterials.

  10. In-situ Scanning Transmission X-Ray Microscopy of Catalytic Solids and Related Nanomaterials

    Energy Technology Data Exchange (ETDEWEB)

    de Groot, F.; Smit, E; van Schooneveld, M; Aramburo, L; Weckhuysen, W

    2010-01-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the experimental boundary conditions that determine the potential applications for in-situ XAS and in-situ STXM studies are discussed. Nanoscale chemical imaging of catalysts under working conditions is outlined using cobalt and iron Fischer-Tropsch catalysts as showcases. In the discussion, we critically compare STXM-XAS and STEM-EELS (scanning transmission electron microscopy-electron energy loss spectroscopy) measurements and indicate some future directions of in-situ nanoscale imaging of catalytic solids and related nanomaterials.

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

    Science.gov (United States)

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

    2015-07-01

    Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles. © The Author 2015. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

  12. 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.

  13. Strains in Thermally Growing Alumina Films Measured in-situ usingSynchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Hou, P.Y.; Paulikas, A.P.; Veal, B.W.

    2006-01-02

    Strains in thermally grown oxides have been measured in-situ, as the oxides develop and evolve. Extensive data have been acquired from oxides grown in air at elevated temperatures on different model alloys that form Al{sub 2}O{sub 3}. Using synchrotron x-rays at the Advanced Photon Source (Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from the oxidizing specimen were recorded every 5 minutes during oxidation and subsequent cooling. The diffraction patterns were analyzed to determine strains in the oxides, as well as phase changes and the degree of texture. To study a specimen's response to stress perturbation, the oxidizing temperature was quickly cooled from 1100 to 950 C to impose a compressive thermal stress in the scale. This paper describes this new experimental approach and gives examples from oxidized {beta}-NiAl, Fe-20Cr-10Al, Fe-28Al-5Cr and H{sub 2}-annealed Fe-28Al-5Cr (all at. %) alloys to illustrate some current understanding of the development and relaxation of growth stresses in Al{sub 2}O{sub 3}.

  14. 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...... over large number of nanowires. Knowing the precise positions of multiple Bragg peaks in reciprocal space we could calculate the average strain and composition. (ii) In the second technique we used a nanofocused X-ray beam of 100 nm in diameter to measure the local variation of strain and tilt...... grow the nanowires and measure X-ray diraction in real time. We studied the initial stage of pure WZ InAs nanowire growth. By measuring the interference fringes in the scattering signal, raising from the nite length of the NWs it was possible to precisely determine the nanowire length evolution at each...

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

    OpenAIRE

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

    2011-01-01

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

  16. A Bayesian Approach to Surface X-ray Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lyman, Paul F.; Saldin, Dilano K.

    2006-11-17

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

  17. Mapping strain fields induced in Zr-based bulk metallic glasses during in-situ nanoindentation by X-ray nanodiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gamcová, J.; Bednarčík, J.; Franz, H. [DESY, Notkestraße 85, Hamburg 22547 (Germany); Mohanty, G.; Wehrs, J.; Michler, J. [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstraße 39, Thun 3602 (Switzerland); Michalik, Š. [Institute of Physics ASCR, Na Slovance 2, Praha 18221 (Czech Republic); Krywka, C. [HZG, Institut für Werkstoffforschung, Notkestraße 85, Hamburg 22547 (Germany); Breguet, J. M. [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstraße 39, Thun 3602 (Switzerland); Alemnis GmbH, Feuerwerkerstraße 39, Thun 3602 (Switzerland)

    2016-01-18

    A pioneer in-situ synchrotron X-ray nanodiffraction approach for characterization and visualization of strain fields induced by nanoindentation in amorphous materials is introduced. In-situ nanoindentation experiments were performed in transmission mode using a monochromatic and highly focused sub-micron X-ray beam on 40 μm thick Zr-based bulk metallic glass under two loading conditions. Spatially resolved X-ray diffraction scans in the deformed volume of Zr-based bulk metallic glass covering an area of 40 × 40 μm{sup 2} beneath the pyramidal indenter revealed two-dimensional map of elastic strains. The largest value of compressive elastic strain calculated from diffraction data at 1 N load was −0.65%. The region of high elastic compressive strains (<−0.3%) is located beneath the indenter tip and has radius of 7 μm.

  18. X-ray micro diffraction study on mesostructured silica thin films

    CERN Document Server

    Noma, T; Miyata, H; Iida, A

    2001-01-01

    The local structure of highly ordered mesostructured silica films was investigated by using a synchrotron X-ray microbeam and a CCD X-ray detector. Two-dimensional X-ray diffraction patterns clearly showed the detailed arrangement of the mesostructures, in which the hexagonal mesochannels aligned uniaxially in the mesostructured silica films formed on a silica glass substrate with a rubbing-treated thin polyimide coating. The alignment direction was shown to be perpendicular to the rubbing direction. The grazing incidence condition revealed the structural anisotropy of the mesostructures, while normal incidence X-ray diffraction data indicated the in-plane structural uniformity of the films. Extra spots were observed in the diffraction patterns. This suggested that the X-ray beam reflected at the boundary of the mesostructured silica film and the substrate.

  19. 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.

  20. 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.

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

    Science.gov (United States)

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

    2000-01-01

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

  2. Local terahertz field enhancement for time-resolved x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kozina, M.; /SLAC; Pancaldi, M.; /CIC nanoGUNE /Stockholm U.; Bernhard, C.; /Fribourg U.; Driel, T.van; Glownia, J.M.; /SLAC; Marsik, P.; /Fribourg U.; Radovic, M.; Vaz, C.A.F.; /PLS, SLS; Zhu, D.; /SLAC; Bonetti, S.; /Stockholm U.; Staub, U.; /PLS, SLS; Hoffmann, M.C.; /SLAC

    2017-02-20

    We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. We find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO3 thin-film sample.

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

    DEFF Research Database (Denmark)

    Buras, B.; Lebech, Bente; Kofoed, W.

    1984-01-01

    A furnace for diffraction studies using synchrotron X-ray radiation is described. The furnace can be operated between ambient temperature and 1 800 °C with a temperature stability better than 5 °C for temperatures above 300 °C. Kapton windows allow almost 360° access for the X-ray beam in the hor...

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

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

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

  5. Neutron and X-ray diffraction study of residual and internal stress evolution in pearlitic steel during cold drawing

    Science.gov (United States)

    Kriška, M.; Tacq, J.; Van Acker, K.; Seefeldt, M.; Van Petegem, S.

    2012-02-01

    Neutron and X-ray diffraction were used to study the residual and internal stress evolution during cold drawing in pearlitic steel wires. A selection of high strength filaments drawn to different reductions has been investigated. In order to compare the evolution of macro and micro residual phase stresses in ferrite, the lattice strain evolution has been studied in axial and transverse direction. In-situ neutron diffraction tests in "Poisson" geometry have been carried out at the TOF strain scanner POLDI at PSI, Switzerland. These tests revealed a significant scatter in mechanical response among differently oriented ferrite grains, including a peculiar response of the {200} reflection, cp. [1, 2].

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

    Science.gov (United States)

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

    2014-03-01

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

  7. Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

    Science.gov (United States)

    Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

    2014-11-17

    We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

  8. Artefacts of X-ray area detectors caused by diffraction

    CERN Document Server

    Gollwitzer, Christian

    2013-01-01

    When an X-ray area detector based on a single crystalline material, for instance a state of the art hybrid-pixel detector, is illuminated from a point source by monochromatic radiation, a pattern of lines appears, which overlays the detected image. These lines can easily be found by scattering experiments with smooth patterns such as small angle X-ray scattering. The origin of this effect is Bragg reflection in the absorber of the detector. We present experimental images over a photon energy range from 3.4 keV to 10 keV together with a theoretical analysis. The patterns can be exploited to check the alignment of the detector surface to the direct beam, and of individual detector modules to each other for modular detectors, as well as for energy calibration of the radiation.

  9. Focusing Optics for High-Energy X-ray Diffraction

    DEFF Research Database (Denmark)

    Leinert, U.; Schulze, C.; Honkimäki, V.;

    1998-01-01

    of the different set-ups are described and potential applications are discussed. First experiments were performed, investigating with high spatial resolution the residual strain gradients in layered polycrystalline materials. The results underline that focused high-energy synchrotron radiation can provide unique...... information on the mesoscopic scale to the materials scientist, complementary to existing techniques based on conventional X-ray sources, neutron scattering or electron microscopy....

  10. Characteristic, parametric, and diffracted transition X-ray radiation for observation of accelerated particle beam profile

    Science.gov (United States)

    Chaikovska, I.; Chehab, R.; Artru, X.; Shchagin, A. V.

    2017-07-01

    The applicability of X-ray radiation for the observation of accelerated particle beam profiles is studied. Three types of quasi-monochromatic X-ray radiation excited by the particles in crystals are considered: characteristic X-ray radiation, parametric X-ray radiation, diffracted transition X-ray radiation. Radiation is collected at the right angle to the particle beam direction. It is show that the most intensive differential yield of X-ray radiation from Si crystal can be provided by characteristic radiation at incident electron energies up to tens MeV, by parametric radiation at incident electron energies from tens to hundreds MeV, by diffracted transition X-ray radiation at GeV and multi-GeV electron energies. Therefore these kinds of radiation are proposed for application to beam profile observation in the corresponding energy ranges of incident electrons. Some elements of X-ray optics for observation of the beam profile are discussed. The application of the DTR as a source of powerful tunable monochromatic linearly polarized X-ray beam excited by a multi-GeV electron beam on the crystal surface is proposed.

  11. Generation of apodized X-ray illumination and its application to scanning and diffraction microscopy.

    Science.gov (United States)

    Khakurel, Krishna P; Kimura, Takashi; Nakamori, Hiroki; Goto, Takumi; Matsuyama, Satoshi; Sasaki, Tomoya; Takei, Masashi; Kohmura, Yoshiki; Ishikawa, Tetsuya; Yamauchi, Kazuto; Nishino, Yoshinori

    2017-01-01

    X-ray science has greatly benefited from the progress in X-ray optics. Advances in the design and the manufacturing techniques of X-ray optics are key to the success of various microscopic and spectroscopic techniques practiced today. Here the generation of apodized X-ray illumination using a two-stage deformable Kirkpatrick-Baez mirror system is presented. Such apodized illumination is marked by the suppression of the side-lobe intensities of the focused beam. Thus generated apodized illumination was employed to improve the image quality in scanning X-ray fluorescence microscopy. Imaging of a non-isolated object by coherent X-ray diffractive imaging with apodized illumination in a non-scanning mode is also presented.

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

    Institute of Scientific and Technical Information of China (English)

    郭鑫; 江舟亚; 陈龙; 陈黎明; 辛建国; 陈洁

    2015-01-01

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

  13. In-situ Scanning Transmission X-ray Microscopy of catalytic materials under reaction conditions

    Science.gov (United States)

    de Smit, Emiel; Creemer, J. Fredrik; Zandbergen, Henny W.; Weckhuysen, Bert M.; de Groot, Frank M. F.

    2009-11-01

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant reaction conditions, and provide detailed information on the morphology and composition of the catalyst material. The nanometer resolution combined with powerful chemical speciation by XAS and the ability to image materials under realistic conditions opens up new opportunities to study many chemical processes.

  14. In-situ Scanning Transmission X-ray Microscopy of catalytic materials under reaction conditions

    Energy Technology Data Exchange (ETDEWEB)

    Smit, Emiel de; Weckhuysen, Bert M; Groot, Frank M F de [Inorganic Chemistry and Catalysis group, Debye Institute for Nanomaterials Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands); Creemer, J Fredrik [DIMES-ECTM, Delft University of Technology, 2600 GB Delft (Netherlands); Zandbergen, Henny W, E-mail: e.desmit@uu.n [Kavli Institute of NanoScience, National Centre for High Resolution Electron Microscopy, Delft University of Technology, 2600 GA Delft (Netherlands)

    2009-11-15

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant reaction conditions, and provide detailed information on the morphology and composition of the catalyst material. The nanometer resolution combined with powerful chemical speciation by XAS and the ability to image materials under realistic conditions opens up new opportunities to study many chemical processes.

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

    Science.gov (United States)

    Chung, Frank H

    2016-08-23

    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.

  16. Synchrotron Radial X-ray Diffraction Studies of Deformation of Polycrystalline MgO

    Science.gov (United States)

    Girard, J.; Tsujino, N.; Mohiuddin, A.; Karato, S. I.

    2016-12-01

    X-ray diffraction analyses have been used for decades to study mechanical properties of polycrystalline samples during in-situ high-pressure deformation. When polycrystalline materials are deformed, stresses develop in grains and lead to lattice distortion. Using X-ray diffraction we can estimate the lattice strain for each (hkl) diffraction plans and calculate the applied stress for each (hkl), using [Singh, 1993] relation. However, this method doesn't take into account plastic anisotropy. As a results of plastic anisotropy present in the material, stress estimated from this method can be largely differ depending on (hkl) diffraction planes [Karato, 2009]. Studying the stress estimate for each (hkl) plane, might help us distinguish dominant deformation mechanisms activated during deformation such as diffusion (we will observe small stress variation as a function of (hkl) diffraction planes) or dislocation creep (we will observe a stress variation as a function of (hkl) diffraction planes that could also give us clues on potential slip system activity). In this study we observed stress evolution in MgO polycrystalline samples deformed under mantle pressure and temperature for (200) and (220) diffraction planes. Using a range MgO grain sizes we were able to control the active deformation mechanism (for e.g. diffusion creep or dislocation creep). For coarse-grained specimens, we observed strong (hkl) dependence of radial strain indicating the operation of dislocation creep. The observed (hkl) dependence changes with pressure suggesting a change in the slip system: at pressures higher than 27 GPa, (200) shows larger stress estimate than (220). In contrast, at lower pressures, (220) shows larger stress estimate than (200). This might indicate a slip system transition in MgO occurring under lower mantle conditions. From {110} plane to {100} plane. This is in good agreement with theoretical predictions and numerical calculation [Amodeo et al., 2012] and has an important

  17. Scanning force microscope for in situ nanofocused X-ray diffraction studies

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Zhe, E-mail: zhe.ren@im2np.fr; Mastropietro, Francesca; Davydok, Anton [Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen – Case 142, F-13397 Marseille (France); Langlais, Simon [Grenoble Institute of Technology and CNRS, BP 75, F-38402 Saint-Martin d’Hères Cedex (France); Richard, Marie-Ingrid [Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen – Case 142, F-13397 Marseille (France); European Synchrotron Radiation Facility (ESRF), 6 rue Jules Horowitz, BP 220, 38043 Grenoble (France); Furter, Jean-Jacques; Thomas, Olivier [Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen – Case 142, F-13397 Marseille (France); Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume [Grenoble Institute of Technology and CNRS, BP 75, F-38402 Saint-Martin d’Hères Cedex (France); Boesecke, Peter [European Synchrotron Radiation Facility (ESRF), 6 rue Jules Horowitz, BP 220, 38043 Grenoble (France); Cornelius, Thomas W. [Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen – Case 142, F-13397 Marseille (France)

    2014-08-06

    An atomic force microscope has been developed for combination with sub-micrometer focused X-ray diffraction at synchrotron beamlines and in situ mechanical tests on single nanostructures. A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials.

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

    Data.gov (United States)

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

  19. X-Ray Diffraction Powder Patterns and Thin Section Observations from the Sierra Madera Impact Structure

    Science.gov (United States)

    Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

    2006-03-01

    X-Ray powder diffraction analysis and thin section observations of carbonate and siliciclastic samples from the Sierra Madera impact structure indicate moderate shock pressures (8 to 30 GPa) were generated during the formation of this crater.

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

    Data.gov (United States)

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

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

    Science.gov (United States)

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

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

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

    Science.gov (United States)

    Berman, R.M.; Cohen, I.

    1988-04-26

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

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

    Science.gov (United States)

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

    2010-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-09-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques [Palais du Louvre, Laboratoire du Centre de Recherche et de Restauration des Musees de France C2RMF CNRS UMR 171, Paris (France)

    2010-09-15

    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.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-08-19

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

  8. 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

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

    Science.gov (United States)

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

    1996-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-10-01

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

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

    Science.gov (United States)

    Hu, Z. W.

    2003-01-01

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

  12. In-situ surface sensitive X-ray investigations of quench condensed thin metal films

    Energy Technology Data Exchange (ETDEWEB)

    Markert, Christian; Luetzenkirchen-Hecht, Dirk; Gertz, Sascha; Frahm, Ronald [Bergische Universitaet Wuppertal, Fachbereich C / Abteilung Physik, Gaussstrasse 20, 42119 Wuppertal (Germany)

    2007-07-01

    We report of ultrahigh vacuum (UHV) experiments on ultra thin Au, Bi and Pb films (thickness less than 10 nm) deposited on atomically flat float-glass substrates which are held at cryogenic temperatures down to 10 K. For deposition temperatures below 100 K the formation of highly disordered or even amorphous metal films can be expected, because thermally activated diffusion of the ad atoms should be inhibited. An UHV chamber was constructed which is suited for grazing incidence X-ray experiments during the quench condensation of the metal films. Various X-ray methods were used for the in-situ investigation of the films growth and their structural evolution with the thickness and an subsequent annealing process. EXAFS (Extended X-ray Absorption Fine Structure) in reflection is used to study the local structure of the films. Furthermore specular and non-specular X-ray reflectivity measurements were performed to get information about the films density and surface roughness parameters (correlation length, hurst parameter etc.). In addition in situ resistivity measurements which are sensitive towards changes of the films microstructure were performed in parallel to the X-ray experiments.

  13. Structural Investigations of Nanowires Using X-Ray Diffraction

    DEFF Research Database (Denmark)

    Stankevic, Tomas

    a very accurate measurements of strain at every point of the single nanowire. We showed that in critical heterostructures the strain distribution can be very inhomogeneous. (iii) Lastly, we have studied in-situ the nanowire growth by molecular beam epitaxy at the synchrotron beamline. With this, we could...

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

    Energy Technology Data Exchange (ETDEWEB)

    Kycia, S.

    1996-04-23

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

  15. Mapping the Strain Distributions in Deformed Bulk Metallic Glasses Using Hard X-Ray Diffraction

    Science.gov (United States)

    Bednarcik, J.; Chen, L. Y.; Wang, X. D.; Jiang, J. Z.; Franz, H.

    2012-05-01

    The deformation behavior of Cu45 Zr46.5 Al7Ti1.5 bulk metallic glass (BMG) under bending was investigated in-situ using high-energy X-ray synchrotron diffraction. Samples were bent using two different benders with radii of 10 and 20 mm. The components of the strain tensor were determined from the change of positions of the first maximum of the diffracted intensity in reciprocal space. The procedure of data treatment was improved by the introduction of direct beam off-center correction. Comparing results for the two different bending radii, we found that the zero stress region does not necessarily lay within the central part of the specimen. Bending with smaller radius resulted in symmetric strain distribution, whereas a larger bending radius revealed strong asymmetry. Furthermore, bending with a smaller radius (10 mm) shows steeper strain gradients as compared with the situation in which the larger bending radius (20 mm) was used. Using a smaller bending radius implies reaching higher tensile/compressive stresses and reveals the signs of the plastic deformation, which are demonstrated as a saturation of elastic strains.

  16. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-06-11

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

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

    CERN Document Server

    Kishimoto, S; Ito, M

    2001-01-01

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

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

    Indian Academy of Sciences (India)

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

    2000-04-01

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

  20. In-situ X-ray diffraction study of the initial dealloying of Cu{sub 3}Au(001) and Cu{sub 0.83}Pd{sub 0.17}(001)

    Energy Technology Data Exchange (ETDEWEB)

    Renner, F.U. [European Synchrotron Radiation Facility, 38043 Grenoble (France)]. E-mail: frank.renner@aist.go.jp; Gruender, Y. [European Synchrotron Radiation Facility, 38043 Grenoble (France); Lyman, P.F. [University of Wisconsin-Milwaukee, Department of Physics, Milwaukee, WI 53201 (United States); Zegenhagen, J. [European Synchrotron Radiation Facility, 38043 Grenoble (France)

    2007-05-23

    Dealloying and selective dissolution are serious corrosion processes, but also employed in technology. We studied the surface structure of Cu{sub 0.83}Pd{sub 0.17}(001) and Cu{sub 3}Au(001) during electrochemical selective Cu dissolution below the critical potential in-situ in 0.1 M H{sub 2}SO{sub 4} (pH = 1) electrolyte. In both cases we observe the formation of an epitaxial layer of nano-scale islands of the noble component of the original alloy (Au or Pd). These islands form a metallic passivation layer suppressing massive dissolution of Cu. The Au islands developed {l_brace}111{r_brace} facets. By re-deposition of Cu ions from the electrolyte solution onto Pd islands, an epitaxial Cu layer is formed.

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

    Directory of Open Access Journals (Sweden)

    Zuliskandar Ramli

    2011-01-01

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

  2. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

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

    2004-02-01

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

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

    Science.gov (United States)

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

    1978-01-01

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

  4. 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 (nanocrystalline powders under pressure. We offer a tentative interpretation of the distribution of macro- and micro-strains in nanoparticles of different grain size.

  5. Carbon Fiber Morphology. 2. Expanded Wide-Angle X-Ray Diffraction Studies of Carbon Fibers

    Science.gov (United States)

    1991-02-01

    X- Ray Diffraction," JPS. Polym. Phys. Ed., 16, 939 (1978). 17. Rosalind E. Franklin , "The Structure of Graphitic Carbons," Acta Cryst., 4, 253 (1951...18. Rosalind E. Franklin , "The Interpretation of Diffuse X-ray Diagrams of Carbon," Acta CrL, 3, 107 (1950). 19. K. Jain and A. S. Abhiraman...been generally mentioned much earlier by Franklin [17,18]. Jain and Abhiraman [19] demonstrated that these corrections can make significant differences

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

    Science.gov (United States)

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

    2016-10-01

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

  7. Ultrahigh vacuum/high pressure chamber for surface x-ray diffraction experiments

    Science.gov (United States)

    Bernard, P.; Peters, K.; Alvarez, J.; Ferrer, S.

    1999-02-01

    We describe an ultrahigh vacuum chamber that can be internally pressurized to several bars and that is designed to perform surface x-ray diffraction experiments on solid-gas interfaces. The chamber has a cylindrical beryllium window that serves as the entrance and exit for the x rays. The sample surface can be ion bombarded with an ancillary ion gun and annealed to 1200 K.

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

    Science.gov (United States)

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

    2016-05-01

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

  9. QUALITATIVE ANALYSIS OF A SERIE OF CEMENT BY X-RAY POWDER DIFFRACTION

    OpenAIRE

    Öztürk Yildirim, Sema; BULMUŞ, Tuğba

    2009-01-01

    Cement is now widely used in every aspect of daily life due to the development of technology and ecological consciousness. In this study, the qualitative analysis of a serie of cement samples were made by using X-ray powder diffraction. The powder diffraction patterns of samples were taken by using copper radiation [λ(CuKα) = 1.54056Å] at room temperature by the RIGAKU type D-MAX 220 model X-ray diffractometer. The data obtained from the powder diffraction patterns was evaluated and the subst...

  10. Nanosecond x-ray Laue diffraction apparatus suitable for laser shock compression experiments.

    Science.gov (United States)

    Suggit, Matthew; Kimminau, Giles; Hawreliak, James; Remington, Bruce; Park, Nigel; Wark, Justin

    2010-08-01

    We have used nanosecond bursts of x-rays emitted from a laser-produced plasma, comprised of a mixture of mid-Z elements, to produce a quasiwhite-light spectrum suitable for performing Laue diffraction from single crystals. The laser-produced plasma emits x-rays ranging in energy from 3 to in excess of 10 keV, and is sufficiently bright for single shot nanosecond diffraction patterns to be recorded. The geometry is suitable for the study of laser-shocked crystals, and single-shot diffraction patterns from both unshocked and shocked silicon crystals are presented.

  11. 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...... 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...

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

    Science.gov (United States)

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

    2014-03-01

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

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

    CERN Document Server

    Li, Zheng; Chapman, Henry; Shih, Yanhua

    2015-01-01

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

  14. 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 diffr

  15. 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 diffr

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

    OpenAIRE

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

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

    Science.gov (United States)

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

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

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

    Science.gov (United States)

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

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

  20. High-resolution X-ray diffraction imaging of non-Bragg diffracting materials using phase retrieval X-ray diffractometry (PRXRD) technique

    Energy Technology Data Exchange (ETDEWEB)

    Nikulin, A.Y.; Darahanau, A.V.; Horney, R.; Ishikawa, T

    2004-06-15

    An X-ray diffraction technique has recently been developed and successfully applied to comprehensively, including both phase and amplitude contrast, map the complex refractive index of non-crystalline materials with submicron spatial resolution. The methodology is based on the measurement of a high angular resolution X-ray Fraunhofer diffraction pattern with further application of the phase-retrieval formalism using a logarithmic dispersion relation. The technique is reviewed from the perspective of its ability to deliver ultra-high, order of several nanometres, spatial resolution and to uniquely determine both the real and imaginary components of the complex refractive index of the material under analysis. Potential niche of practical applications is discussed in terms of the spatial resolution and field of view achievable by the method.

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

    Science.gov (United States)

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

    2003-01-01

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

  2. 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 (< 30 nm) are discussed. It is shown that due to the complex structure, constituting a two-phase, core/surface shell system, no unique lattice parameter value and, consequently, no unique compressibility coefficient can satisfactorily describe the behavior of nanocrystalline powders under pressure. We offer a tentative interpretation of the distribution of macro- and micro-strains in nanoparticles of different grain size.

  3. Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

    Science.gov (United States)

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

    2014-04-01

    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 Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

  4. 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.

  5. Firing of Clays Studied by X-ray Diffraction and Moessbauer Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Haeusler, W. [Technische Universitaet Muenchen, Physik-Department E15 (Germany)

    2004-06-15

    Three bentonites of varying purity were fired in air under controlled conditions up to 1300{sup o}C in an attempt to provide data for the assessment of firing techniques used in prehistoric pottery making. X-ray diffraction of samples heated at increasing temperatures allows to study the mineral transformations, the breakdown of the clay structure and the formation of new minerals in the high-temperature region. Moessbauer spectroscopy reveals the change of valence state and of the environment of the iron atoms on heating. Non iron-bearing minerals are only accessible by X-ray diffraction, while iron-containing oxidic and amorphous phases may be difficult to detect, due to poor crystallinity and small particle size. The combination of X-ray diffraction and Moessbauer spectroscopy therefore has a considerable potential in the study of the chemical and physical transformations occurring in pottery clays during firing.

  6. Firing of Clays Studied by X-ray Diffraction and Mössbauer Spectroscopy

    Science.gov (United States)

    Häusler, W.

    2004-06-01

    Three bentonites of varying purity were fired in air under controlled conditions up to 1300°C in an attempt to provide data for the assessment of firing techniques used in prehistoric pottery making. X-ray diffraction of samples heated at increasing temperatures allows to study the mineral transformations, the breakdown of the clay structure and the formation of new minerals in the high-temperature region. Mössbauer spectroscopy reveals the change of valence state and of the environment of the iron atoms on heating. Non iron-bearing minerals are only accessible by X-ray diffraction, while iron-containing oxidic and amorphous phases may be difficult to detect, due to poor crystallinity and small particle size. The combination of X-ray diffraction and Mössbauer spectroscopy therefore has a considerable potential in the study of the chemical and physical transformations occurring in pottery clays during firing.

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

    Science.gov (United States)

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

    2009-08-03

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

  8. Long-Wavelength X-Ray Diffraction and Its Applications in Macromolecular Crystallography.

    Science.gov (United States)

    Weiss, Manfred S

    2017-01-01

    For many years, diffraction experiments in macromolecular crystallography at X-ray wavelengths longer than that of Cu-K α (1.54 Å) have been largely underappreciated. Effects caused by increased X-ray absorption result in the fact that these experiments are more difficult than the standard diffraction experiments at short wavelengths. However, due to the also increased anomalous scattering of many biologically relevant atoms, important additional structural information can be obtained. This information, in turn, can be used for phase determination, for substructure identification, in molecular replacement approaches, as well as in structure refinement. This chapter reviews the possibilities and the difficulties associated with such experiments, and it provides a short description of two macromolecular crystallography synchrotron beam lines dedicated to long-wavelength X-ray diffraction experiments.

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

    Science.gov (United States)

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

    2016-09-01

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

  10. 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.)

  11. In-laboratory diffraction-enhanced X-ray imaging for articular cartilage.

    Science.gov (United States)

    Muehleman, Carol; Fogarty, Daniel; Reinhart, Benjamin; Tzvetkov, Tochko; Li, Jun; Nesch, Ivan

    2010-07-01

    The loss of articular cartilage characteristic of osteoarthritis can only be diagnosed by joint space narrowing when conventional radiography is used. This is due to the lack of X-ray contrast of soft tissues. Whereas conventional radiography harnesses the X-ray attenuation properties of tissues, Diffraction Enhanced Imaging (DEI), a novel radiographic technique, allows the visualization of soft tissues simultaneous with calcified tissues by virtue of its ability to not only harness X-ray attenuation but also the X-ray refraction from tissue boundaries. Previously, DEI was dependent upon synchrotron X-rays, but more recently, the development of nonsynchrotron DEI units has been explored. These developments serve to elaborate the full potential of radiography. Here, we tested the potential of an in-laboratory DEI system, called Diffraction-Enhanced X-ray Imaging (DEXI), to render images of articular cartilage displaying varying degrees of degradation, ex vivo. DEXI allowed visualization of even early stages of cartilage degeneration such as surface fibrillation. This may be of eventual clinical significance for the diagnosis of early stages of degeneration, or at the very least, to visualize soft tissue degeneration simultaneous with bone changes.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-12-30

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

  13. Ultra-fast in-situ X-ray studies of evolving columnar dendrites in solidifying steel weld pools

    Science.gov (United States)

    Mirihanage, W. U.; Di Michiel, M.; Mathiesen, R. H.

    2015-06-01

    High-brilliance polychromatic synchrotron radiation has been used to conduct in-situ studies of the solidification microstructure evolution during simulated welding. The welding simulations were realized by rapidly fusing ∼ 5 mm spot in Fe-Cr-Ni steel. During the solid- liquid-solid phase transformations, a section of the weld pool was placed in an incident 50-150 keV polychromatic synchrotron X-ray beam, in a near-horizontal position at a very low inclination angle. Multiple high-resolution 2D detectors with very high frame rates were utilized to capture time resolved X-ray diffraction data from suitably oriented solid dendrites evolving in the weld pool. Comprehensive analysis of the diffraction data revealed individual and overall dendritic growth characteristics and relevant melt and solid flow dynamics during weld pool solidification, which was completed within 1.5 s. Columnar dendrite tip velocities were estimated from the experimental data and during early stages of solidification were exceeded 4 mm/s. The most remarkable observation revealed through the time-resolved reciprocal space observations are correlated to significant tilting of columnar type dendrites at their root during solidification, presumably caused by convective currents in the weld pool. When the columnar dendrite tilting are transformed to respective metric linear tilting velocities at the dendrite tip; tilting velocities are found to be in the same order of magnitude as the columnar tip growth velocities, suggesting a highly transient nature of growth conditions.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-10-19

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

  15. 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

  16. 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.

  17. Diffraction crystal for sagittally focusing x-rays

    Science.gov (United States)

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

    1984-01-01

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

  18. Diffraction crystals for sagittally focusing x-rays

    Science.gov (United States)

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

    1982-06-07

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

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

    Science.gov (United States)

    Marshall, J.; Keaten, R.

    1999-09-01

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

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

    Science.gov (United States)

    Marshall, J.; Keaten, R.

    1999-01-01

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

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

    CERN Document Server

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2010-01-01

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

  3. Phase Sensitive X-Ray Diffraction Imaging of Defects in Biological Macromolecular Crystals

    Science.gov (United States)

    Hu, Z. W.; Lai, B.; Chu, Y. S.; Cai, Z.; Mancini, D. C.; Thomas, B. R.; Chernov, A. A.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

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

    DEFF Research Database (Denmark)

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

    1998-01-01

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

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

    Science.gov (United States)

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

    2008-02-01

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

  7. X-ray fluorescence and energy dispersive x-ray diffraction for the quantification of elemental concentrations in breast tissue.

    Science.gov (United States)

    Geraki, K; Farquharson, M J; Bradley, D A

    2004-01-07

    This paper presents improvements on a previously reported method for the measurement of elements in breast tissue specimens (Geraki et al 2002 Phys. Med. Biol. 47 2327-39). A synchrotron-based system was used for the detection of the x-ray fluorescence (XRF) emitted from iron, copper, zinc and potassium in breast tissue specimens, healthy and cancerous. Calibration models resulting from the irradiation of standard aqueous solutions were used for the quantification of the elements. The present developments concentrate on increasing the convergence between the tissue samples and the calibration models, therefore improving accuracy. For this purpose the composition of the samples in terms of adipose and fibrous tissue was evaluated, using an energy dispersive x-ray diffraction (EDXRD) system. The relationships between the attenuation and scatter properties of the two tissue components and water were determined through Monte Carlo simulations. The results from the simulations and the EDXRD measurements allowed the XRF data from each specimen to be corrected according to its composition. The statistical analysis of the elemental concentrations of the different groups of specimens reveals that all four elements are found in elevated levels in the tumour specimens. The increase is less pronounced for iron and copper and most for potassium and zinc. Other observed features include the substantial degree of inhomogeneity of elemental distributions within the volume of the specimens, varying between 4% and 36% of the mean, depending on the element and the type of the sample. The accuracy of the technique, based on the measurement of a standard reference material, proved to be between 3% and 22% depending on the element, which presents only a marginal improvement (1%-3%) compared to the accuracy of the previously reported results. The measurement precision was between 1% and 9% while the calculated uncertainties on the final elemental concentrations ranged between 10% and 16%.

  8. X-ray diffraction in temporally and spatially resolved biomolecular science.

    Science.gov (United States)

    Helliwell, John R; Brink, Alice; Kaenket, Surasak; Starkey, Victoria Laurina; Tanley, Simon W M

    2015-01-01

    Time-resolved Laue protein crystallography at the European Synchrotron Radiation Facility (ESRF) opened up the field of sub-nanosecond protein crystal structure analyses. There are a limited number of such time-resolved studies in the literature. Why is this? The X-ray laser now gives us femtosecond (fs) duration pulses, typically 10 fs up to ∼50 fs. Their use is attractive for the fastest time-resolved protein crystallography studies. It has been proposed that single molecules could even be studied with the advantage of being able to measure X-ray diffraction from a 'crystal lattice free' single molecule, with or without temporal resolved structural changes. This is altogether very challenging R&D. So as to assist this effort we have undertaken studies of metal clusters that bind to proteins, both 'fresh' and after repeated X-ray irradiation to assess their X-ray-photo-dynamics, namely Ta6Br12, K2PtI6 and K2PtBr6 bound to a test protein, hen egg white lysozyme. These metal complexes have the major advantage of being very recognisable shapes (pseudo spherical or octahedral) and thereby offer a start to (probably very difficult) single molecule electron density map interpretations, both static and dynamic. A further approach is to investigate the X-ray laser beam diffraction strength of a well scattering nano-cluster; an example from nature being the iron containing ferritin. Electron crystallography and single particle electron microscopy imaging offers alternatives to X-ray structural studies; our structural studies of crustacyanin, a 320 kDa protein carotenoid complex, can be extended either by electron based techniques or with the X-ray laser representing a fascinating range of options. General outlook remarks concerning X-ray, electron and neutron macromolecular crystallography as well as 'NMR crystallography' conclude the article.

  9. X-Ray induced radiation damage in taurine: a combined X-ray diffraction and Raman study.

    Science.gov (United States)

    Beukes, J A; Mo, F; van Beek, W

    2007-09-07

    The impact of X-radiation on crystalline taurine has been investigated by time resolved synchrotron X-ray powder and single crystal diffraction and Raman spectroscopy. Multiple data sets have been collected at 120 and 296 K. All the observed effects of radiation, i.e. broadening and shifts of Raman and diffraction lines, a dose dependent irreversible increase in the atomic displacement parameters (ADPs) as well as in one of the unit-cell axes, and an apparent enhancement of electron density in the SO(3) group can be tentatively attributed to primary radical formation predominantly involving the SO(3) group. In secondary reactions molecular species that are distinct from taurine are created in minute quantities, thereby introducing local departure from crystalline order, i.e. enhanced static disorder and a build-up of local strain. Our study provides evidence for ascribing the linear increase in ADPs as well as the expansion of the c axis to the accumulation of foreign species in the crystal, and not to a thermal effect. Once initiated, this process appears to continue also without radiation, however, then at a much reduced rate.

  10. Structural Studies of Matrix Metalloproteinase by X-Ray Diffraction.

    Science.gov (United States)

    Decaneto, Elena; Lubitz, Wolfgang; Ogata, Hideaki

    2017-01-01

    Matrix Metalloproteinases (MMPs) are a family of proteolytic enzymes whose endopeptidase activity is dependent on the presence of specific metal ions. MT1-MMP (or MMP-14), which has been implicated in tumor progression and cellular invasion, contains a membrane-spanning region located C-terminal to a hemopexin-like domain and an N-terminal catalytic domain. We recombinantly expressed the catalytic domain of human MT1-MMP in E. coli and purified it from inclusion bodies using a refolding protocol that yielded significant quantities of active protein. Crystals of MT1-MMP were obtained using the vapour diffusion method. Here, we describe the protocols used for crystallization and the data analysis together with the resulting diffraction pattern.

  11. Confocal X-ray fluorescence spectrometer for in-situ analyses of paintings

    Science.gov (United States)

    Trojek, Tomáš; Prokeš, Radek; Šefců, Radka; Bilavčíková, Hana; Čechák, Tomáš

    2017-08-01

    This paper describes the properties of the newly constructed device for confocal X-ray fluorescence analysis that was tested with a sample plate consisting of 19 combinations of two single pigment layers. The preparation of this experimental wooden board with layered systems was based on knowledge of the panel painting techniques of Bohemian collections from the National Gallery in Prague dating back to the 14th and 15th centuries. The design of the confocal setup allows its transport and the in-situ measurement of paintings in depositories or even in exhibition areas. The advantages of our confocal setup with movable collimating optics are also described.

  12. XDS: a flexible beamline for X-ray diffraction and spectroscopy at the Brazilian synchrotron.

    Science.gov (United States)

    Lima, F A; Saleta, M E; Pagliuca, R J S; Eleotério, M A; Reis, R D; Fonseca Júnior, J; Meyer, B; Bittar, E M; Souza-Neto, N M; Granado, E

    2016-11-01

    The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage-ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X-ray spectrum (above ∼10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi-purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X-ray absorption spectroscopy at energies above 18 keV and high-resolution diffraction experiments. More recently, new setups and photon-hungry experiments such as total X-ray scattering, X-ray diffraction under high pressures, resonant X-ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    1999-01-01

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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    Science.gov (United States)

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

    2016-02-01

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

  17. MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTITATIVE X-RAY DIFFRACTION PHASE ANALYSIS

    Institute of Scientific and Technical Information of China (English)

    G. Chu; Y.F. Cong; H.J. You

    2003-01-01

    A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

  18. 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.

  19. 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.

  20. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-10-31

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed.

  1. 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.

  2. Spectrometer for Hard X-Ray Free Electron Laser Based on Diffraction Focusing

    CERN Document Server

    Kohn, V G; Vartanyants, I A

    2012-01-01

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

  3. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Elsaesser, T.; Woerner, M. [Max-Born-Institut für Nichtlineare Optik und Kurzzeitspektroskopie, 12489 Berlin (Germany)

    2014-01-14

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

  5. 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.

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

    Science.gov (United States)

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

    2014-10-01

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

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

    Science.gov (United States)

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

    2009-09-01

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

  8. In-situ assessment of metal contamination via portable X-ray fluorescence spectroscopy: Zlatna, Romania.

    Science.gov (United States)

    Weindorf, David C; Paulette, Laura; Man, Titus

    2013-11-01

    Zlatna, Romania is the site of longtime mining/smelting operations which have resulted in widespread metal pollution of the entire area. Previous studies have documented the contamination using traditional methods involving soil sample collection, digestion, and quantification via inductively coupled plasma atomic emission spectroscopy or atomic absorption. However, field portable X-ray fluorescence spectroscopy (PXRF) can accurately quantify contamination in-situ, in seconds. A PXRF spectrometer was used to scan 69 soil samples in Zlatna across multiple land use types. Each site was georeferenced with data inputted into a geographic information system for high resolution spatial interpolations. These models were laid over contemporary aerial imagery to evaluate the extent of pollution on an individual elemental basis. Pb, As, Co, Cu, and Cd exceeded governmental action limits in >50% of the sites scanned. The use of georeferenced PXRF data offers a powerful new tool for in-situ assessment of contaminated soils.

  9. High-resolution diffraction microscopy using the plane-wave field of a nearly diffraction limited focused x-ray beam

    OpenAIRE

    Takahashi, Yukio; Nishino, Yoshinori; Tsutsumi, Ryosuke; Kubo, Hideto; Furukawa, Hayato; Mimura, Hidekazu; MATSUYAMA, Satoshi; Zettsu, Nobuyuki; Matsubara, Eiichiro; Ishikawa, Tetsuya; Yamauchi, Kazuto

    2009-01-01

    X-ray waves in the center of the beam waist of nearly diffraction limited focused x-ray beams can be considered to have amplitude and phase that are both almost uniform, i.e., they are x-ray plane waves. Here we report the results of an experimental demonstration of high-resolution diffraction microscopy using the x-ray plane wave of the synchrotron x-ray beam focused using Kirkpatrik-Baez mirrors. A silver nanocube with an edge length of ∼100 nm is illuminated with the x-ray beam focused to ...

  10. High-energy X-ray diffraction using the Pixium 4700 flat-panel detector.

    Science.gov (United States)

    Daniels, J E; Drakopoulos, M

    2009-07-01

    The Pixium 4700 detector represents a significant step forward in detector technology for high-energy X-ray diffraction. The detector design is based on digital flat-panel technology, combining an amorphous Si panel with a CsI scintillator. The detector has a useful pixel array of 1910 x 2480 pixels with a pixel size of 154 microm x 154 microm, and thus it covers an effective area of 294 mm x 379 mm. Designed for medical imaging, the detector has good efficiency at high X-ray energies. Furthermore, it is capable of acquiring sequences of images at 7.5 frames per second in full image mode, and up to 60 frames per second in binned region of interest modes. Here, the basic properties of this detector applied to high-energy X-ray diffraction are presented. Quantitative comparisons with a widespread high-energy detector, the MAR345 image plate scanner, are shown. Other properties of the Pixium 4700 detector, including a narrow point-spread function and distortion-free image, allows for the acquisition of high-quality diffraction data at high X-ray energies. In addition, high frame rates and shutterless operation open new experimental possibilities. Also provided are the necessary data for the correction of images collected using the Pixium 4700 for diffraction purposes.

  11. Crystallization and preliminary X-ray diffraction of malate dehydrogenase from Plasmodium falciparum

    NARCIS (Netherlands)

    Wrenger, Carsten; Mueller, Ingrid B.; Butzloff, Sabine; Jordanova, Rositsa; Lunev, Sergey; Groves, Matthew R.

    2012-01-01

    The expression, purification, crystallization and preliminary X-ray diffraction characterization of malate dehydrogenase (MDH) from the malarial parasite Plasmodium falciparum (PfMDH) are reported. In order to gain a deeper understanding of the function and role of PfMDH, the protein was purified to

  12. 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 procedu...

  13. 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...

  14. High pressure behaviour of TbN: an X-ray diffraction and computational study

    DEFF Research Database (Denmark)

    Jakobsen, J.M.; Madsen, G.K.H.; Jorgensen, J.E.;

    2002-01-01

    In the present work, we report an X-ray powder diffraction study of TbN up to an applied hydrostatic pressure of 43 GPa. TbN was found to be stable in the 131 (NaCl structure) within the examined pressure interval, and the zero pressure bulk modulus was determined to be 176(7) GPa. The electronic...

  15. Determination of the Cu(110)-c(6X2)-O structure by x-ray diffraction

    DEFF Research Database (Denmark)

    Feidenhans'l, R.; Grey, F.; Johnson, R.L.

    1991-01-01

    We have performed a structural determination of the Cu(110)-c(6 X 2)-O surface by x-ray diffraction. A model including only copper atoms is found on the basis of the Patterson function; the positions of the oxygen atoms are revealed in an electron-density-difference map. The final structure has a...

  16. X-ray diffraction results from mars science laboratory: Mineralogy of rocknest at Gale crater

    NARCIS (Netherlands)

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

    2013-01-01

    The Mars Science Laboratory rover Curiosity scooped samples of soil from the Rocknest aeolian bedform in Gale crater. Analysis of the soil with the Chemistry and Mineralogy (CheMin) x-ray diffraction (XRD) instrument revealed plagioclase (~An57), forsteritic olivine (~Fo62), augite, and pigeonite, w

  17. Monolayers of CF4 Adsorbed on Graphite, Studied by Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Kjær, Kristian; Nielsen, Mourits; Bohr, Jakob;

    1982-01-01

    With synchrotron x-ray diffraction we have measured the phase diagram of CF4 monolayers adsorbed on the graphite substrate UCAR-ZYX. We have found four two-dimensional crystalline phases including the 2×2 commensurate structure. Between this and the denser incommensurate hexagonal phase we find...

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

    Science.gov (United States)

    Lucas, Amand A.

    2008-01-01

    A-DNA and B-DNA are two secondary molecular conformations (among other allomorphs) that double-stranded DNA drawn into a fiber can assume, depending on the relative water content and other chemical parameters of the fiber. They were the first two forms to be observed by X-ray fiber diffraction in the early 1950s, respectively by Wilkins and…

  19. 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...

  20. 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 penet....... © 2012 International Union of Crystallography Printed in Singapore-all rights reserved....

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

    Science.gov (United States)

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

    2010-12-01

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

  2. 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)

  3. 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 stack...

  4. 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...

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

    Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

    2007-01-01

    A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

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

    Science.gov (United States)

    Ohsumi, K. O.; Hagiya, K. H.; Zolensky, M. E.

    2002-01-01

    X-ray diffraction study revealed the existence of magnetite and new type of pyrrhotite with the chemical formula of Fe0.56S in L2005 AG17. Considering the total chemical formula of Fe0.83S, residual iron in amorphous state might exist in this sample. Additional information is contained in the original extended abstract.

  8. 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 the ...

  9. Structure Factors of Berly for the Use in Dynamical Diffraction Studies with X-rays

    OpenAIRE

    Yoshimura, Junichi; Okamura, Mitsuru; Taki, Sadao

    1985-01-01

    For the use in dynamical diffraction works with X-rays, structure factors corresponding to the real and imaginary parts, respectively, of atomic scattering factors were calculated for beryl (Be_3Al_2Si_6O_) from previously reported structural data.

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

    Science.gov (United States)

    Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

    2007-01-01

    A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

  11. High-pressure X-ray diffraction study of bulk- and nanocrystalline GaN

    DEFF Research Database (Denmark)

    Jorgensen, J.E.; Jakobsen, J.M.; Jiang, Jianzhong

    2003-01-01

    Bulk- and nanocrystalline GaN have been studied by high-pressure energy-dispersive X-ray diffraction. Pressure-induced structural phase transitions from the wurtzite to the NaCl phase were observed in both materials. The transition pressure was found to be 40 GPa for the bulk-crystalline GaN, while...

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

    Science.gov (United States)

    Lucas, Amand A.

    2008-01-01

    A-DNA and B-DNA are two secondary molecular conformations (among other allomorphs) that double-stranded DNA drawn into a fiber can assume, depending on the relative water content and other chemical parameters of the fiber. They were the first two forms to be observed by X-ray fiber diffraction in the early 1950s, respectively by Wilkins and…

  13. 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...

  14. 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...

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

    Science.gov (United States)

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

    2012-10-01

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

  16. X-ray and Electron Diffraction Study of MgO

    NARCIS (Netherlands)

    Tsirelson, V.G.; Asilov, A.S.; Abramov, Yu. A.; Belokoneva, E.L.; Kitaneh, R.; Feil, D.

    1998-01-01

    Precise X-ray and high-energy transmission electron diffraction methods were used for the study of electron density and electrostatic potential in MgO crystals. The structure amplitudes were determined and their accuracy estimated using ab initio Hartree-Fock structure amplitudes as criteria. The el

  17. 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 ...

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

    Science.gov (United States)

    Smither, Robert K.

    2011-05-17

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

  19. Microcavity arrays for X-ray diffraction studies of ordering phenomena in confined colloid solutions

    NARCIS (Netherlands)

    Diaz, A.; David, C.; Guo, H.; Keymeulen, H.; Pfeiffer, F.; Wegdam, G.; Weitkamp, T.; van der Veen, J.F.

    2005-01-01

    We present a way to fabricate high-aspect-ratio silicon microcavity arrays which can be used for the investigation of confinement-induced ordering phenomena within colloid solutions. In these studies, the microcavity arrays serve as containers for confinement of the colloid. X-ray diffraction measur

  20. X-ray powder diffraction data and unit cells of ammonium paratungstate tetrahydrate

    NARCIS (Netherlands)

    Put, J.W. van; Verkroost, T.W.; Sonneveld, E.J.

    1990-01-01

    X-Ray powder diffraction data and unit cell parameters of industrially produced, as well as bench scale prepared, ammonium paratungstate tetrahydrate are reported and compared with current Powder Data file (PDF) (1989) patterns. A least-squares refinement resulted in two slightly different unit cell

  1. Electrostatic Molecular Interaction from X-ray Diffraction Data. II. Test on Theoretical Pyrazine Data

    NARCIS (Netherlands)

    Feil, Dirk; Moss, Grant

    1983-01-01

    In a previous paper [Moss & Feil (1981). Acta Cryst. A37, 414-421] a method was reported to calculate the electrostatic potential and the electrostatic interaction energy from single-crystal X-ray diffraction data. The method was applied to experimental pyrazine data; however, owing to the relativel

  2. Origin of nondetectable x-ray diffraction peaks in nanocomposite CuTiZr alloys

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Kato, H.; Ohsuna, T.

    2003-01-01

    Microscopic structures of Cu60Ti10+xZr30-x (x=0 and 10) alloys have been investigated by transmission electron microscopy, x-ray diffraction (XRD) and differential scanning calorimeter (DSC). In the Cu60Ti10Zr30 samples annealed at 708 K for times ranging from 0 to 130 min, where the enthalpy of ...

  3. An X-ray diffraction study of direct-bonded silicon interfaces

    DEFF Research Database (Denmark)

    Howes, P.B.; Benamara, M.; Grey, F.

    1998-01-01

    Semiconductor wafer bonding techniques have been used to create a giant twist grain boundary from two Si(001) wafers. We show, using X-ray diffraction measurements that after annealing the interface forms a highly ordered superstructure with relaxations extending to many layers into the crystals...

  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...

  5. 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.

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

    Science.gov (United States)

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

    2016-08-01

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

  7. X-Ray and Neutron Diffraction Studies on Thermal Parameters of Thalous Bromide

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Thermal parameters of TIBr were determined using both X-ray and neutron diffraction techniques. The data was analysed by Rietveld profile refinement procedure. From the neutron diffraction data, due to weak odd-order reflections, it was not possible to determine the individual thermal parameters. The X-ray diffraction measurements yielded BT1=0.296(5) nm2 and BBr=0.162(5) nm2. The overall isotropic value, B was 0.252(7) nm2 which is in good agreement with B=0.230(8) nm2 obtained from present neutron diffraction measurements. The present values are also in good agreement with theoretical estimates obtained from the shell models.

  8. Twisted X-rays: incoming waveforms yielding discrete diffraction patterns for helical structures

    CERN Document Server

    Friesecke, Gero; Jüstel, Dominik

    2015-01-01

    Conventional X-ray methods use incoming plane waves and result in discrete diffraction patterns when scattered at crystals. Here we find, by a systematic method, incoming waveforms which exhibit discrete diffraction patterns when scattered at helical structures. As examples we present simulated diffraction patterns of carbon nanotubes and tobacco mosaic virus. The new incoming waveforms, which we call twisted waves due to their geometric shape, are found theoretically as closed-form solutions to Maxwell's equations. The theory of the ensuing diffraction patterns is developed in detail. A twisted analogue of the Von Laue condition is seen to hold, with the peak locations encoding the symmetry and the helix parameters, and the peak intensities indicating the electronic structure in the unit cell. If suitable twisted X-ray sources can in the future be realized experimentally, it appears from our mathematical results that they will provide a powerful tool for directly determining the detailed atomic structure of ...

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

    Science.gov (United States)

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

    1988-04-01

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

  10. Femtosecond powder diffraction with a laser-driven hard X-ray source.

    Science.gov (United States)

    Zamponi, F; Ansari, Z; Woerner, M; Elsaesser, T

    2010-01-18

    X-ray powder diffraction with a femtosecond time resolution is introduced to map ultrafast structural dynamics of polycrystalline condensed matter. Our pump-probe approach is based on photoexcitation of a powder sample with a femtosecond optical pulse and probing changes of its structure by diffracting a hard X-ray pulse generated in a laser-driven plasma source. We discuss the key aspects of this scheme including an analysis of detection sensitivity and angular resolution. Applying this technique to the prototype molecular material ammonium sulfate, up to 20 powder diffraction rings are recorded simultaneously with a time resolution of 100 fs. We describe how to derive transient charge density maps of the material from the extensive set of diffraction data in a quantitative way.

  11. 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 (La3Ga5SiO14) 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.

  12. Influence of anions on dealloying of Cu3Au (111): An in-situ x-ray study

    Energy Technology Data Exchange (ETDEWEB)

    Pareek, Aparna; Ankah, Genesis; Huemann, Sascha; Rohwerder, Michael; Renner, Frank [Max-Planck Institut fuer Eisenforschung, Max-Planck Strasse 1, 40237 Duesseldorf (Germany)

    2009-07-01

    Dealloying is a well-known process occurring at the alloy surfaces, which are composed of elements with widely different Nernst potentials. The dealloying behaviour of Cu3Au in 0.1M H2SO4 was previously investigated using electrochemical measurements combined with in-situ X-ray diffraction. We reported the formation of an ultra-thin epitaxial passive Au layer at lower overpotentials with a reversed stacking sequence, which transforms to thicker Au islands at higher overpotentials. Here we investigated the influence of various anionic species (Br, I) dissolved in 0.1M H2SO4 on the above electrochemical corrosion process. Presence of these anionic additives influences the potential where the ultra-thin passive layer transforms to the thicker Au islands. To corroborate the results obtained from X-ray measurements, ex-situ AFM measurements were performed, where the topographical changes with the potential change were recorded. In addition, we present first results of high resolution TEM studies.

  13. X-ray diffraction measurements for solid methane at high pressures

    CERN Document Server

    Umemoto, S; Akahama, Y; Kawamura, H

    2002-01-01

    X-ray powder diffraction and Raman scattering experiments for solid methane were carried out at pressures up to 37 GPa and room temperature. The diffraction pattern of phase B at 16.9 GPa is assigned to a cubic lattice with lattice constant of 7.914 A (B. At the transition from phase B to the HP phase, the pressure-volume curve shows an anomaly without the structural change.

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

    Indian Academy of Sciences (India)

    K K Pandey; H K Poswal; A K Mishra; Abhilash Dwivedi; R Vasanthi; Nandini Garg; Surinder M Sharma

    2013-04-01

    An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic powdered samples. A few recent high-pressure investigations are presented to demonstrate the capabilities of the beamline.

  15. An ultrahigh-vacuum chamber for surface X-ray diffraction combined with MBE

    Science.gov (United States)

    Vlieg, E.; Van't Ent, A.; De Jongh, A. P.; Neerings, H.; Van Der Veen, J. F.

    1987-12-01

    An ultrahigh-vacuum chamber has been built which can be coupled to a diffractometer via a rotary feedthrough. X-rays enter and leave the chamber through a large beryllium window. In addition to standard equipment for surface preparation and reflection high-energy electron diffraction, the chamber contains Knudsen evaporation cells for MBE crystal growth. This arrangement allows in situ diffraction experiments to be performed on growing surfaces and thin films.

  16. X-ray detectors for diffraction studies and their use with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    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.

  17. Quantitative x-ray diffraction phase analysis of coarse airborne particulate collected by cascade impactor sampling

    Science.gov (United States)

    Esteve, V.; Rius, J.; Ochando, L. E.; Amigó, J. M.

    Mineralogical composition of Castellon (Spanish Mediterranean coast) atmospheric aerosol was studied by X-ray diffraction by sampling with a cascade impactor without filters. Quantitative phase analysis of natural phases present in the atmospheric coarse aerosol was performed using a modified version of the computer program MENGE, that uses the standardless X-ray method developed by Rius for the quantitative analysis of multiphase mixtures, adapted for PC running. Presence of quartz, calcite and gypsum was identified in the atmospheric aerosol and we have quantified their amounts using the standardless method.

  18. Content analyses in GaMnAs by double-crystal X-ray diffraction

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A model for analyzing point defects in compound crystals was improved. Based on this modified model,a method for measuring Mn content in GaMnAs was established. A technique for eliminating the zero-drift-error was also established in the experiments of X-ray diffraction. With these methods, the Mn content in GaMnAs single crystals fabricated by the ion-beam epitaxy system was analyzed.Kevwords: GaMnAs, diluted magnetic semiconductor, X-ray dff fraction, lattice parameter, content of Mn.

  19. 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 approximately...... 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....

  20. Ultrafast coherent diffractive imaging of nanoparticles using X-ray free-electron laser radiation

    Energy Technology Data Exchange (ETDEWEB)

    Kassemeyer, Stephan

    2014-05-20

    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

  1. Composition variations in Cu{sub 2}ZnSnSe{sub 4} thin films analyzed by X-ray diffraction, energy dispersive X-ray spectroscopy, particle induced X-ray emission, photoluminescence, and Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Dahyun [Department of Physics, Sogang University, Seoul 121-742 (Korea, Republic of); Opanasyuk, A.S.; Koval, P.V.; Ponomarev, A.G. [Department of Electronics and Computer Technology, Sumy State University, Sumy UA-40007 (Ukraine); Jeong, Ah Reum; Kim, Gee Yeong; Jo, William [Department of Physics, Ewha Womans University, Seoul 120-750 (Korea, Republic of); Cheong, Hyeonsik, E-mail: hcheong@sogang.ac.kr [Department of Physics, Sogang University, Seoul 121-742 (Korea, Republic of)

    2014-07-01

    Compositional and structural studies of Cu{sub 2}ZnSnSe{sub 4} (CZTSe) thin films were carried out by X-ray diffraction, energy dispersive X-ray spectroscopy (EDS), particle induced X-ray emission (PIXE), photoluminescence, and Raman spectroscopy. CZTSe thin films with different compositions were deposited on sodalime glass by co-evaporation. The composition of the films measured by two different methods, EDS and PIXE, showed significant differences. Generally, the Zn/Sn ratio measured by EDS is larger than that measured by PIXE. Both the micro-PIXE and the micro-Raman imaging results indicated the compositional and structural inhomogeneity of the sample. - Highlights: • Particle induced X-ray emission was used to analyze the composition of CZTSe films. • Energy dispersive X-ray spectroscopy tends to underestimate the Sn composition. • Local Raman intensity is related with the composition rather than the crystallinity.

  2. Application of confocal technology based on polycapillary X-ray optics in three-dimensional diffraction scanning analysis

    Energy Technology Data Exchange (ETDEWEB)

    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); Liu, Hehe; Liu, Zhiguo; 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; Luo, Ping; 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)

    2014-03-15

    The confocal technology based on a polycapillary focusing X-ray lens in the excitation channel and a polycapillary parallel X-ray lens in the detection channel was used to perform three-dimensional energy dispersive X-ray diffraction scanning analysis of a copper film on a silicon substrate. A theoretical model of correcting the intensity of the diffracted X-rays from different parts of the sample in the confocal volume was designed. The point-to-point 3D diffraction information of the sample was obtained.

  3. Energy-windowed, pixellated X-ray diffraction using the Pixirad CdTe detector

    Science.gov (United States)

    O'Flynn, D.; Bellazzini, R.; Minuti, M.; Brez, A.; Pinchera, M.; Spandre, G.; Moss, R.; Speller, R. D.

    2017-01-01

    X-ray diffraction (XRD) is a powerful tool for material identification. In order to interpret XRD data, knowledge is required of the scattering angles and energies of X-rays which interact with the sample. By using a pixellated, energy-resolving detector, this knowledge can be gained when using a spectrum of unfiltered X-rays, and without the need to collimate the scattered radiation. Here we present results of XRD measurements taken with the Pixirad detector and a laboratory-based X-ray source. The cadmium telluride sensor allows energy windows to be selected, and the 62 μm pixel pitch enables accurate spatial information to be preserved for XRD measurements, in addition to the ability to take high resolution radiographic images. Diffraction data are presented for a variety of samples to demonstrate the capability of the technique for materials discrimination in laboratory, security and pharmaceutical environments. Distinct diffraction patterns were obtained, from which details on the molecular structures of the items under study were determined.

  4. A laboratory based system for Laue micro x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Advanced Light Source; Tamura, Nobumichi; Lynch, P.A.; Stevenson, A.W.; Liang, D.; Parry, D.; Wilkins, S.; Tamura, N.

    2007-02-28

    A laboratory diffraction system capable of illuminating individual grains in a polycrystalline matrix is described. Using a microfocus x-ray source equipped with a tungsten anode and prefigured monocapillary optic, a micro-x-ray diffraction system with a 10 mum beam was developed. The beam profile generated by the ellipsoidal capillary was determined using the"knife edge" approach. Measurement of the capillary performance, indicated a beam divergence of 14 mrad and a useable energy bandpass from 5.5 to 19 keV. Utilizing the polychromatic nature of the incident x-ray beam and application of the Laue indexing software package X-Ray Micro-Diffraction Analysis Software, the orientation and deviatoric strain of single grains in a polycrystalline material can be studied. To highlight the system potential the grain orientation and strain distribution of individual grains in a polycrystalline magnesium alloy (Mg 0.2 wt percent Nd) was mapped before and after tensile loading. A basal (0002) orientation was identified in the as-rolled annealed alloy; after tensile loading some grains were observed to undergo an orientation change of 30 degrees with respect to (0002). The applied uniaxial load was measured as an increase in the deviatoric tensile strain parallel to the load axis (37 References).

  5. Crystallization and X-ray diffraction data of Thermus flavus 5S rRNA helices

    Science.gov (United States)

    Vallazza, Marco; Senge, Andrea; Lippmann, Corinna; Perbandt, Markus; Betzel, Christian; Bald, Rolf; Erdmann, Volker A.

    2001-11-01

    5S rRNA is an essential component of the large ribosomal subunit in prokaryotes and eukaryotes. Its unknown function in the ribosome will eventually be revealed in part by structural studies. To promote crystallization and enhance resolution in X-ray diffraction the molecule was subdivided into five domains A-E. Several RNA oligonucleotides were chemically produced by solid-phase phosphoramidite synthesis in order to construct the domains of the 5S rRNA. An improved RNA-MPD-screen was applied in crystallization which covers a complete 2D matrix for the components used. Crystallization analysis resulted in preferred combinations of pH, polyamine, monovalent and divalent cations for short RNA molecules. Six types of crystals corresponding to the domains B, C and E of Thermus flavus 5S rRNA could be obtained which were suitable for X-ray diffraction. Four RNA helices consist of seven base pairs and two of eight base pairs. As special features, they contain two adenines in a bulge position or G : U wobble base pairs assumed to be involved in RNA-protein recognition. With an increase in crystal size an increase in resolution by X-ray analysis was observed. X-ray diffraction data were collected to 1.5 Å resolution using synchrotron radiation and cryogenic cooling techniques.

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

    Energy Technology Data Exchange (ETDEWEB)

    Kovalevsky, Andrey [Los Alamos National Laboratory (LANL); Erskine, Peter T. [University of Southampton, England; Cooper, Jon [University of Southampton, England

    2008-01-01

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

  7. A novel setup for time-resolved X-ray diffraction on gas gun experiments

    Science.gov (United States)

    Zucchini, Frédéric; Chauvin, Camille; Loyen, Arnaud; Combes, Philippe; Petit, Jacques; Bland, Simon

    2017-01-01

    Polymorphic phase transitions in metals have been investigated for a long time under dynamic loadings through usual dynamic compression diagnostics such as velocity and temperature measurements. Such measurements were valuable for revealing the key role of kinetic effects in most phase transition mechanisms. However, the information extracted was mostly macroscopic. Obtaining direct insight about the crystallographic structure under dynamic loadings is critical for understanding mechanisms governing shock-induced structural changes. For example, in order to evidence a mixture phase or to determine the time scale of a transition, structural information may be extremely valuable. Over the last 20 years a significant number of X-ray diffraction experiments were carried under dynamic loading, either using laboratory X-ray sources or synchrotron radiation. We are developing a novel experimental setup based on a compact High Pulsed Power generator capable of producing intense X radiation through an X-pinch X-ray source. This source is specifically designed for time-resolved X-ray diffraction in Bragg geometry on gas gun experiments. Promising preliminary diffraction data obtained under static conditions are presented.

  8. Thermal transport in thin films measured by time-resolved, grazing incidence x-ray diffraction.

    Energy Technology Data Exchange (ETDEWEB)

    Walko, D. A.; Sheu, Y.-M.; Trigo, M.; Reis, D. A. (X-Ray Science Division); (Univ. of Michigan,); (SLAC National Accelerator Lab.); (Stanford Univ.)

    2011-01-01

    We use depth- and time-resolved x-ray diffraction to study thermal transport across single crystal Bi films grown on sapphire in order to determine the thermal conductivity of the film and the Kapitza conductance of the interface. Ultrafast Ti:sapphire laser pulses were used to heat the films; x-ray diffraction then measured the film's lattice expansion. Use of grazing incidence diffraction geometry provided depth sensitivity, as the x-ray angle of incidence was varied near the critical angle. The shift of the film's Bragg peak position with time was used to determine the film temperature averaged over an x-ray penetration depth that could be selected by choice of the angle of incidence. For films that were thick compared to the laser penetration depth, we observed a large temperature gradient at early times. In this case, measurements with the incident angle near or well above the critical angle were more sensitive to the film conductivity or Kapitza conductance, respectively. For thinner films, however, cooling was dominated by the Kapitza conductance at all accessible time scales.

  9. 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.

  10. Development of synchrotron radiation as a high-intensity source for X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Huxley, H.E. [Brandeis Univ., Rosenstiel Center, Waltham, Massachusetts (United States); Holmes, K.C. [Max-Planck-Inst. fuer Medizinische Forschung, Heidelberg (Germany)

    1997-11-01

    Interest in the molecular mechanism of muscle contraction led to the search for an intense source of X-rays of 1-2 Aa wavelength so as to be able to examine the rich X-ray diffraction patterns given by muscles during contraction. This led to the first X-ray diffraction experiments using synchrotron radiation, carried out by Holmes, Rosenbaum and Witz at DESY, Hamburg, in September 1970. In the following years, the EMBL Outstation, to utilize synchrotron radiation for biological structure determination, was established at DESY and preliminary experiments on muscle were also carried out at NINA (Daresbury). The development of time-resolved techniques for muscle diffraction was first started in the MRC Molecular Biology Laboratory in Cambridge, using rotating-anode X-ray tubes, and was then greatly extended at the EMBL Outstation, Hamburg, using the storage ring DORIS. This was a very successful venture, and helped to drive the whole technology development and to interest other potential users in the technique. (au).

  11. 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.

  12. Heterodyne-Detected Ultrafast X-Ray Diffraction and Scattering from Nonstationary States

    CERN Document Server

    Bennett, Kochise; Mukamel, Shaul

    2016-01-01

    Free-electron laser hard X-ray light sources can provide high fluence, femtosecond pulses, enabling the time-resolved probing of structural dynamics and elementary relaxation processes in molecules. Traditional X-ray elastic scattering from crystals in the ground state consists of sharp Bragg diffraction peaks that arise from pairs of molecules and reveal the ground state charge density. Scattering of ultrashort X-ray pulses from gases, liquids, and even single molecules is more complex and involves both single- and two- molecule contributions, diffuse (non-Bragg) features, elastic and inelastic components, contributions of electronic coherences in nonstationary states, and interferences between scattering off different states (heterodyne detection). We present a unified description that covers all these processes and discuss their relative magnitudes for gas-phase NaI. Conditions for the observation of holographic (heterodyne) interference, which has been recently discussed [1], are clarified.

  13. Double-slit dynamical diffraction of X-rays in ideal crystals (Laue case).

    Science.gov (United States)

    Balyan, Minas K

    2010-11-01

    The theoretical investigation of double-slit dynamical X-ray diffraction in ideal crystals shows that, on the exit surface of crystals, interference fringes similar to Young's fringes are formed. An expression for the period of the fringes was obtained. The visibility of the fringes depending on temporal and spatial coherent properties of the incident beam is studied. The polarization state of the incident beam also affects the visibility of the fringes, which in turn depends on the size of the slits. The deviation from Bragg's exact angle causes a shift of the fringes and can also affect the amplitude of the intensity. One of the parameters on which the visibility of the fringes depends is the source-crystal distance. The proposed scheme can be used as a Rayleigh X-ray interferometer. Use of the scheme as a Michelson X-ray stellar interferometer is also possible.

  14. Imaging of Biological Materials and Cells by X-ray Scattering and Diffraction.

    Science.gov (United States)

    Hémonnot, Clément Y J; Köster, Sarah

    2017-09-26

    Cells and biological materials are large objects in comparison to the size of internal components such as organelles and proteins. An understanding of the functions of these nanoscale elements is key to elucidating cellular function. In this review, we describe the advances in X-ray scattering and diffraction techniques for imaging biological systems at the nanoscale. We present a number of principal technological advances in X-ray optics and development of sample environments. We identify radiation damage as one of the most severe challenges in the field, thus rendering the dose an important parameter when putting different X-ray methods in perspective. Furthermore, we describe different successful approaches, including scanning and full-field techniques, along with prominent examples. Finally, we present a few recent studies that combined several techniques in one experiment in order to collect highly complementary data for a multidimensional sample characterization.

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

    Energy Technology Data Exchange (ETDEWEB)

    Malinovschi, V. [University of Pitesti, Research Center for Advanced Materials, Targul din Vale Street, No.1, 110040 Pitesti, Arges (Romania)]. E-mail: malinov@electra.upit.ro; Ducu, C. [University of Pitesti, Research Center for Advanced Materials, Targul din Vale Street, No.1, 110040 Pitesti, Arges (Romania); Aldea, N. [National Institutes for Research and Development for Isotopic and Molecular Technologies, P.O. Box 700, 3400 Cluj-Napoca (Romania); Fulger, M. [Institutes for Nuclear Research, P.O. Box 0402, 0300 Pitesti (Romania)

    2006-06-30

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vekemans, Bart [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Verhaeven, Eddy [Antwerp University, Faculty of Design Sciences, Mutsaardstraat 31, B-2000 Antwerpen (Belgium); Tack, Pieter; De Wolf, Robin; Garrevoet, Jan [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium)

    2015-08-01

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

  17. The structure of liquid semiconductors, superionic conductors and glasses by neutron scattering, X-ray diffraction and extended X-ray absorption fine structure

    CERN Document Server

    Buchanan, P

    2001-01-01

    NDIS technique alone. The structure of liquid FeTe sub 2 was determined at the total structure factor level using neutron diffraction in order to estimate the effect of chalcogenide ion size on the structure. The results demonstrate the feasibility of the additional structural determination techniques for disordered materials made possible through the development of third generation X-ray synchrotron sources. A study of the applicability of modern X-ray and neutron scattering techniques to the study of the structure of liquid semiconductors and glasses has been made. The results demonstrate how neutron scattering with isotopic substitution (NDIS), anomalous X-ray scattering and Extended X-ray Absorption Fine Structure (EXAFS) can be successfully used to elucidate the structure of materials that cannot be studied by NDIS alone. The local coordination structure of Ag sub 2 Se in its room temperature, superionic and liquid phases has been determined using the EXAFS technique. This EXAFS data have been combined w...

  18. 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.

  19. 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.

  20. Slow scan sit detector for x-ray diffraction studies using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Milch, J R

    1978-10-18

    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/sup 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.

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

    Science.gov (United States)

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

    2000-01-01

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

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

    DEFF Research Database (Denmark)

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

    2014-01-01

    X-ray diffraction is a superior technique for structural characterization of crystalline matter. Here we review the use of in situ powder X-ray diffraction (PXD) mainly for real-time studies of solid/gas reactions, data analysis and the extraction of valuable knowledge of structural, chemical...... and physical properties. Furthermore, the diffraction data may also provide knowledge on reaction mechanisms, kinetics and thermodynamic properties. Thus, in situ PXD simultaneously provides properties as a function of pressure, temperature and/or time at different length scales, i.e. nanoscale structural data...... and bulk sample properties. Initially, a brief description of experimental and methodological details is provided, followed by a variety of examples of different designs of experiments and methods of data analysis. Additionally, it is discussed how a range of physical properties can be accessed...

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

    Science.gov (United States)

    Ferguson, Milton W.

    1994-01-01

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

  4. 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 t

  5. 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...

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2014-07-17

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. © 2014 The Author(s) Published by the Royal Society. All rights reserved.

  8. Application of Cryo-SEM Microscopy and In-situ X-ray Diffraction for the Investigation of Building Material Hydration%低温SEM和原位XRD技术在建筑材料水化中的应用研究

    Institute of Scientific and Technical Information of China (English)

    Herbert P(o)llmann

    2011-01-01

    New methods and improved techniques are increasingly used for better investigation of hydration reactions and also for testing of properties This paper describes the use and application of cryo-microscopy, in-situ X-ray technology and calorimetry for investigation of hydration reactions of cements and building materials.%为更好地研究水泥水化反应及测试其性能,需应用新的方法和改良技术.阐述了应用低温SEM和原位XRD技术及量热学研究水泥和建筑材料的新方法.

  9. Study of transmission grating diffraction efficiencies for soft X-ray

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    Tansmission grating spectrometers are extensively used tomeasure absolute X-ray spectra in a photon-energy rangebelow 1000 eV. The transmission grating, as its dispersive element, must be calibrated to obtain its diffraction efficiencies.Calibrations of absolute diffraction efficiencies of the transmissiongrating at photon energy of 844 eV have been carried out onBeijing Synchrotron Radiation Facility. With the aid of gratingmodel, all of the grating structure parameters have been determinedand the absolute diffraction efficiencies in a photon-energy rangebelow 2000 eV have also been calculated and discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

    McGonegle, David, E-mail: d.mcgonegle1@physics.ox.ac.uk; Wark, Justin S.; Higginbotham, Andrew [Department of Physics, Clarendon Laboratory University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Milathianaki, Despina [Linac Coherent Light Source, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Remington, Bruce A. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States)

    2015-08-14

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

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

    Directory of Open Access Journals (Sweden)

    E. Han Dao

    2015-07-01

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

  12. 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)

  13. 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)

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

    Science.gov (United States)

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

    2013-01-01

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

  15. In-situ x-ray characterization of wurtzite formation in GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Krogstrup, Peter; Hannibal Madsen, Morten; Nygaard, Jesper; Feidenhans' l, Robert [Nano-Science Center, Niels Bohr Institute, University of Copenhagen, Copenhagen (Denmark); Hu Wen [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); Kozu, Miwa; Nakata, Yuka [University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan); Takahasi, Masamitu [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan)

    2012-02-27

    In-situ monitoring of the crystal structure formation during Ga-assisted GaAs nanowire growth on Si(111) substrates has been performed in a combined molecular beam epitaxy growth and x-ray characterization experiment. Under Ga rich conditions, we show that an increase in the V/III ratio increases the formation rate of the wurtzite structure. Moreover, the response time for changes in the structural phase formation to changes in the beam fluxes is observed to be much longer than predicted time scales of adatom kinetics and liquid diffusion. This suggests that the morphology of the growth interface plays the key role for the relative growth structure formation rates.

  16. Bayesian orientation estimate and structure information from sparse single-molecule x-ray diffraction images.

    Science.gov (United States)

    Walczak, Michał; Grubmüller, Helmut

    2014-08-01

    We developed a Bayesian method to extract macromolecular structure information from sparse single-molecule x-ray free-electron laser diffraction images. The method addresses two possible scenarios. First, using a "seed" structural model, the molecular orientation is determined for each of the provided diffraction images, which are then averaged in three-dimensional reciprocal space. Subsequently, the real space electron density is determined using a relaxed averaged alternating reflections algorithm. In the second approach, the probability that the "seed" model fits to the given set of diffraction images as a whole is determined and used to distinguish between proposed structures. We show that for a given x-ray intensity, unexpectedly, the achievable resolution increases with molecular mass such that structure determination should be more challenging for small molecules than for larger ones. For a sufficiently large number of recorded photons (>200) per diffraction image an M^{1/6} scaling is seen. Using synthetic diffraction data for a small glutathione molecule as a challenging test case, successful determination of electron density was demonstrated for 20000 diffraction patterns with random orientations and an average of 82 elastically scattered and recorded photons per image, also in the presence of up to 50% background noise. The second scenario is exemplified and assessed for three biomolecules of different sizes. In all cases, determining the probability of a structure given set of diffraction patterns allowed successful discrimination between different conformations of the test molecules. A structure model of the glutathione tripeptide was refined in a Monte Carlo simulation from a random starting conformation. Further, effective distinguishing between three differently arranged immunoglobulin domains of a titin molecule and also different states of a ribosome in a tRNA translocation process was demonstrated. These results show that the proposed method is

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

    Science.gov (United States)

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

    2012-01-01

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

  18. Direct observation of bi-alkali antimonide photocathodes growth via in operando x-ray diffraction studies

    Directory of Open Access Journals (Sweden)

    M. Ruiz-Osés

    2014-12-01

    Full Text Available Alkali antimonides have a long history as visible-light-sensitive photocathodes. This work focuses on the process of fabrication of the bi-alkali photocathodes, K2CsSb. In-situ synchrotron x-ray diffraction and photoresponse measurements were used to monitor phase evolution during sequential photocathode growth mode on Si(100 substrates. The amorphous-to-crystalline transition for the initial antimony layer was observed at a film thickness of 40 Å . The antimony crystalline structure dissolved upon potassium deposition, eventually recrystallizing upon further deposition into K-Sb crystalline modifications. This transition, as well as the conversion of potassium antimonide to K2CsSb upon cesium deposition, is correlated with changes in the quantum efficiency.

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

    Science.gov (United States)

    De Caro, Liberato; Jark, Werner

    2008-03-01

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

  20. X-ray diffraction and Raman studies on Ho: Eu2O3

    Science.gov (United States)

    Irshad, K. A.; Chandra Shekar, N. V.; Ravindran, T. R.; Srihari, V.; Pandey, K. K.

    2017-01-01

    In this paper the structural parameters of mixed rare earth sesquioxides (Eu1-xHox)2O3 (0 ≤ x ≤ 1) is reported for the first time. The oxide samples are characterized by angle dispersive X-ray diffraction (ADXRD) and Raman scattering techniques. ADXRD measurements confirmed the formation of single phase in the cubic bixbyite structure with space group Ia-3. Complete miscibility of the two components is confirmed by the Vegard's law. A random distribution of the two cations in the two rare earth (RE) ion sites is observed. Symmetry modes are assigned for the observed 13 out of 22 expected Raman bands and the dependency of average cationic radii, RRE, is discussed. A low frequency band shows an anomalous mode softening with decrease in Eu content. This mode disappears above x = 0.8, which coincides with a distinct slope change observed in the RE(24d) positional coordinate estimated from refined x-ray diffraction data.

  1. Microfibril angle variability in Masson Pine (Pinus massoniana Lamb.) using X-ray diffraction

    Institute of Scientific and Technical Information of China (English)

    Zhang Bo; Fei Ben-hua; Yu Yan; Zhao Rong-jun

    2007-01-01

    The microfibril angle of fiber walls is an ultra-microscopic feature affecting the performance of wood products. It is therefore essential to get more definitive information to improve selection and utilization. X-ray diffraction is a rapid method for measuring micro fibril angles. In this paper, the variability of microfibril angle in plantation-grown Masson pine was investigated by peak-fitting method. This method was compared with the traditional hand-drawn method, 40% peak height method and half peak height method. X-ray diffraction measurements indicated that the microfibril angle changed as a function of the position in the tree.The mean micro fibril angle decreased more gradually as the distance increased from the pith and reached the same level in mature wood. The microfibril angle also seemed to decrease clearly from the base upward. Differences of angle-intensity curves between heartwood and sapwood were also examined.

  2. Synchrotron radiation X-ray powder diffraction techniques applied in hydrogen storage materials - A review

    Directory of Open Access Journals (Sweden)

    Honghui Cheng

    2017-02-01

    Full Text Available Synchrotron radiation is an advanced collimated light source with high intensity. It has particular advantages in structural characterization of materials on the atomic or molecular scale. Synchrotron radiation X-ray powder diffraction (SR-XRPD has been successfully exploited to various areas of hydrogen storage materials. In the paper, we will give a brief introduction on hydrogen storage materials, X-ray powder diffraction (XRPD, and synchrotron radiation light source. The applications of ex situ and in situ time-resolved SR-XRPD in hydrogen storage materials, are reviewed in detail. Future trends and proposals in the applications of the advanced XRPD techniques in hydrogen storage materials are also discussed.

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    Daniel Schick

    2014-11-01

    Full Text Available Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates.

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

    DEFF Research Database (Denmark)

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

    2012-01-01

    High-throughput crystallisation and characterisation platforms provide an efficient means to carry out solid-form screening during the pre-formulation phase. To determine the crystal structures of identified new solid phases, however, usually requires independent crystallisation trials to produce...... single crystals or bulk samples of sufficient quantity to carry out high-quality X-ray diffraction measurements. This process could be made more efficient by a robust procedure for crystal structure determination directly from high-throughput X-ray powder diffraction (XRPD) data. Quantum......-chemical calculations based on dispersion-corrected density functional theory (DFT-D) have now become feasible for typical small organic molecules used as active pharmaceutical ingredients. We demonstrate how these calculations can be applied to complement high-throughput XRPD data by determining the crystal structure...

  6. Introduction to Advanced X-ray Diffraction Techniques for Polymeric Thin Films

    Directory of Open Access Journals (Sweden)

    Nicodemus Edwin Widjonarko

    2016-11-01

    Full Text Available X-ray diffraction has been a standard technique for investigating structural properties of materials. However, most common applications in the organic materials community have been restricted to either chemical identification or qualitative strain analysis. Moreover, its use for polymeric thin films has been challenging because of the low structure factor of carbon and the thin film nature of the sample. Here, we provide a short review of advanced X-ray diffraction (XRD techniques suitable for polymeric thin films, including the type of analysis that can be done and measurement geometries that would compensate low signals due to low carbon structure factor and the thin film nature of the sample. We will also briefly cover the χ -pole figure for texture analysis of ultra-thin film that has recently become commonly used. A brief review of XRD theory is also presented.

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

    Science.gov (United States)

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

    2016-01-01

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

  8. In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization

    Science.gov (United States)

    Yano, Yohko F.; Douguchi, Junya; Kumagai, Atsushi; Iijima, Takao; Tomida, Yukinobu; Miyamoto, Toshiaki; Matsuura, Kazuo

    2006-11-01

    In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20mol% ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist.

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

    DEFF Research Database (Denmark)

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

    1999-01-01

    The structural phase transition from the hexagonal to a distorted-hexagonal (centered rectangular) phase (the LS-S transition) in Langmuir monolayers of octadecanol is studied in a grazing incidence x-ray diffraction experiment. We find algebraic decay of positional correlations, which suggests...... solid-like order in both phases at the distances accessible in the present x-ray diffraction experiment. The transition is accompanied by strong positional disorder, which is evident from the drastic increase of the exponent eta to values eta>2 close to the transition. Remarkably, on approaching...... the transition, the continuous increase of eta is apparent already at 20 degrees C above it. The positional disorder is attributed to elastic distortions around pretransitional fluctuations. [S1063-651X(99)10102-8]....

  10. 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.

  11. Modelling studies of carbon nanotubes-Comparison of simulations and X-ray diffraction data

    Energy Technology Data Exchange (ETDEWEB)

    Koloczek, J. [A. Chelkowski Institute of Physics, University of Silesia, ul. Uniwersytecka 4, 40-007 Katowice (Poland); Hawelek, L. [A. Chelkowski Institute of Physics, University of Silesia, ul. Uniwersytecka 4, 40-007 Katowice (Poland); Burian, A. [A. Chelkowski Institute of Physics, University of Silesia, ul. Uniwersytecka 4, 40-007 Katowice (Poland)]. E-mail: burian@us.edu.pl; Dore, J.C. [School of Physical Sciences, University of Kent, Canterbury CT2 7NR (United Kingdom); Honkimaeki, V. [European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble (France); Kyotani, T. [Institute of Multidisciplinary Research and Advanced Materials, Tohoku University, Katahira, Sendai 980-8577 (Japan)

    2005-09-29

    Computer simulations of the powder diffraction profiles for multi-wall carbon nanotubes were performed using the Debye equation including a generalized Debye-Waller factor. The X-ray diffraction data were recorded using high-energy synchrotron radiation and an image plate as a detector for the carbon nanotubes produced by a template chemical vapour deposition (CVD) process. The computed and experimental structure factors were converted to real-space via the Fourier transform. The results of computation, obtained in the form of the structure factor and the pair correlation function, are compared with the X-ray experimental data in both reciprocal and real-space. The nanotube model consisting of five layers with the length of 12 A has proved to account very well for the experimental data.

  12. 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.

  13. 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

  14. Secondary Extinction in Cylindrical and Spherical Crystals for X-Ray and Neutron Diffraction

    Institute of Scientific and Technical Information of China (English)

    胡华琛; 李兆桓; 杨斌; 沈彩万; 乔英

    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.

  15. 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

  16. 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.

  17. Structural instability of EuTiO3 from X-ray powder diffraction

    OpenAIRE

    Köhler, J; Dinnebier, R.; Bussmann-Holder, A.

    2012-01-01

    We have recently predicted and subsequently verified experimentally by specific heat measurements that EuTiO3 undergoes a structural phase transition at elevated temperature TS = 282 K. The origin of the phase transition has been attributed to the softening of a transverse acoustic mode stemming from an oxygen octahedral rotation analogous to SrTiO3. Here we demonstrate that the theoretical interpretation is correct by using high resolution laboratory X-ray powder diffraction which evidences ...

  18. The application of a novel detector for X-ray diffraction study of breast cancer

    OpenAIRE

    Zheng, Y.

    2016-01-01

    Current imaging methods - mammography, digital breast tomosynthesis, ultrasound and magnetic resonance images (MRI), fail to provide an accurate breast tumour size measurement. X-ray diffraction (XRD) can provide better contrast than mammography and digital breast tomosynthesis, better spatial resolution than ultrasound and is more cost effective than MRI. However, its use is limited by high radiation dose. Previous breast XRD research often fails to investigate samples with a realistic thick...

  19. Structural studies of BSCCO/Ag-tapes by high-energy synchrotron X-ray diffraction

    DEFF Research Database (Denmark)

    Poulsen, H.F.; Frello, T.; Andersen, N.H.

    1998-01-01

    High-energy (100 keV) synchrotron X-ray diffraction has been identified as a powerful tool for characterizing texture and structural phases,within Ag clad high T-c, superconducting tapes of the (Bi,Pb)-Sr-Ca-Cu-O (BSSCO) type during synthesis of (Bi,Pb)(2)Sr2Ca2Cu3Ox (Bi-2223) from (Bi,Pb)(2)Sr2CaCu...

  20. In-lab X-ray fluorescence and diffraction techniques for pathological calcifications

    OpenAIRE

    Rouzière, Stéphan; Bazin, Dominique; Daudon, Michel

    2016-01-01

    International audience; If imaging by physical methods is probably the best well-known link between physics and medicine, other ways such as X-ray fluorescence and diffraction techniques give significant information to clinicians. In this contribution, we would like to assess different results obtained through such techniques on three main problems in urology namely Randall's plaque, brushite kidney stones and phase conversion between weddellite and whewellite. Randall's plaque is a mineral d...

  1. Nitrogen-gas-stream cryostat for general X-ray diffraction studies

    Energy Technology Data Exchange (ETDEWEB)

    Cosier, J.; Glazer, A.M.

    1986-04-01

    A continuous nitrogen-flow cooling device, generally applicable to X-ray diffraction studies, is described. The device works in the range 77.4 to 323.0 K with a precision of +-0.1 K and a liquid-nitrogen constant consumption rate of 0.5 l h/sup -1/ over the whole temperature range. The supply vessel is unpressurised, so that refilling can be done without any observable influence on the cooling of the sample.

  2. Guiding synchrotron X-ray diffraction by multimodal video-rate protein crystal imaging

    OpenAIRE

    Newman, Justin A.; ZHANG, Shijie; Sullivan, Shane Z.; Dow, Ximeng Y.; Becker, Michael; Sheedlo, Michael J.; Stepanov, Sergey; Carlsen, Mark S.; Everly, R. Michael; Das, Chittaranjan; Fischetti, Robert F.; Simpson, Garth J.

    2016-01-01

    Synchronous digitization, in which an optical sensor is probed synchronously with the firing of an ultrafast laser, was integrated into an optical imaging station for macromolecular crystal positioning prior to synchrotron X-ray diffraction. Using the synchronous digitization instrument, second-harmonic generation, two-photon-excited fluorescence, one-photon-excited fluorescence, two-photon-excited ultraviolet fluorescence and bright field by laser transmittance were all acquired with perfect...

  3. Analysis of diatomite sediments from a paleolake in central Mexico using PIXE, X-ray tomography and X-ray diffraction

    Science.gov (United States)

    Miranda, J.; Oliver, A.; Vilaclara, G.; Rico-Montiel, R.; Macías, V. M.; Ruvalcaba, J. L.; Zenteno, M. A.

    1994-03-01

    Diatomite samples from paleolake Tlaxcala, in Central Mexico, have been analyzed using proton induced X-ray emission (PIXE), X-ray tomography and X-ray diffraction. Chiseled blocks were scanned with a 0.7 MeV proton beam, 0.1 mm in diameter, in 0.25 mm steps across the sediments. X-ray tomography with the same step sizes was then applied, in order to compare the concentrations obtained with PIXE and the material density in the sediment layers. Three different kinds of layers were found, related to their colors: dark, white and gray. The composition of the layers is fairly uniform. The dark zone is enriched in Al, K, Ca, Ti, Mn, and Fe. This dark layer may be associated with eruptions of the Malitzin volcano. The white zone is found to contain diatomite of a high purity, with traces of K, Ca, and Fe, while the gray zones are also Al enriched, suggesting a clay contamination of the diatomite. X-ray diffraction of materials obtained from each main layer showed that the white and gray phases are highly amorphous, with a small component of cristobalite, as expected from the diatom sediment diagenesis, while the dark layer contains also important amounts of anorthite and orthoclase, supporting the volcanic origin of this layer.

  4. Advancements in X-ray waveguides and their applications in coherent diffraction imaging

    Energy Technology Data Exchange (ETDEWEB)

    Pelliccia, D. [Institut fuer Synchrotronstrahlung-ANKA Forschungszentrum Karlsruhe Herman-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen (Germany)], E-mail: daniele.pelliccia@iss.fzk.de; Bukreeva, I. [Istituto di Fotonica e Nanotecnologie-CNR, Via Cineto Romano 42, 00156 Roma (Italy); Giannini, C.; De Caro, L. [Istituto di Cristallografia-CNR, Via Amendola 122/O, 70126 Bari (Italy); Cedola, A.; Scarinci, F.; Lagomarsino, S. [Istituto di Fotonica e Nanotecnologie-CNR, Via Cineto Romano 42, 00156 Roma (Italy)

    2009-10-15

    X-ray planar waveguides are currently used tools, in synchrotron radiation facilities, to produce a coherent beam with typical dimensions in the range of tens or hundreds of nanometers. The properties of waveguided beams such as divergence and coherence turns out to be very interesting for several applications both in synchrotron and in laboratory sources. These features will be reviewed in the present paper for different coupling methods of the radiation field with the waveguide channel. Details of fabrication procedures and experimental results concerning front coupling waveguide are reported. The waveguide properties can be estimated from the far-field diffracted beam by a Fourier analysis giving the autocorrelation function of the exit field. Due to the high degree of coherence of the exiting beam, X-ray waveguides can be successfully exploited in coherent diffraction imaging experiments. We review results concerning Fresnel coherent diffraction imaging experiments with hard X-rays, using planar waveguides as optical elements in one and two dimensions.

  5. Femtosecond Diffractive Imaging with a Soft-X-Ray Free-Electron Laser

    Energy Technology Data Exchange (ETDEWEB)

    Chapman, Henry N.; /LLNL, Livermore /UC, Davis; Barty, Anton: AUTHOR = Bogan, Michael J.; /LLNL, Livermore; Boutet, Sebastian; /LLNL, Livermore /SLAC /Uppsala U., Biomed. Ctr.; Frank, Matthias; Hau-Riege, Stefan P.; /LLNL, Livermore; Marchesini, Stefano; /LLNL, Livermore /UC, Davis; Woods, Bruce W.; Bajt, Sasa; Benner, W.Henry; /LLNL, Livermore; London, Richard A.; /LLNL, Livermore /UC, Davis; Plonjes, Elke; Kuhlmann, Marion; Treusch, Rolf; Dusterer, Stefan; Tschentscher, Thomas; Schneider, Jochen R.; /CERN; Spiller, Eberhard; /Spiller X-ray Optics, Livermore; Moller, Thomas; Bostedt, Christoph; Hoener, Matthias; /Berlin, Tech. U.; Shapiro, David A.; /UC, Davis /SLAC /Uppsala U. /LLNL, Livermore /Uppsala U. /Uppsala U. /SLAC /Uppsala U.

    2010-10-07

    Theory predicts that with an ultrashort and extremely bright coherent X-ray pulse, a single diffraction pattern may be recorded from a large macromolecule, a virus, or a cell before the sample explodes and turns into a plasma. Here we report the first experimental demonstration of this principle using the FLASH soft X-ray free-electron laser. An intense 25 fs, 4 x 10{sup 13} W/cm{sup 2} pulse, containing 10{sup 12} photons at 32 nm wavelength, produced a coherent diffraction pattern from a nano-structured non-periodic object, before destroying it at 60,000 K. A novel X-ray camera assured single photon detection sensitivity by filtering out parasitic scattering and plasma radiation. The reconstructed image, obtained directly from the coherent pattern by phase retrieval through oversampling, shows no measurable damage, and extends to diffraction-limited resolution. A three-dimensional data set may be assembled from such images when copies of a reproducible sample are exposed to the beam one by one.

  6. Study of microstructure in vanadium–palladium alloys by X-ray diffraction technique

    Indian Academy of Sciences (India)

    J Ghosh; S K Chattopadhyay; A K Meikap; S K Chatterjee; P Chatterjee

    2007-10-01

    Present study considers microstructural characterization of vanadium-based palladium (V–Pd) alloys, which are widely used in marine environment due to their high corrosion resistance. The X-ray diffraction line profile analysis (XRDLPA) have been used to assess the microstructure in body centred cubic (bcc) V–Pd alloys having four different nominal compositions in wt.%. X-ray diffraction line broadening analysis on V–Pd alloys has been performed by using different methods like the Warren–Averbach, double-Voigt and Rietveld methods. Finally microstructural defect parameters such as domain size (), r.m.s. microstrain 〈 2 〉1/2, twin fault ('), spacing fault () and deformation stacking fault () were evaluated in these alloys by Fourier line shape analysis using Rietveld method in which the X-ray diffraction profiles of these alloys were described by the pseudo-Voigt function to fit the experimental data. From analysis it has been observed that twin fault, ', and the spacing fault, , are totally absent in these bcc alloy systems because the twin fault, ', has been observed to be either negative or very small (within experimental error limit) for these alloy systems and the spacing fault, , appears to be negative. This analysis also revealed that the deformation stacking fault, , is significantly present in this alloy system and increases with Pd content.

  7. A X-ray diffraction analysis on graphene layers of Assam coal

    Indian Academy of Sciences (India)

    Binoy K Saikia; Rajani K Boruah; Pradip K Gogoi

    2009-01-01

    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 Å) and a high S region (S > 3 Å) where = 4 -1 sin. 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 and are 64.99 Å and 22.63 Å for Tirap-2 and 55.54 Å and 23.80 Å for that of Tirap-1 coals respectively. The position of band was found to be at 4.34 Å and 4.13 Å 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-03-13

    Theory predicts that with an ultrashort and extremely bright coherent X-ray pulse, a single diffraction pattern may be recorded from a large macromolecule, a virus, or a cell before the sample explodes and turns into a plasma. Here we report the first experimental demonstration of this principle using the FLASH soft X-ray free-electron laser. An intense 25 fs, 4 x 10{sup 13} W/cm{sup 2} pulse, containing 10{sup 12} photons at 32 nm wavelength, produced a coherent diffraction pattern from a nano-structured non-periodic object, before destroying it at 60,000 K. A novel X-ray camera assured single photon detection sensitivity by filtering out parasitic scattering and plasma radiation. The reconstructed image, obtained directly from the coherent pattern by phase retrieval through oversampling, shows no measurable damage, and extends to diffraction-limited resolution. A three-dimensional data set may be assembled from such images when copies of a reproducible sample are exposed to the beam one by one.

  9. Modelisation of strains measured by X-ray diffraction in composites with spherical particles

    Energy Technology Data Exchange (ETDEWEB)

    Durand, L.; Lavelle, B.; Drira-Halouani, R.; Altibelli, A. [CNRS, Toulouse (France). CEMES

    2000-07-01

    In a particle composite, elaboration residual stresses have two main origins : differences between thermal expansion coefficients of particles and matrix on the one hand, and volume changes induced by reactions at particles / matrix interface on the other hand. We have compared calculated thermal stresses, and experimental measures on two composites, one presenting an interface reactivity and the other none. The two composites with a nickel matrix and spherical particles either of silica or of alumina have been sintered at 1400 C and analyzed between room temperature and 240 C by X-ray diffraction (Cu K{alpha} radiation). In the semi-infinite composite model, spherical particles have been distributed at the points of a simple cubic lattice. Modelised thickness is larger in comparison of the thickness analyzed by X-ray diffraction. Calculations are based on elastic theory and the difference of coefficients of thermal expansion between the matrix and the particles. Materials are supposed isotropic. At a given temperature, the strain to be observed by X-ray diffraction in a given directions calculated from the distribution of strains in matrix; absorption phenomena are taken into account. Effects of the free surface and of interfacial reactivity are thus shown off. (orig.)

  10. X-Ray Diffraction Analysis of NLO Crystals: Traditional Applications and More New Opportunities

    Science.gov (United States)

    Antipin, Mikhail Yu.; Clark, Ronald D.; Nesterov, Vladimir N.

    1998-01-01

    Single crystal X-ray diffraction analysis is one of the more important methods for the molecular and crystal structure determination of matter and therefore it has a great importance in material science including design and engineering of different compounds with non-linear optical (NLO) properties. It was shown in our previous publications that this method provides unique information about molecular structure of NLO compounds, their crystal symmetry and crystal packing arrays, molecular conformation and geometries and many other structural and electronic characteristics that are important for understanding the nature of NLO properties of solids. A very new application of the X-ray diffraction method is related to analysis of the electron density distribution p(r) in crystals and some of its characteristics (atomic and group charges, dipole and higher multipole moments, etc.), that may be obtained directly form the diffraction measurements. In the present work, we will discuss our preliminary low temperature high-resolution X-ray data for the m-nitroaniline (mNA) single crystal (VI). This is one of the "classical" organic NLO materials and electron density distribution analysis in this simple compound has a great scientific interest.

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

    Science.gov (United States)

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

    2014-09-01

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

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

    Science.gov (United States)

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

    2014-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

  14. 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.

  15. 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.

  16. 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.

  17. Cloning, expression, purification and crystallization as well as X-ray fluorescence and preliminary X-ray diffraction analyses of human ADP-ribosylhydrolase 1.

    Science.gov (United States)

    Kernstock, Stefan; Koch-Nolte, Friedrich; Mueller-Dieckmann, Jochen; Weiss, Manfred S; Mueller-Dieckmann, Christoph

    2009-05-01

    Human ADP-ribosylhydrolase 1 (hARH1, ADPRH) cleaves the glycosidic bond of ADP-ribose attached to an Arg residue of a protein. hARH1 has been cloned, expressed heterologously in Escherichia coli, purified and crystallized in complex with K(+) and ADP. The orthorhombic crystals contained one monomer per asymmetric unit, exhibited a solvent content of 43% and diffracted X-rays to a resolution of 1.9 A. A prerequisite for obtaining well diffracting crystals was the performance of X-ray fluorescence analysis on poorly diffracting apo hARH1 crystals, which revealed the presence of trace amounts of K(+) in the crystal. Adding K-ADP to the crystallization cocktail then resulted in a crystal of different morphology and with dramatically improved diffraction properties.

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

    CERN Document Server

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

    2014-01-01

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

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

    Science.gov (United States)

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

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

  20. 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...

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

    Science.gov (United States)

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

    2016-09-01

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

  2. 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.

  3. Thickness measurement of GaN epilayer using high resolution X-ray diffraction technique

    Institute of Scientific and Technical Information of China (English)

    冯淦; 朱建军; 沈晓明; 张宝顺; 赵德刚; 王玉田; 杨辉; 梁骏吾

    2003-01-01

    In this paper we propose a new method for measuring the thickness of the GaN epilayer, by using the ratio of the integrated intensity of the GaN epilayer X-ray diffraction peaks to that of the sapphire substrate ones. This ratio shows a linear dependence on the GaN epilayer thickness up to 2 μm. The new method is more accurate and convenient than those of using the relationship between the integrated intensity of GaN epilayer diffraction peaks and the GaN thickness. Besides, it can eliminate the absorption effect of the GaN epilayer.

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

    Science.gov (United States)

    Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J R; Krenner, Hubert J; Wixforth, Achim; Salditt, Tim

    2014-10-01

    Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length).

  5. High-pressure X-ray diffraction studies on {beta}-Ni(OH){sub 2}

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-06-15

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

  6. High resolution X-ray diffraction imaging of lead tin telluride

    Science.gov (United States)

    Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Spal, Richard; Simchick, Richard; Fripp, Archibald

    1991-01-01

    High resolution X-ray diffraction images of two directly comparable crystals of lead tin telluride, one Bridgman-grown on Space Shuttle STS 61A and the other terrestrially Bridgman-grown under similar conditions from identical material, present different subgrain structure. In the terrestrial, sample 1 the appearance of an elaborate array of subgrains is closely associated with the intrusion of regions that are out of diffraction in all of the various images. The formation of this elaborate subgrain structure is inhibited by growth in microgravity.

  7. Understanding the instrumental profile of synchrotron radiation X-ray powder diffraction beamlines.

    Science.gov (United States)

    Rebuffi, Luca; Sánchez Del Río, Manuel; Busetto, Edoardo; Scardi, Paolo

    2017-05-01

    A Monte Carlo algorithm has been developed to calculate the instrumental profile function of a powder diffraction synchrotron beamline. Realistic models of all optical elements are implemented in a ray-tracing software. The proposed approach and the emerging paradigm have been investigated and verified for several existing X-ray powder diffraction beamlines. The results, which can be extended to further facilities, show a new and general way of assessing the contribution of instrumental broadening to synchrotron radiation data, based on ab initio simulations.

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

    Science.gov (United States)

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

    2010-05-01

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

  9. In-situ real-time x-ray scattering for probing the processing-structure-performance relation

    KAUST Repository

    Smilgies, Detlef-M.

    2014-01-01

    © 2014 Materials Research Society. In-situ X-ray scattering methodology is discussed, in order to analyze the microstructure development of soft functional materials during coating, annealing, and drying processes in real-time. The relevance of a fundamental understanding of coating processes for future industrial production is pointed out.

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

    Science.gov (United States)

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

    2014-01-01

    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. PMID:24763651

  11. The Study of Shock Waves and Laser Excited Lattice Dynamics using Ultrafast X-ray Diffraction

    Science.gov (United States)

    Funk, David J.; Hur, N.; Wark, J.

    2005-07-01

    We have studied the picosecond lattice dynamics of optically pumped hexagonal manganite LuMnO3 using ultrafast x-ray diffraction. The results show a shift and broadening of the diffraction curve due to the stimulated lattice expansion. To understand the transient response of the lattice, the measured time- and angle-resolved diffraction curves are compared with a theoretical calculation based on dynamical diffraction theory modified for the hexagonal crystal structure of LuMnO3. Our simulations reveal that a large coupling coefficient between the a-b plane and the c-axis (c13) is required to the data. We compare this result to our previous coherent phonon studies of LuMnO3 using optical pump-probe spectroscopy. We have also performed preliminary experiments of shock waves traversing thin (approximately one micron) metal single-crystals, characterizing the shock wave using ultrafast spatial interferometry and with ultrafast x-ray diffraction. A summary of our current results will be presented.

  12. Imaging whole Escherichia coli bacteria by using single-particle x-ray diffraction.

    Science.gov (United States)

    Miao, Jianwei; Hodgson, Keith O; Ishikawa, Tetsuya; Larabell, Carolyn A; LeGros, Mark A; Nishino, Yoshinori

    2003-01-07

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Miao, J.

    2004-06-04

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

  14. X-Ray Diffraction Study of Carbon Nanotubes Under High Pressure

    Institute of Scientific and Technical Information of China (English)

    CHEN Liang-Chen; WANG Li-Jun; TANG Dong-Sheng; XIE Si-Shen; JIN Chang-Qing

    2001-01-01

    The structure and physical properties of carbon nanotubes have been investigated by using in situ high pressureenergy dispersive x-ray diffraction with synchrotron radiation at pressures up to 50.7 Gpa. At atmosphericpressure, the structure of carbon nanotubes is similar to the hexagonal close-packed lattice of graphite with theinterplanar spacing of the diffraction line (002) d002 = 0.3404nm and that of the line (100) d100 = 0.2116nm.According to the high pressure x-ray diffraction results, the diffraction line (002) is broadened and weakenedabove 8 Gpa, and carbon nanotubes become partly amorphous. When the pressures of 10 and 20 Gpa aredecreased to zero, the diffraction line (002) is partly recovered. While at the maximum pressure of 50.7 Gpa,they become entirely amorphous and this amorphous transition is irreversible. We used the equation of state ofBirch-Murnaghan to fit the P-V data of carbon nanotubes and obtained the bulk modulus K0 = 54.3 ± 3.2 Gpa(at K1o = 4.0).C

  15. In situ monitoring of the electrochemical absorption of deuterium into palladium by x-ray diffraction using synchrotron-wiggler radiation

    Energy Technology Data Exchange (ETDEWEB)

    Dominguez, D.D.; Hagans, P.L.; Skelton, E.F.; Qadri, S.B.; Nagel, D.J. [Naval Research Lab., Washington, DC (United States)

    1998-12-31

    With low energy x-rays, such as those from a Cu x-ray tube, only the outer few microns of a metallic sample can be probed. This low penetrating power prohibits structural studies from being carried out on the interior of an electrode in an electrochemical cell because of absorption by the cell material, electrodes and the electrolyte. The work described in this paper circumvents this problem by utilizing high energy, high brightness x-rays produced on the superconducting wiggler beam line, X-17C, at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory. The penetrating power of the higher energy x-rays allowed Pd diffraction spectra to be obtained in-situ on a 1 mm diameter Pd wire cathode during electrolysis of heavy water. Moreover, the beam (28 x 28 {micro}m in cross-section) allowed diffraction spectra to be acquired as a function of distance across the sample. Spectra were recorded in 50 {micro}m steps from the edge of the Pd wire to its core. This was done at 2 minute intervals as a function of electrolysis time. The {alpha}-{beta} phase transition induced in the Pd while deuterium was electrochemically absorbed was observed by monitoring the Pd-(422) diffraction peaks. Results allowed the diffusion rate and the diffusivity of deuterium atoms in the Pd wire to be determined. Other features of the structural changes associated with the absorption of deuterium into Pd are reported.

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

    Science.gov (United States)

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

    2010-02-01

    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 2ψ 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 of

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

    Science.gov (United States)

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

    2015-11-03

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

  18. 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 (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

  19. Time-resolved X-ray diffraction with accelerator- and laser-plasma-based X-ray sources

    Energy Technology Data Exchange (ETDEWEB)

    Nicoul, Matthieu

    2010-09-01

    Femtosecond X-ray pulses are a powerful tool to investigate atomic motions triggered by femtosecond pump pulses. This thesis is dedicated to the production of such pulses and their use in optical pump - X-ray probe measurement. This thesis describes the laser-plasma-based sources available at the University of Duisburg-Essen. Part of it consists of the description of the design, built-up and characterization of a new ''modular'' X-ray source dedicated to optimize the X-ray flux onto the sample under investigation. The acoustic wave generation in femtosecond optically excited semiconductor (gallium arsenide) and metal (gold) was performed using the sources of the University of Duisburg-Essen. The physical answer of the material was modeled by a simple strain model for the semiconductor, pressure model for the metal, in order to gain information on the interplay of the electronic and thermal pressures rising after excitation. Whereas no reliable information could be obtain in gallium arsenide (principally due to the use of a bulk), the model for gold achieved very good agreement, providing useful information. The relaxation time of the electron to lattice energy was found to be (5.0{+-}0.3) ps, and the ratio of the Grueneisen parameters was found to be {gamma}{sub e} / {gamma}{sub i} = (0.5{+-}0.1). This thesis also describes the Sub-Picosecond Pulse Source (SPPS) which existed at the (formally) Stanford Linear Accelerator Center, an accelerator-based X-ray source, and two measurements performed with it. The first one is the detailed investigation of the phonon softening of the A{sub 1g} mode launch in bismuth upon fluence excitation. Detailed information concerning the new equilibrium position and phonon frequency were obtained over extended laser pump fluences. The second measurement concerned the study of the liquid phase dynamics in a newly formed liquid phase following ultrafast melting in indium antimonide. The formation of the liquid phase

  20. Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

    Science.gov (United States)

    Nikonow, Wilhelm; Rammlmair, Dieter

    2016-11-01

    Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

  1. Quantitative determination of minerals in Nevada Test Site samples by x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Pawloski, G.A.

    1983-07-01

    The external standard intensity ratio technique has been developed into a routine procedure for quantitatively determining mineralogic compositions of Nevada Test Site (NTS) samples by x-ray diffraction. This technique used ratios of x-ray intensity peaks from the same run which eliminates many possible errors. Constants have been determined for each of thirteen minerals commonly found in NTS samples - quartz, montmorillonite, illite, clinoptilolite, cristobalite, feldspars, calcite, dolomite, hornblende, kaolinite, muscovite, biotite, and amorphous glass. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of quartz are used to calculate sample composition. The technique has been tested on samples with three to eleven components representative of geologic environments at NTS, and is accurate to 7.0 wt % of the total sample. The minimum amount of each of these minerals detectable by x-ray diffraction has also been determined. QUANTS is a computer code that calculates mineral contents and produces a report sheet. Constants for minerals in NTS samples other than those listed above can easily be determined, and added to QUANTS at any time.

  2. High resolution X-ray diffraction studies on unirradiated and irradiated strontium hexaferrite crystals

    Indian Academy of Sciences (India)

    Balwinder Kaur; Monita Bhat; F Licci; Ravi Kumar; K K Bamzai; P N Kotru

    2012-04-01

    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 irradiated crystals suggest the possibility of creation of low angle grain boundaries and other point/clusters of defects causing amorphization in the irradiated crystals. The perfection of the irradiated and unirradiated (0001) cleaved surfaces of the crystals is studied using the bulk method of X-ray topography. The topographs supplement the findings suggestive of modifications in the crystalline quality of SrFe12O19 on irradiation with SHI of Li3+. Etching of the (0001) cleaved surfaces in H3PO4 at 120°C suggests that the dissolution characteristics of the surfaces get affected on irradiation with SHI of Li3+, besides supporting the findings of HRXRD and X-ray topography regarding modifications in the perfection of SrFe12O19 on irradiation.

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

    Science.gov (United States)

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

    2014-01-01

    Emerging X-ray free-electron lasers with femtosecond pulse duration enable single-shot snapshot imaging almost free from sample damage by outrunning major radiation damage processes. In bioimaging, it is essential to keep the sample close to its natural state. Conventional high-resolution imaging, however, suffers from severe radiation damage that hinders live cell imaging. Here we present a method for capturing snapshots of live cells kept in a micro-liquid enclosure array by X-ray laser diffraction. We place living Microbacterium lacticum cells in an enclosure array and successively expose each enclosure to a single X-ray laser pulse from the SPring-8 Angstrom Compact Free-Electron Laser. The enclosure itself works as a guard slit and allows us to record a coherent diffraction pattern from a weakly-scattering submicrometre-sized cell with a clear fringe extending up to a 28-nm full-period resolution. The reconstructed image reveals living whole-cell structures without any staining, which helps advance understanding of intracellular phenomena. PMID:24394916

  4. Investigation of electronic order using resonant soft X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Schlappa, J.

    2006-12-01

    The aim of this PhD work was the application of resonant soft X-ray diffraction technique for the investigation of electronic order in transition metal oxides at the TM L{sub 2,3}-edge, trying to obtain a quantitative understanding of the data. The method was first systematically explored through application to a model system in order to test the feasibility of the technique and to understand of how X-ray optical effects have to be taken into account. Two more complex systems were investigated; stripe order in La{sub 1.8}Sr{sub 0.2}NiO{sub 4} and charge and orbital order in Fe{sub 3}O{sub 4}. The main focus of the work was on the spectroscopic potential of the technique, trying to obtain a level of quantitative description of the data. For X-ray absorption spectroscopy (XAS) from transition metal oxides, cluster configuration interaction calculation provides a powerful and realistic microscopic theory. In the frame work of this thesis cluster theory, considering explicit hybridization effects between the TM-ion and the surrounding oxygen ligands, has been applied for the first time to describe resonant diffraction data. (orig.)

  5. Crystallization and preliminary X-ray diffraction experiments of arylmalonate decarboxylase from Alcaligenes bronchisepticus

    Energy Technology Data Exchange (ETDEWEB)

    Nakasako, Masayoshi, E-mail: nakasako@phys.keio.ac.jp [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); The RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Obata, Rika; Okubo, Ryosuke; Nakayama, Shyuichi [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); Miyamoto, Kenji; Ohta, Hiromichi [Department of Biosciences and Informatics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan)

    2008-07-01

    Crystals of arylmalonate decarboxylase from A. bronchisepticus were obtained which diffracted X-rays to a resolution of at least 3.0 Å. Arylmalonate decarboxylase catalyses the enantioselective decarboxylation of α-aryl-α-methylmalonates to produce optically pure α-arylpropionates. The enzyme was crystallized with ammonium sulfate under alkaline pH conditions with the aim of understanding the mechanism of the enantioselective reaction. X-ray diffraction data collected to a resolution of 3.0 Å at cryogenic temperature showed that the crystals belonged to the orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 83.13, b = 99.62, c = 139.64 Å. This suggested that the asymmetric unit would contain between four and six molecules. Small-angle X-ray scattering revealed that the enzyme exists as a monomer in solution. Thus, the assembly of molecules in the asymmetric unit was likely to have been induced during the crystallization process.

  6. In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

    Energy Technology Data Exchange (ETDEWEB)

    Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

    2016-03-31

    Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

  7. Mineral identification in Colombian coals using Moessbauer spectroscopy and X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fajardo, M. [Universidad del Valle, A.A, Departamento de Fisica (Colombia); Mojica, J. [Instituto Nacional de Investigaciones en Geociencia, Mineria y Quimica (INGEOMINAS) (Colombia); Barraza, J. [Universidad del Valle, A.A, Departamento de Procesos Quimicos, Facultad de Ingenieria (Colombia); Perez Alcazar, G.A.; Tabares, J.A. [Universidad del Valle, A.A, Departamento de Fisica (Colombia)

    1999-11-15

    Minerals were identified in three Colombian coal samples from the Southwest of the country using Moessbauer spectroscopy and X-ray diffraction. Original and sink separated coal fractions of specific gravity 1.40 and 1.60 with particle size less than 600 {mu}m were used in the study. Using Moessbauer spectroscopy, the minerals identified in the original coal samples were pyrite jarosite, ankerite, illite and ferrous sulfate, whereas by means of X-ray diffraction, minerals identified were kaolinite, quartz, pyrite, and jarosite. Differences in mineral composition were found in the original and sink separated fractions using both techniques. Moessbauer spectra show that the mineral phases in low concentrations such as illite, ankerite and ferrous sulfate do not always appear in the spectra of sink coals, despite of those minerals occurring in the original coal, due to the fact that they are associated with the organic matter and not liberated in the grinding process. X-ray results show that the peak intensity grows as the specific gravity is increased indicating that the density separation method could be an effective process to clean coal.

  8. APPLICATION OF THE MOMENT METHODS TO ANALYSIS OF X-RAY DIFFRACTION LINE PROFILE FOR PA1010-BMI SYSTEM

    Institute of Scientific and Technical Information of China (English)

    ZHANG Hongfang; YU Li; ZHANG Lihua; MO Zhishen; MU Zhongchen

    1995-01-01

    Pure X-ray diffraction profiles have been analysed for polyamide 1010 and PA1010-BMI system by means of multipeak fitting resolution of X-ray diffraction. The methods of variance and fourth moment have been applied to determine the particle size and strain values for the paracrystalline materials. The results indicated that both variance and fourth moment of X-ray diffraction line profile yielded approximately the same values of the particle size and the strain. The particle sizes of (100) reflection have been found to decrease with increasing BMI content, whereas the strain values increased.

  9. X-rays diffraction on a new chromium oxide single-crystal thin film prepared by molecular beam epitaxy

    NARCIS (Netherlands)

    Du, X. S.; Hak, S.; Hibma, T.; Rogojanu, O. C.; Struth, B.

    2006-01-01

    Chromium oxide films were prepared on MgO substrates by molecular beam epitaxy. The crystalline structure of the films was characterized by X-ray diffraction (XRD) with conventional as well as synchrotron X-ray sources. The theta-2 theta spectra showed that the film was a new chromium oxide epitaxia

  10. The architecture of amyloid-like peptide fibrils revealed by X-ray scattering, diffraction and electron microscopy

    DEFF Research Database (Denmark)

    Langkilde, Annette Eva; Morris, Kyle L; Serpell, Louise C;

    2015-01-01

    of the GNNQQNY peptide fragment of a yeast prion protein. Data from small-angle X-ray solution scattering, fibre diffraction and electron microscopy are combined with existing high-resolution X-ray crystallographic structures to investigate the fibrillation process and the hierarchical fibril structure...

  11. The use of X-ray diffraction for analyzing biomodification of crystalline cellulose by wood decay fungi

    DEFF Research Database (Denmark)

    Howell, Caitlin; Hastrup, Anne Christine Steenkjær; Jellison, Jody

    2007-01-01

    X-ray diffraction (XRD) is based on the creation of an interference pattern by x-rays when they encounter a regularly spaced matrix. In wood, this process has been used to determine, among other things, the average width of the cellulose microcrystals, the percent of crystalline cellulose within...

  12. X-ray powder diffraction characterization of the large-volume unit cell of the M8 murataite polytype

    OpenAIRE

    MAKI, Ryosuke S. S.; Morgan, Peter E. D.; Suzuki, Yoshikazu

    2016-01-01

    We have used conventional X-ray powder diffraction to study one of the largest volume inorganic mixed oxide unit-supercell structures done so far. This necessitated some small-angle X-ray scattering-like observations at low angles from

  13. X-rays diffraction on a new chromium oxide single-crystal thin film prepared by molecular beam epitaxy

    NARCIS (Netherlands)

    Du, X. S.; Hak, S.; Hibma, T.; Rogojanu, O. C.; Struth, B.

    2006-01-01

    Chromium oxide films were prepared on MgO substrates by molecular beam epitaxy. The crystalline structure of the films was characterized by X-ray diffraction (XRD) with conventional as well as synchrotron X-ray sources. The theta-2 theta spectra showed that the film was a new chromium oxide

  14. A novel wafer-scale CMOS APS X-ray detector for breast cancer diagnosis using X-ray diffraction studies

    Science.gov (United States)

    Konstantinidis, A.; Zheng, Y.; Philip, D.; Vinnicombe, S.; Speller, R.

    2012-12-01

    The current study uses a novel large area (12.8 cm × 13.1 cm) complementary metal-oxide-semiconductor (CMOS) active pixel sensor (APS) X-ray detector, named Dynamic range Adjustable for Medical Imaging Technology (DynAMITe), for breast cancer diagnosis. The detector consists of two geometrically superimposed grids: a) 2560 × 2624 fine-pitch grid of pixels (50 μm pitch), named Sub-Pixels (SP camera), for low intrinsic noise and high spatial resolution and b) 1280 × 1312 large-pitch grid of pixels (100 μm pitch), named Pixels (P camera), for high dynamic range. X-ray performance characterization measurements show that the detective quantum efficiency (DQE) of the SP camera is in the range 0.7-0.75 at low spatial frequencies using a tungsten (W) anode X-ray source at 28 kV. Hence, the detector is suitable for mammography. Furthermore, we used the SP camera to combine mammograms with angle dispersive X-ray diffraction (ADXRD) measurements in order to apply the X-ray biopsy concept in one examination. The results show that ADXRD technique indicates the presence of cancer in suspicious areas on the mammogram. Hence, it could be used to determine the region affected by cancer and assist in planning surgery. This study is the proof of concept that mammography and ADXRD can be combined in one examination.

  15. Time-, Frequency-, and Wavevector-Resolved X-Ray Diffraction from Single Molecules

    CERN Document Server

    Bennett, Kochise; Zhang, Yu; Dorfman, Konstantin E; Mukamel, Shaul

    2014-01-01

    Using a quantum electrodynamic framework, we calculate the off-resonant scattering of a broad-band X-ray pulse from a sample initially prepared in an arbitrary superposition of electronic states. The signal consists of single-particle (incoherent) and two-particle (coherent) contributions that carry different particle form factors that involve different material transitions. Single-molecule experiments involving incoherent scattering are more influenced by inelastic processes compared to bulk measurements. The conditions under which the technique directly measures charge densities (and can be considered as diffraction) as opposed to correlation functions of the charge-density are specified. The results are illustrated with time- and wavevector-resolved signals from a single amino acid molecule (cysteine) following an impulsive excitation by a stimulated X-ray Raman process resonant with the sulfur K-edge. Our theory and simulations can guide future experimental studies on the structures of nano-particles and ...

  16. Diffraction data of core-shell nanoparticles from an X-ray free electron laser.

    Science.gov (United States)

    Li, Xuanxuan; Chiu, Chun-Ya; Wang, Hsiang-Ju; Kassemeyer, Stephan; Botha, Sabine; Shoeman, Robert L; Lawrence, Robert M; Kupitz, Christopher; Kirian, Richard; James, Daniel; Wang, Dingjie; Nelson, Garrett; Messerschmidt, Marc; Boutet, Sébastien; Williams, Garth J; Hartmann, Elisabeth; Jafarpour, Aliakbar; Foucar, Lutz M; Barty, Anton; Chapman, Henry; Liang, Mengning; Menzel, Andreas; Wang, Fenglin; Basu, Shibom; Fromme, Raimund; Doak, R Bruce; Fromme, Petra; Weierstall, Uwe; Huang, Michael H; Spence, John C H; Schlichting, Ilme; Hogue, Brenda G; Liu, Haiguang

    2017-04-11

    X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Scattering patterns resulting from single particles were selected and compiled into a dataset which can be valuable for algorithm developments in single particle scattering research.

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

    Science.gov (United States)

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

    2007-01-01

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

  18. X-ray diffraction results from Mars Science Laboratory: mineralogy of Rocknest at Gale crater.

    Science.gov (United States)

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

    2013-09-27

    The Mars Science Laboratory rover Curiosity scooped samples of soil from the Rocknest aeolian bedform in Gale crater. Analysis of the soil with the Chemistry and Mineralogy (CheMin) x-ray diffraction (XRD) instrument revealed plagioclase (~An57), forsteritic olivine (~Fo62), augite, and pigeonite, with minor K-feldspar, magnetite, quartz, anhydrite, hematite, and ilmenite. The minor phases are present at, or near, detection limits. The soil also contains 27 ± 14 weight percent x-ray amorphous material, likely containing multiple Fe(3+)- and volatile-bearing phases, including possibly a substance resembling hisingerite. The crystalline component is similar to the normative mineralogy of certain basaltic rocks from Gusev crater on Mars and of martian basaltic meteorites. The amorphous component is similar to that found on Earth in places such as soils on the Mauna Kea volcano, Hawaii.

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

    Science.gov (United States)

    Karunaratne, B. S. B.

    2012-07-01

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

  20. Imaging of complex density in silver nanocubes by coherent x-ray diffraction

    Science.gov (United States)

    Harder, R.; Liang, M.; Sun, Y.; Xia, Y.; Robinson, I. K.

    2010-03-01

    When using coherent x-rays to perform lensless imaging, it is the complex wave field exiting the sample or, in the case of the Bragg geometry, the deformed electron density distribution of a crystal, that is being sought. For most samples, to some extent, the image will be complex, containing both an amplitude and phase variation across the sample. We have developed versions of the hybrid input-output (HIO) and error reduction (ER) algorithms that are very robust for the inversion to complex objects from three-dimensional (3D) coherent x-ray diffraction (CXD) data measured around a Bragg spot of a small crystal. The development and behavior of these algorithms will be discussed in the context of inverting a 3D CXD pattern measured around a (111) Bragg spot of a silver nanocube.

  1. A Mössbauer and X-ray powder diffraction study of some ferrous hematinics.

    Science.gov (United States)

    Coe, E M; Bowen, L H; Bereman, R D

    1995-06-01

    Iron deficiency anemia is a relatively common illness that can arise from a number of different causes. Three ferrous salts are usually used in its treatment: ferrous fumarate, gluconate, and sulfate. They are administered orally and are relatively well tolerated. These hematinics have been studied by Mössbauer spectroscopy and X-ray powder diffraction, and can easily be distinguished by both techniques. It was found that the two ferrous sulfates studied (Eckerd and SmithKline Beckman Co.) most closely resemble the monohydrate by comparison of the X-ray powder pattern with those of the JCPDS. Both the ferrous fumarate (Femiron) and gluconate (Spring Valley) had approximately 10% ferric iron present. To the authors' knowledge, this is the first reported Mössbauer spectrum for ferrous fumarate.

  2. Structure determination of thin CoFe films by anomalous x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gloskovskii, Andrei; Stryganyuk, Gregory; Ouardi, Siham [Institut fuer Anorganische und Analytische Chemie, Johannes Gutenberg-Universitaet, 55099 Mainz (Germany); Fecher, Gerhard H.; Felser, Claudia [Institut fuer Anorganische und Analytische Chemie, Johannes Gutenberg-Universitaet, 55099 Mainz (Germany); Max Planck Institute for Chemical Physics of Solids, D-01187 Dresden (Germany); Hamrle, Jaroslav; Pistora, Jaromir [Department of Physics and Nanotechnology Centre, VSB-Technical University of Ostrava, 70833 Ostrava (Czech Republic); Bosu, Subrojati; Saito, Kesami; Sakuraba, Yuya; Takanashi, Koki [Institute for Materials Research (IMR), Tohoku University, Sendai 980-8577 (Japan)

    2012-10-01

    This work reports on the investigation of structure-property relationships in thin CoFe films grown on MgO. Because of the very similar scattering factors of Fe and Co, it is not possible to distinguish the random A2 (W-type) structure from the ordered B2 (CsCl-type) structure with commonly used x-ray sources. Synchrotron radiation based anomalous x-ray diffraction overcomes this problem. It is shown that as grown thin films and 300 K post annealed films exhibit the A2 structure with a random distribution of Co and Fe. In contrast, films annealed at 400 K adopt the ordered B2 structure.

  3. RASOR: An advanced instrument for soft x-ray reflectivity and diffraction

    Science.gov (United States)

    Beale, T. A. W.; Hase, T. P. A.; Iida, T.; Endo, K.; Steadman, P.; Marshall, A. R.; Dhesi, S. S.; van der Laan, G.; Hatton, P. D.

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (θ, 2θ, and χ) diffractometer with an additional removable rotation (ϕ) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.

  4. Automated high pressure cell for pressure jump x-ray diffraction

    Science.gov (United States)

    Brooks, Nicholas J.; Gauthe, Beatrice L. L. E.; Terrill, Nick J.; Rogers, Sarah E.; Templer, Richard H.; Ces, Oscar; Seddon, John M.

    2010-06-01

    A high pressure cell for small and wide-angle x-ray diffraction measurements of soft condensed matter samples has been developed, incorporating a fully automated pressure generating network. The system allows both static and pressure jump measurements in the range of 0.1-500 MPa. Pressure jumps can be performed as quickly as 5 ms, both with increasing and decreasing pressures. Pressure is generated by a motorized high pressure pump, and the system is controlled remotely via a graphical user interface to allow operation by a broad user base, many of whom may have little previous experience of high pressure technology. Samples are loaded through a dedicated port allowing the x-ray windows to remain in place throughout an experiment; this facilitates accurate subtraction of background scattering. The system has been designed specifically for use at beamline I22 at the Diamond Light Source, United Kingdom, and has been fully integrated with the I22 beamline control systems.

  5. Evaluation of x-ray diffraction enhanced imaging in the diagnosis of breast cancer.

    Science.gov (United States)

    Liu, Chenglin; Yan, Xiaohui; Zhang, Xinyi; Yang, Wentao; Peng, Weijun; Shi, Daren; Zhu, Peiping; Huang, Wanxia; Yuan, Qingxi

    2007-01-21

    The significance of the x-ray diffraction enhanced imaging (DEI) technique in the diagnosis of breast cancer and its feasibility in clinical medical imaging are evaluated. Different massive specimens including normal breast tissues, benign breast tumour tissues and malignant breast tumour tissues are imaged with the DEI method. The images are recorded respectively by CCD or x-ray film at different positions of the rocking curve and processed with a pixel-by-pixel algorithm. The characteristics of the DEI images about the normal and diseased tissues are compared. The rocking curves of a double-crystal diffractometer with various tissues are also studied. The differences in DEI images and their rocking curves are evaluated for early diagnosis of breast cancers.

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

    Science.gov (United States)

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

    2010-03-31

    Many proteins, sugars and pharmaceuticals crystallize into two forms that are mirror images of each other (enantiomers) like our right and left hands. Tellurium is one enantiomer having a space group pair, P3(1)21 (right-handed screw) and P3(2)21 (left-handed screw). X-ray diffraction with dispersion correction terms has been playing an important role in determining the handedness of enantiomers for a long time. However, this approach is not applicable for an elemental crystal such as tellurium or selenium. We have demonstrated that positive and negative circularly polarized x-rays at the resonant energy of tellurium can be used to absolutely distinguish right from left tellurium. This method is applicable to chiral motifs that occur in biomolecules, liquid crystals, ferroelectrics and antiferroelectrics, multiferroics, etc.

  7. On radiation damage in FIB-prepared softwood samples measured by scanning X-ray diffraction.

    Science.gov (United States)

    Storm, Selina; Ogurreck, Malte; Laipple, Daniel; Krywka, Christina; Burghammer, Manfred; Di Cola, Emanuela; Müller, Martin

    2015-03-01

    The high flux density encountered in scanning X-ray nanodiffraction experiments can lead to severe radiation damage to biological samples. However, this technique is a suitable tool for investigating samples to high spatial resolution. The layered cell wall structure of softwood tracheids is an interesting system which has been extensively studied using this method. The tracheid cell has a complex geometry, which requires the sample to be prepared by cutting it perpendicularly to the cell wall axis. Focused ion beam (FIB) milling in combination with scanning electron microscopy allows precise alignment and cutting without splintering. Here, results of a scanning X-ray diffraction experiment performed on a biological sample prepared with a focused ion beam of gallium atoms are reported for the first time. It is shown that samples prepared and measured in this way suffer from the incorporation of gallium atoms up to a surprisingly large depth of 1 µm.

  8. Source assemblage types for cratonic diamonds from X-ray synchrotron diffraction

    Science.gov (United States)

    Nestola, F.; Alvaro, M.; Casati, M. N.; Wilhelm, H.; Kleppe, A. K.; Jephcoat, A. P.; Domeneghetti, M. C.; Harris, J. W.

    2016-11-01

    Three single crystals of clinopyroxene trapped within three different gem-quality diamonds from the Udachnaya kimberlite (Siberia, Russia) were analysed in situ by single-crystal synchrotron X-ray diffraction in order to obtain information on their chemical composition and infer source assemblage type. A non-destructive approach was used with high-energy (≈ 60 keV; λ ≈ 0.206 Å) at I15, the extreme-conditions beamline at Diamond Light Source. A dedicated protocol was used to center the mineral inclusions located deep inside the diamonds in the X-ray beam. Our results reveal that two of the inclusions can be associated with peridotitic paragenesis whereas the third is eclogitic. This study also demonstrates that this non-destructive experimental approach is extremely efficient in evaluating the origin of minerals trapped in their diamond hosts.

  9. Automated high pressure cell for pressure jump x-ray diffraction.

    Science.gov (United States)

    Brooks, Nicholas J; Gauthe, Beatrice L L E; Terrill, Nick J; Rogers, Sarah E; Templer, Richard H; Ces, Oscar; Seddon, John M

    2010-06-01

    A high pressure cell for small and wide-angle x-ray diffraction measurements of soft condensed matter samples has been developed, incorporating a fully automated pressure generating network. The system allows both static and pressure jump measurements in the range of 0.1-500 MPa. Pressure jumps can be performed as quickly as 5 ms, both with increasing and decreasing pressures. Pressure is generated by a motorized high pressure pump, and the system is controlled remotely via a graphical user interface to allow operation by a broad user base, many of whom may have little previous experience of high pressure technology. Samples are loaded through a dedicated port allowing the x-ray windows to remain in place throughout an experiment; this facilitates accurate subtraction of background scattering. The system has been designed specifically for use at beamline I22 at the Diamond Light Source, United Kingdom, and has been fully integrated with the I22 beamline control systems.

  10. RASOR: an advanced instrument for soft x-ray reflectivity and diffraction.

    Science.gov (United States)

    Beale, T A W; Hase, T P A; Iida, T; Endo, K; Steadman, P; Marshall, A R; Dhesi, S S; van der Laan, G; Hatton, P D

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (theta, 2theta, and chi) diffractometer with an additional removable rotation (phi) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.

  11. Crystal structure of Pigment Red 254 from X-ray powder diffraction data

    Directory of Open Access Journals (Sweden)

    Svetlana N. Ivashevskaya

    2017-04-01

    Full Text Available The crystal structure of Pigment Red 254 [P.R. 254, C18H10Cl2N2O2; systematic name: 3,6-bis(4-chlorophenyl-2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione] was solved from laboratory X-ray powder diffraction data using the simulated annealing method followed by Rietveld refinement because the very low solubility of the pigment in all solvents impedes the growth of single crystals suitable for X-ray analysis. The molecule lies across an inversion center. The dihedral angle between the benzene ring and the pyrrole ring in the unique part of the molecule is 11.1 (2°. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming chains along [110] incorporating R22(8 rings.

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

    Science.gov (United States)

    Balyan, Minas K

    2014-03-01

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

  13. Evaluation of multiaxial stress in textured cubic films by x-ray diffraction

    Institute of Scientific and Technical Information of China (English)

    Zhang Jian-Min; Xu Ke-Wei

    2005-01-01

    X-ray diffraction is used extensively to determine the residual stress in bulk or thin film materials on the assumptions that the material is composed of fine crystals with random orientation and the stress state is biaxial and homogeneous through the x-ray penetrating region. The stress is calculated from the gradient of ε~ sin2 ψ linear relation. But the method cannot be used in textured films due to nonlinear relation. In this paper, a novel method is proposed for measuring the multiaxial stresses in cubic films with any [hkl] fibre texture. As an example, a detailed analysis is given for measuring three-dimensional stresses in FCC films with [111] fibre texture.

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

    KAUST Repository

    Misra, Sumohan

    2012-06-26

    Figure Persented: Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-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, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes. © 2012 American Chemical Society.

  15. Monitoring protein precipitates by in-house X-ray powder diffraction

    DEFF Research Database (Denmark)

    Ståhl, Kenny; Frankær, Christian Grundahl; Petersen, Jakob

    2013-01-01

    Powder diffraction from protein powders using in-house diffractometers is an effective tool for identification and monitoring of protein crystal forms and artifacts. As an alternative to conventional powder diffractometers a single crystal diffractometer equipped with an X-ray micro-source can...... of protein data sets in the database some problems can be foreseen due to the large number of overlapping peaks in the low-angle region, and small differences in unit cell parameters between pdb-data and powder data. It is suggested that protein entries are supplied with more searchable keywords as protein...... be used to collect powder patterns from 1 l samples. Using a small-angle X-ray scattering (SAXS) camera it is possible to collect data within minutes. A streamlined program has been developed for the calculation of powder patterns from pdb-coordinates, and includes correction for bulk-solvent. A number...

  16. An In-situ X-ray Scattering Study During Uniaxial Stretching of Ionic Liquid/Ultra-high Molecular Weight Polyethylene Blends

    Energy Technology Data Exchange (ETDEWEB)

    X Li; Y Mao; H Ma; F Zuo; B Hsiao; B Chu

    2011-12-31

    An ionic liquid (IL) 1-docosanyl-3-methylimidazolium bromide was incorporated into ultra-high molecular weight polyethylene (UHMWPE) and formed IL/UHMWPE blends by solution mixing. The structure evolution of these blends during uniaxial stretching was followed by in-situ synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. During deformation at room temperature, deformation-induced phase transformation from orthorhombic to monoclinic phase was observed in both IL/UHMWPE blends and neat UHMWPE. The elongation-to-break ratios of IL/UHMWPE blends were found to increase by 2-3 times compared with that of pure UHMWPE, while the tensile strength remained about the same. In contrast, during deformation at high temperature (120 C), no phase transformation was observed. However, the blend samples showed much better toughness, higher crystal orientation and higher tilting extent of lamellar structure at high strains.

  17. Optically Induced Lattice Dynamics of hexagonal manganite using Ultrafast X-ray Diffraction

    Science.gov (United States)

    Lee, Hae Ja; Workman, J. B.; Hur, N.

    2005-03-01

    We have studied the picosecond lattice dynamics of optically pumped hexagonal manganite LuMnO3 using ultrafast x-ray diffraction. The results show a shift and broadening of the diffraction curve due to the stimulated lattice expansion. To understand the transient response of the lattice, the measured time- and angle-resolved diffraction curves are compared with a theoretical calculation based on dynamical diffraction theory modified for the hexagonal crystal structure of LuMnO3. Our simulations reveal that a large coupling coefficient between the a-b plane and the c-axis (c13) is required to the data. We compare this result to our previous coherent phonon studies of LuMnO3 using optical pump-probe spectroscopy.

  18. Crystal structure of defect-containing semiconductor nanocrystals. An X-ray diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Buljan, Maja [Karlova Univ., Prague (Czech Republic). Fakulta Matematicko-Fyzikalni; Institut Rudjer Boskovic, Zagreb (Croatia); Desnica, Uros V.; Radic, Nikola [Institut Rudjer Boskovic, Zagreb (Croatia); Drazic, Goran [Institut Jozef Stefan, Ljubljana (Slovenia); Matej, Zdenek; Vales, Vaclav; Holy, Vaclav [Karlova Univ., Prague (Czech Republic). Fakulta Matematicko-Fyzikalni

    2009-08-15

    Defects of crystal structure in semiconductor nanocrystals embedded in an amorphous matrix are studied by X-ray diffraction and a full-profile analysis of the diffraction curves based on the Debye formula. A new theoretical model is proposed, describing the diffraction from randomly distributed intrinsic and extrinsic stacking faults and twin blocks in the nanocrystals. The application of the model to full-profile analysis of experimental diffraction curves enables the determination of the concentrations of individual defect types in the nanocrystals. The method has been applied for the investigation of selforganized Ge nanocrystals in an SiO{sub 2} matrix, and the dependence of the structure quality of the nanocrystals on their deposition and annealing parameters was obtained. (orig.)

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

    Institute of Scientific and Technical Information of China (English)

    Zichun Le; Kai Liu; Jingqiu Liang

    2005-01-01

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

  20. X-ray, synchrotron, and neutron diffraction analysis of Roman cavalry parade helmet fragment

    Energy Technology Data Exchange (ETDEWEB)

    Smrcok, L' . [Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dubravska cesta 9, 84536 Bratislava (Slovakia); Petrik, I. [Geological Institute, Slovak Academy of Sciences, Dubravska cesta 9, 84005 Bratislava (Slovakia); Langer, V. [Environmental Inorganic Chemistry, Chalmers University of Technology, 412 96 Gothenburg (Sweden); Filinchuk, Y. [Swiss-Norwegian Beam Lines, European Synchrotron Radiation Facility, 6 rue Jules Horowitz, BP-220, 38043 Grenoble CEDEX (France); Beran, P. [Nuclear Physics Institute ASCR v.v.i. and Research Centre Rez Ltd., 25068 Rez (Czech Republic)

    2010-10-15

    A partially corroded fragment of the neck guard of a Roman cavalry helmet excavated in the former military camp of Gerulata, a part of the Limes Romanus on the River Danube, was analysed by laboratory X-ray, synchrotron and neutron powder diffraction. The approximate phase composition determined by the neutron diffraction of the bulk, 82% (wt) of the copper alloy phase, 12 % (wt) of cuprite and 6% of nantokite indicate a significant degree of corrosion of the artefact. Elemental EDX analysis of cleaned surface showed that the chemical composition of the original alloy is 78 to 82 % (wt) of Cu and 21.4 to 16.5 % of Zn with minute amounts of Sn, Si and S. High contents of Cu and Zn with the negligible amount of Sn showed that the body of the helmet was made of brass and not of bronze as expected before. The amount of zinc in the copper alloy calculated from the refined lattice parameter agrees fairly well with the value determined by EDX. The most abundant phase in the synchrotron powder diffraction pattern of the corrosion products scrapped from the artefact is cuprite, but presence of atacamite, malachite, brochantite, nantokite, mixed Cu-Zn hydroxyl carbonates and probably also of simonkolleite (Zn{sub 5}(OH){sub 8}Cl{sub 2}.H{sub 2}O) have been detected. In contrast, the X-ray pattern taken directly from the surface of the artefact is dominated by atacamite with some traces of malachite and quartz. Because the penetration depth of laboratory X-rays is in order of tens of microns, the phase analysis based only on a diffraction pattern taken from a surface can lead to erroneous conclusions concerning the phase composition of the patina. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)