Intermediate-range order in mesoporous silicas investigated by a high-energy X-ray diffraction technique

International Nuclear Information System (INIS)

Wakihara, Toru; Fan, Wei; Ogura, Masaru; Okubo, Tatsuya; Kohara, Shinji; Sankar, Gopinathan

2008-01-01

We perform a high-energy X-ray diffraction study comparing bulk amorphous silica with MCM-41 and SBA-15 that are representative mesoporous silicas prepared in basic and acidic conditions, respectively. It is revealed that mesoporous silicas, especially SBA-15, have less ordered structures and contain larger fractions of three- and four-membered rings than does bulk amorphous silica. (author)

Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

Science.gov (United States)

Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

2004-03-01

We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

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

Indian Academy of Sciences (India)

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

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

International Nuclear Information System (INIS)

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

1992-01-01

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

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

International Nuclear Information System (INIS)

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

1981-02-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-02-01

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

Characterization of neutron-irradiated HT-UPS steel by high-energy X-ray diffraction microscopy

Energy Technology Data Exchange (ETDEWEB)

Zhang, Xuan, E-mail: xuanzhang@anl.gov [Nuclear Engineering Division, Argonne National Laboratory, Lemont, IL 60439 (United States); Park, Jun-Sang; Almer, Jonathan [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Li, Meimei [Nuclear Engineering Division, Argonne National Laboratory, Lemont, IL 60439 (United States)

2016-04-01

This paper presents the first measurement of neutron-irradiated microstructure using far-field high-energy X-ray diffraction microscopy (FF-HEDM) in a high-temperature ultrafine-precipitate-strengthened (HT-UPS) austenitic stainless steel. Grain center of mass, grain size distribution, crystallographic orientation (texture), diffraction spot broadening and lattice constant distributions of individual grains were obtained for samples in three different conditions: non-irradiated, neutron-irradiated (3dpa/500 °C), and irradiated + annealed (3dpa/500 °C + 600 °C/1 h). It was found that irradiation caused significant increase in grain-level diffraction spot broadening, modified the texture, reduced the grain-averaged lattice constant, but had nearly no effect on the average grain size and grain size distribution, as well as the grain size-dependent lattice constant variations. Post-irradiation annealing largely reversed the irradiation effects on texture and average lattice constant, but inadequately restored the microstrain.

High resolution X-ray diffraction studies on unirradiated

Indian Academy of Sciences (India)

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

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

Indian Academy of Sciences (India)

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

A spectrometer for X-ray energy-dispersive diffraction using synchrotron radiation

International Nuclear Information System (INIS)

Buras, B.; Gerward, L.; Staun Olsen, J.; Steenstrup, S.

1981-10-01

The paper describes a white-beam X-ray energy dispersive diffractometer using the synchroton radiation from the DORIS ESR. The following features of the instrument are discussed: Horizontal or vertical scattering plane, collimators, sample environment, remote control of gonimeter, data acquisition, energy-sensitive detectors using small-area and large-area detector crystals, modes of operation, powder and single crystal diffraction. An example is given from a high-pressure study of YbH 2 using a diamond anvil cell. (orig./HP)

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.

Hard x-ray monochromator with milli-electron volt bandwidth for high-resolution diffraction studies of diamond crystals

Energy Technology Data Exchange (ETDEWEB)

Stoupin, Stanislav; Shvyd' ko, Yuri; Shu Deming; Khachatryan, Ruben; Xiao, Xianghui; DeCarlo, Francesco; Goetze, Kurt; Roberts, Timothy; Roehrig, Christian; Deriy, Alexey [Advanced Photon Source, Argonne National Laboratory, Illinois 60439 (United States)

2012-02-15

We report on design and performance of a high-resolution x-ray monochromator with a spectral bandwidth of {Delta}E{sub X}{approx_equal} 1.5 meV, which operates at x-ray energies in the vicinity of the backscattering (Bragg) energy E{sub H} = 13.903 keV of the (008) reflection in diamond. The monochromator is utilized for high-energy-resolution diffraction characterization of diamond crystals as elements of advanced x-ray crystal optics for synchrotrons and x-ray free-electron lasers. The monochromator and the related controls are made portable such that they can be installed and operated at any appropriate synchrotron beamline equipped with a pre-monochromator.

The high-energy x-ray diffraction and scattering beamline at the Canadian Light Source

Science.gov (United States)

Gomez, A.; Dina, G.; Kycia, S.

2018-06-01

The optical design for the high-energy x-ray diffraction and scattering beamline of the Brockhouse sector at the Canadian Light Source is described. The design is based on a single side-bounce silicon focusing monochromator that steers the central part of a high-field permanent magnet wiggler beam into the experimental station. Two different configurations are proposed: a higher energy resolution with vertical focusing and a lower energy resolution with horizontal and vertical focusing. The monochromator will have the possibility of mounting three crystals: one crystal optimized for 35 keV that focuses in the horizontal and vertical directions using reflection (1,1,1) and two other crystals both covering the energies above 40 keV: one with only vertical focusing and another one with horizontal and vertical focusing. The geometry of the last two monochromator crystals was optimized to use reflections (4,2,2) and (5,3,3) to cover the broad energy range from 40 to 95 keV.

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

Energy Technology Data Exchange (ETDEWEB)

Cook, Emily [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)]. E-mail: ecook@medphys.ucl.ac.uk; Fong, Ruby [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Horrocks, Julie [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Wilkinson, David [HOSDB, Woodcock Hill, Sandridge, Herts. AL4 9HQ (United Kingdom); Speller, Robert [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)

2007-08-15

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra.

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

International Nuclear Information System (INIS)

Cook, Emily; Fong, Ruby; Horrocks, Julie; Wilkinson, David; Speller, Robert

2007-01-01

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra

Three-Dimensional X-Ray Diffraction Technique for Metals Science

DEFF Research Database (Denmark)

Zhang, Yubin; Fan, Guohua

2017-01-01

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

A high resolution, high counting rate bidimensional, MWPC imaging detector for small angle X-ray diffraction studies

International Nuclear Information System (INIS)

Bateman, J.E.; Connolly, J.F.; Sawyer, E.C.; Stephenson, R.

1981-07-01

The performance is reported of a 200 mm x 200 mm X-ray imaging MWPC aimed at applications in small angle X-ray diffraction and scattering. With quantum energies of approximately 8 keV high spatial resolution (+- 0.5 mm x +- 0.14 mm) with a capability for data taking at >approximately 350 kHz is reported. The detection efficiency is approximately 75% and the detector operates as a sealed unit with a long lifetime. (author)

Surface and interface strains studied by x-ray diffraction

International Nuclear Information System (INIS)

Akimoto, Koichi; Emoto, Takashi; Ichimiya, Ayahiko

1998-01-01

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

Direct observation of radial distribution change during tensile deformation of metallic glass by high energy X-ray diffraction method

Energy Technology Data Exchange (ETDEWEB)

Nasu, Toshio, E-mail: nasu@kekexafs.kj.yamagata-u.ac.j [Faculty of Education, Arts and Science, Yamagata University, 1-4-12 Kojirakawa, Yamagata, Yamagata, 990-8560 (Japan); Sasaki, Motokatsu [Faculty of Education, Arts and Science, Yamagata University, 1-4-12 Kojirakawa, Yamagata, Yamagata, 990-8560 (Japan); Usuki, Takeshi; Sekine, Mai [Faculty of Science, Yamagata University, Yamagata 990-8560 (Japan); Takigawa, Yorinobu; Higashi, Kenji [Graduate School of Engineering, Osaka Prefecture University, Sakai 599-8531 (Japan); Kohara, Shinji [Japan Synchrotron Radiation Research Institute, Harima Science Garden City, Sayo town, Hyogo 679-5198 (Japan); Sakurai, Masaki; Wei Zhang; Inoue, Akihisa [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan)

2009-08-26

The purpose of this research is to investigate the micro-mechanism of deformation behavior of metallic glasses. We report the results of direct observations of short-range and medium-range structural change during tensile deformation of metallic glasses by high energy X-ray diffraction method. Cu{sub 50}Zr{sub 50} and Ni{sub 30}Zr{sub 70} metallic glass samples in the ribbon shape (1.5 mm width and 25 mum) were made by using rapid quenching method. Tensile deformation added to the sample was made by using special equipment adopted for measuring the high energy X-ray diffraction. The peaks in pair distribution function g(r) for Cu{sub 50}Zr{sub 50} and N{sub 30}iZr{sub 70} metallic glasses move zigzag into front and into rear during tensile deformation. These results of direct observation on atomic distribution change for Cu{sub 50}Zr{sub 50} and Ni{sub 30}Zr{sub 70} metallic glass ribbons during tensile deformation suggest that the micro-relaxations occur.

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}).

Submicron X-ray diffraction

International Nuclear Information System (INIS)

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

2000-01-01

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

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

Introducing the ARL X'Tra x-ray diffraction system

International Nuclear Information System (INIS)

Harris, L.

2002-01-01

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

Radiation processing with high-energy X-rays

International Nuclear Information System (INIS)

Cleland, Marshall R.; Stichelbaut, Frederic

2009-01-01

The physical, chemical or biological characteristics of selected commercial products and materials can be improved by radiation processing. The ionizing energy can be provided by accelerated electrons with energies between 75 keV and 10 MeV, gamma rays from cobalt-60 with average energies of 1.25 MeV or X-rays with maximum energies up to 7.5 MeV. Electron beams are preferred for thin products, which are processed at high speeds. Gamma rays are used for products that are too thick for treatment with electron beams. High-energy X-rays can also be used for these purposes because their penetration in solid materials is similar to or even slightly greater than that of gamma rays. Previously, the use of X-rays had been inhibited by their slower processing rates and higher costs when compared with gamma rays. Since then, the price of cobalt-60 sources has been increased and the radiation intensity from high-energy, high-power X-ray generators has also increased. For facilities requiring at least 2 MCi of cobalt-60, the capital and operating costs of X-ray facilities with equivalent processing rates can be less than that of gamma-ray irradiators. Several high-energy electron beam facilities have been equipped with removable X-ray targets so that irradiation processes can be done with either type of ionizing energy. A new facility is now being built which will be used exclusively in the X-ray mode to sterilize medical products. Operation of this facility will show that high-energy, high-power X-ray generators are practical alternatives to large gamma-ray sources. (author)

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.

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.

Energy dispersive X-ray diffraction at high pressure in CHESS

International Nuclear Information System (INIS)

Ruoff, A.L.; Baublitz, M.A. Jr.

1981-01-01

Energy dispersive X-ray techniques were used with a diamond anvil cell in the Cornell High Energy Synchrotron Source (CHESS). It was shown that quantitative relative intensity measurement could be made when the pressure was hydrostatic and the crystals were relatively defect free. The crystal structures of the high pressure polymorphs of Ge, GaAs, GaP, and AlSb were studied. Ge exhibits the β-tetragonal structure as found by Jamieson; however, the transition pressure is 80 +- 5 kbars. GaAs exhibits an orthorhombic structure above 172 +- 7 kbars, GaP the β-Sn structure above 215 +- 8 kbars, and AlSb an orthorhombic structure above 77 +- 5 kbars. (Auth.)

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-08-15

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

High-resolution X-ray diffraction with no sample preparation.

Science.gov (United States)

Hansford, G M; Turner, S M R; Degryse, P; Shortland, A J

2017-07-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.

Complete k-space visualization of x-ray photoelectron diffraction

International Nuclear Information System (INIS)

Denlinger, J.D.; Lawrence Berkeley Lab., CA; Rotenberg, E.; Lawrence Berkeley Lab., CA; Kevan, S.D.; Tonner, B.P.

1996-01-01

A highly detailed x-ray photoelectron diffraction data set has been acquired for crystalline Cu(001). The data set for bulk Cu 3p emission encompasses a large k-space volume (k = 3--10 angstrom -1 ) with sufficient energy and angular sampling to monitor the continuous variation of diffraction intensities. The evolution of back-scattered intensity oscillations is visualized by energy and angular slices of this volume data set. Large diffraction data sets such as this will provide rigorous experimental tests of real-space reconstruction algorithms and multiple-scattering simulations

Crystallized solids characterization by X-ray diffraction

International Nuclear Information System (INIS)

Broll, N.

1996-01-01

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

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-10-15

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

A diamond-anvil high-pressure cell for X-ray diffraction on a single crystal

International Nuclear Information System (INIS)

Malinowski, M.

1987-01-01

A new diamond-anvil high-pressure cell is described which can be used in single-crystal X-ray diffraction instruments to collect X-ray intensity data from single-crystal samples up to hydrostatic pressures of about 10 GPa. A unique design allows two types of diffraction geometry to be applied in single-crystal high-pressure diffraction experiments. More than 85% of the Ewald sphere is accessible, and a continuous range of 2θ values is available from 0 up to about 160 0 . Pressure may be calibrated by the ruby fluorescence technique or by the use of an internal X-ray-standard single crystal. The design of our diamond-anvil cell would allow, with little or no modification, operation at high and low temperatures, optical studies and powder diffractometer work. (orig.)

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

International Nuclear Information System (INIS)

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

1977-01-01

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

Characterization of breast tissue using energy-dispersive X-ray diffraction computed tomography

International Nuclear Information System (INIS)

Pani, S.; Cook, E.J.; Horrocks, J.A.; Jones, J.L.; Speller, R.D.

2010-01-01

A method for sample characterization using energy-dispersive X-ray diffraction computed tomography (EDXRDCT) is presented. The procedures for extracting diffraction patterns from the data and the corrections applied are discussed. The procedures were applied to the characterization of breast tissue samples, 6 mm in diameter. Comparison with histological sections of the samples confirmed the possibility of grouping the patterns into five families, corresponding to adipose tissue, fibrosis, poorly differentiated cancer, well differentiated cancer and benign tumour.

Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

International Nuclear Information System (INIS)

Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima; Guimaraes, Luciana; Vieira Filho, Sidney A.

2012-01-01

Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

Energy Technology Data Exchange (ETDEWEB)

Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Quimica; Guimaraes, Luciana [Universidade Federal de Sao Joao Del-Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Vieira Filho, Sidney A., E-mail: bibo@ef.ufop.br [Universidade Federal de Ouro Preto (UFOP), MG (Brazil). Dept. de Farmacia

2012-07-01

Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

X-CHIP: an integrated platform for high-throughput protein crystallization and on-the-chip X-ray diffraction data collection

International Nuclear Information System (INIS)

Kisselman, Gera; Qiu, Wei; Romanov, Vladimir; Thompson, Christine M.; Lam, Robert; Battaile, Kevin P.; Pai, Emil F.; Chirgadze, Nickolay Y.

2011-01-01

The X-CHIP (X-ray Crystallography High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The X-CHIP (X-ray Crystallization High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The system has been designed for crystallization condition screening, visual crystal inspection, initial X-ray screening and data collection in a high-throughput fashion. X-ray diffraction data acquisition can be performed directly on-the-chip at room temperature using an in situ approach. The capabilities of the chip eliminate the necessity for manual crystal handling and cryoprotection of crystal samples, while allowing data collection from multiple crystals in the same drop. This technology would be especially beneficial for projects with large volumes of data, such as protein-complex studies and fragment-based screening. The platform employs hydrophilic and hydrophobic concentric ring surfaces on a miniature plate transparent to visible light and X-rays to create a well defined and stable microbatch crystallization environment. The results of crystallization and data-collection experiments demonstrate that high-quality well diffracting crystals can be grown and high-resolution diffraction data sets can be collected using this technology. Furthermore, the quality of a single-wavelength anomalous dispersion data set collected with the X-CHIP at room temperature was sufficient to generate interpretable electron-density maps. This technology is highly resource-efficient owing to the use of nanolitre-scale drop volumes. It does not require any modification for most in-house and synchrotron beamline systems and offers

X-CHIP: an integrated platform for high-throughput protein crystallization and on-the-chip X-ray diffraction data collection

Energy Technology Data Exchange (ETDEWEB)

Kisselman, Gera; Qiu, Wei; Romanov, Vladimir; Thompson, Christine M.; Lam, Robert [Ontario Cancer Institute, Princess Margaret Hospital, University Health Network, Toronto, Ontario M5G 2C4 (Canada); Battaile, Kevin P. [Argonne National Laboratory, Argonne, Illinois 60439 (United States); Pai, Emil F.; Chirgadze, Nickolay Y., E-mail: nchirgad@uhnresearch.ca [Ontario Cancer Institute, Princess Margaret Hospital, University Health Network, Toronto, Ontario M5G 2C4 (Canada); University of Toronto, Toronto, Ontario M5S 1A8 (Canada)

2011-06-01

The X-CHIP (X-ray Crystallography High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The X-CHIP (X-ray Crystallization High-throughput Integrated Platform) is a novel microchip that has been developed to combine multiple steps of the crystallographic pipeline from crystallization to diffraction data collection on a single device to streamline the entire process. The system has been designed for crystallization condition screening, visual crystal inspection, initial X-ray screening and data collection in a high-throughput fashion. X-ray diffraction data acquisition can be performed directly on-the-chip at room temperature using an in situ approach. The capabilities of the chip eliminate the necessity for manual crystal handling and cryoprotection of crystal samples, while allowing data collection from multiple crystals in the same drop. This technology would be especially beneficial for projects with large volumes of data, such as protein-complex studies and fragment-based screening. The platform employs hydrophilic and hydrophobic concentric ring surfaces on a miniature plate transparent to visible light and X-rays to create a well defined and stable microbatch crystallization environment. The results of crystallization and data-collection experiments demonstrate that high-quality well diffracting crystals can be grown and high-resolution diffraction data sets can be collected using this technology. Furthermore, the quality of a single-wavelength anomalous dispersion data set collected with the X-CHIP at room temperature was sufficient to generate interpretable electron-density maps. This technology is highly resource-efficient owing to the use of nanolitre-scale drop volumes. It does not require any modification for most in-house and synchrotron beamline systems and offers

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

Energy Technology Data Exchange (ETDEWEB)

Murray, Thomas D. [University of California, Berkeley, CA 94720 (United States); Johns Hopkins University School of Medicine, Baltimore, MD 21205 (United States); Lyubimov, Artem Y. [Stanford University, Stanford, CA 94305 (United States); Ogata, Craig M. [Argonne National Laboratory, Argonne, IL 60439 (United States); Vo, Huy [Johns Hopkins University, Baltimore, MD 21205 (United States); Uervirojnangkoorn, Monarin; Brunger, Axel T., E-mail: brunger@stanford.edu [Stanford University, Stanford, CA 94305 (United States); Berger, James M., E-mail: brunger@stanford.edu [Johns Hopkins University School of Medicine, Baltimore, MD 21205 (United States); University of California, Berkeley, CA 94720 (United States)

2015-09-26

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

X-ray topography and multiple diffraction

International Nuclear Information System (INIS)

Chang, S.-L.

1983-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1975-01-07

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Short-time X-ray diffraction with an efficient-optimized, high repetition-rate laser-plasma X-ray-source

International Nuclear Information System (INIS)

Kaehle, Stephan

2009-01-01

This thesis deals with the production and application of ultrashort X-ray pulses. In the beginning different possibilities for the production of X-ray pulses with pulse durations of below one picosecond are presented, whereby the main topic lies on the so called laser-plasma X-ray sources with high repetition rate. In this case ultrashort laser pulses are focused on a metal, so that in the focus intensities of above 10 16 W/cm 2 dominate. In the ideal case in such way ultrafast electrons are produced, which are responsible for line radiation. In these experiments titanium K α radiation is produced, thes photons possess an energy of 4.51 keV. For the efficient production of line radiation here the Ti:Sa laser is optimized in view of the laser energy and the pulse shape and the influence of the different parameters on the K α production systematically studied. The influences of laser intensity, system-conditioned pre-pulses and of phase modulation are checked. It turns out that beside the increasement of the K α radiation by a suited laser intensity a reduction of the X-ray background radiation is of deciding importance for the obtaining of clear diffraction images. This background radiation is mainly composed of bremsstrahlung. It can be suppressed by the avoidance of intrinsic pre-pulses and by means of 2nd-order phase modulation. By means of optical excitation and X-ray exploration experiments the production of acoustic waves after ultrashort optical excitation in a 150 nm thick Ge(111) film on Si(111) is studied. These acoustic waves are driven by thermal (in this time scale time-independent) and electronic (time dependent) pressure amounts. As essential results it turns out that the relative amount of the electronic pressure increases with decreasing excitation density [de

X-ray diffraction studies of NbTe 2 single crystal

Indian Academy of Sciences (India)

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

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.

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

International Nuclear Information System (INIS)

1992-02-01

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

Diffraction enhanced x-ray imaging

International Nuclear Information System (INIS)

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

1997-09-01

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

In-situ high-energy X-ray diffraction and batch Rietveld refinement of phase changes in titanium aluminides

International Nuclear Information System (INIS)

Whitfield, R.

2007-01-01

Full text: We have used the Rietveld refinement method for the analysis of high-energy X-ray power diffraction for quantitatve phase analysis. This method has the advantage of being able to model the multiple phases appearing in the diffraction pattern and tell us about the composition of the phases of a sample as we change the temperature. It has been applied to various TiAl compounds allowing us to follow in detail the phase transitions of the intermetallics when heated to around 1400 0 Cand subsequently cooled. Small amounts of additives like V, Cr and Gd as well as signatures from different production processes can be seen to have an effect on the phase transitions. With increasing temperature we can see the evolution of the unit cell due to thermal expansion, chemical segregation and the relative proportion of phase changes

Development of Compton X-ray spectrometer for high energy resolution single-shot high-flux hard X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Kojima, Sadaoki, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Ikenouchi, Takahito; Arikawa, Yasunobu; Sakata, Shohei; Zhang, Zhe; Abe, Yuki; Nakai, Mitsuo; Nishimura, Hiroaki; Shiraga, Hiroyuki; Fujioka, Shinsuke, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Azechi, Hiroshi [Institute of Laser Engineering, Osaka University, 2-6 Yamada-oka, Suita, Osaka 565-0871 (Japan); Ozaki, Tetsuo [National Institute for Fusion Science, 322-6 Oroshi, Toki, Gifu 509-5292 (Japan); Miyamoto, Shuji; Yamaguchi, Masashi; Takemoto, Akinori [Laboratory of Advanced Science and Technology for Industry, University of Hyogo, 3-1-2 Kouto, Kamigori-cho, Ako-gun, Hyogo 678-1205 (Japan)

2016-04-15

Hard X-ray spectroscopy is an essential diagnostics used to understand physical processes that take place in high energy density plasmas produced by intense laser-plasma interactions. A bundle of hard X-ray detectors, of which the responses have different energy thresholds, is used as a conventional single-shot spectrometer for high-flux (>10{sup 13} photons/shot) hard X-rays. However, high energy resolution (Δhv/hv < 0.1) is not achievable with a differential energy threshold (DET) X-ray spectrometer because its energy resolution is limited by energy differences between the response thresholds. Experimental demonstration of a Compton X-ray spectrometer has already been performed for obtaining higher energy resolution than that of DET spectrometers. In this paper, we describe design details of the Compton X-ray spectrometer, especially dependence of energy resolution and absolute response on photon-electron converter design and its background reduction scheme, and also its application to the laser-plasma interaction experiment. The developed spectrometer was used for spectroscopy of bremsstrahlung X-rays generated by intense laser-plasma interactions using a 200 μm thickness SiO{sub 2} converter. The X-ray spectrum obtained with the Compton X-ray spectrometer is consistent with that obtained with a DET X-ray spectrometer, furthermore higher certainly of a spectral intensity is obtained with the Compton X-ray spectrometer than that with the DET X-ray spectrometer in the photon energy range above 5 MeV.

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Opalescence of quartz: a study by high energy x-ray diffraction

Science.gov (United States)

Bastie, P.; Dolino, G.; Hamelin, B.

2003-05-01

The origin of the opalescence observed at the α-β transition of quartz remains an open question. This intense light scattering occurs during the coexistence, at the first order transition, of the α and incommensurate (inc) phases, in the vicinity of the phase interface. New hard x-ray diffraction experiment shows that the large angle light scattering is mainly in the α-phase region of the crystal and reveals the existence of an intermediate structure between the α-phase and the 3q inc phase.

Opalescence of quartz: a study by high energy x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Bastie, P [Laboratoire de Spectrometrie Physique, Universite Joseph Fourier-Grenoble 1 - CNRS, UMR No 5588, BP 87, 38402 Saint Martin d' Heres Cedex (France); Dolino, G [Laboratoire de Spectrometrie Physique, Universite Joseph Fourier-Grenoble 1 - CNRS, UMR No 5588, BP 87, 38402 Saint Martin d' Heres Cedex (France); Hamelin, B [Institut Laue Langevin, BP 156X, 38042 Grenoble Cedex 9 (France)

2003-05-21

The origin of the opalescence observed at the {alpha}-{beta} transition of quartz remains an open question. This intense light scattering occurs during the coexistence, at the first order transition, of the {alpha} and incommensurate (inc) phases, in the vicinity of the phase interface. New hard x-ray diffraction experiment shows that the large angle light scattering is mainly in the {alpha}-phase region of the crystal and reveals the existence of an intermediate structure between the {alpha}-phase and the 3q inc phase.

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.

X-ray Microprobe for Fluorescence and Diffraction Analysis

International Nuclear Information System (INIS)

Ice, G.E.

2005-01-01

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

X-ray topography under conditions of monochromatic spherical wave diffraction

International Nuclear Information System (INIS)

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

1981-01-01

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

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

International Nuclear Information System (INIS)

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

1994-01-01

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

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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.

Treatment of foods with high-energy X rays

International Nuclear Information System (INIS)

Cleland, M.R.; Meissner, J.; Herer, A.S.; Beers, E.W.

2001-01-01

The treatment of foods with ionizing energy in the form of gamma rays, accelerated electrons, and X rays can produce beneficial effects, such as inhibiting the sprouting in potatoes, onions, and garlic, controlling insects in fruits, vegetables, and grains, inhibiting the growth of fungi, pasteurizing fresh meat, poultry, and seafood, and sterilizing spices and food additives. After many years of research, these processes have been approved by regulatory authorities in many countries and commercial applications have been increasing. High-energy X rays are especially useful for treating large packages of food. The most attractive features are product penetration, absorbed dose uniformity, high utilization efficiency and short processing time. The ability to energize the X-ray source only when needed enhances the safety and convenience of this technique. The availability of high-energy, high-power electron accelerators, which can be used as X-ray generators, makes it feasible to process large quantities of food economically. Several industrial accelerator facilities already have X-ray conversion equipment and several more will soon be built with product conveying systems designed to take advantage of the unique characteristics of high-energy X rays. These concepts will be reviewed briefly in this paper

Treatment of foods with high-energy X rays

Science.gov (United States)

Cleland, M. R.; Meissner, J.; Herer, A. S.; Beers, E. W.

2001-07-01

The treatment of foods with ionizing energy in the form of gamma rays, accelerated electrons, and X rays can produce beneficial effects, such as inhibiting the sprouting in potatoes, onions, and garlic, controlling insects in fruits, vegetables, and grains, inhibiting the growth of fungi, pasteurizing fresh meat, poultry, and seafood, and sterilizing spices and food additives. After many years of research, these processes have been approved by regulatory authorities in many countries and commercial applications have been increasing. High-energy X rays are especially useful for treating large packages of food. The most attractive features are product penetration, absorbed dose uniformity, high utilization efficiency and short processing time. The ability to energize the X-ray source only when needed enhances the safety and convenience of this technique. The availability of high-energy, high-power electron accelerators, which can be used as X-ray generators, makes it feasible to process large quantities of food economically. Several industrial accelerator facilities already have X-ray conversion equipment and several more will soon be built with product conveying systems designed to take advantage of the unique characteristics of high-energy X rays. These concepts will be reviewed briefly in this paper.

Diffraction enhanced kinetic depth X-ray imaging

Science.gov (United States)

Dicken, A.

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

High-speed classification of coherent X-ray diffraction patterns on the K computer for high-resolution single biomolecule imaging

Energy Technology Data Exchange (ETDEWEB)

Tokuhisa, Atsushi [RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Arai, Junya [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Joti, Yasumasa [JASRI, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Ohno, Yoshiyuki; Kameyama, Toyohisa; Yamamoto, Keiji; Hatanaka, Masayuki; Gerofi, Balazs; Shimada, Akio; Kurokawa, Motoyoshi; Shoji, Fumiyoshi [RIKEN Advanced Institute for Computational Science, 7-1-26 Minatojima-minami-machi, Chuo-ku, Kobe, Hyogo 650-0047 (Japan); Okada, Kensuke [RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Sugimoto, Takashi [JASRI, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Yamaga, Mitsuhiro; Tanaka, Ryotaro [RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Yokokawa, Mitsuo; Hori, Atsushi [RIKEN Advanced Institute for Computational Science, 7-1-26 Minatojima-minami-machi, Chuo-ku, Kobe, Hyogo 650-0047 (Japan); Ishikawa, Yutaka, E-mail: ishikawa@is.s.u-tokyo.ac.jp [The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Hatsui, Takaki, E-mail: ishikawa@is.s.u-tokyo.ac.jp [RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Go, Nobuhiro [Japan Atomic Energy Agency, 8-1-7 Umemidai, Kizugawa, Kyoto 619-0215 (Japan)

2013-11-01

A code with an algorithm for high-speed classification of X-ray diffraction patterns has been developed. Results obtained for a set of 1 × 10{sup 6} simulated diffraction patterns are also reported. Single-particle coherent X-ray diffraction imaging using an X-ray free-electron laser has the potential to reveal the three-dimensional structure of a biological supra-molecule at sub-nanometer resolution. In order to realise this method, it is necessary to analyze as many as 1 × 10{sup 6} noisy X-ray diffraction patterns, each for an unknown random target orientation. To cope with the severe quantum noise, patterns need to be classified according to their similarities and average similar patterns to improve the signal-to-noise ratio. A high-speed scalable scheme has been developed to carry out classification on the K computer, a 10PFLOPS supercomputer at RIKEN Advanced Institute for Computational Science. It is designed to work on the real-time basis with the experimental diffraction pattern collection at the X-ray free-electron laser facility SACLA so that the result of classification can be feedback for optimizing experimental parameters during the experiment. The present status of our effort developing the system and also a result of application to a set of simulated diffraction patterns is reported. About 1 × 10{sup 6} diffraction patterns were successfully classificatied by running 255 separate 1 h jobs in 385-node mode.

X-ray diffraction

International Nuclear Information System (INIS)

Vries, J.L. de.

1976-01-01

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

Powder X-ray diffraction study af alkali alanates

DEFF Research Database (Denmark)

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

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

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

Science.gov (United States)

Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

2017-06-01

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

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

International Nuclear Information System (INIS)

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

2004-01-01

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

HIGH ENERGY, HIGH BRIGHTNESS X-RAYS PRODUCED BY COMPTON BACKSCATTERING AT THE LIVERMORE PLEIADES FACILITY

International Nuclear Information System (INIS)

Tremaine, A M; Anderson, S G; Betts, S; Crane, J; Gibson, D J; Hartemann, F V; Jacob, J S; Frigola, P; Lim, J; Rosenzweig, J; Travish, G

2005-01-01

PLEIADES (Picosecond Laser Electron Interaction for the Dynamic Evaluation of Structures) produces tunable 30-140 keV x-rays with 0.3-5 ps pulse lengths and up to 10 7 photons/pulse by colliding a high brightness electron beam with a high power laser. The electron beam is created by an rf photo-injector system, accelerated by a 120 MeV linac, and focused to 20 (micro)m with novel permanent magnet quadrupoles. To produce Compton back scattered x-rays, the electron bunch is overlapped with a Ti:Sapphire laser that delivers 500 mJ, 100 fs, pulses to the interaction point. K-edge radiography at 115 keV on Uranium has verified the angle correlated energy spectrum inherent in Compton scattering and high-energy tunability of the Livermore source. Current upgrades to the facility will allow laser pumping of targets synchronized to the x-ray source enabling dynamic diffraction and time-resolved studies of high Z materials. Near future plans include extending the radiation energies to >400 keV, allowing for nuclear fluorescence studies of materials

X-ray powder diffraction camera for high-field experiments

International Nuclear Information System (INIS)

Koyama, K; Mitsui, Y; Takahashi, K; Watanabe, K

2009-01-01

We have designed a high-field X-ray diffraction (HF-XRD) camera which will be inserted into an experimental room temperature bore (100 mm) of a conventional solenoid-type cryocooled superconducting magnet (10T-CSM). Using the prototype camera that is same size of the HF-XRD camera, a XRD pattern of Si is taken at room temperature in a zero magnetic field. From the obtained results, the expected ability of the designed HF-XRD camera is presented.

ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

International Nuclear Information System (INIS)

Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

1987-01-01

A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

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

International Nuclear Information System (INIS)

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

2016-01-01

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

Applications of a pnCCD detector coupled to columnar structure CsI(Tl) scintillator system in ultra high energy X-ray Laue diffraction

Science.gov (United States)

Shokr, M.; Schlosser, D.; Abboud, A.; Algashi, A.; Tosson, A.; Conka, T.; Hartmann, R.; Klaus, M.; Genzel, C.; Strüder, L.; Pietsch, U.

2017-12-01

Most charge coupled devices (CCDs) are made of silicon (Si) with typical active layer thicknesses of several microns. In case of a pnCCD detector the sensitive Si thickness is 450 μm. However, for silicon based detectors the quantum efficiency for hard X-rays drops significantly for photon energies above 10 keV . This drawback can be overcome by combining a pixelated silicon-based detector system with a columnar scintillator. Here we report on the characterization of a low noise, fully depleted 128×128 pixels pnCCD detector with 75×75 μm2 pixel size coupled to a 700 μm thick columnar CsI(Tl) scintillator in the photon range between 1 keV to 130 keV . The excellent performance of the detection system in the hard X-ray range is demonstrated in a Laue type X-ray diffraction experiment performed at EDDI beamline of the BESSY II synchrotron taken at a set of several GaAs single crystals irradiated by white synchrotron radiation. With the columnar structure of the scintillator, the position resolution of the whole system reaches a value of less than one pixel. Using the presented detector system and considering the functional relation between indirect and direct photon events Laue diffraction peaks with X-ray energies up to 120 keV were efficiently detected. As one of possible applications of the combined CsI-pnCCD system we demonstrate that the accuracy of X-ray structure factors extracted from Laue diffraction peaks can be significantly improved in hard X-ray range using the combined CsI(Tl)-pnCCD system compared to a bare pnCCD.

Structural investigation of GaInP nanowires using X-ray diffraction

DEFF Research Database (Denmark)

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

2013-01-01

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

Effect of strontium on liquid structure of Al-Si hypoeutectic alloys using high-energy X-ray diffraction

International Nuclear Information System (INIS)

Srirangam, P.; Kramer, M.J.; Shankar, S.

2011-01-01

High-energy X-ray diffraction experiments were performed using a synchrotron beam source to investigate the effect of strontium on the liquid atomic structure of Al-Si hypoeutectic alloys. The high-temperature liquid diffraction experiments were carried out on Al alloys with 3, 7, 10 and 12.5 (eutectic) wt.% Si, respectively, with 0 and 0.04 wt.% addition of Sr to each of the alloys. Further, the diffraction data for all the alloys were obtained at various melt temperatures (5-220 K) above the respective liquidus temperature. It was observed that the addition of 0.04 wt.% Sr results in significant change in the liquid structure parameters, such as structure factor, pair distribution function, radial distribution function, coordination number and packing density, at any given melt temperature of the alloy. Salient observations were that, for any specific alloy and temperature, addition of Sr significantly decreases coordination number and packing density. Further, with the addition of Sr in the liquid alloy, the atomic coordination number and packing density increases with decreasing temperature and decreasing Si content of the alloy. The results coupled with prior knowledge have enabled an in-depth understanding of the nucleation environment of the solidifying phases, specifically the role of Sr in delaying the clustering tendencies (nucleation) of the eutectic Si phase.

100 years of discovery of X-ray diffraction

International Nuclear Information System (INIS)

Zhang Tao

2012-01-01

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

A super-high angular resolution principle for coded-mask X-ray imaging beyond the diffraction limit of a single pinhole

International Nuclear Information System (INIS)

Zhang Chen; Zhang Shuangnan

2009-01-01

High angular resolution X-ray imaging is always useful in astrophysics and solar physics. In principle, it can be performed by using coded-mask imaging with a very long mask-detector distance. Previously, the diffraction-interference effect was thought to degrade coded-mask imaging performance dramatically at the low energy end with its very long mask-detector distance. The diffraction-interference effect is described with numerical calculations, and the diffraction-interference cross correlation reconstruction method (DICC) is developed in order to overcome the imaging performance degradation. Based on the DICC, a super-high angular resolution principle (SHARP) for coded-mask X-ray imaging is proposed. The feasibility of coded mask imaging beyond the diffraction limit of a single pinhole is demonstrated with simulations. With the specification that the mask element size is 50 x 50 μm 2 and the mask-detector distance is 50 m, the achieved angular resolution is 0.32 arcsec above about 10 keV and 0.36 arcsec at 1.24 keV (λ = 1 nm), where diffraction cannot be neglected. The on-axis source location accuracy is better than 0.02 arcsec. Potential applications for solar observations and wide-field X-ray monitors are also briefly discussed. (invited reviews)

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

CERN Document Server

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

2001-01-01

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

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

International Nuclear Information System (INIS)

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

2001-01-01

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

High pressure x-ray diffraction studies on U-Al systems

International Nuclear Information System (INIS)

Sahu, P.Ch.; Chandra Shekar, N.V.; Subramanian, N.; Yousuf, Mohammad; Govinda Rajan, K.

1995-01-01

In this paper, high pressure x-ray diffraction studies of the three U-Al compounds, namely, UAl 2 , UAl 3 and UAl 4 are presented. The experiments are carried out using a unique diamond anvil high pressure x-ray diffraction system in the Guinier geometry up to a maximum pressure of ∼ 35 GPa. The compressibility behaviour of UAl 2 is consistent with its itinerant 5f states, whereas that of UAl 3 and UAl 4 indicate more towards their localized nature. Among these three compounds, a structural phase transition in UAl 2 has been observed at ∼ 11 GPa and the structure of the high pressure phase has been identified to be of MgNi 2 type with space group P6 3 /mmc. The structure of UAl 2 at NTP is of MgCu 2 type with space group Fd3m. From the electron to atom ratio (e/α) consideration, another structural phase transition, namely, MgNi 2 -MgCu 2 at a higher pressure is proposed. Further, on a similar consideration, a new pressure induced structural sequence, namely, MgCu 2 -MgNi 2 (or MgZn 2 -MgCu 2 ) in the AB 2 type compounds of the f electron based systems is suggested. (author)

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

International Nuclear Information System (INIS)

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

2004-01-01

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

Structural investigations of interfaces in Fe{sub 90}Sc{sub 10} nanoglasses using high-energy x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Ghafari, M.; Gleiter, H.; Feng, T. [Karlsruhe Institute of Technology (KIT), Institute for Nanotechnology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Kohara, S. [Research and Utilization Division, Japan Synchrotron Radiation Research Institute/SPring-8, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Hahn, H.; Witte, R. [Karlsruhe Institute of Technology (KIT), Institute for Nanotechnology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); KIT-TUD Joint Research Laboratory Nanomaterials, Technische Universitaet Darmstadt, Petersenstr. 32, 64287 Darmstadt (Germany); Kamali, S. [Department of Chemistry, University of California, One Shields Ave., Davis, California 95616 (United States)

2012-03-26

High-resolution diffraction experiments of Fe{sub 90}Sc{sub 10} nanoglasses and rapidly quenched metallic glasses as reference materials have been performed using high-energy x-rays with a wavelength of 0.21 Angst from a synchrotron radiation source. Nanoglasses are amorphous alloys with a significant fraction of interfaces on the nanometer scale. The short- and intermediate-range orders of a nanoglass are different from the well known amorphous materials produced by rapid quenching from the melt. These structural modifications have significant influence on the physical properties. In this paper, the short- and intermediate-range orders of the nanoglass Fe{sub 90}Sc{sub 10} and the reference metallic glass Fe{sub 90}Sc{sub 10} alloy prepared by rapid quenching are discussed.

One dimensional detector for X-ray diffraction with superior energy resolution based on silicon strip detector technology

International Nuclear Information System (INIS)

Dąbrowski, W; Fiutowski, T; Wiącek, P; Fink, J; Krane, H-G

2012-01-01

1-D position sensitive X-ray detectors based on silicon strip detector technology have become standard instruments in X-ray diffraction and are available from several vendors. As these devices have been proven to be very useful and efficient further improvement of their performance is investigated. The silicon strip detectors in X-ray diffraction are primarily used as counting devices and the requirements concerning the spatial resolution, dynamic range and count rate capability are of primary importance. However, there are several experimental issues in which a good energy resolution is important. The energy resolution of silicon strip detectors is limited by the charge sharing effects in the sensor as well as by noise of the front-end electronics. The charge sharing effects in the sensor and various aspects of the electronics, including the baseline fluctuations, which affect the energy resolution, have been analyzed in detail and a new readout concept has been developed. A front-end ASIC with a novel scheme of baseline restoration and novel interstrip logic circuitry has been designed. The interstrip logic is used to reject the events resulting in significant charge sharing between neighboring strips. At the expense of rejecting small fraction of photons entering the detector one can obtain single strip energy spectra almost free of charge sharing effects. In the paper we present the design considerations and measured performance of the detector being developed. The electronic noise of the system at room temperature is typically of the order of 70 el rms for 17 mm long silicon strips and a peaking time of about 1 μs. The energy resolution of 600 eV FWHM has been achieved including the non-reducible charge sharing effects and the electronic noise. This energy resolution is sufficient to address a common problem in X-ray diffraction, i.e. electronic suppression of the fluorescence radiation from samples containing iron or cobalt while irradiated with 8.04 ke

A new X-ray pinhole camera for energy dispersive X-ray fluorescence imaging with high-energy and high-spatial resolution

Energy Technology Data Exchange (ETDEWEB)

Romano, F.P., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Altana, C. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy); Cosentino, L.; Celona, L.; Gammino, S.; Mascali, D. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Pappalardo, L. [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Rizzo, F. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy)

2013-08-01

A new X-ray pinhole camera for the Energy Dispersive X-ray Fluorescence (ED-XRF) imaging of materials with high-energy and high-spatial resolution, was designed and developed. It consists of a back-illuminated and deep depleted CCD detector (composed of 1024 × 1024 pixels with a lateral size of 13 μm) coupled to a 70 μm laser-drilled pinhole-collimator, positioned between the sample under analysis and the CCD. The X-ray pinhole camera works in a coaxial geometry allowing a wide range of magnification values. The characteristic X-ray fluorescence is induced on the samples by irradiation with an external X-ray tube working at a maximum power of 100 W (50 kV and 2 mA operating conditions). The spectroscopic capabilities of the X-ray pinhole camera were accurately investigated. Energy response and energy calibration of the CCD detector were determined by irradiating pure target-materials emitting characteristic X-rays in the energy working-domain of the system (between 3 keV and 30 keV). Measurements were performed by using a multi-frame acquisition in single-photon counting. The characteristic X-ray spectra were obtained by an automated processing of the acquired images. The energy resolution measured at the Fe–Kα line is 157 eV. The use of the X-ray pinhole camera for the 2D resolved elemental analysis was investigated by using reference-patterns of different materials and geometries. The possibility of the elemental mapping of samples up to an area of 3 × 3 cm{sup 2} was demonstrated. Finally, the spatial resolution of the pinhole camera was measured by analyzing the profile function of a sharp-edge. The spatial resolution determined at the magnification values of 3.2 × and 0.8 × (used as testing values) is about 90 μm and 190 μm respectively. - Highlights: • We developed an X-ray pinhole camera for the 2D X-ray fluorescence imaging. • X-ray spectra are obtained by a multi-frame acquisition in single photon mode. • The energy resolution in the X-ray

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...... the wurtzite phase was retained up to 60 GPa in the case of nanocrystalline GaN. The bulk moduli for the wurtzite phases were determined to be 187 ( 7) and 319 ( 10) GPa for the bulk- and nanocrystalline phases, respectively, while the respective NaCl phases were found to have very similar bulk moduli [ 208...

Diffraction anomalous fine structure using X-ray anomalous dispersion

International Nuclear Information System (INIS)

Soejima, Yuji; Kuwajima, Shuichiro

1998-01-01

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

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

International Nuclear Information System (INIS)

Tanaka, M; Katsuya, Y; Matsushita, Y

2013-01-01

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

X-ray diffraction identification of clay minerals by microcomputer

International Nuclear Information System (INIS)

Rodrigues, S.; Imasava, F.J.

1988-01-01

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

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.

Automated high pressure cell for pressure jump x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Brooks, Nicholas J.; Gauthe, Beatrice L. L. E.; Templer, Richard H.; Ces, Oscar; Seddon, John M. [Department of Chemistry, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Terrill, Nick J. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Rogers, Sarah E. [ISIS, Rutherford Appleton Laboratory, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0QX (United Kingdom)

2010-06-15

A high pressure cell for small and wide-angle x-ray diffraction measurements of soft condensed matter samples has been developed, incorporating a fully automated pressure generating network. The system allows both static and pressure jump measurements in the range of 0.1-500 MPa. Pressure jumps can be performed as quickly as 5 ms, both with increasing and decreasing pressures. Pressure is generated by a motorized high pressure pump, and the system is controlled remotely via a graphical user interface to allow operation by a broad user base, many of whom may have little previous experience of high pressure technology. Samples are loaded through a dedicated port allowing the x-ray windows to remain in place throughout an experiment; this facilitates accurate subtraction of background scattering. The system has been designed specifically for use at beamline I22 at the Diamond Light Source, United Kingdom, and has been fully integrated with the I22 beamline control systems.

Automated high pressure cell for pressure jump x-ray diffraction

International Nuclear Information System (INIS)

Brooks, Nicholas J.; Gauthe, Beatrice L. L. E.; Templer, Richard H.; Ces, Oscar; Seddon, John M.; Terrill, Nick J.; Rogers, Sarah E.

2010-01-01

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.

X-ray diffraction at high pressure and high/low temperatures using synchrotron radiation. Applications in the study of spinel structures

International Nuclear Information System (INIS)

Gerward, L.; Jiang, J.Z.; Olsen, J.S.; Recio, J.M.; Wakowska, A.

2004-01-01

High-pressure x-ray diffraction made a quantum leap in the 1960's with the advent of the diamond-anvil cell. This ingenious device, where two opposing diamond faces apply pressure to a tiny sample, made it possible to replicate the pressure near the core of the Earth by turning a thumbscrew. Multianvil cells, such as the Japanese MAX80 press, were developed for combined high-pressure and high-temperature studies. The availability n at about the same time n of dedicated synchrotron radiation sources of hard x-rays was another big step forward. Since then, the white-beam energy-dispersive method has been the workhorse for high pressure, high-temperature x-ray diffraction, although it is now gradually being replaced by high-resolution monochromatic methods based on the image plate, the CCD camera or other electronic area detectors. The first part of the paper is a review of high-pressure x-ray diffraction (HPXRD), covering roughly the last three decades. Physical parameters, such as the bulk modulus, the compressibility and the equation of state, are defined. The diamond-anvil cell, the multianvil press and other high-pressure devices are described, as well as synchrotron radiation sources and recording techniques. Examples are drawn from current experimental and theoretical research on crystal structures of the spinel type. Accurate structural parameters have been determined at ambient conditions and at low temperatures using single-crystal diffraction and four-circle diffractometers. The uniform high-pressure behavior of the oxide spinels has been investigated in detail and compared with the corresponding behavior of selenium-based spinels. The synthesis of advanced novel materials is exemplified in the case of the cubic spinel Si 3 N 4 . This and other nitrogen spinels, which have a bulk modulus of about 300 GPa modulated by the actual cation, are opening a road towards superhard materials. The paper finishes off with an outlook into the future, where new

Three-dimensional x-ray diffraction detection and visualization

International Nuclear Information System (INIS)

Allahkarami, Masoud; Hanan, Jay C

2014-01-01

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

The structure of molten CuCl: Reverse Monte Carlo modeling with high-energy X-ray diffraction data and molecular dynamics of a polarizable ion model

Energy Technology Data Exchange (ETDEWEB)

Alcaraz, Olga; Trullàs, Joaquim, E-mail: quim.trullas@upc.edu [Departament de Física i Enginyeria Nuclear, Universitat Politècnica de Catalunya, Campus Nord UPC B4-B5, 08034 Barcelona (Spain); Tahara, Shuta [Department of Physics and Earth Sciences, Faculty of Science, University of the Ryukyus, Okinawa 903-0213 (Japan); Kawakita, Yukinobu [J-PARC Center, Japan Atomic Energy Agency (JAEA), Ibaraki 319-1195 (Japan); Takeda, Shin’ichi [Department of Physics, Faculty of Sciences, Kyushu University, Fukuoka 819-0395 (Japan)

2016-09-07

The results of the structural properties of molten copper chloride are reported from high-energy X-ray diffraction measurements, reverse Monte Carlo modeling method, and molecular dynamics simulations using a polarizable ion model. The simulated X-ray structure factor reproduces all trends observed experimentally, in particular the shoulder at around 1 Å{sup −1} related to intermediate range ordering, as well as the partial copper-copper correlations from the reverse Monte Carlo modeling, which cannot be reproduced by using a simple rigid ion model. It is shown that the shoulder comes from intermediate range copper-copper correlations caused by the polarized chlorides.

The structure of molten CuCl: Reverse Monte Carlo modeling with high-energy X-ray diffraction data and molecular dynamics of a polarizable ion model

International Nuclear Information System (INIS)

Alcaraz, Olga; Trullàs, Joaquim; Tahara, Shuta; Kawakita, Yukinobu; Takeda, Shin’ichi

2016-01-01

The results of the structural properties of molten copper chloride are reported from high-energy X-ray diffraction measurements, reverse Monte Carlo modeling method, and molecular dynamics simulations using a polarizable ion model. The simulated X-ray structure factor reproduces all trends observed experimentally, in particular the shoulder at around 1 Å −1 related to intermediate range ordering, as well as the partial copper-copper correlations from the reverse Monte Carlo modeling, which cannot be reproduced by using a simple rigid ion model. It is shown that the shoulder comes from intermediate range copper-copper correlations caused by the polarized chlorides.

Highly sensitive x-ray detectors in the low-energy range on n-type 4H-SiC epitaxial layers

Energy Technology Data Exchange (ETDEWEB)

Mandal, Krishna C.; Muzykov, Peter G. [Department of Electrical Engineering, University of South Carolina, Columbia, South Carolina 29208 (United States); Russell Terry, J. [Space Science and Applications Group (ISR-1), Intelligence and Space Research Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

2012-07-30

Schottky diodes on n-type 4H-SiC epitaxial layers have been fabricated for low-energy x-ray detection. The detectors were highly sensitive to soft x-rays and showed improved response compared to the commercial SiC UV photodiodes. Current-voltage characteristics at 475 K showed low leakage current revealing the possibility of high temperature operation. The high quality of the epi-layer was confirmed by x-ray diffraction and chemical etching. Thermally stimulated current measurements performed at 94-550 K revealed low density of deep levels which may cause charge trapping. No charge trapping on detectors' responsivity in the low x-ray energy was found.

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr 0.67 Sr 0.33 MnO 3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam

Thin film characterisation by advanced X-ray diffraction techniques

International Nuclear Information System (INIS)

Cappuccio, G.; Terranova, M.L.

1996-09-01

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

An introduction to three-dimensional X-ray diffraction microscopy

DEFF Research Database (Denmark)

Poulsen, Henning Friis

2012-01-01

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

Multiple x-ray diffraction simulation and applications

International Nuclear Information System (INIS)

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

1989-09-01

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

30-lens interferometer for high energy x-rays

Energy Technology Data Exchange (ETDEWEB)

Lyubomirskiy, M., E-mail: lyubomir@esrf.fr; Snigireva, I., E-mail: irina@esrf.fr; Vaughan, G. [European Synchrotron Radiation facility (ESRF), CS 40220, 71, av des Martyrs, F-38043, Grenoble (France); Kohn, V. [National Research Centre “Kurchatov Institute”, 123182, Moscow (Russian Federation); Kuznetsov, S.; Yunkin, V. [Institute of Microelectronics Technology RAS, 142432, Chernogolovka (Russian Federation); Snigirev, A. [Baltic Federal University, 236041, Kaliningrad (Russian Federation)

2016-07-27

We report a hard X-ray multilens interferometer consisting of 30 parallel compound refractive lenses. Under coherent illumination each CRL creates a diffraction limited focal spot - secondary source. An overlapping of coherent beams from these sources resulting in the interference pattern which has a rich longitudinal structure in accordance with the Talbot imaging formalism. The proposed interferometer was experimentally tested at ID11 ESRF beamline for the photon energies 32 keV and 65 keV. The fundamental and fractional Talbot images were recorded with the high resolution CCD camera. An effective source size in the order of 15 µm was determined from the first Talbot image proving that the multilens interferometer can be used as a high resolution beam diagnostic tool.

X-ray diffraction microtomography using synchrotron radiation

CERN Document Server

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

2001-01-01

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

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

International Nuclear Information System (INIS)

Ito, K.; Amemiya, Y.

1999-01-01

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

X-ray absorption intensity at high-energy region

International Nuclear Information System (INIS)

Fujikawa, Takashi; Kaneko, Katsumi

2012-01-01

We theoretically discuss X-ray absorption intensity in high-energy region far from the deepest core threshold to explain the morphology-dependent mass attenuation coefficient of some carbon systems, carbon nanotubes (CNTs), highly oriented pyrolytic graphite (HOPG) and fullerenes (C 60 ). The present theoretical approach is based on the many-body X-ray absorption theory including the intrinsic losses (shake-up losses). In the high-energy region the absorption coefficient has correction term dependent on the solid state effects given in terms of the polarization part of the screened Coulomb interaction W p . We also discuss the tail of the valence band X-ray absorption intensity. In the carbon systems C 2s contribution has some influence on the attenuation coefficient even in the high energy region at 20 keV.

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

International Nuclear Information System (INIS)

Masiello, F.

2011-05-01

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

Molecular beam epitaxial growth mechanism of ZnSe epilayers on (100) GaAs as determined by reflection high-energy electron diffraction, transmission electron microscopy and X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Ruppert, P.; Hommel, D.; Behr, T.; Heinke, H.; Waag, A.; Landwehr, G. (Physikalisches Inst., Univ. Wuerzburg (Germany))

1994-04-14

The properties of molecular beam epitaxial growth of ZnSe epilayers deposited directly on a GaAs substrate are compared to those grown on a GaAs buffer layer. The superior quality of the latter is confirmed by RHEED, TEM and X-ray diffraction. Based on RHEED oscillation studies, a model explaining the dependence of the ZnSe growth rate on Zn and Se fluxes and the substrate temperature is developed taking into account physisorbed and chemisorbed states. For partially relaxed epilayers, the correlation between the relaxation state and the crystalline mosaicity, as found by high resolution X-ray diffraction, is discussed

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

X-ray diffraction

International Nuclear Information System (INIS)

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

1982-01-01

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

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

NARCIS (Netherlands)

1996-01-01

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

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

DEFF Research Database (Denmark)

Frankær, Christian Grundahl

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

Refractive x-ray lens for high pressure diffraction

International Nuclear Information System (INIS)

Ohishi, Yasuo

2001-01-01

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

X-ray diffraction patterns and diffracted intensity of Kα spectral lines of He-like ions

Science.gov (United States)

Goyal, Arun; Khatri, Indu; Singh, A. K.; Sharma, Rinku; Mohan, Man

2017-09-01

In the present paper, we have calculated fine-structure energy levels related to the configurations 1s2s, 1s2p, 1s3s and 1s3p by employing GRASP2K code. We have also computed radiative data for transitions from 1s2p 1 P1o, 1s2p 3 P2o, 1s2p 3 P1o and 1s2s 3S1 to the ground state 1s2. We have made comparisons of our presented energy levels and transition wavelengths with available results compiled by NIST and good agreement is achieved. We have also provided X-ray diffraction (XRD) patterns of Kα spectral lines, namely w, x, y and z of Cu XXVIII, Kr XXXV and Mo with diffraction angle and maximum diffracted intensity which is not published elsewhere in the literature. We believe that our presented results may be beneficial in determination of the order parameter, X-ray crystallography, solid-state drug analysis, forensic science, geological and medical applications.

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...

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Prospects of high-resolution resonant X-ray inelastic scattering studies on solid materials, liquids and gases at diffraction-limited storage rings

International Nuclear Information System (INIS)

Schmitt, Thorsten; Groot, Frank M. F. de; Rubensson, Jan-Erik

2014-01-01

Diffraction-limited storage rings will allow for pushing the achievable energy resolution, signal intensity and the sampled spot size in resonant inelastic X-ray scattering (RIXS) experiments to new limits. In this article the types of improved soft X-ray RIXS studies that will become possible with these instrumental improvements are envisioned. The spectroscopic technique of resonant inelastic X-ray scattering (RIXS) will particularly profit from immensely improved brilliance of diffraction-limited storage rings (DLSRs). In RIXS one measures the intensities of excitations as a function of energy and momentum transfer. DLSRs will allow for pushing the achievable energy resolution, signal intensity and the sampled spot size to new limits. With RIXS one nowadays probes a broad range of electronic systems reaching from simple molecules to complex materials displaying phenomena like peculiar magnetism, two-dimensional electron gases, superconductivity, photovoltaic energy conversion and heterogeneous catalysis. In this article the types of improved RIXS studies that will become possible with X-ray beams from DLSRs are envisioned

Study of the Elasto-plastic Properties of Mineralized Biomaterials via Synchrotron High-energy X-ray Diffraction

Science.gov (United States)

Deymier-Black, Alix Christine

Synchrotron high-energy X-ray diffraction was employed to investigate the strains in the hydroxyapatite (HAP) platelets and mineralized collagen fibrils in bovine dentin and cortical bone. The HAP and the fibrillar apparent moduli, defined as the applied stress divided by the phase strain, in dentin were measured as 27+/-7.2 and 16+/-4.9 GPa. The HAP apparent modulus ( EHAPapp ) is less than the lower bound calculated for EHAPapp from the Voigt model. This discrepancy is probably due to stress concentrators or decreases in the HAP Young's modulus due to size or composition effects. EHAPapp and Efibapp in dentin vary significantly within a single tooth in both the apical-cervical direction and the buccal-lingual direction. However, the variation between teeth is minimal. The HAP and fibrillar apparent moduli are not affected by freezing in dentin or by X-ray irradiation in bone and dentin. X-ray irradiation causes a decrease in HAP residual strain in bone. This decrease suggests the presence of HAP-collagen interfacial damage. It was determined from the HAP 00.2 peak broadening that irradiation damage mostly affects the HAP unit cells which are under the highest strain. From this it was theorized that irradiation may damage highly-strained bonds at stress concentrators and/or calcium-mediated electrostatic bonds. The fact that the apparent modulus does not change with irradiation suggests that the interfacial damage must be reversible. Bone and dentin both undergo creep when loaded to high stresses. At low irradiation doses, both the fibrillar and HAP strains increase with creep time indicating that load is being transferred from the matrix to the HAP. However, at high doses, the strain on the HAP decreases with creep time. This supports the interfacial damage theory which would allow the HAP to release its elastic load upon interfacial debonding. At -80 MPa, beyond a dose of 50 kGy, the rate of change in HAP strain with time begins to increase, becoming positive at

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

NARCIS (Netherlands)

Rijn, Richard van

2012-01-01

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

Structure evolutions in a Ti–6Al–4V matrix composite reinforced with TiB, characterised using high energy X-ray diffraction

International Nuclear Information System (INIS)

Ropars, Ludovic; Dehmas, Moukrane; Gourdet, Sophie; Delfosse, Jérôme; Tricker, David; Aeby-Gautier, Elisabeth

2015-01-01

Highlights: • In-situ high energy X-ray diffraction used during different thermal treatments. • Kinetics of phase evolutions characterised for the matrix and for the borides. • Conversion from TiB 2 to TiB-B27 via a metastable structure TiB-B f . • Strong effect of the process on the matrix phases evolutions and microstructure. - Abstract: A titanium matrix composite reinforced with TiB was produced using powder metallurgy. A Ti–6Al–4V alloy was chosen to be the matrix, and 12 wt.% of TiB 2 was used as the boron source for the solid state formation of TiB. The TiB 2 to TiB conversion reaction was studied using an in situ high energy X-ray diffraction technique while heat treating the composite. The TiB 2 (space group: P6/mmm) converts into TiB-B27 (Pnma), via TiB-B f (Cmcm). The metastable character of B f is confirmed here; it is the first phase formed during the conversion and it progressively converts into B27 during elevated temperature heat treatment. A modification of the phase transformation kinetics in the matrix and of the composite β transus temperature (T β = 1275 °C) was also observed, mainly due to gas contamination and intensive work hardening as a result of the mechanical alloying process used to manufacture the material and to a modification of the matrix equilibria

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.

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

Directory of Open Access Journals (Sweden)

Katharina Fucke

2010-07-01

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

Femtosecond X-ray diffraction from an aerosolized beam of protein nanocrystals.

Science.gov (United States)

Awel, Salah; Kirian, Richard A; Wiedorn, Max O; Beyerlein, Kenneth R; Roth, Nils; Horke, Daniel A; Oberthür, Dominik; Knoska, Juraj; Mariani, Valerio; Morgan, Andrew; Adriano, Luigi; Tolstikova, Alexandra; Xavier, P Lourdu; Yefanov, Oleksandr; Aquila, Andrew; Barty, Anton; Roy-Chowdhury, Shatabdi; Hunter, Mark S; James, Daniel; Robinson, Joseph S; Weierstall, Uwe; Rode, Andrei V; Bajt, Saša; Küpper, Jochen; Chapman, Henry N

2018-02-01

High-resolution Bragg diffraction from aerosolized single granulovirus nanocrystals using an X-ray free-electron laser is demonstrated. The outer dimensions of the in-vacuum aerosol injector components are identical to conventional liquid-microjet nozzles used in serial diffraction experiments, which allows the injector to be utilized with standard mountings. As compared with liquid-jet injection, the X-ray scattering background is reduced by several orders of magnitude by the use of helium carrier gas rather than liquid. Such reduction is required for diffraction measurements of small macromolecular nanocrystals and single particles. High particle speeds are achieved, making the approach suitable for use at upcoming high-repetition-rate facilities.

Assessment of the out-plane and in-plane ordering of high quality ZnO nanorods by X-ray multiple diffraction

International Nuclear Information System (INIS)

Martínez-Tomás, M.C.; Montenegro, D.N.; Agouram, S.; Sallet, V.; Muñoz-Sanjosé, V.

2013-01-01

ZnO nanorods grown on buffered and non buffered sapphire substrates have been investigated by X-ray multiple diffraction using Renninger scans of the ZnO(0001) and ZnO(0003) forbidden reflections. In this technique the diffracted X-ray beam is simultaneously diffracted by several sets of planes, providing information on the broadening in different directions, as well as from nanorods, and from the layer on which they grow. The intensities and angular widths of peaks obtained by azimuthal and omega scans have been analyzed, making a direct comparison with conventional measurements of the full width at half-maximum of symmetric and asymmetric reflections. The analysis leads to establish that the peaks of the Renninger scan are highly sensitive to structural characteristics, providing information related with both the out-plane and in-plane ordering of nanostructured samples with a single scan. - Highlights: ► Structural characteristics of ZnO nanorods have been analyzed by X-ray multiple diffraction. ► X-ray multiple diffraction can provide mosaic structure characteristics from a single scan. ► Peaks of Renninger scan result to be very sensitive to structural characteristics. ► X-ray multiple diffraction can be an alternative analysis method to X-ray diffraction

Assessment of the out-plane and in-plane ordering of high quality ZnO nanorods by X-ray multiple diffraction

Energy Technology Data Exchange (ETDEWEB)

Martínez-Tomás, M.C., E-mail: Carmen.Martinez-tomas@uv.es [Departamento de Física Aplicada y Electromagnetismo, Universitat de Valencia, Dr. Moliner 50, 46100 Burjassot (Spain); Montenegro, D.N.; Agouram, S. [Departamento de Física Aplicada y Electromagnetismo, Universitat de Valencia, Dr. Moliner 50, 46100 Burjassot (Spain); Sallet, V. [Groupe d' Etude de la Matière Condensée (GEMAC), CNRS-Université de Versailles St-Quentin, 45 avenue des Etats-Unis, 78035 Versailles Cedex (France); Muñoz-Sanjosé, V. [Departamento de Física Aplicada y Electromagnetismo, Universitat de Valencia, Dr. Moliner 50, 46100 Burjassot (Spain)

2013-08-31

ZnO nanorods grown on buffered and non buffered sapphire substrates have been investigated by X-ray multiple diffraction using Renninger scans of the ZnO(0001) and ZnO(0003) forbidden reflections. In this technique the diffracted X-ray beam is simultaneously diffracted by several sets of planes, providing information on the broadening in different directions, as well as from nanorods, and from the layer on which they grow. The intensities and angular widths of peaks obtained by azimuthal and omega scans have been analyzed, making a direct comparison with conventional measurements of the full width at half-maximum of symmetric and asymmetric reflections. The analysis leads to establish that the peaks of the Renninger scan are highly sensitive to structural characteristics, providing information related with both the out-plane and in-plane ordering of nanostructured samples with a single scan. - Highlights: ► Structural characteristics of ZnO nanorods have been analyzed by X-ray multiple diffraction. ► X-ray multiple diffraction can provide mosaic structure characteristics from a single scan. ► Peaks of Renninger scan result to be very sensitive to structural characteristics. ► X-ray multiple diffraction can be an alternative analysis method to X-ray diffraction.

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

International Nuclear Information System (INIS)

Stern, Stephan

2013-12-01

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

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

High-pressure powder x-ray diffraction experiments on Zn at low temperature

CERN Document Server

Takemura, K; Fujihisa, H; Kikegawa, T

2002-01-01

High-pressure powder x-ray diffraction experiments have been performed on Zn with a He-pressure medium at low temperature. When the sample was compressed in the He medium at low temperature, large nonhydrostaticity developed, yielding erroneous lattice parameters. On the other hand, when the pressure was changed at high temperatures, good hydrostaticity was maintained. No anomaly in the volume dependence of the c/a axial ratio has been found.

X-ray diffraction without sample preparation: Proof-of-principle experiments

International Nuclear Information System (INIS)

Hansford, Graeme M.

2013-01-01

The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

Advances in thin film diffraction instrumentation by X-ray optics

International Nuclear Information System (INIS)

Haase, A.

1996-01-01

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

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.

Structural refinement and extraction of hydrogen atomic positions in polyoxymethylene crystal based on the first successful measurements of 2-dimensional high-energy synchrotron X-ray diffraction and wide-angle neutron diffraction patterns of hydrogenated and deuterated species

International Nuclear Information System (INIS)

Tashiro, Kohji; Hanesaka, Makoto; Ohhara, Takashi; Kurihara, Kazuo; Tamada, Taro; Kuroki, Ryota; Fujiwara, Satoru; Ozeki, Tomoji; Kitano, Toshiaki; Nishu, Takashi; Tanaka, Ichiro; Niimura, Nobuo

2007-01-01

2-Dimensional X-ray and neutron diffraction patterns have been successfully measured for deuterated and hydrogenated polyoxymethylene (POM) samples obtained by γ-ray induced solid-state polymerization reaction. More than 700 reflections were collected from the X-ray diffraction data at -150degC by utilizing a high-energy synchrotron X-ray beam at SPring-8, Japan, from which the crystal structure of POM has been refined thoroughly including the extraction of hydrogen atomic positions at clearly seen in the difference Fourier synthesis map. As the first trial the nonuniform (9/5) helical model was analyzed with the reliability factor (R factor) 6.9%. The structural analysis was made also using the X-ray reflections of about 400 observed at room temperature (R 8.8%), and the thermal parameters of constituent atoms were compared between the low and high temperatures to discuss the librational thermal motion of the chains. The 2-dimensional neutron diffraction data, collected for the deuterated and hydrogenated POM samples using an imaging plate system specifically built-up for neutron scattering experiment, have allowed us to pick up the D and H atomic positions clearly in the Fourier synthesis maps. Another possible model, (29/16) helix, which was proposed by several researches, has been also investigated on the basis of the X-ray diffraction data at -150degC. The direct method succeeded in extracting this (29/16) model straightforwardly. The R factor was 8.6%, essentially the same as that of (9/5) helical model. This means that the comparison of the diffraction intensity between the data collected from the full-rotation X-ray diffraction pattern and the intensity calculated for both the (9/5) and (29/16) models cannot be used for the unique determination of the superiority of the model, (9/5) or (29/16) helix. However, we have found the existence of 001 and 002 reflections which give the longer repeating period 55.7 A. Besides there observed a series of meridional

Polarisation resonance in X-ray diffraction

International Nuclear Information System (INIS)

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

1994-01-01

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

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...

Superiority of Low Energy 160 KV X-Rays Compared to High Energy 6 MV X-Rays in Heavy Element Radiosensitization for Cancer Treatment

Science.gov (United States)

Lim, Sara N.; Pradhan, Anil K.; Nahar, Sultana N.; Barth, Rolf F.; Yang, Weilian; Nakkula, Robin J.; Palmer, Alycia; Turro, Claudia

2013-06-01

High energy X-rays in the MeV range are generally employed in conventional radiation therapy from linear accelerators (LINAC) to ensure sufficient penetration depths. However, lower energy X-rays in the keV range may be more effective when coupled with heavy element (high-Z or HZ) radiosensitizers. Numerical simulations of X-ray energy deposition for tumor phantoms sensitized with HZ radiosensitizers were performed using the Monte Carlo code Geant4. The results showed enhancement in energy deposition to radiosensitized phantoms relative to unsensitized phantoms for low energy X-rays in the keV range. In contrast, minimal enhancement was seen using high energy X-rays in the MeV range. Dose enhancement factors (DEFs) were computed and showed radiosensitization only in the low energy range nitrate, was initially used because it was 7x less toxic that an equivalent amount of carboplatin in vitro studies. This would allow us to separate the radiotoxic and the chemotoxic effects of HZ sensitizers. Results from this study showed a 10-fold dose dependent reduction in surviving fractions (SF) of radiosensitized cells treated with low energy 160 kV X-rays compared to those treated with 6 MV X-rays. This is in agreement with our simulations that show an increase in dose deposition in radiosensitized tumors for low energy X-rays. Due to unforeen in vivo toxicity, however, another in vitro study was performed using the commonly used, Pt-based chemotherapeutic drug carboplatin which confirmed earlier results. This lays the ground work for a planned in vivo study using F98 glioma bearing rats. This study demonstrates that while high energy X-rays are commonly used in cancer radiotherapy, low energy keV X-rays might be much more effective with HZ radiosensitization.

High-speed X-ray topography

International Nuclear Information System (INIS)

Eckers, W.; Oppolzer, H.

1977-01-01

The investigation of lattice defects in semiconductor crystals by conventional X-ray diffraction topography is very time-consuming. Exposure times can be reduced by using high-intensity X-rays and X-ray image intensifiers. The described system comprises a high-power rotating-anode X-ray tube, a remote-controlled X-ray topography camera, and a television system operating with an X-ray sensing VIDICON. System performance is demonstrated with reference to exploratory examples. The exposure time for photographic plates is reduced to 1/20 and for the X-ray TV system (resolution of the order of 30 μm) to 1/100 relative to that required when using a conventional topography system. (orig.) [de

The phase problem and perspectives of surface X-ray diffraction

International Nuclear Information System (INIS)

Tajiri, Hiroo; Takahashi, Toshio

2009-01-01

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

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...... is greatly improved by introducing an orbital dependent U term into the energy-functional. The 4f electrons in TbN-B1 are atomic like and highly correlated, and ferro-magnetic TbN-B1 is found to be a magnetic half-metal. Calculations find the spindown f-electrons in a hypothetical TbN-B2 (CsCl) structure...

Correlation between X-ray and high energy gamma-ray emission form Cygnus X-3

International Nuclear Information System (INIS)

Weekes, T.C.; Danaher, S.; Fegan, D.J.; Porter, N.A.

1981-01-01

In May-June 1980, the 4.8 hour modulated X-ray flux from Cygnus X-3 underwent a significant change in the shape of the light curve; this change correlates with the peak in the high-energy (E > 2 x 10 12 eV) gamma ray emission at the same epoch. (orig.)

Diagnostic Spectrometers for High Energy Density X-Ray Sources

International Nuclear Information System (INIS)

Hudson, L. T.; Henins, A.; Seely, J. F.; Holland, G. E.

2007-01-01

A new generation of advanced laser, accelerator, and plasma confinement devices are emerging that are producing extreme states of light and matter that are unprecedented for laboratory study. Examples of such sources that will produce laboratory x-ray emissions with unprecedented characteristics include megajoule-class and ultrafast, ultraintense petawatt laser-produced plasmas; tabletop high-harmonic-generation x-ray sources; high-brightness zeta-pinch and magnetically confined plasma sources; and coherent x-ray free electron lasers and compact inverse-Compton x-ray sources. Characterizing the spectra, time structure, and intensity of x rays emitted by these and other novel sources is critical to assessing system performance and progress as well as pursuing the new and unpredictable physical interactions of interest to basic and applied high-energy-density (HED) science. As these technologies mature, increased emphasis will need to be placed on advanced diagnostic instrumentation and metrology, standard reference data, absolute calibrations and traceability of results.We are actively designing, fabricating, and fielding wavelength-calibrated x-ray spectrometers that have been employed to register spectra from a variety of exotic x-ray sources (electron beam ion trap, electron cyclotron resonance ion source, terawatt pulsed-power-driven accelerator, laser-produced plasmas). These instruments employ a variety of curved-crystal optics, detector technologies, and data acquisition strategies. In anticipation of the trends mentioned above, this paper will focus primarily on optical designs that can accommodate the high background signals produced in HED experiments while also registering their high-energy spectral emissions. In particular, we review the results of recent laboratory testing that explores off-Rowland circle imaging in an effort to reclaim the instrumental resolving power that is increasingly elusive at higher energies when using wavelength

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....

Diffractive sub-picosecond manipulation of x-rays

International Nuclear Information System (INIS)

Adams, B.

2004-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-02-15

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

Femtosecond x-ray photoelectron diffraction on gas-phase dibromobenzene molecules

International Nuclear Information System (INIS)

Rolles, D; Boll, R; Epp, S W; Erk, B; Foucar, L; Hömke, A; Adolph, M; Gorkhover, T; Aquila, A; Chapman, H N; Coppola, N; Delmas, T; Gumprecht, L; Holmegaard, L; Bostedt, C; Bozek, J D; Coffee, R; Decleva, P; Filsinger, F; Johnsson, P

2014-01-01

We present time-resolved femtosecond photoelectron momentum images and angular distributions of dissociating, laser-aligned 1,4-dibromobenzene (C 6 H 4 Br 2 ) molecules measured in a near-infrared pump, soft-x-ray probe experiment performed at an x-ray free-electron laser. The observed alignment dependence of the bromine 2p photoelectron angular distributions is compared to density functional theory calculations and interpreted in terms of photoelectron diffraction. While no clear time-dependent effects are observed in the angular distribution of the Br(2p) photoelectrons, other, low-energy electrons show a pronounced dependence on the time delay between the near-infrared laser and the x-ray pulse. (paper)

The high energy X-ray spectra of supernova remnants

Science.gov (United States)

Pravdo, S. H.; Nugent, J. J.

The results of fitting an ionization-nonequilibrium (INE) model to the high-energy (above 5-keV) X-ray spectra of the young supernova remnants Cas A and Tycho are presented. As an additional constraint, the models must simultaneously fit lower-energy, higher-resolution data. For Cas A, a single INE component cannot adequately reproduce the features for the entire X-ray spectrum because the ionization structure of iron ions responsible for the K emission is inconsistent with that of the ions responsible for the lower-energy lines, and the flux of the highest-energy X-rays is underestimated. The iron K line and the high-energy continuum could arise from the same INE component, but the identification of this component with either the blast wave or the ejecta in the standard model is difficult. In Tycho, the high-energy data rule out a class of models for the lower-energy data which have too large a continuum contribution.

An ultrahigh-vacuum apparatus for resonant diffraction experiments using soft x rays (hν=300-2000 eV)

International Nuclear Information System (INIS)

Takeuchi, T.; Chainani, A.; Takata, Y.; Tanaka, Y.; Oura, M.; Tsubota, M.; Senba, Y.; Ohashi, H.; Mochiku, T.; Hirata, K.; Shin, S.

2009-01-01

We have developed an ultrahigh-vacuum instrument for resonant diffraction experiments using polarized soft x rays in the energy range of hν=300-2000 eV at beamline BL17SU of SPring-8. The diffractometer consists of modified differentially pumped rotary feedthroughs for θ-2θ stages, a sample manipulator with motor-controlled x-y-z-, tilt (χ)-, and azimuth (φ)-axes, and a liquid helium flow-type cryostat for temperature dependent measurements between 30 and 300 K. Test results indicate that the diffractometer exhibits high reproducibility (better than 0.001 deg.) for a Bragg reflection of α-quartz 100 at a photon energy of hν=1950 eV. Typical off- and on-resonance Bragg reflections in the energy range of 530-1950 eV could be measured using the apparatus. The results show that x-ray diffraction experiments with energy-, azimuth-, and incident photon polarization-dependence can be reliably measured using soft x rays in the energy range of ∼300-2000 eV. The facility can be used for resonant diffraction experiments across the L-edge of transition metals, M-edge of lanthanides, and up to the Si K-edge of materials.

Structure evolutions in a Ti–6Al–4V matrix composite reinforced with TiB, characterised using high energy X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Ropars, Ludovic, E-mail: ludovic.ropars@airbus.com [Airbus Group SAS, Airbus Group Innovations, 12 rue Pasteur, BP-76, 92152 Suresnes Cedex (France); Institut Jean Lamour (IJL), SI2M Dpt., CNRS UMR 7198, Université de Lorraine, Parc de Saurupt, CS 50840, F-54011 Nancy Cedex (France); Dehmas, Moukrane, E-mail: ismoukrane.dehmas@univlorraine.fr [Institut Jean Lamour (IJL), SI2M Dpt., CNRS UMR 7198, Université de Lorraine, Parc de Saurupt, CS 50840, F-54011 Nancy Cedex (France); Laboratory of Excellence for Design of Alloy Metals for Low-mass Structures (‘DAMAS’ Labex), Université de Lorraine (France); Gourdet, Sophie; Delfosse, Jérôme [Airbus Group SAS, Airbus Group Innovations, 12 rue Pasteur, BP-76, 92152 Suresnes Cedex (France); Tricker, David [Materion AMC, RAE Road, Farnborough, Hampshire GU14 6XE (United Kingdom); Aeby-Gautier, Elisabeth [Institut Jean Lamour (IJL), SI2M Dpt., CNRS UMR 7198, Université de Lorraine, Parc de Saurupt, CS 50840, F-54011 Nancy Cedex (France); Laboratory of Excellence for Design of Alloy Metals for Low-mass Structures (‘DAMAS’ Labex), Université de Lorraine (France)

2015-03-05

Highlights: • In-situ high energy X-ray diffraction used during different thermal treatments. • Kinetics of phase evolutions characterised for the matrix and for the borides. • Conversion from TiB{sub 2} to TiB-B27 via a metastable structure TiB-B{sub f}. • Strong effect of the process on the matrix phases evolutions and microstructure. - Abstract: A titanium matrix composite reinforced with TiB was produced using powder metallurgy. A Ti–6Al–4V alloy was chosen to be the matrix, and 12 wt.% of TiB{sub 2} was used as the boron source for the solid state formation of TiB. The TiB{sub 2} to TiB conversion reaction was studied using an in situ high energy X-ray diffraction technique while heat treating the composite. The TiB{sub 2} (space group: P6/mmm) converts into TiB-B27 (Pnma), via TiB-B{sub f} (Cmcm). The metastable character of B{sub f} is confirmed here; it is the first phase formed during the conversion and it progressively converts into B27 during elevated temperature heat treatment. A modification of the phase transformation kinetics in the matrix and of the composite β transus temperature (T{sub β} = 1275 °C) was also observed, mainly due to gas contamination and intensive work hardening as a result of the mechanical alloying process used to manufacture the material and to a modification of the matrix equilibria.

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-03-07

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

Coherent X-ray diffraction studies of mesoscopic materials

International Nuclear Information System (INIS)

Shabalin, Anatoly

2015-12-01

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

X-ray diffraction analysis of InAs nanowires

International Nuclear Information System (INIS)

Davydok, Anton

2013-01-01

Si substrate. MBE provides the opportunity to combine a group III-V material with nearly any semiconductor substrate independent from lattice mismatch. Vertically aligned nanowire ensembles were studied performing X-ray diffraction experiments in different scattering geometries. Considering the nanowires are composed by structural units of zinc-blende and wurtzite the latter one was found to be affected by a high density of stacking faults already at nanowires with short growth time. The stacking faults density was estimated by Monte-Carlo simulations based on model of ensemble average. A strong signal of unique zinc-blende reflection was observed as well. Coherent X-ray diffraction experiments with the use of a nano-focus setup have shown 'bar-code' patterning due to stacking fault arrangement within the nanowire. The found highly defective structure cannot be attributed to wurtzite or zinc-blende phases alone. Also parasitic islands were found on the samples surfaces and characterized as pure zinc-blende objects.

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

International Nuclear Information System (INIS)

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

2001-01-01

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

X-ray diffraction diagnostic design for the National Ignition Facility

Science.gov (United States)

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

2013-09-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-05-15

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

High energy resolution off-resonant X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Wojciech, Blachucki [Univ. of Fribourg (Switzerland). Dept. of Physics

2015-10-16

This work treats of the high energy resolution off-resonant X-ray spectroscopy (HEROS) method of determining the density of unoccupied electronic states in the vicinity of the absorption edge. HEROS is an alternative to the existing X-ray absorption spectroscopy (XAS) methods and opens the way for new studies not achievable before.

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

International Nuclear Information System (INIS)

Banos L, L.

2004-01-01

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

X-ray diffraction 2 - diffraction principles

International Nuclear Information System (INIS)

O'Connor, B.

1999-01-01

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

Design and fabrication of micro X-ray diffraction system

International Nuclear Information System (INIS)

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

2006-10-01

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

Design and fabrication of micro X-ray diffraction system

Energy Technology Data Exchange (ETDEWEB)

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

2006-10-15

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

Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

DEFF Research Database (Denmark)

Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

2015-01-01

For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

The comparative study of contents of zinc and lead in ore samples of Namtu-Bawdwin Mine by wet analysis, X-ray fluorescence and X-ray diffraction methods

Energy Technology Data Exchange (ETDEWEB)

Kyaw-Soe,

1990-05-01

Lead-zinc ores taken from Namtu-Bawdwin area had been analyzed by wet processes in the Department of Chemistry, 1984. These ore samples have been analyzed by energy dispersive X-ray fluorescence method in the Department of Physics and X-ray diffraction method is also used to determine elements of lead and zinc compounds in these ore samples in the University`s Research Centre. In brief, we study comparatively the contents of lead and zinc and their compounds using the methods of wet processes, X-ray fluorescence and X-ray diffraction. (author).

Plasma instability control toward high fluence, high energy x-ray continuum source

Science.gov (United States)

Poole, Patrick; Kirkwood, Robert; Wilks, Scott; Blue, Brent

2017-10-01

X-ray source development at Omega and NIF seeks to produce powerful radiation with high conversion efficiency for material effects studies in extreme fluence environments. While current K-shell emission sources can achieve tens of kJ on NIF up to 22 keV, the conversion efficiency drops rapidly for higher Z K-alpha energies. Pulsed power devices are efficient generators of MeV bremsstrahlung x-rays but are unable to produce lower energy photons in isolation, and so a capability gap exists for high fluence x-rays in the 30 - 100 keV range. A continuum source under development utilizes instabilities like Stimulated Raman Scattering (SRS) to generate plasma waves that accelerate electrons into high-Z converter walls. Optimizing instabilities using existing knowledge on their elimination will allow sufficiently hot and high yield electron distributions to create a superior bremsstrahlung x-ray source. An Omega experiment has been performed to investigate the optimization of SRS and high energy x-rays using Au hohlraums with parylene inner lining and foam fills, producing 10× greater x-ray yield at 50 keV than conventional direct drive experiments on the facility. Experiment and simulation details on this campaign will be presented. This work was performed under the auspices of the US DoE by LLNL under Contract No. DE-AC52-07NA27344.

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

International Nuclear Information System (INIS)

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

1999-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-04-01

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

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

Science.gov (United States)

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

2005-08-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-08-15

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-10-15

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

In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

DEFF Research Database (Denmark)

Amri, Mahrez; Fitch, Andy; Norby, Poul

2015-01-01

allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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....

Time-resolved x-ray diffraction analysis of the experimental dehydration of serpentine at high pressure

International Nuclear Information System (INIS)

Inoue, Toru; Yoshimi, Isamu; Yamada, Akihiro; Kikegawa, Takumi

2009-01-01

Time-resolved, in situ X-ray diffraction analysis was used to determine the dehydration rate and kinetics of serpentine during experimental dehydration at high pressures. The capsule used comprises a diamond sleeve fitted with Au or Pt lids in order to provide high-quality, time-resolved X-ray diffraction data. Antigorite quickly dehydrated to enstatite + forsterite + fluid within 2 h at 650degC below ∼6 GPa. Avrami modeling of the results and SEM observations of the partially dehydrated sample revealed that the nucleation rate was quite high for enstatite but low for forsterite, showing incubation periods of ∼10 min before appearing. The crystallization of these minerals is controlled largely by the composition of the fluid generated from serpentine dehydration. The dehydration boundary determined below 6 GPa in the present study is consistent with the results of previous phase equilibrium studies. This study indicates that serpentine in a subducting slab dehydrates rapidly below 6 GPa when the slab intersects the dehydration boundary conditions. (author)

Synchrotron X-ray diffraction and imaging of ancient Chinese bronzes

International Nuclear Information System (INIS)

Young, M.L.; Dunand, D.C.; Casadio, F.; Schnepp, S.; Almer, J.; Haeffner, D.R.

2006-01-01

High-energy synchrotron X-ray diffraction and imaging experiments were performed at the Advanced Photon Source on two ancient Chinese bronzes from the Art Institute of Chicago with the goal to nondestructively study their microstructure. The first object, a bronze fragment from an early Western Zhou dynasty vessel (Hu, 11th/10th century B.C.), was investigated with spatially-resolved diffraction to reveal the depth and composition of the surface corrosion layer as well as the composition and grain size of the underlying bronze core. The second object, a bronze dagger-axe (Ge, 3rd/2nd century B.C.) with a silver-inlaid sheath, was studied under both diffraction and imaging conditions. It was found to have been cast as a single object, answering longstanding scholars' questions on whether the ceremonial object concealed an interior blade. (orig.)

X-ray diffraction imaging of biological cells

CERN Document Server

Nakasako, Masayoshi

2018-01-01

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

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Novel X-ray imaging diagnostics of high energy nanosecond pulse accelerators

International Nuclear Information System (INIS)

Smith, Graham W.; Gallegos, Roque Rosauro; Hohlfelder, Robert James; Beutler, David Eric; Dudley, John; Seymour, Calvin L.G.; Bell, John D.

2004-01-01

Pioneering x-ray imaging has been undertaken on a number of AWE's and Sandia National Laboratories radiation effects x-ray simulators. These simulators typically yield a single very short (<50ns) pulse of high-energy (MeV endpoint energy bremsstrahlung) x-ray radiation with doses in the kilorad (krad(Si)) region. X-ray source targets vary in size from 2 to 25cm diameter, dependent upon the particular simulator. Electronic imaging of the source x-ray emission under dynamic conditions yields valuable information upon how the simulator is performing. The resultant images are of interest to the simulator designer who may configure new x-ray source converter targets and diode designs. The images can provide quantitative information about machine performance during radiation effects testing of components under active conditions. The effects testing program is a valuable interface for validation of high performance computer codes and models for the radiation effects community. A novel high-energy x-ray imaging spectrometer is described whereby the spectral energy (0.1 to 2.5MeV) profile may be discerned from the digitally recorded and viewable images via a pinhole/scintillator/CCD imaging system and knowledge of the filtration parameters. Unique images, analysis and a preliminary evaluation of the capability of the spectrometer are presented. Further, a novel time resolved imaging system is described that captures a sequence of high spatial resolution temporal images, with zero interframe time, in the nanosecond timeframe, of our source x-rays.

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

International Nuclear Information System (INIS)

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

1989-01-01

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

In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

International Nuclear Information System (INIS)

Thomas, D.; Mainz, R.; Rodriguez-Alvarez, H.; Marsen, B.; Abou-Ras, D.; Klaus, M.; Genzel, Ch.; Schock, H.-W.

2011-01-01

Recrystallization processes during the sulfurization of CuInS 2 (CIS) thin films have been studied in-situ using energy dispersive X-ray diffraction (EDXRD) with synchrotron radiation. In order to observe the recrystallization isolated from other reactions occurring during film growth, Cu-poor, small grained CIS layers covered with CuS on top were heated in a vacuum chamber equipped with windows for synchrotron radiation in order to analyze the grain growth mechanism within the CIS layer. In-situ monitoring of the grain size based on diffraction line profile analysis of the CIS-112 reflection was utilized to interrupt the recrystallization process at different points. Ex-situ studies by electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX) performed on samples of intermediate recrystallization states reveal that during the heat treatment Cu and In interdiffuse inside the layer indicating the importance of the mobility of these two elements during CuInS 2 grain growth.

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

International Nuclear Information System (INIS)

Freyer, Benjamin

2013-01-01

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

Measurement of rocking curve wings at high x-ray energies

International Nuclear Information System (INIS)

Chapman, D.; Hastings, J.; Moulin, H.; Siddons, D.P.; Garrett, R.F.; Nachaliel, E.; Dilmanian, F.A.

1991-01-01

Measurements done recently at the NSLS have indicated that the level of intensity found in the wings of diffraction peaks from silicon at higher x-ray energies (>20keV) far exceeds the value which would be predicted based on the dynamical theory. We have measured Si(220) double crystal rocking curves at the 40keV fundamental and harmonics with various crystal scattering geometries: Bragg-Bragg, Laue-Bragg, Laue-Lauel. The comparison of the Bragg and Laue case diffraction geometries was done to determine scattering volume effects. Comparisons with dynamical theory calculations will be discussed. These measurements have been carried out in order to assess the level of harmonic contamination which will be present from a double crystal monochromator being designed for the X17 Superconducting Wiggler Beamline

EPR and X-ray diffraction investigation of some Greek marbles and limestones

International Nuclear Information System (INIS)

Duliu, Octavian; Grecu, Maria Nicoleta; Cristea, Corina

2009-01-01

Twelve different marble and limestone samples collected from well-known Greek quarries have been investigated by X-ray diffraction and electron paramagnetic resonance (EPR). X-ray diffraction spectra permitted to determine both major (calcite and dolomite) and minor (quartz or magnesite) mineralogical components. EPR has been used to investigate the same samples unirradiated and after 10 kGy gamma-ray irradiation. The unirradiated samples display typical EPR spectra of Mn 2+ in calcite and dolomite as well as a superposition of these while some samples displayed EPR free radicals signals of centers (low field signal) and centers (high field signal). From X-ray diffraction and EPR spectra it was possible to extract numerical values of several numerical parameters such as dolomite to calcite ratio, EPR intensity parameter, and low field to high field EPR signals intensity ratio. These values as well as the correlation coefficients between the digital functions that described the low field Mn 2+ ions EPR line have been used as entry data for cluster analysis to quantify the resemblance and differences between analyzed samples. (authors)

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)....

Historical development of synchrotron x-ray diffraction topography

International Nuclear Information System (INIS)

Kawado, Seiji

2011-01-01

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

X-ray fluorescence in Member States (Italy): Full field X-ray fluorescence imaging with high-energy and high-spatial resolution

Energy Technology Data Exchange (ETDEWEB)

Romano, F. P.; Masini, N.; Pappalardo, L., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); Cosentino, L.; Gammino, S.; Mascali, D.; Rizzo, F. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy)

2014-02-15

A full field X-ray camera for the X-Ray Fluorescence imaging of materials with high-energy and high-spatial resolution was designed and developed. The system was realized by coupling a pinhole collimator with a positionsensitive CCD detector. X-Ray fluorescence is induced on the samples by irradiation with an external X-ray tube. The characteristic X-ray spectra of the investigated materials are obtained by using a multi-frames acquisition in single-photon counting. The energy resolution measured at the Fe-Kα line was 157 eV. The spatial resolution of the system was determined by the analysis of a sharp-edge at different magnification values; it was estimated to be 90 μm at a magnification value of 3.2x and 190 μm at 0.8x. The present set-up of the system is suited to analyze samples with dimensions up to 5x4 cm{sup 2}. Typical measurement time is in the range between 1h to 4 h. (author)

Measurements of internal stresses in bond coating using high energy x-rays from synchrotron radiation source

CERN Document Server

Suzuki, K; Akiniwa, Y; Nishio, K; Kawamura, M; Okado, H

2002-01-01

Thermal barrier coating (TBC) techniques enable high temperature combustion of turbines made of Ni-base alloy. TBC is made of zirconia top coating on NiCoCrAlY bond coating. The internal stresses in the bond coating play essential role in the delamination or fracture of TBC in service. With the X-rays from laboratory equipments, it is impossible to measure nondestructively the internal stress in the bond coating under the top coating. synchrotron radiations with a high energy and high brightness have a large penetration depth as compared with laboratory X-rays. Using the high energy X-rays from the synchrotron radiation, it is possible to measure the internal stress in the bond coating through the top coating. In this study, the furnace, which can heat a specimen to 1473 K, was developed for the stress measurement of the thermal barrier coatings. The internal stresses in the bond coating were measured at the room temperature, 773 K, 1073 K and 1373 K by using the 311 diffraction from Ni sub 3 Al with about 73...

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-27

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

X-ray optics and X-ray microscopes: new challenges

International Nuclear Information System (INIS)

Susini, J.

2004-01-01

main fields of applications are driven by the unique attributes of X-ray microscopy in the multi-keV energy range: i) access to K-absorption edges and fluorescence emission lines of medium-light elements and L,M - edges of heavy materials for micro-spectroscopy (e.g. XANES), chemical or trace element mapping ii) higher penetration depths compared to soft X-rays allowing imaging of thicker samples, iii) favorable wavelengths for diffraction studies and iv) generally large focal lengths and depths of focus which are advantageous for the use of specific sample environments (high pressure, controlled temperatures....). Typical experiments can be broadly divided into two categories: i) morphological studies which require high spatial resolution and are therefore well adapted to 2D or 3D transmission full-field microscopy. ii) studies dealing with co-localization and/or speciation of trace elements in heterogeneous matrices at the micron scale. Following a brief account on the basic principles and methods, strengths and weaknesses of X-ray microscopy and spectro-microscopy techniques in the 1 - 30 keV range will be discussed and illustrated by examples of applications. The main technical developments, involving new focusing lenses or novel phase contrast geometry, will be presented. (author)

Surface structure of Bi₂Se₃(111) determined by low-energy electron diffraction and surface x-ray diffraction

DEFF Research Database (Denmark)

dos Reis, Diogo Duarte; Barreto, Lucas; Bianchi, Marco

2013-01-01

The surface structure of the prototypical topological insulator Bi2Se3 is determined by low-energy electron diffraction and surface x-ray diffraction at room temperature. Both approaches show that the crystal is terminated by an intact quintuple layer. Specifically, an alternative termination by ...... by a bismuth bilayer is ruled out. Surface relaxations obtained by both techniques are in good agreement with each other and found to be small. This includes the relaxation of the van der Waals gap between the first two quintuple layers....

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

DEFF Research Database (Denmark)

Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

2008-01-01

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

Measurement of the energy distribution of parametric X-ray radiation from a double-crystal system

International Nuclear Information System (INIS)

Mori, Akira; Hayakawa, Yasushi; Kidokoro, Akio; Sato, Isamu; Tanaka, Toshinari; Hayakawa, Ken; Kobayashi, Kouji; Ohshima, Hisashi

2006-01-01

A parametric X-ray radiation (PXR) generator system was developed at the Laboratory for Electron Beam Research and Applications (LEBRA) at Nihon University; this PXR generator system is a tunable wavelength and quasi-monochromatic X-ray source constructed as one of the advanced applications of the LEBRA 125-MeV electron linear accelerator. The PXR beam which has characteristic of energy distribution. The theoretical values of energy distribution obtained at the output port were calculated to be approximately 300 eV and 2 keV at the central X-ray energies of 7 keV and 20 keV, respectively. In order to investigate the energy distribution, several measurements of the X-ray energy were carried out. The X-ray absorption of known materials and that of thin aluminum has been evaluated based on analyses of images taken using an imaging plate. The X-ray energy was deduced base on the identification of the absorption edges, and the energy distribution was estimated based on measurements using aluminum step method. In addition, an X-ray diffraction method using a perfect silicon crystal was employed, and spectra were measured using a solid state detector (SSD). The results of these experiments agreed with the calculated results. In particular, the well-defined absorption edges in the X-ray images and the typical rocking curves obtained by the measurement of the X-ray diffraction indicated that the distribution has a high-energy resolution

High-energy X-ray production in a boundary layer of an accreting neutron star

International Nuclear Information System (INIS)

Hanawa, Tomoyuki

1991-01-01

It is shown by Monte Carlo simulation that high-energy X-rays are produced through Compton scattering in a boundary layer of an accreting neutron star. The following is the mechanism for the high-energy X-ray production. An accreting neutron star has a boundary layer rotating rapidly on the surface. X-rays radiated from the star's surface are scattered in part in the boundary layer. Since the boundary layer rotates at a semirelativistic speed, the scattered X-ray energy is changed by the Compton effect. Some X-rays are scattered repeatedly between the neutron star and the boundary layer and become high-energy X-rays. This mechanism is a photon analog of the second-order Fermi acceleration of cosmic rays. When the boundary layer is semitransparent, high-energy X-rays are produced efficiently. 17 refs

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

International Nuclear Information System (INIS)

Kassemeyer, Stephan

2014-01-01

Coherent diffractive imaging with X-ray free-electron lasers (X-FEL) promises high-resolution structure determination of single microscopic particles without the need for crystallization. The diffraction signal of small samples can be very weak, a difficulty that can not be countered by merely increasing the number of photons because the sample would be damaged by a high absorbed radiation dose. Traditional X-ray crystallography avoids this problem by bringing many sample particles into a periodic arrangement, which amplifies the individual signals while distributing the absorbed dose. Depending on the sample, however, crystallization can be very difficult or even impossible. This thesis presents algorithms for a new imaging approach using X-FEL radiation that works with single, non-crystalline sample particles. X-FELs can deliver X-rays with a peak brilliance many orders of magnitude higher than conventional X-ray sources, compensating for their weak interaction cross sections. At the same time, FELs can produce ultra-short pulses down to a few femtoseconds. In this way it is possible to perform ultra-fast imaging, essentially ''freezing'' the atomic positions in time and terminating the imaging process before the sample is destroyed by the absorbed radiation. This thesis primarily focuses on the three-dimensional reconstruction of single (and not necessarily crystalline) particles using coherent diffractive imaging at X-FELs: in order to extract three-dimensional information from scattering data, two-dimensional diffraction patterns from many different viewing angles must be combined. Therefore, the diffraction signal of many identical sample copies in random orientations is measured. The main result of this work is a globally optimal algorithm that can recover the sample orientations solely based on the diffraction signal, enabling three-dimensional imaging for arbitrary samples. The problem of finding three-dimensional orientations is

X-ray diffraction using the time structure of the SRS

International Nuclear Information System (INIS)

Tanner, B.K.

1983-01-01

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

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

DEFF Research Database (Denmark)

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

2010-01-01

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

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.

X-ray diffraction at Bragg angles around π/2

International Nuclear Information System (INIS)

Mayolo, C.M.G. de.

1991-01-01

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

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

International Nuclear Information System (INIS)

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

1979-07-01

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

Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

Energy Technology Data Exchange (ETDEWEB)

Huang, Xian-Rong; Gog, Thomas; Kim, Jungho; Kasman, Elina; Said, Ayman H.; Casa, Diego M.; Wieczorek, Michael; Hönnicke, Marcelo G.; Assoufid, Lahsen

2018-02-01

Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h₁h₂h₃L} and {h₂h₁h₃L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystals therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.

ICF ignition capsule neutron, gamma ray, and high energy x-ray images

Science.gov (United States)

Bradley, P. A.; Wilson, D. C.; Swenson, F. J.; Morgan, G. L.

2003-03-01

Post-processed total neutron, RIF neutron, gamma-ray, and x-ray images from 2D LASNEX calculations of burning ignition capsules are presented. The capsules have yields ranging from tens of kilojoules (failures) to over 16 MJ (ignition), and their implosion symmetry ranges from prolate (flattest at the hohlraum equator) to oblate (flattest towards the laser entrance hole). The simulated total neutron images emphasize regions of high DT density and temperature; the reaction-in-flight neutrons emphasize regions of high DT density; the gamma rays emphasize regions of high shell density; and the high energy x rays (>10 keV) emphasize regions of high temperature.

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

International Nuclear Information System (INIS)

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

1998-01-01

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

High-pressure powder X-ray diffraction at the turn of the century

International Nuclear Information System (INIS)

Paszkowicz, W.

2002-01-01

Studies at extreme pressures and temperatures are helpful for understanding the physical properties of the solid state, including such classes of materials as semiconductors, superconductors or minerals. This is connected with the opportunity of tuning the pressure by many orders of magnitude. Diamond-anvil and large-anvil pressure cells installed at dedicated synchrotron beamlines are efficient tools for examination of crystal structure, equation of state, compressibility and phase transitions. One of basic methods in such studies is powder diffraction. This review is devoted to methods of powder X-ray diffraction at high-pressures generated by devices installed at synchrotron radiation sources, in particular to the principles of operation of high-pressure-high-temperature cells. General information on high-pressure diffraction facilities installed at 11 synchrotron storage rings in the world is provided. Measurement aspects are considered, including (i) pressure generation and calibration, (ii) strain in the sample, the pressure marker and the pressure-transmitting medium and (iii) pressure and temperature distributions within the cells. Sources of interest in high-pressure diffraction studies (design of new materials, observation of new phenomena, confrontation of theory with experiment) are briefly discussed. Recent developments of high-pressure methods make that pressure becomes a variable playing a key role in investigation of condensed matter. The paper ends with some remarks on the possible future developments of the technique

Rapid, low dose X-ray diffractive imaging of the malaria parasite Plasmodium falciparum

International Nuclear Information System (INIS)

Jones, Michael W.M.; Dearnley, Megan K.; Riessen, Grant A. van; Abbey, Brian; Putkunz, Corey T.; Junker, Mark D.; Vine, David J.; McNulty, Ian; Nugent, Keith A.; Peele, Andrew G.; Tilley, Leann

2014-01-01

Phase-diverse X-ray coherent diffractive imaging (CDI) provides a route to high sensitivity and spatial resolution with moderate radiation dose. It also provides a robust solution to the well-known phase-problem, making on-line image reconstruction feasible. Here we apply phase-diverse CDI to a cellular sample, obtaining images of an erythrocyte infected by the sexual stage of the malaria parasite, Plasmodium falciparum, with a radiation dose significantly lower than the lowest dose previously reported for cellular imaging using CDI. The high sensitivity and resolution allow key biological features to be identified within intact cells, providing complementary information to optical and electron microscopy. This high throughput method could be used for fast tomographic imaging, or to generate multiple replicates in two-dimensions of hydrated biological systems without freezing or fixing. This work demonstrates that phase-diverse CDI is a valuable complementary imaging method for the biological sciences and ready for immediate application. - Highlights: • Phase-diverse coherent X-ray diffraction microscopy provides high-resolution and high-contrast images of intact biological samples. • Rapid nanoscale resolution imaging is demonstrated at orders of magnitude lower dose than previously possible. • Phase-diverse coherent X-ray diffraction microscopy is a robust technique for rapid, quantitative, and correlative X-ray phase imaging

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.

Processing of Bi-2212 and Nb$_3$Sn studied in situ by high energy synchrotron diffraction and micro-tomography

CERN Document Server

Kadar, Julian

Next generation superconducting wires have been studied to obtain more information on the evolution of phase growth, crystallite size and strain state during wire processing. The high energy scattering beam line ID15 at the European Synchrotron Radiation Facility provides a very high flux of high energy photons for very fast in situ X-ray diffraction and micro-tomography studies of Bi-2212/Ag and Nb$_3$S/Cu wire samples. The typical wire processing conditions could be imitated in the X-ray transparent furnace at ID15 for diffraction and tomography studies. Efficient data analysis is mandatory in order to handle the very fast data acquisition rate. For this purpose an Excel-VBA based program was developed that allows a semi-automated fitting and tracking of peaks with pre-set constraints. With this method, more than one thousand diffraction patterns have been analysed to extract d-spacing, peak intensity and peak width values. X ray absorption micro tomograms were recorded simultaneously with the X-ray diffrac...

X-ray characterization of curved crystals for hard x-ray astronomy

Science.gov (United States)

Buffagni, Elisa; Bonnini, Elisa; Ferrari, Claudio; Virgilli, Enrico; Frontera, Filippo

2015-05-01

Among the methods to focus photons the diffraction in crystals results as one of the most effective for high energy photons. An assembling of properly oriented crystals can form a lens able to focus x-rays at high energy via Laue diffraction in transmission geometry; this is a Laue lens. The x-ray diffraction theory provides that the maximum diffraction efficiency is achieved in ideal mosaic crystals, but real mosaic crystals show diffraction efficiencies several times lower than the ideal case due to technological problems. An alternative and convenient approach is the use of curved crystals. We have recently optimized an efficient method based on the surface damage of crystals to produce self-standing uniformly curved Si, GaAs and Ge tiles of thickness up to 2-3 mm and curvature radii R down to a few meters. We show that, for curved diffracting planes, such crystals have a diffraction efficiency nearly forty times higher than the diffraction efficiency of perfect similar flat crystals, thus very close to that of ideal mosaic crystals. Moreover, in an alternative configuration where the diffracting planes are perpendicular to the curved ones, a focusing effect occurs and will be shown. These results were obtained for several energies between 17 and 120 keV with lab sources or at high energy facilities such as LARIX at Ferrara (Italy), ESRF at Grenoble (France), and ANKA at Karlsruhe (Germany).

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Kinetics of the main phase transition of hydrated lecithin monitored by real-time x-ray diffraction

International Nuclear Information System (INIS)

Caffrey, M.; Bilderback, D.H.

1984-01-01

A method is described for observing and recording in real-time x-ray diffraction from an unoriented hydrated membrane lipid, dipalmitoylphosphatidylcholine (DPPC), through its thermotropic gel/liquid crystal phase transition. Synchrotron radiation from the Cornell High Energy Synchrotron Source (Ithaca, New York) was used as an x-ray source of extremely high brilliance and the dynamic display of the diffraction image was effected using a three-stage image intensifier tube coupled to an external fluorescent screen. The image on the output phosphor was sufficiently intense to be recorded cinematographically and to be displayed on a television monitor using a vidicon camera at 30 frames x s -1 . These measurements set an upper limit of 2 s on the DPPC gel → liquid crystal phase transition and indicate that the transition is a two-state process. The real-time method couples the power of x-ray diffraction as a structural probe with the ability to follow kinetics of structural changes. The method does not require an exogenous probe, is relatively nonperturbing, and can be used with membranes in a variety of physical states and with unstable samples. The method has the additional advantage over its static measurement counterpart in that it is more likely to detect transiently stable intermediates if present

Modern trends in x-ray powder diffraction

International Nuclear Information System (INIS)

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

1985-01-01

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

Investigations of the phase transition in V3O5 using energy dispersive X-ray diffraction and synchrotron radiation white beam X-ray topography

International Nuclear Information System (INIS)

Asbrink, S.; Gerward, L.; Staun Olsen, J.

1985-01-01

The reversible first order phase transition in V 3 O 5 at T t =155 0 C has been studied using a specially constructed oven, where the temperature can be kept constant within a few hundredths of a degree for several hours. Energy dispersive diffraction measurements have beem made in a temperature region around the phase transition with the fixed crystal method and the θ/2θ scanning method. White beam X-ray topographs have been obtained from the same crystal in the same temperature region using synchrotron radiation. The integrated intensities of the strong h 0 0 reflections show anomalies that are correlated with the corresponding X-ray topographs. Thus, an unexpected increase of crystal perfection is observed a few hundredths of a degree below T t . The energy dependence of the intensity maximum at T t for strong reflections has been determined and semi-quantitatively explained on the basis of extinction theory. (orig.)

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

Science.gov (United States)

Girardin, E; Millet, P; Lodini, A

2000-02-01

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

Structural studies of metal nanoparticles using high-energy x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Kumara, L. S. R., E-mail: KUMARA.Rosantha@nims.go.jp; Yang, Anli; Song, Chulho [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS) 1-1-1 Kouto, Sayo, Hyogo, 679-5148 (Japan); Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS) 1-1-1 Kouto, Sayo, Hyogo, 679-5148 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo, 679-5148 (Japan); Department of Innovative and Engineered Materials, Tokyo Institute of Technology, 4259-J3-16, Nagatsuta, Midori, Yokohama 226-8502 (Japan); Kohara, Shinji [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS) 1-1-1 Kouto, Sayo, Hyogo, 679-5148 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo, 679-5148 (Japan); Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Kusada, Kohei; Kobayashi, Hirokazu [Division of Chemistry, Graduate School of Science, Kyoto University, Kitashirakawa Oiwake-cho, Sakyo-ku, Kyoto 606-8502 Japan (Japan); Kitagawa, Hiroshi [Division of Chemistry, Graduate School of Science, Kyoto University, Kitashirakawa Oiwake-cho, Sakyo-ku, Kyoto 606-8502 Japan (Japan); INAMORI Frontier Research Center, Kyushu University, 744 Motooka, Nishi-ku, Fukuoka 819-0395 Japan (Japan); Institute for Integrated Cell-Material Sciences (iCeMS), Kyoto University, Yoshida, Sakyo-ku, Kyoto 606-8501 Japan (Japan)

2016-07-27

The XRD patterns of nanoparticles exhibit broad Bragg peaks because of small size, where the contribution of diffuse component provides us with inherent structural information. Therefore, pair distribution function obtained from a Fourier transformation of high-energy XRD data and structure modeling on the basis of diffraction data becomes an essential tool to understand the structure of nanoparticles. This promising tool was utilized to obtain structural information of Pd/Pt bimetallic core/shell and solid-solution nanoparticles, which show much attention due to their improved hydrogen storage capacity and catalytic activity.

Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

Energy Technology Data Exchange (ETDEWEB)

Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

2010-07-19

Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

White-Beam X-ray Diffraction and Radiography Studies on High-Boron Containing Borosilicate Glass at High Pressures

Science.gov (United States)

Ham, Kathryn; Vohra, Yogesh; Kono, Yoshio; Wereszczak, Andrew; Patel, Parimal

Multi-angle energy-dispersive x-ray diffraction studies and white-beam x-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron content borosilicate glass sample (17.6% B2O3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å-1, is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed an overall uniaxial compression of 22.5 % at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si-O, O-O, and Si-Si bond distances were measured as a function of pressure. Raman spectroscopy of pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and B3O6 boroxol rings. US Army Research Office under Grant No. W911NF-15-1-0614.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

International Nuclear Information System (INIS)

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

1999-01-01

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

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

International Nuclear Information System (INIS)

YangDai, Tianyi; Zhang, Li

2016-01-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Energy Technology Data Exchange (ETDEWEB)

YangDai, Tianyi [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China); Zhang, Li, E-mail: zhangli@nuctech.com [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China)

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Science.gov (United States)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

High-energy synchrotron X-ray radiography of shock-compressed materials

Science.gov (United States)

Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

2015-06-01

This presentation will discuss the development and application of a high-energy (50 to 250 keV) synchrotron X-ray imaging method to study shock-compressed, high-Z samples at Beamline I12 at the Diamond Light Source synchrotron (Rutherford-Appleton Laboratory, UK). Shock waves are driven into materials using a portable, single-stage gas gun designed by the Institute of Shock Physics. Following plate impact, material deformation is probed in-situ by white-beam X-ray radiography and complimentary velocimetry diagnostics. The high energies, large beam size (13 x 13 mm), and appreciable sample volumes (~ 1 cm3) viable for study at Beamline I12 compliment existing in-house pulsed X-ray capabilities and studies at the Dynamic Compression Sector. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

Synchrotron high energy X-ray diffraction study of microstructure evolution of severely cold drawn NiTi wire during annealing

International Nuclear Information System (INIS)

Yu, Cun; Aoun, Bachir; Cui, Lishan; Liu, Yinong; Yang, Hong; Jiang, Xiaohua; Cai, Song; Jiang, Daqiang; Liu, Zunping; Brown, Dennis E.; Ren, Yang

2016-01-01

Microstructure evolution of a cold-drawn NiTi shape memory alloy wire was investigated by means of in-situ synchrotron high-energy X-ray diffraction during continuous heating. The cold-drawn wire contained amorphous regions and nano-crystalline domains in its microstructure. Pair distribution function analysis revealed that the amorphous regions underwent structural relaxation via atomic rearrangement when heated above 100 °C. The nano-crystalline domains were found to exhibit a strong cold work induced lattice strain anisotropy along 〈111〉, which coincides with the crystallographic fiber orientation of the domains along the wire axial direction. The lattice strain anisotropy systematically decreased upon heating above 200 °C, implying a structural recovery. Crystallization of the amorphous phase led to a broadening of the angular distribution of 〈111〉 preferential orientations of grains along the axial direction as relative to the original 〈111〉 axial fiber texture of the nanocrystalline domains produced by the severe cold wire drawing deformation.

Study of the earth's deep interior and crystallography. X-ray and neutron diffraction experiments under high pressures

International Nuclear Information System (INIS)

Yagi, Takehiko

2014-01-01

History of the study of the Earth's deep interior was reviewed. In order to understand Earth's deep interior from the view point of materials science, X-ray diffraction under high pressure and high temperature played very important role. Use of synchrotron radiation dramatically advanced this experimental technique and it is now possible to make precise X-ray study under the P-T conditions corresponding even to the center of the Earth. In order to clarify the behavior of light elements such as hydrogen, however, studies using neutron diffraction are also required. A new neutron beam line dedicated for high-pressure science is constructed at J-PARC and is now ready for use. (author)

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

International Nuclear Information System (INIS)

Zolotoyabko, E.; Quintana, J.P.

2004-01-01

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

X-ray diffraction investigation of spin reorientation in SmFe2

International Nuclear Information System (INIS)

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

1996-01-01

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

Thermal expansion studies on Inconel-600[reg] by high temperature X-ray diffraction

International Nuclear Information System (INIS)

Raju, S.; Sivasubramanian, K.; Divakar, R.; Panneerselvam, G.; Banerjee, A.; Mohandas, E.; Antony, M.P.

2004-01-01

The lattice thermal expansion characteristics of Inconel-600[reg] have been studied by high temperature X-ray diffraction (HT-XRD) technique in the temperature range 298-1200 K. Altogether four experimental runs were conducted on thin foils of about 75-100 μm thickness. The diffraction profiles have been accurately calibrated to offset the shift in 2θ values introduced by sample buckling at elevated temperatures. The corrected lattice parameter data have been used to estimate the instantaneous and mean linear thermal expansion coefficients as a function of temperature. The thermal expansion values estimated in the present study show a fair degree of agreement with other existing dilatometer based bulk thermal expansion estimates. The lattice parameter for this alloy at 300 K is found to be 0.3549(1) nm. The mean linear thermal expansivity is found to be 11.4 x 10 -6 K -1

High-pressure X-ray diffraction experiments on US using synchrotron radiation

International Nuclear Information System (INIS)

Olsen, J.S.; Steenstrup, S.

1983-12-01

High-pressure X-ray diffraction studies have been performed on US up to 40 GPa using synchrotron radiation and a diamond anvil cell. The measured value of the bulk modulus B 0 = 92 GPa is in reasonable agreement with calculations. The high-pressure behaviour indicates a phase transformation to US III at about 15 GPa. The transformation is a smooth deformation process, which starts with a tetragonal structure asub(tetr) = asub(cub)/√2, csub(tetr) = 2asub(cub) and continues with an orthorhombic structure with a = 375(3)pm, b = 345(3)pm, c = 1069 (24)pm at 35 GPa; it is of second order nature within experimental errors and it should involve some contributions from uranium f electrons. (orig.)

High pressure in-situ X-ray diffraction study on Zn-doped magnetite nanoparticles

Science.gov (United States)

Ferrari, S.; Bilovol, V.; Pampillo, L. G.; Grinblat, F.; Errandonea, D.

2018-03-01

We have performed high pressure synchrotron X-ray powder diffraction experiments on two different samples of Zn-doped magnetite nanoparticles (formula Fe(3-x)ZnxO4; x = 0.2, 0.5). The structural behavior of then a noparticles was studied up to 13.5 GPa for x = 0.2, and up to 17.4 GPa for x = 0.5. We have found that both systems remain in the cubic spinel structure as expected for this range of applied pressures. The analysis of the unit cell volume vs. pressure results in bulk modulus values lower than in both end-members, magnetite (Fe3O4) and zinc ferrite (ZnFe2O4), suggesting that chemical disorder may favor compressibility, which is expected to improve the increase of the Neel temperature under compression.

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

Science.gov (United States)

2013-01-01

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

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

Science.gov (United States)

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

2002-03-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Patel, J. R.

2002-08-16

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2002-03-26

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

Fatigue life assessment for pipeline welds by x-ray diffraction technique

International Nuclear Information System (INIS)

Lee, Sang Guk; Yoo, Keun Bong

2006-01-01

The objective of this study is to estimate the feasibility of X-ray diffraction method application for fatigue life assessment of the high-temperature pipeline steel such as main steam pipe, re-heater pipe and header etc. in power plant. In this study, X-ray diffraction tests using various types of specimen simulated low cycle fatigue damage were performed in order to analyze fatigue properties when fatigue damage conditions become various stages such as 1/4, l/2 and 3/4 of fatigue life, respectively. As a result off-ray diffraction tests for specimens simulated fatigue damages, we conformed that the variation of the full width at half maximum intensity decreased in proportion to the increase of fatigue life ratio. And also, He ratio of the full width at half maximum intensity due to fatigue damage has linear relationship with fatigue life ratio algebraically. From this relationship, it was suggested that direct expectation of the life consumption rate was feasible.

High energy x-ray scattering studies of strongly correlated oxides

International Nuclear Information System (INIS)

Hatton, Peter D; Wilkins, S B; Spencer, P D; Zimmermann, M v; D'Almeida, T

2003-01-01

Many transition metal oxides display strongly correlated charge, spin, or orbital ordering resulting in varied phenomena such as colossal magnetoresistance, high temperature superconductivity, metal-insulator transitions etc. X-ray scattering is one of the principle techniques for probing the structural response to such effects. In this paper, we discuss and review the use of synchrotron radiation high energy x-rays (50-200 keV) for the study of transition metal oxides such as nickelates (La 2-x Sr x NiO 4 ) and manganites (La 2-2x Sr 1+2x Mn 2 O 7 ). High energy x-rays have sufficient penetration to allow us to study large flux-grown single crystals. The huge increase in sample scattering volume means that extremely weak peaks can be observed. This allows us to study very weak charge ordering. Measurements of the intensity, width and position of the charge ordering satellites as a function of temperature provide us with quantitative measures of the charge amplitude, inverse correlation length and wavevector of the charge ordering

High temperature X-ray diffraction studies on HfO2-Gd2O3 system

International Nuclear Information System (INIS)

Panneerselvam, G.; Antony, M.P.; Ananthasivan, K.; Joseph, M.

2016-01-01

High temperature X-ray diffraction (HTXRD) technique is an important experimental tool for measuring thermal expansion of materials of interest. A series of solid solutions containing GdO 1.5 in HfO 2 ,Hf 1-y Gd y )O 2 (y = 0.15, 0.2, 0.3, 0.41 and 0.505) were prepared by solid state method. Structural characterization and computation of lattice parameter was carried out by using room temperature X-ray diffraction measurements. The room temperature lattice parameter estimated for (Hf 1-y Gd y )O 2 (y=0.15, 0.2, 0.3, 0.41 and 0.505) are 0.51714 nm, 0.51929 nm, 0.52359nm, 0.52789nm and 0.53241 nm, respectively. Thermal expansion coefficients and percentage linear thermal expansion of the HfO 2 -Gd 2 O 3 solid solutions containing 20 and 41 mol% GdO 1.5 were determined using HTXRD in the temperature range 298 to 1673K. The mean linear thermal expansion coefficients of the solid solutions containing 20 and 41 mol. %Gd are 11.65 x 10 -6 K -1 and 12.07 x 10 -6 K -1 , respectively. (author)

Elasticity of Tantalum to 105 Gpa using a stress and angle-resolved x-ray diffraction

International Nuclear Information System (INIS)

Cynn, H; Yoo, C S

1999-01-01

Determining the mechanical properties such as elastic constants of metals at Mbar pressures has been a difficult task in experiment. Following the development of anisotropic elastic theory by Singh et al.[l], Mao et a1.[2] have recently developed a novel experimental technique to determine the elastic constants of Fe by using the stress and energy-dispersive x-ray diffraction (SEX). In this paper, we present an improved complementary technique, stress and angle-resolved x-ray diffraction (SAX), which we have applied to determine the elastic constants of tantalum to 105 GPa. The extrapolation of the tantalum elastic data shows an excellent agreement with the low-pressure ultrasonic data[3]. We also discuss the improvement of this SAX method over the previous SEX.[elastic constant, anisotropic elastic theory, angle-dispersive synchrotron x-ray diffraction, mechanical properties

High thermal efficiency x-ray energy conversion scheme for advanced fusion reactors

International Nuclear Information System (INIS)

Quimby, D.C.; Taussig, R.T.; Hertzberg, A.

1977-01-01

This paper reports on a new radiation energy conversion scheme which appears to be capable of producing electricity from the high quality x-ray energy with efficiencies of 60 to 70 percent. This new reactor concept incorporates a novel x-ray radiation boiler and a new thermal conversion device known as an energy exchanger. The low-Z first walls of the radiation boiler are semi-transparent to x-rays, and are kept cool by incoming working fluid, which is subsequently heated to temperatures of 2000 to 3000 0 K in the interior of the boiler by volumetric x-ray absorption. The radiation boiler may be a compact part of the reactor shell since x-rays are readily absorbed in high-Z materials. The energy exchanger transfers the high-temperature working fluid energy to a lower temperature gas which drives a conventional turbine. The overall efficiency of the cycle is characterized by the high temperature of the working fluid. The high thermal efficiencies which appear achievable with this cycle would make an otherwise marginal advanced fusion reactor into an attractive net power producer. The operating principles, initial conceptual design, and engineering problems of the radiation boiler and thermal cycle are presented

New imaging technique based on diffraction of a focused x-ray beam

Energy Technology Data Exchange (ETDEWEB)

Kazimirov, A [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853 (United States); Kohn, V G [Russian Research Center ' Kurchatov Institute, 123182 Moscow (Russian Federation); Cai, Z-H [Advanced Photon Source, 9700 S. Cass Avenue, Argonne, IL 60439 (United States)], E-mail: ayk7@cornell.edu

2009-01-07

We present first experimental results from a new diffraction depth-sensitive imaging technique. It is based on the diffraction of a focused x-ray beam from a crystalline sample and recording the intensity pattern on a high-resolution CCD detector positioned at a focal plane. Structural non-uniformity inside the sample results in a region of enhanced intensity in the diffraction pattern. The technique was applied to study silicon-on-insulator thin layers of various thicknesses which revealed a complex strain profile within the layers. A circular Fresnel zone plate was used as a focusing optic. Incoherent diffuse scattering spreads out of the diffraction plane and results in intensity recorded outside of the focal spot providing a new approach to separately register x-rays scattered coherently and incoherently from the sample. (fast track communication)

High-Resolution Detector For X-Ray Diffraction

Science.gov (United States)

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

1988-01-01

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

Dual-energy X-ray radiography for automatic high-Z material detection

International Nuclear Information System (INIS)

Chen Gongyin; Bennett, Gordon; Perticone, David

2007-01-01

There is an urgent need for high-Z material detection in cargo. Materials with Z > 74 can indicate the presence of fissile materials or radiation shielding. Dual (high) energy X-ray material discrimination is based on the fact that different materials have different energy dependence in X-ray attenuation coefficients. This paper introduces the basic physics and analyzes the factors that affect dual-energy material discrimination performance. A detection algorithm is also discussed

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.

High energy X-ray phase and dark-field imaging using a random absorption mask.

Science.gov (United States)

Wang, Hongchang; Kashyap, Yogesh; Cai, Biao; Sawhney, Kawal

2016-07-28

High energy X-ray imaging has unique advantage over conventional X-ray imaging, since it enables higher penetration into materials with significantly reduced radiation damage. However, the absorption contrast in high energy region is considerably low due to the reduced X-ray absorption cross section for most materials. Even though the X-ray phase and dark-field imaging techniques can provide substantially increased contrast and complementary information, fabricating dedicated optics for high energies still remain a challenge. To address this issue, we present an alternative X-ray imaging approach to produce transmission, phase and scattering signals at high X-ray energies by using a random absorption mask. Importantly, in addition to the synchrotron radiation source, this approach has been demonstrated for practical imaging application with a laboratory-based microfocus X-ray source. This new imaging method could be potentially useful for studying thick samples or heavy materials for advanced research in materials science.

Comparison of neutron and high-energy X-ray dual-beam radiography for air cargo inspection

International Nuclear Information System (INIS)

Liu, Y.; Sowerby, B.D.; Tickner, J.R.

2008-01-01

Dual-beam radiography techniques utilising various combinations of high-energy X-rays and neutrons are attractive for screening bulk cargo for contraband such as narcotics and explosives. Dual-beam radiography is an important enhancement to conventional single-beam X-ray radiography systems in that it provides additional information on the composition of the object being imaged. By comparing the attenuations of transmitted dual high-energy beams, it is possible to build a 2D image, colour coded to indicate material. Only high-energy X-rays, gamma-rays and neutrons have the required penetration to screen cargo containers. This paper reviews recent developments and applications of dual-beam radiography for air cargo inspection. These developments include dual high-energy X-ray techniques as well as fast neutron and gamma-ray (or X-ray) radiography systems. High-energy X-ray systems have the advantage of generally better penetration than neutron systems, depending on the material being interrogated. However, neutron systems have the advantage of much better sensitivity to material composition compared to dual high-energy X-ray techniques. In particular, fast neutron radiography offers the potential to discriminate between various classes of organic material, unlike dual energy X-ray techniques that realistically only offer the ability to discriminate between organic and metal objects

Characterization of Brazilian asphalt using X-ray diffraction

International Nuclear Information System (INIS)

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

2007-01-01

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

Intergranular stress study of TC11 titanium alloy after laser shock peening by synchrotron-based high-energy X-ray diffraction

Science.gov (United States)

Su, R.; Li, L.; Wang, Y. D.; Nie, Z. H.; Ren, Y.; Zhou, X.; Wang, J.

2018-05-01

The distribution of residual lattice strain as a function of depth were carefully investigated by synchrotron-based high energy X-ray diffraction (HEXRD) in TC11 titanium alloy after laser shock peening (LSP). The results presented big compressive residual lattice strains at surface and subsurface, then tensile residual lattice strains in deeper region, and finally close to zero lattice strains in further deep interior with no plastic deformation thereafter. These evolutions in residual lattice strains were attributed to the balance of direct load effect from laser shock wave and the derivative restriction force effect from surrounding material. Significant intergranular stress was evidenced in the processed sample. The intergranular stress exhibited the largest value at surface, and rapidly decreased with depth increase. The magnitude of intergranular stress was proportional to the severity of the plastic deformation caused by LSP. Two shocks generated larger intergranular stress than one shock.

Effect of Boron Doping on High-Resolution X-Ray Diffraction Metrology

Science.gov (United States)

Faheem, M.; Zhang, Y.; Dai, X.

2018-03-01

The effect of boron (B) doping on high-resolution X-ray diffraction (HXRD) metrology has been investigated. Twelve samples of Si1-xGex films were epitaxially grown on Si (100) substrates with different thicknesses, germanium (Ge) concentrations and with/without B dopants. Secondary ion mass spectroscopy (SIMS) and HXRD were employed for measurements of B doping, Ge concentration, strain, and thickness of the layers. The SIMS results show the absence of B in two samples while the rest of the samples have B doping in the range of 8.40 × 1018-8.7 × 1020 atoms/cm3 with Ge concentration of 13.3-55.2 at.%. The HXRD measurements indicate the layers thickness of 7.07-108.13 nm along with Ge concentration of 12.82-49.09 at.%. The difference in the Ge concentration measured by SIMS and HXRD was found to deend on B doping. For the undoped samples, the difference is 0.5 at.% and increases with B doping but with no linear proportionality. The difference in the Ge concentration was 7.11 at.% for the highly B-doped (8.7 × 1020 atoms/cm3) sample. The B doping influences the Si1-xGex structure, causing a change in the lattice parameter and producing tensile strains shifting Si1-xGex peaks towards Si (100) substrate peaks in the HXRD diffraction patterns. As a result, Vegard's law is no longer effective and makes a high impact on the HXRD measurement. The comparison between symmetric (004) and asymmetric (+113, +224) reciprocal space mappings (RSM) showed a slight difference in Ge concentration between the undoped and lower B-doped samples. However, there is a change of 0.21 at.% observed for the highly doped Si1-xGex samples. RSM's (+113) demonstrate the small SiGe peak broadening as B doping increases, which indicates a minor crystal distortion.

Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

Science.gov (United States)

Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

2004-11-01

The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

High resolution x-ray diffraction analysis of annealed low-temperature gallium arsenide

Science.gov (United States)

Matyi, R. J.; Melloch, M. R.; Woodall, J. M.

1992-05-01

High resolution x-ray diffraction methods have been used to characterize GaAs grown at low substrate temperatures by molecular beam epitaxy and to examine the effects of post-growth annealing on the structure of the layers. Double crystal rocking curves from the as-deposited epitaxial layer show well-defined interference fringes, indicating a high level of structural perfection despite the presence of excess arsenic. Annealing at temperatures from 700 to 900 °C resulted in a decrease in the perpendicular lattice mismatch between the GaAs grown at low temperature and the substrate from 0.133% to 0.016% and a decrease (but not total elimination) of the visibility of the interference fringes. Triple-crystal diffraction scans around the 004 point in reciprocal space exhibited an increase in the apparent mosaic spread of the epitaxial layer with increasing anneal temperature. The observations are explained in terms of the growth of arsenic precipitates in the epitaxial layer.

X-ray powder diffraction data on miscellaneous lanthanide compounds

International Nuclear Information System (INIS)

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

1978-08-01

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

X-ray diffraction of multilayers and superlattices

International Nuclear Information System (INIS)

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

1986-01-01

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

Time-resolved x-ray diffraction measurement of C60 under high pressure and temperature using synchrotron radiation

International Nuclear Information System (INIS)

Horikawa, T; Suito, K; Kobayashi, M; Onodera, A

2002-01-01

C 60 has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C 60 structure are presented and the relevance to the hardness of materials derived from C 60 is discussed

X-ray diffraction and chemical bonding

International Nuclear Information System (INIS)

Bats, J.W.

1976-01-01

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

Mineralogical analysis of clays in hardsetting soil horizons, by X-ray fluorescence and X-ray diffraction using Rietveld method

International Nuclear Information System (INIS)

Prandel, L.V.; Saab, S.C.; Brinatti, A.M.; Giarola, N.F.B.; Leite, W.C.; Cassaro, F.A.M.

2014-01-01

Diffraction and spectroscopic techniques have been shown to be suitable for obtaining physical and mineralogical properties in polycrystalline soil samples, and also in their precursor compounds. For instance, the X-ray fluorescence (XRF) spectroscopy allows obtaining the elemental composition of an investigated sample, while the X-ray diffraction (XRD) technique permits obtaining qualitative and quantitative composition of the soil minerals through the Rietveld method (RM). In this study Yellow Latosol (Oxisol), Yellow Argisol (Ultisol) and Gray Argisol (Ultisol) soil samples, classified as “hardsetting soils”, extracted from areas located at Northeast and Southeast of Brazilian coast were investigated. The soils and their fractions were analyzed in an EDX-700 and an XRD-6000 (Cu K α radiation). XRF results indicate high percentages of Si and Al, and small percentage of Fe and Ti in the investigated samples. The DRX data and RM indicate that there was a predominance of kaolinite and halloysite minerals (kaolin group minerals) in the clay fractions, which are presumably responsible for the formation of kaolinitic plasma in these soils. Also, the obtained results showed that the XRF, XRD techniques and RM were very helpful for investigating the mineralogical composition of a hardsetting soil. - Highlights: ► Elemental composition of soil samples through X-Ray fluorescence. ► Mineralogical quantification through X-ray diffraction and Rietveld method. ► Oxisol and Ultisol, Brazil ‘Barreiras’ formation. ► High amounts of Si and Al oxides and low amounts of Fe and Ti oxides. ► Predominance of kaolinite in the clay fraction

Stability of dislocation structures in copper towards stress relaxation investigated by high angular resolution 3D X-ray diffraction

DEFF Research Database (Denmark)

Jakobsen, Bo; Poulsen, Henning Friis; Lienert, Ulrich

2009-01-01

A 300 µm thick tensile specimen of OFHC copper is subjected to a tensile loading sequence and deformed to a maximal strain of 3.11%. Using the novel three-dimensional X-ray diffraction method High angular resolution 3DXRD', the evolution of the microstructure within a deeply embedded grain....... In contrast to the deformation stages, during each stress relaxation stage, number, size and orientation of subgrains are found to be constant, while a minor amount of clean-up of the microstructure is observed as narrowing of the radial X-ray diffraction line profile. The associated decrease in the width...

High energy X-ray observations of COS-B gamma-ray sources from OSO-8

Science.gov (United States)

Dolan, J. F.; Crannell, C. J.; Dennis, B. R.; Frost, K. J.; Orwig, L. E.; Caraveo, P. A.

1985-01-01

During the three years between satellite launch in June 1975 and turn-off in October 1978, the high energy X-ray spectrometer on board OSO-8 observed nearly all of the COS-B gamma-ray source positions given in the 2CG catalog (Swanenburg et al., 1981). An X-ray source was detected at energies above 20 keV at the 6-sigma level of significance in the gamma-ray error box containing 2CG342 - 02 and at the 3-sigma level of significance in the error boxes containing 2CG065 + 00, 2CG195 + 04, and 2CG311 - 01. No definite association between the X-ray and gamma-ray sources can be made from these data alone. Upper limits are given for the 2CG sources from which no X-ray flux was detected above 20 keV.

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…

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...

Clinopyroxenes still trapped in diamonds: high-energy synchrotron X-ray diffraction as a chemical probe

Science.gov (United States)

Casati, Nicola; Nestola, Fabrizio; Alvaro, Matteo; Wilhelm, Heribert; Kleppe, Annette; Nimis, Paolo; Harris, Jeffrey W.

2014-05-01

Clinopyroxenes are mainly Ca-Na-Fe-Mg-silicates constituting a significant portion of the Earth's upper mantle up to 20% of such shell of our planet. They could be found as typical mineral inclusions in diamonds being diopsidic and omphacitic in composition and, together with garnets, cover a key role in providing indications concerning the source rock in which the diamond crystallize. In detail, it is well known that eclogitic diamonds are characterized by clinopyroxenes with omphacitic compositions (about Ca0.5Na0.5Mg0.5Al0.5Si2O6) whereas peridotitic diamonds show clinopyroxenes very rich in the diopside end-member (CaMgSi2O6). In order to get direct chemical composition on the inclusions, and therefore on the diamond origin source, it is obviously necessary to extract them breaking and/or polishing the diamond host. However, a non-destructive investigation of an inclusion still trapped in a diamond is useful and important for different reasons: (1) the inclusions could be under pressure and their crystal structure can be modified if the pressure is released by the extraction; (2) the residual pressure on the inclusion can provide information about the formation pressure of the diamond (e.g. Nestola et al. 2011 and references therein); (3) the morphology and growth relationships of the inclusion with the host diamond can provide indications about its protogenetic vs. syngenetic and/or epigenetic nature; and (4) preservation of the diamond surface growth features can maintain crucial information on late oxidation processes (Fedortchouk et al. 2011). However the available methods to measure the composition of the inclusions implies to destroy the sample. The aim of this work is to obtain chemical information on the inclusions still trapped in their diamond host and therefore to indicate the diamond origin without extracting the inclusions. The work was carried out by single crystal X-ray diffraction using a new experimental approach by high energy synchrotron

Raman spectroscopy and X-ray diffraction studies on celestite

International Nuclear Information System (INIS)

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

2010-01-01

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

Quantitative determination of mineral composition by powder X-ray diffraction

International Nuclear Information System (INIS)

Pawloski, G.A.

1986-01-01

A method is described of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where mless than or equal ton, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K/sub j/=(X/sub j//X/sub l/)(I/sub l//I/sub j/) for each mineral (j=2...n) in the group of known minerals (j=2...n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; identifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X/sub j//X/sub l/ for each mineral (j=2...m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I/sub j/ of each mineral in the test sample to the measured highest integrated intensity peak I/sub l/ of the reference mineral in the test sample, and from the previously determined standard coefficients, X/sub j//X/sub l/=K/sub j/(I/sub j//I/sub l/

Individual GaAs nanorods imaged by coherent X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Pietsch, Ullrich; Biermanns, Andreas; Davydok, Anton [Universitaet Siegen (Germany); Paetzelt, Hendrik [Universitaet Leipzig (Germany); IOM Leipzig (Germany); Diaz, Ana; Metzger, Hartmut [ID01 Beamline, ESRF (France); Gottschalch, Volker [Universitaet Leipzig (Germany)

2010-07-01

Semiconductor nanorods are of particular interest for new semiconductor devices because the nanorod approach can be used to form heterostructures of materials with a large lattice mismatch and to define nanorod arrays with tailored inter-rod distance. However, all applications require objects with uniform physical properties based on uniform morphology. Complementary to electron microscopy techniques, destruction free X-ray diffraction techniques can be used to determine structural and morphological details. Using scanning X-ray diffraction microscopy with a spot size of 220 x 600 nm{sup 2} we were able to inspect individual GaAs nanorods grown by seed-free MOVPE through circular openings in a SiN{sub x} mask in a periodic array with 3 {mu}m spacing on GaAs[111]B. The focussed X-ray beam allows the determination of the strain state of individual rods and in combination with coherent diffraction imaging, we were able to characterize also morphological details. Rods grown at different positions in the array show significant differences in shape, size and strain state.

High energy x-ray and neutron studies of disordered energy-related materials at extreme conditions

International Nuclear Information System (INIS)

Parise, John

2016-01-01

The fundamental scientific accomplishments are: (1) advances in a general description of the liquid state by employing structural models constrained by measurements to interpret experimental results and extend them to liquids in general, with special emphasis on (2) The structure of the high-temperature crystal and molten UO_2 and 3) water. Specifically, samples of UO_2 and water were probed using high-energy x-rays at the Advanced Photon Source. The high Z of UO_2, and the 2-3mm diameter droplet shape of the molten sample, means that >100keV X-rays are required to minimize absorption and multiple scattering, which can distort the measured structure factor. A high flux of x-rays is also required to obtain sufficient statistical accuracy in short (a few seconds) measurement times. The scattered x-ray data were analyzed and pair distribution functions, extracted that characterize the local and long-range atomic structure of the material. The measurements of the hot UO_2 solid show a substantial increase in oxygen disorder and, upon melting, the average U-O coordination was found to decrease from 8 to 6.7±0.5. The research incorporated development of diffraction techniques, sample environment optimization and state-of-the-art simulation techniques. The symbiotic nature of the advances in simulation and experiment allowed for a more focused and informed development of future experiments, effective use of expensive beam time and generated new research agendas for the growing number of research groups, within the US and internationally, that focus on the structure of liquids. Molecular dynamics (MD) provided detailed information when combined with high-quality XN data including addressing key issues in liquids; the relationship between cooling path, structure and fictive temperature, and the trade-offs between network over connectedness in liquids containing low-coordination cations.

High energy x-ray and neutron studies of disordered energy-related materials at extreme conditions

Energy Technology Data Exchange (ETDEWEB)

Parise, John [Stony Brook Univ., NY (United States)

2016-05-16

The fundamental scientific accomplishments are: (1) advances in a general description of the liquid state by employing structural models constrained by measurements to interpret experimental results and extend them to liquids in general, with special emphasis on (2) The structure of the high-temperature crystal and molten UO₂ and 3) water. Specifically, samples of UO₂ and water were probed using high-energy x-rays at the Advanced Photon Source. The high Z of UO₂, and the 2-3mm diameter droplet shape of the molten sample, means that >100keV X-rays are required to minimize absorption and multiple scattering, which can distort the measured structure factor. A high flux of x-rays is also required to obtain sufficient statistical accuracy in short (a few seconds) measurement times. The scattered x-ray data were analyzed and pair distribution functions, extracted that characterize the local and long-range atomic structure of the material. The measurements of the hot UO₂ solid show a substantial increase in oxygen disorder and, upon melting, the average U-O coordination was found to decrease from 8 to 6.7±0.5. The research incorporated development of diffraction techniques, sample environment optimization and state-of-the-art simulation techniques. The symbiotic nature of the advances in simulation and experiment allowed for a more focused and informed development of future experiments, effective use of expensive beam time and generated new research agendas for the growing number of research groups, within the US and internationally, that focus on the structure of liquids. Molecular dynamics (MD) provided detailed information when combined with high-quality XN data including addressing key issues in liquids; the relationship between cooling path, structure and fictive temperature, and the trade-offs between network over connectedness in liquids containing low-coordination cations.

Biological imaging by soft X-ray diffraction microscopy

Science.gov (United States)

Shapiro, David

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

High-Pressure X-ray Diffraction Study of Tungsten Diselenide

International Nuclear Information System (INIS)

Selvi, E.; Aksoy, R.; Knudson, R.; Ma, Y.

2008-01-01

Synchrotron X-ray diffraction was used in conjunction with a diamond anvil cell to investigate the properties of a tungsten diselenide (WSe2) sample to 35.8 GPa at room temperature. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus, K0T, of WSe2 was determined to be 72±1 GPa with its pressure derivative, K(prime) 0T , being 4.1±0.1. It was also found that the c-direction of the hexagonal structure is significantly more compressible than the a-direction. No phase transformation was clearly observed in the pressure range of our measurements.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

Energy Technology Data Exchange (ETDEWEB)

Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031 (China); Huang, J. W.; Zeng, X. L.; Li, Y.; E, J. C.; Huang, J. Y. [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Sun, T.; Fezzaa, K. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Wang, Z. [Physics Division P-25, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

2016-05-15

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.

X-Ray Diffraction Project Final Report, Fiscal Year 2006

International Nuclear Information System (INIS)

Dane V. Morgan

2006-01-01

An x-ray diffraction diagnostic system was developed for determining real-time shock-driven lattice parameter shifts in single crystals at the gas gun at TA-IV at Sandia National Laboratories (SNL). The signal-to-noise ratio and resolution of the system were measured using imaging plates as the detector and by varying the slit width. This report includes tests of the x-ray diffraction system using a phosphor coupled to a charge-coupled device (CCD) camera by a coherent fiber-optic bundle. The system timing delay was measured with a newly installed transistor-transistor logic (TTL) bypass designed to reduce the x-ray delay time. The axial misalignment of the Bragg planes was determined with respect to the optical axis for a set of eight LiF [lithium fluoride] crystals provided by SNL to determine their suitability for gas gun experiments

Contribution of x-ray topography and high-resolution diffraction to the study of defects in SiC

International Nuclear Information System (INIS)

Dudley, Michael; Huang Xianrong; Vetter, William M

2003-01-01

A short review is presented of the various synchrotron white beam x-ray topography (SWBXT) imaging techniques developed for characterization of silicon carbide (SiC) crystals and thin films. These techniques, including back-reflection topography, reticulography, transmission topography, and a set of section topography techniques, are demonstrated to be particularly powerful for imaging hollow-core screw dislocations (micropipes) and closed-core threading screw dislocations, as well as other defects, in SiC. The geometrical diffraction mechanism commonly underlying these imaging processes is emphasized for understanding the nature and origins of these defects. Also introduced is the application of SWBXT combined with high-resolution x-ray diffraction techniques to complete characterization of 3C/4H or 3C/6H SiC heterostructures, including polytype identification, 3C variant mapping, and accurate lattice mismatch measurements

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.

High Resolution Higher Energy X-ray Microscope for Mesoscopic Materials

International Nuclear Information System (INIS)

Snigireva, I; Snigirev, A

2013-01-01

We developed a novel X-ray microscopy technique to study mesoscopically structured materials, employing compound refractive lenses. The easily seen advantage of lens-based methodology is the possibility to retrieve high resolution diffraction pattern and real-space images in the same experimental setup. Methodologically the proposed approach is similar to the studies of crystals by high resolution transmission electron microscopy. The proposed microscope was applied for studying of mesoscopic materials such as natural and synthetic opals, inverted photonic crystals

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

Science.gov (United States)

Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

2011-03-01

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

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

Science.gov (United States)

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

2016-05-01

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

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.

New methods of X-ray diffraction spectrometry. II

International Nuclear Information System (INIS)

Soerum, H.; Bremer, J.

1980-01-01

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

Energy spectrum measurement of high power and high energy(6 and 9 MeV) pulsed x-ray source for industrial use

Energy Technology Data Exchange (ETDEWEB)

Takagi, Hiroyuki [Hitachi, Ltd. Power Systems Company, Ibaraki (Japan); Murata, Isao [Graduate School of Engineering, Osaka University, Osaka (Japan)

2016-06-15

Industrial X-ray CT system is normally applied to non-destructive testing (NDT) for industrial product made from metal. Furthermore there are some special CT systems, which have an ability to inspect nuclear fuel assemblies or rocket motors, using high power and high energy (more than 6 MeV) pulsed X-ray source. In these case, pulsed X-ray are produced by the electron linear accelerator, and a huge number of photons with a wide energy spectrum are produced within a very short period. Consequently, it is difficult to measure the X-ray energy spectrum for such accelerator-based X-ray sources using simple spectrometry. Due to this difficulty, unexpected images and artifacts which lead to incorrect density information and dimensions of specimens cannot be avoided in CT images. For getting highly precise CT images, it is important to know the precise energy spectrum of emitted X-rays. In order to realize it we investigated a new approach utilizing the Bayesian estimation method combined with an attenuation curve measurement using step shaped attenuation material. This method was validated by precise measurement of energy spectrum from a 1 MeV electron accelerator. In this study, to extend the applicable X-ray energy range we tried to measure energy spectra of X-ray sources from 6 and 9 MeV linear accelerators by using the recently developed method. In this study, an attenuation curves are measured by using a step-shaped attenuation materials of aluminum and steel individually, and the each X-ray spectrum is reconstructed from the measured attenuation curve by the spectrum type Bayesian estimation method. The obtained result shows good agreement with simulated spectra, and the presently developed technique is adaptable for high energy X-ray source more than 6 MeV.

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

DEFF Research Database (Denmark)

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

2009-01-01

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

High-pressure phases of uranium monophosphide studied by synchrotron x-ray diffraction

DEFF Research Database (Denmark)

Olsen, J. Staun; Gerward, Leif; Benedict, U.

1988-01-01

X-ray diffraction studies have been performed on UP powder for pressures up to 51 GPa using synchrotron radiation and a diamond-anvil cell. At ambient pressure UP has the rocksalt structure. The bulk modulus has been determined to B0=102(4) GPa and its pressure derivative to B0’=4.0(8). The cubic...

Determination of the stacking fault energies of face centured cubic metals and alloys by X-rays diffraction

International Nuclear Information System (INIS)

Borges, J.F.A.; Padilha, A.F.; Imakuma, K.

1988-03-01

An X-rays diffraction method was applied to measure the Stacking Fault Energies (SFE) of the AISI 304, AISI 316, AISI 347 and DIN-WERKSTOFF 1.4970 Austenitic Stainless Steels. The SFE determination plays an important role in the research of the mecanichal behaviour of the Metal and Alloys, their deformation mechanisms, stability of micro-structure and electronic configuration. The method is based on the relationship between the SFE and the ratio of the Mean Square Strains to the Stacking-Fault probability. The Mean Square Strain was evaluated by Fourier Analysis of X-rays Diffaction profiles, corrected to reduce instrumental effects, followed by the application of the Warren-Averbach method to the Fourier Coefficients. The Stacking-Fault probabilities were derived from the changes of peak separations between cold-worked and annealed specimens. (author) [pt

Accidental exposure with X-ray diffraction equipment

International Nuclear Information System (INIS)

Montanez, O.; Blanco, D.

1991-01-01

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

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

International Nuclear Information System (INIS)

Milch, J.R.

1978-01-01

A TV-type x-ray detector using a SIT vidicon has been used for biological diffraction studies at the EMBL outstation at DESY, Hamburg, Germany. The detector converts the two-dimensional diffraction pattern to a charge pattern on the vidicon target, which is read out in the slow-scan mode. This detector has high DOE, no count-rate limit, and is simple and inexpensive to construct. Radiation from the storage ring DORIS was used to study the structure of live muscle at various phases of contraction. Typically the count-rate on the detector was 10 6 x-rays/sec and a total exposure of a few seconds was needed to record the weak diffraction from muscle. This compares with usual exposure times of several hours using a rotating anode generator and film

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

NARCIS (Netherlands)

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

1994-01-01

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

Basic of X-ray diffraction

International Nuclear Information System (INIS)

Giacovazzo, C.

1996-01-01

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

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.

Residual stress characterization of welds using x-ray diffraction techniques

International Nuclear Information System (INIS)

Pineault, J.A.; Brauss, M.E.

1996-01-01

Neglect of residual stresses created during processes lead to stress corrosion cracking, distortion, fatigue cracking, premature failures in components, and instances of over design. Automated residual stress mapping and truly portable equipment have now made the characterization of residual stresses using x-ray diffraction (XRI) practical. The nondestructive nature of the x-ray diffraction technique has made the tile residual stress characterization of welds a useful tool for process optimization and failure analysis, particularly since components can be measured before and after welding and post welding processes. This paper illustrates the importance of residual stress characterization in welds and presents examples where x-ray diffraction techniques were applied in the characterization of various kinds of welds. arc welds, TIG welds, resistance welds, laser welds and electron beam welds. Numerous techniques are available to help manage potentially harmfull residual stresses created during the welding process thus, the effects of a few example post weld processes such as grinding, heat treating and shot peening are also addressed

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.

Compact energy dispersive X-ray microdiffractometer for diagnosis of neoplastic tissues

Science.gov (United States)

Sosa, C.; Malezan, A.; Poletti, M. E.; Perez, R. D.

2017-08-01

An energy dispersive X-ray microdiffractometer with capillary optics has been developed for characterizing breast cancer. The employment of low divergence capillary optics helps to reduce the setup size to a few centimeters, while providing a lateral spatial resolution of 100 μm. The system angular calibration and momentum transfer resolution were assessed by a detailed study of a polycrystalline reference material. The performance of the system was tested by means of the analysis of tissue-equivalent samples previously characterized by conventional X-ray diffraction. In addition, a simplified correction model for an appropriate comparison of the diffraction spectra was developed and validated. Finally, the system was employed to evaluate normal and neoplastic human breast samples, in order to determine their X-ray scatter signatures. The initial results indicate that the use of this compact energy dispersive X-ray microdiffractometer combined with a simplified correction procedure is able to provide additional information to breast cancer diagnosis.

Detectors for X-ray diffraction and scattering: current technology and future challenges

International Nuclear Information System (INIS)

Bahr, D.; Brugemann, L.; Gerndt, E.

2003-01-01

Full text: Detectors are crucial devices determining the quality, the reliability and the throughput of x-ray diffraction (XRD) and scattering investigations. This is of utmost importance in an industrial environment where in many cases untrained personnel or even without human intervention the experiments and data evaluations are running. The currently used technology of 0-dimensional to 2-dim XRD detectors is presented using selected examples. The application specific requirements on e.g. energy range and resolution, count rate limit, background and dynamic range, and size versus price are discussed. Due to the fact that x-ray diffraction investigations are becoming increasingly attractive in science, research and industry the advance in detector technology is pushed beyond existing limits. The discussion of the resultant market opportunities versus the cost of ownership and market entrance barrier is the final section of the presentation

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.

Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

CERN Document Server

Ellmer, K; Weiss, V; Rossner, H

2001-01-01

A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3 deg. and 10 deg., is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

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

International Nuclear Information System (INIS)

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

2002-01-01

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

Contained x-ray diffraction goniometer for examination of radioactive materials

International Nuclear Information System (INIS)

Smith, P.K.; Osgood, B.C.; Blaser, D.E.; Howell, R.E.; Stuhler, H.; Stauver, J.

1987-11-01

Radioactive materials are being characterized for chemical form and certain physical properties with an x-ray diffraction goniometer customized for containment in a shielded alpha glovebox. A Siemens D500 goniometer was customized by Siemens to locate the associated electronics and x-ray generator outside the glovebox to minimize corrosion and facilitate maintenance. A graphite monochromator is used with a shielded scintillation detector to separate diffracted x-radiation from nuclear radiation. The diffraction system is computer automated for data acquisition and reduction. The facility is designed to handle primarily alpha- and beta-emitting samples with moderate neutron and gamma radiation. Samples containing plutonium, enriched uranium, and other transuranic elements are analyzed in support of site nuclear operations and development programs on nuclear waste, chemical separations, reactor fuels, and product forms

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Yanagisawa, Yasuhide [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Chatake, Toshiyuki [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Chiba-Kamoshida, Kaori [National Institute of Advanced Industrial Science and Technology (AIST), Umezono 1-1-1, Tsukuba, Ibaraki 305-8568 (Japan); Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki [Kurashiki University of Science and Arts, Nishinoura 2640, Tsurajima-cho, Kurashiki, Okayama 712-8505 (Japan); Yasuda, Ichiro [Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan); Morimoto, Yukio [Research Reactor Institute, Kyoto University, Asashironishi 2, Kumatori, Sennan, Osaka 590-0494 (Japan); Faculty of Pharmaceutical Sciences, Chiba Institute of Science, 15-8 Shiomi-cho, Choshi, Chiba 288-0025 (Japan)

2010-12-01

Nattokinase, a protein found in high levels in the traditional Japanese food natto, has been reported to have high thrombolytic activity. In the present study, the crystallization of native nattokinase and the collection of X-ray diffraction date from a nattokinase crystal to a resolution of 1.74 Å are reported. Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27 724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b = 49.9, c = 56.3 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å with an R{sub merge} of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase.

On the measurement of the stacking-fault energies of face centered cubic metal and austenitic stainless steels by X-ray diffraction

International Nuclear Information System (INIS)

Borges, J.F.A.

1985-01-01

An X-rays diffraction method was applied to measure the Stacking-Fault Energies (SFE) of the AISI 304, AISI 316, AISI 347 and DIN-WERKSTOFF 1.4970 Austenitic Stainless Steels. The SFE determination plays an important role in the research of the mechanical behaviour of the Metal and Alloys, their deformation mechanisms, stability of microstructure amd electronic configuration. The method is based on the relationship between the SFE and the ratio of the Mean Square Strain to the Stacking-Fault probability. The Mean Square Strain was evaluated by Fourier Analysis of X-rays Diffraction profiles, corrected to reduce instrumental effects, followed by the application of the Warren-Averbach method to the Fourier Coefficients. The Stacking-Fault probabilities were derived from the changes of peak separations between cold-worked and annealed specimens. (author) [pt

A differential scanning calorimetric and X-ray diffraction

Indian Academy of Sciences (India)

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-05-06

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

Competing orbital ordering in RVO3 compounds: High-resolution x-ray diffraction and thermal expansion

International Nuclear Information System (INIS)

Sage, M. H.; Blake, G. R.; Palstra, T. T. M.; Marquina, C.

2007-01-01

We report evidence for the phase coexistence of orbital orderings of different symmetry in RVO 3 compounds with intermediate-size rare earths. Through a study by high-resolution x-ray powder diffraction and thermal expansion, we show that the competing orbital orderings are associated with the magnitude of the VO 6 octahedral tilting and magnetic exchange striction in these compounds and that the phase-separated state is stabilized by lattice strains

High-pressure x-ray diffraction study on lithium borohydride using a synchrotron radiation

Science.gov (United States)

Nakano, S.; Nakayama, A.; Kikegawa, T.

2008-07-01

Lithium borohydride (LiBH4) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P42/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH4.

High-pressure x-ray diffraction study on lithium borohydride using a synchrotron radiation

Energy Technology Data Exchange (ETDEWEB)

Nakano, S [National Institute for Materials Science, Tsukuba, Ibaraki 305-0044 (Japan); Nakayama, A [Department of Materials Science and Engineering, Meijo University, Nagoya 468-8502 (Japan); Kikegawa, T [Photon Factory (PF), Institute of Materials Structure Science, High Energy Accelerator Research Organization (KEK), Ibaraki 305-0801 (Japan)], E-mail: NAKANO.Satoshi@nims.go.jp

2008-07-15

Lithium borohydride (LiBH{sub 4}) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P4{sub 2}/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH{sub 4}.

X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

Science.gov (United States)

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

2002-07-01

Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

Discovery and development of x-ray diffraction

Science.gov (United States)

Jeong, Yeuncheol; Yin, Ming; Datta, Timir

2013-03-01

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

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.

Glancing angle synchrotron X-ray diffraction

International Nuclear Information System (INIS)

Cernik, R.J.

1996-01-01

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

Determination of densities from chemical composition and X-Ray diffraction

International Nuclear Information System (INIS)

Azevedo, A.L.T. de

1980-01-01

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

New medical imaging systems exploiting the energy dispersive X-ray diffraction with spectrometric CdZnTe based detector

International Nuclear Information System (INIS)

Barbes, Damien

2016-01-01

This thesis studies the interest of measuring the coherent scattering of X-rays for breast diagnosis imaging. Nowadays, most of X-ray-based medical imaging techniques use the information of X-rays attenuation through the tissues. It is the case for mammography, the most common breast imaging modality. The recent emergence of energy resolved detectors (based on semiconductors in particular) allows to consider using another phenomenon: the coherent X-ray scattering. Measurement of diffracted spectra can provide new information related to the molecular structure of the examined tissues, in order to improve their characterization and therefore improve the final diagnosis. Two modalities are considered: the breast cancer detection in vivo, following a suspicious mammography result, or biopsy analysis. The coherent scattering measurement system developed during this thesis work uses energy-resolved CdZnTe-based detectors, these detectors combining performances (energy resolution, sensitivity, spatial resolution, and compactness) promising for clinical application. This system is also based on the detector pixelation, which allows to provide an imaging modality capable of characterizing analyzed materials or tissues in one direction without any translation or rotation. A complete study of the measurement system is proposed in this thesis, structured in three main parts: modeling and simulation of the system, development of the processing of the data measured by the detector in order to image and characterize the analyzed sample and finally, designing of a new and more complex experimental setup based on a whole detector and multi-slit collimation system. An experimental validation is proposed for each of these three parts. (author) [fr

High-pressure pair distribution function (PDF) measurement using high-energy focused x-ray beam

Energy Technology Data Exchange (ETDEWEB)

Hong, Xinguo, E-mail: xhong@bnl.gov; Weidner, Donald J. [Mineral Physics Institute, Stony Brook University, Stony Brook, NY 11794 (United States); Ehm, Lars [Mineral Physics Institute, Stony Brook University, Stony Brook, NY 11794 (United States); National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Zhong, Zhong; Ghose, Sanjit [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Duffy, Thomas S. [Department of Geosciences, Princeton University, Princeton, NJ 08544 (United States)

2016-07-27

In this paper, we report recent development of the high-pressure pair distribution function (HP-PDF) measurement technique using a focused high-energy X-ray beam coupled with a diamond anvil cell (DAC). The focusing optics consist of a sagittally bent Laue monochromator and Kirkpatrick-Baez (K–B) mirrors. This combination provides a clean high-energy X-ray beam suitable for HP-PDF research. Demonstration of the HP-PDF technique for nanocrystalline platinum under quasi-hydrostatic condition above 30 GPa is presented.

High-energy particle diffraction

International Nuclear Information System (INIS)

Barone, V.; Predazzi, E.

2002-01-01

This monograph gives a comprehensive and up-to-date overview of soft and hard diffraction processes in strong interaction physics. The first part covers the general formalism (the optical analogy, the eikonal picture, high-energy kinematics, S-matrix theory) and soft hadron-hadron scattering (including the Regge theory) in a complete and mature presentation. It can be used as a textbook in particle physics classes. The remainder of the book is devoted to the 'new diffraction': the pomeron in QCD, low-x physics, diffractive deep inelastic scattering and related processes, jet production etc. It presents recent results and experimental findings and their phenomenological interpretations. This part addresses graduate students as well as researchers. (orig.)

Processing two-dimensional X-ray diffraction and small-angle scattering data in DAWN 2.

Science.gov (United States)

Filik, J; Ashton, A W; Chang, P C Y; Chater, P A; Day, S J; Drakopoulos, M; Gerring, M W; Hart, M L; Magdysyuk, O V; Michalik, S; Smith, A; Tang, C C; Terrill, N J; Wharmby, M T; Wilhelm, H

2017-06-01

A software package for the calibration and processing of powder X-ray diffraction and small-angle X-ray scattering data is presented. It provides a multitude of data processing and visualization tools as well as a command-line scripting interface for on-the-fly processing and the incorporation of complex data treatment tasks. Customizable processing chains permit the execution of many data processing steps to convert a single image or a batch of raw two-dimensional data into meaningful data and one-dimensional diffractograms. The processed data files contain the full data provenance of each process applied to the data. The calibration routines can run automatically even for high energies and also for large detector tilt angles. Some of the functionalities are highlighted by specific use cases.

Time-resolved x-ray diffraction measurement of C{sub 60} under high pressure and temperature using synchrotron radiation

Energy Technology Data Exchange (ETDEWEB)

Horikawa, T [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Suito, K [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Kobayashi, M [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Onodera, A [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan)

2002-11-11

C{sub 60} has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C{sub 60} structure are presented and the relevance to the hardness of materials derived from C{sub 60} is discussed.

X-ray diffraction studies of NbTe2 single crystal

Indian Academy of Sciences (India)

Unknown

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

Experimental coherent X-ray diffractive imaging: capabilities and limitations of the technique

International Nuclear Information System (INIS)

Schropp, Andreas

2008-08-01

The investigations pursued during this work were focused on the testing of the applicability of the coherent X-ray diffractive imaging(CXDI)-method in the hard X-ray regime and different measurements were carried out at photon energies between 7 keV and 10 keV. The samples investigated were lithographically prepared two-dimensional gold structures with a size ranging from 3 μm to 10 μm as well as a cluster of gold spheres with a lateral extension of about 3.5 μm. Continuous diffraction patterns were recorded in small angle scattering geometry. In some of the measurements a scattering signal up to the edge of the detector could be measured which corresponds to a lateral resolution of about 30 nm. For certain samples it was possible to reconstruct the object from the measured diffraction data. Since the scattered intensity of non-periodic objects is weak at large scattering angles, the available photon flux is finally the main limitation of the method with regard to the achievable resolution. The experimental data were used to get an estimate of photon flux required for sub-nanometer resolution. The ptychographic iterative phase retrieval algorithm proposed by J. M. Rodenburg et al. (2004) was implemented and tested on simulated diffraction data. Additionally, a genetic algorithm has been developed and implemented for phase retrieval. This algorithm is very different from state-of-the-art algorithms and allows to introduce further experimentally important parameters such as a certain illumination function and partial coherence of the X-ray light. (orig.)

High energy X-ray observation of Cyg X-3

International Nuclear Information System (INIS)

Kendziorra, E.; Pietsch, W.; Staubert, R.; Truemper, J.

1975-01-01

On Feb. 20, 1975 Cyg X-3 was observed in the energy range of 29-70 keV during a 5 hour observation of the Cyg region. An intensity variation consistent with a 4.8 h sinusoidal modulation has been found, in phase with low energy X-ray observations and with a relative amplitude of 0.37 +- 0.19. (orig.) [de

Extending the methodology of X-ray crystallography to allow X-ray microscopy without X-ray optics

International Nuclear Information System (INIS)

Miao Jianwei; Kirz, Janos; Sayre, David; Charalambous, Pambos

2000-01-01

We demonstrate that the soft X-ray diffraction pattern from a micron-size noncrystalline specimen can be recorded and inverted to form a high-resolution image. The phase problem is overcome by oversampling the diffraction pattern. The image is obtained using an iterative algorithm. The technique provides a method for X-ray microscopy requiring no high-resolution X-ray optical elements or detectors. In the present work, a resolution of approximately 60 nm was obtained, but we believe that considerably higher resolution can be achieved

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

Energy Technology Data Exchange (ETDEWEB)

Ludwig, W., E-mail: ludwig@esrf.fr [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); King, A. [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); School of Materials, University of Manchester, Manchester, M13 9PL (United Kingdom); Reischig, P. [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); Herbig, M. [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); Lauridsen, E.M.; Schmidt, S. [Riso National Laboratory for Sustainable Energy, Technical University of Denmark, P.O. Box 49, DK-4000 Roskilde (Denmark); Proudhon, H.; Forest, S. [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Cloetens, P.; Roscoat, S. Rolland du [European Synchrotron Radiation Facility, BP220, 38043 Grenoble (France); Buffiere, J.Y. [Universite de Lyon, INSA-Lyon, MATEIS CNRS UMR 5510, 69621Villeurbanne (France); Marrow, T.J. [School of Materials, University of Manchester, Manchester, M13 9PL (United Kingdom); Poulsen, H.F. [Riso National Laboratory for Sustainable Energy, Technical University of Denmark, P.O. Box 49, DK-4000 Roskilde (Denmark)

2009-10-25

Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes and crystallographic orientations for certain categories of polycrystalline materials. Direct visualisation of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques may be possible, but is restricted to specific material systems. A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape, crystallographic orientation and local attenuation coefficient distribution. The technique applies to the larger range of plastically undeformed, polycrystalline mono-phase materials, provided some conditions on grain size and texture are fulfilled. The straightforward combination with high-resolution microtomography opens interesting new possibilities for the observation of microstructure related damage and deformation mechanisms in these materials.

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

International Nuclear Information System (INIS)

Ludwig, W.; King, A.; Reischig, P.; Herbig, M.; Lauridsen, E.M.; Schmidt, S.; Proudhon, H.; Forest, S.; Cloetens, P.; Roscoat, S. Rolland du; Buffiere, J.Y.; Marrow, T.J.; Poulsen, H.F.

2009-01-01

Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes and crystallographic orientations for certain categories of polycrystalline materials. Direct visualisation of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques may be possible, but is restricted to specific material systems. A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape, crystallographic orientation and local attenuation coefficient distribution. The technique applies to the larger range of plastically undeformed, polycrystalline mono-phase materials, provided some conditions on grain size and texture are fulfilled. The straightforward combination with high-resolution microtomography opens interesting new possibilities for the observation of microstructure related damage and deformation mechanisms in these materials.

X-ray diffraction study of WO3 at high pressure

International Nuclear Information System (INIS)

Bouvier, P.; Crichton, W.A.; Boulova, M.; Lucazeau, G.

2002-01-01

The high-pressure behaviour of microcrystalline tungsten oxide (WO 3 ) has been investigated with angle-dispersive synchrotron x-ray powder diffraction in a diamond anvil cell up to 40 GPa at room temperature. Up to 21 GPa, the pressure dependence of the volume of the monoclinic high-pressure (P2 1 /c) phase is described by a third-order Birch-Murnaghan equation of state with parameters V 0 =210.9(7)A 3 , K T =27(2)GP a and K'=9.4(5). At 24 GPa, a first-order phase transition occurs with an approximate Δ V of 7.4% to a monoclinic P2 1 /a unit cell with a=6.1669(8)A, b=4.5758(6)A, c=5.3159(6)A, β=101.440(9) deg. A second transition is observed at pressures higher than 31 GPa with an approximate Δ V of 12% to a phase described by a third monoclinic unit cell, with a=10.3633(22)A, b=3.9065(8)A, c=9.3459(18)A and β=98.539(14) deg. (author)

A high pressure x-ray diffraction study of titanium disulfide

International Nuclear Information System (INIS)

Aksoy, Resul; Selvi, Emre; Knudson, Russell; Ma Yanzhang

2009-01-01

A high pressure angle dispersive synchrotron x-ray diffraction study of titanium disulfide (TiS 2 ) was carried out to pressures of 45.5 GPa in a diamond-anvil cell. We observed a phase transformation of TiS 2 beginning at about 20.7 GPa. The structure of the high pressure phase needs further identification. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus, K 0T , was determined to be 45.9 ± 0.7 GPa with its pressure derivative, K' 0T , being 9.5 ± 0.3 at pressures lower than 17.8 GPa. It was found that the compression behavior of TiS 2 is anisotropic along the different axes. The compression ratio of the c-axis is about nine times larger than the a-axis when pressures are lower than 1 GPa. It suddenly decreases to three times larger at pressures of about 3 GPa. This ratio shows a linear decrease with a slope of negative 0.048 at pressures below phase transformation.

X-ray filter for x-ray powder diffraction

Science.gov (United States)

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

2018-01-23

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

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

International Nuclear Information System (INIS)

Farrahi, G.H.

1996-01-01

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

X-Rays from NGC 3256: High-Energy Emission in Starburst Galaxies and Their Contribution to the Cosmic X-Ray Background

International Nuclear Information System (INIS)

Moran, Edward C.; Lehnert, Matthew D.; Helfand, David J.

1999-01-01

The infrared-luminous galaxy NGC 3256 is a classic example of a merger-induced nuclear starburst system. We find here that it is the most X-ray-luminous star-forming galaxy yet detected (L 0.5-10keV =1.6x10 42 ergs s-1). Long-slit optical spectroscopy and a deep, high-resolution ROSAT X-ray image show that the starburst is driving a ''superwind'' which accounts for ∼20% of the observed soft X-ray emission. Analysis of X-ray spectral data from ASCA indicates this gas has a characteristic temperature of kT≅0.3 keV. Our model for the broadband X-ray emission of NGC 3256 contains two additional components: a warm thermal plasma (kT≅0.8 keV) associated with the central starburst, and a hard power-law component with an energy index of α X ≅0.7. We discuss the energy budget for the two thermal plasmas and find that the input of mechanical energy from the starburst is more than sufficient to sustain the observed level of emission. We also examine possible origins for the power-law component, concluding that neither a buried AGN nor the expected population of high-mass X-ray binaries can account for this emission. Inverse Compton scattering, involving the galaxy's copious flux of infrared photons and the relativistic electrons produced by supernovae, is likely to make a substantial contribution to the hard X-ray flux. Such a model is consistent with the observed radio and IR fluxes and the radio and X-ray spectral indices. We explore the role of X-ray-luminous starbursts in the production of the cosmic X-ray background radiation. The number counts and spectral index distribution of the faint radio source population, thought to be dominated by star-forming galaxies, suggest that a significant fraction of the hard X-ray background could arise from starbursts at moderate redshift. (c) (c) 1999. The American Astronomical Society

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

International Nuclear Information System (INIS)

Andreeva, N. S.

2006-01-01

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

Quantitative determination of phases by X-ray diffraction

International Nuclear Information System (INIS)

Azevedo, A.L.T.

1979-01-01

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

Direct methods for surface X-ray diffraction

International Nuclear Information System (INIS)

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

2000-01-01

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

X-ray absorption spectroscopy and high-energy XRD study of the local environment of copper in antibacterial copper-releasing degradable phosphate glasses

OpenAIRE

Pickup, David M.; Ahmed, Ifty; Fitzgerald, Victoria; Moss, Rob M.; Wetherall, Karen; Knowles, Jonathan C.; Smith, Mark E.; Newport, Robert J.

2006-01-01

Phosphate-based glasses of the general formula Na2O-CaO-P2O5 are degradable in an aqueous environment, and therefore can act as antibacterial materials through the inclusion of ions such as copper. In this study, CuO and Cu2O were added to Na2O-CaO-P2O5 glasses (1-20 mol% Cu) and X-ray absorption spectroscopy (XAS) and high-energy X-ray diffraction (HEXRD) used to probe the local environment of the copper ions. Copper K-edge X-ray absorption near-edge structure (XANES) spectra confirm the oxi...

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

International Nuclear Information System (INIS)

Yoo, Keun Bong; Kim, Jae Hoon

2009-01-01

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

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

Science.gov (United States)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

Dynamics of oxygen ordering in YBa2CU3O6+x studied by neutron and high-energy synchrotron x-ray diffiaction.

Science.gov (United States)

Frello, T.; Andersen, N. H.; Madsen, J.; Ka¨ll, M.; von Zimmermann, M.; Schmidt, O.; Poulsen, H. F.; Schneider, J. R.; Wolf, Th.

1997-08-01

The dynamics of the ortho-II oxygen structure in a high purity YBa 2Cu 3O 6+ x single crystal with x=0.50 has been studied by neutron and by X-ray diffraction with a photon energy of 100 keV. Our data show that the oxygen order develops on two different time-scales, one of the order of seconds and a much slower of the order of weeks and months. The mechanism dominating the slow time-scale is related to oxygen diffusion, while the fast mechanism may result from a temperature-dependent change in the average oxygen chain length.

Diamond Thermal Expansion Measurement Using Transmitted X-ray Back-diffraction.

OpenAIRE

Giles, Carlos; Adriano, Cris; Lubambo, Adriana Freire; Cusatis, Cesar; Mazzaro, Irineu; Hönnicke, Marcelo Goncalves

2015-01-01

The linear thermal expansion coefficient of diamond has been measured using forward-diffracted profiles in X-ray backscattering. This experimental technique is presented as an alternative way of measuring thermal expansion coefficients of solids in the high-resolution Bragg backscattering geometry without the intrinsic difficulty of detecting the reflected beam. The temperature dependence of the lattice parameter is obtained from the high sensitivity of the transmitted profiles to the Bragg a...

X-ray diffraction characteristics of curved monochromators for sychrotron radiation

International Nuclear Information System (INIS)

Boeuf, A.; Rustichelli, F.; Mazkedian, S.; Puliti, P.; Melone, S.

1978-01-01

A theoretical study is presented concerning the diffraction characteristics of curved monochromators for X-ray synchrotron radiation used at the laboratories of Hamburg, Orsay and Stanford. The investigation was performed by extending to the X-ray case a simple model recently developed and fruitfully employed to describe the neutron diffraction properties of curved monochromators. Several diffraction patterns were obtained corresponding to different monochromator materials (Ge, Si) used by the different laboratories, for different reflecting planes (111), (220), asymmetry angles, X-ray wave-lengths (Mo Kα, Cu Kα, Cr Kα) and curvature radii. The results are discussed in physical terms and their implications on the design of curved monochromators for synchrotron radiation are presented. In particular, the study shows that all the monochromators used in the different laboratories should behave practically as perfect crystals and therefore should have a very low integrated reflectivity corresponding to an optimized wavelength passband Δlambda/lambda approximately 10 -4 . The gain that can be obtained by increasing the curvature, by introducing a gradient in the lattice spacing or by any other kind of imperfection is quite limited and much lower than the desirable value. The adopted model can help in obtaining a possible moderate gain in intensity by also taking into consideration other parameters, such as crystal material, reflecting plane, asymmetry of the reflection and X-ray wavelength. (Auth.)

submitter Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

CERN Document Server

Zhang, Hongjia; Salvati, Enrico; Daisenberger, Dominik; Lunt, Alexander J G; Fong, Kai Soon; Song, Xu; Korsunsky, Alexander M

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated...

Hard X-ray nanoimaging method using local diffraction from metal wire

Energy Technology Data Exchange (ETDEWEB)

Takano, Hidekazu, E-mail: htakano@sci.u-hyogo.ac.jp; Konishi, Shigeki; Shimomura, Sho; Azuma, Hiroaki; Tsusaka, Yoshiyuki; Kagoshima, Yasushi [Center for Novel Material Science under Multi-Extreme Conditions, Graduate School of Material Science, University of Hyogo, Kamigori, Hyogo 678-1297 (Japan)

2014-01-13

A simple hard X-ray imaging method achieving a high spatial resolution is proposed. Images are obtained by scanning a metal wire through the wave field to be measured and rotating the sample to collect data for back projection calculations; the local diffraction occurring at the edges of the metal wire operates as a narrow line probe. In-line holograms of a test sample were obtained with a spatial resolution of better than 100 nm. The potential high spatial resolution of this method is shown by calculations using diffraction theory.

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

Czech Academy of Sciences Publication Activity Database

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

2011-01-01

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

X-ray diffraction topography. Stages and tendencies of development

International Nuclear Information System (INIS)

Shul'pina, I.L.

2000-01-01

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

Variable-metric diffraction crystals for x-ray optics

International Nuclear Information System (INIS)

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

1992-01-01

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

Dehydration reactions of gypsum: A neutron and X-ray diffraction study

Science.gov (United States)

Abriel, W.; Reisdorf, K.; Pannetier, J.

1990-03-01

The kinetics of the dehydration of gypsum was investigated by powder diffraction methods. Using the incoherent scattering effect of H with the neutron beam, the background intensity as a measure of the water content was checked in the temperature range 295-623 K. The superposed Bragg peaks yielded four major phases: Gypsum, subhydratesCaSO 4(H 2O) x (1 > x > 0),AIII-CaSO 4, AII-CaSO 4. For the subhydrates a maximum water content of x > = 0.74was determined. A different kinetic was found using Guinier X-ray technique with the heated sample prepared on a thin foil. Only with high local H 2O steam pressure, produced in the comparable larger sample container of the neutron diffraction experiment, could this high H 2O occupation of the subhydrate tunnel structure be found. A topotactic mechanism can describe the phase transitions for this reaction.

Extinction correction in white X-ray and neutron diffraction

International Nuclear Information System (INIS)

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

1980-01-01

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

High-pressure X-ray diffraction studies on ThS up to 40 GPa using synchrotron radiation

International Nuclear Information System (INIS)

Benedict, U.; Spirlet, J.C.; Gerward, L.; Olsen, J.S.

1983-12-01

High-pressure X-ray diffraction studies have been performed on ThS up to 40 GPa using synchrotron radiation and a diamond anvil cell. The measured value of the bulk modulus B 0 =145 GPa is in disagreement with a previous measurement. The high-pressure behaviour indicates a phase transformation to ThS II starting at 15 to 20 GPa. The transformation is of second order nature, the resulting structure can be described as distorted fcc. (orig.)

High pressure X-ray diffraction studies on ThS up to 40 GPa using synchrotron radiation

International Nuclear Information System (INIS)

Benedict, U.; Spirlet, J.C.; Gerward, L.; Olsen, J.S.

1984-01-01

High pressure X-ray diffraction studies (up to 40 GPa) were performed on ThS using synchrotron radiation and a diamond anvil cell. The measured value of 145 GPa for the bulk modulus B 0 disagrees with a previous measurement. The high pressure behaviour indicates a phase transformation to ThS II starting at 15 - 20 GPa. The transformation is of the second-order type, and the resulting structure can be described as distorted f.c.c. (Auth.)

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

DEFF Research Database (Denmark)

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

1993-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-06-24

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

Secondary-source energy-dispersive x-ray spectrometer

International Nuclear Information System (INIS)

Larsen, R.P.; Tisue, G.T.

1975-01-01

A secondary-source energy-dispersive x-ray spectrometer has been built and tested. In this instrument the primary source of x rays is a tungsten-target tube powered by a high-voltage (75 kV), a high-power (3.7 kW) generator from a wavelength spectrometer (G.E. XRD-6). The primary polychromatic x rays irradiate an elemental foil, the secondary source. Its characteristic essentially monochromatic x rays are used to irradiate the sample. Fluorescent x rays from the sample are detected and resolved by a lithium-drifted silicon detector, multichannel-analyzer system. The design of the instrument provides a convenient means for changing the secondary, and hence, the energy of the excitation radiation

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

International Nuclear Information System (INIS)

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

2009-01-01

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

High pressure X-ray studies

International Nuclear Information System (INIS)

Sikka, S.K.

1981-01-01

High pressure research has already led to new insights in the physical properties of materials and at times to the synthesis of new ones. In all this, X-ray diffraction has been a valuable diagnostic experimental tool. In particular, X-rays in high pressure field have been used (a) for crystallographic identification of high pressure polymorphs and (b) for study of the effect of pressure on lattice parameters and volume under isothermal conditions. The results in the area (a) are reviewed. The techniques of applying high pressures are described. These include both static and dynamic shockwave X-ray apparatus. To illustrate the effect of pressure, some of the pressure induced phase transitions in pure metals are described. It has been found that there is a clear trend for elements in any group of the periodic table to adopt similar structures at high pressures. These studies have enabled to construct generalized phase diagrams for many groups. In the case of alloys, the high pressure work done on Ti-V alloys is presented. (author)

Quantitative mineralogical analysis of sandstones using x-ray diffraction techniques

International Nuclear Information System (INIS)

Ward, C.R.; Taylor, J.C.

1999-01-01

Full text: X-ray diffraction has long been used as a definitive technique for mineral identification based on the measuring the internal atomic or crystal structures present in powdered rocks; soils and other mineral mixtures. Recent developments in data gathering and processing, however, have provided an improved basis for its use as a quantitative tool, determining not only the nature of the minerals but also the relative proportions of the different minerals present. The mineralogy of a series of sandstone samples from the Sydney and Bowen Basins of eastern Australia has been evaluated by X-ray diffraction (XRD) on a quantitative basis using the Australian-developed SIROQUANT data processing technique. Based on Rietveld principles, this technique generates a synthetic X-ray diffractogram by adjusting and combining full-profile patterns of minerals nominated as being present in the sample and interactively matches the synthetic diffractogram under operator instructions to the observed diffractogram of the sample being analysed. The individual mineral patterns may be refined in the process, to allow for variations in crystal structure of individual components or for factors such as preferred orientation in the sample mount. The resulting output provides mass percentages of the different minerals in the mixture, and an estimate of the error associated with each individual percentage determination. The chemical composition of the mineral mixtures indicated by SIROQUANT for each individual sandstone studied was estimated using a spreadsheet routine, and the indicated proportion of each oxide in each sample compared to the actual chemical analysis of the same sandstone as determined independently by X-ray fluorescence spectrometry. The results show a high level of agreement for all major chemical constituents, indicating consistency between the SIROQUANT XRD data and the whole-rock chemical composition. Supplementary testing with a synthetic corundum spike further

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....

High-pressure optical spectroscopy and X-ray diffraction studies on synthetic cobalt aluminum silicate garnet

DEFF Research Database (Denmark)

N. Taran, Michail; Nestola, Fabrizio; Ohashi, Haruo

2007-01-01

The pressure-induced behavior of spin-allowed dd-bands of VIIICo2+ in the absorption spectra of synthetic Co3Al2Si3O12 garnet was studied from 10-4 to 13 GPa. The plots of the peak energy vs. pressure for the three sharpest well resolved bands at ca. 5160, 17 680, and 18 740 cm-1 display small...... but discernible breaks in linear relations between 4 and 5 GPa. Datafromsingle-crystalX-raydiffractionData from single-crystal X-ray diffraction likewise show discontinuities in trends of CoO8 polyhedral volume and distortion, and Co-O and Si-O bond distances over this pressure range. These effects are related...... to a pressure-induced phase transition from the ß- to a-isostructural polymorph of Co3Al2Si3O12....

Modulated High-Energy Gamma-Ray Emission from the Micro-quasar Cygnus X-3

International Nuclear Information System (INIS)

Abdo, A.A.; Cheung, C.C.; Dermer, C.D.; Grove, J.E.; Johnson, W.N.; Lovellette, M.N.; Makeev, A.; Ray, P.S.; Strickman, M.S.; Wood, K.S.; Abdo, A.A.; Cheung, C.C.; Ackermann, M.; Ajello, M.; Bechtol, K.; Berenji, B.; Blandford, R.D.; Bloom, E.D.; Borgland, A.W.; Cameron, R.A.; Chiang, J.; Claus, R.; Digel, S.W.; Silva, E.D.E.; Drell, P.S.; Dubois, R.; Focke, W.B.; Glanzman, T.; Godfrey, G.; Hayashida, M.; Johannesson, G.; Johnson, A.S.; Kamae, T.; Kocian, M.L.; Lande, J.; Madejski, G.M.; Michelson, P.F.; Mitthumsiri, W.; Monzani, M.E.; Moskalenko, I.V.; Murgia, S.; Nolan, P.L.; Paneque, D.; Reimer, A.; Reimer, O.; Rochester, L.S.; Romani, R.W.; Tanaka, T.; Thayer, J.B.; Tramacere, A.; Uchiyama, Y.; Usher, T.L.; Waite, A.P.; Wang, P.; Ackermann, M.; Ajello, M.; Bechtol, K.; Berenji, B.; Blandford, R.D.; Bloom, E.D.; Borgland, A.W.; Cameron, R.A.; Chiang, J.; Claus, R.; Digel, S.W.; Silva, E.D.E.; Drell, P.S.; Dubois, R.; Focke, W.B.; Glanzman, T.; Godfrey, G.; Hayashida, M.; Johannesson, G.; Johnson, A.S.; Kamae, T.; Kocian, M.L.; Lande, J.; Madejski, G.M.; Michelson, P.F.; Mitthumsiri, W.; Monzani, M.E.; Moskalenko, I.V.; Murgia, S.; Nolan, P.L.; Paneque, D.; Reimer, A.; Reimer, O.; Rochester, L.S.; Romani, R.W.; Tanaka, T.; Thayer, J.B.; Tramacere, A.; Uchiyama, Y.; Usher, T.L.; Waite, A.P.; Wang, P.; Axelsson, M.; Hjalmarsdotter, L.; Axelsson, M.; Conrad, J.; Hjalmarsdotter, L.; Jackson, M.S.; Meurer, C.; Ryde, F.; Ylinen, T.; Baldini, L.; Bellazzini, R.; Brez, A.; Kuss, M.; Latronico, L.; Omodei, N.; Pesce-Rollins, M.; Razzano, M.; Sgro, C.; Ballet, J.; Casandjian, J.M.; Chaty, S.; Corbel, S.; Grenier, I.A.; Koerding, E.; Rodriguez, J.; Starck, J.L.; Tibaldo, L.

2009-01-01

Micro-quasars are accreting black holes or neutron stars in binary systems with associated relativistic jets. Despite their frequent outburst activity, they have never been unambiguously detected emitting high-energy gamma rays. The Fermi Large Area Telescope (LAT) has detected a variable high-energy source coinciding with the position of the x-ray binary and micro-quasar Cygnus X-3. Its identification with Cygnus X-3 is secured by the detection of its orbital period in gamma rays, as well as the correlation of the LAT flux with radio emission from the relativistic jets of Cygnus X-3. The gamma-ray emission probably originates from within the binary system, opening new areas in which to study the formation of relativistic jets. (authors)

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

International Nuclear Information System (INIS)

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

1984-01-01

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

High-pressure x-ray diffraction of icosahedral Zr-Al-Ni-Cu-Ag quasicrystals

DEFF Research Database (Denmark)

Jiang, Jianzhong; Saksl, Karel; Rasmussen, Helge Kildahl