Microstructural characterization of reservoir rocks by X-ray microtomography

International Nuclear Information System (INIS)

Fernandes, Jaquiel Salvi; Appoloni, Carlos Roberto

2007-01-01

The evaluation of microstructural parameters from reservoir rocks is of great importance for petroleum industries. This work presents measurements of total porosity and pore size distribution of a sandstone sample from Tumblagooda geological formation, extracted from the Kalbari National Park in Australia. X-ray microtomography technique was used for determining porosity and pore size distribution. Other techniques, such as mercury intrusion porosimetry and Archimedes method have also been applied for those determinations but since they are regarded destructive techniques, samples cannot usually be used for further analyses. X-ray microtomography, besides allowing future analyses of a sample already evaluated, also provides tridimensional images of the sample. The experimental configuration included a SkysCan 1172 from CENPES-PETROBRAS, Rio de Janeiro, Brazil. The spatial resolution of this equipment is 2.9 μm. Images have been reconstructed using NRecon software and analysed with the IMAGO software developed by the Laboratory of Porous Materials and Thermophysical Properties of the Department of Mechanical Engineering / Federal University of Santa Catarina, Florianopolis, Brazil

Identification of ginseng root using quantitative X-ray microtomography

Directory of Open Access Journals (Sweden)

Linlin Ye

2017-07-01

Conclusion: This study is the first to provide evidence of the distribution characteristics of COCCs to identify four types of ginseng, with regard to species authentication and age identification, by X-ray phase-contrast microtomography quantitative imaging. This method is also expected to reveal important relationships between COCCs and the occurrence of the effective medicinal components of ginseng.

X-ray micro-Tomography at the Advanced Light Source

Science.gov (United States)

The X-ray micro-Tomography Facility at the Advanced Light Source has been in operation since 2004. The source is a superconducting bend magnet of critical energy 10.5KeV; photon energy coverage is 8-45 KeV in monochromatic mode, and a filtered white light option yields useful photons up to 50 KeV. A...

Soft x-ray scanning microtomography with submicron resolution

International Nuclear Information System (INIS)

McNulty, I.; Haddad, W.S.; Trebes, J.E.; Anderson, E.H.

1994-01-01

Scanning soft x-ray microtomography was used to obtain high-resolution three-dimensional images of a microfabricated test object. Using a special rotation stage mounted on the scanning transmission x-ray microscope at the XIA Beamline at the National Synchrotron Light Source, we recorded nine two-dimensional projections of the 3D test object over an angular range of -50 degrees to +55 degrees. The x-ray wavelength was 3.6 nm and the radiation dose to the object per projection was approximately 2 x 10 6 Gy. The object consisted of two gold patterns supported on transparent silicon nitride membranes, separated by 4.75 Jim, with 100 to 300-nm wide and 65-nm thick features. We reconstructed a volumetric data set of the test object from the two-dimensional projections using an algebraic reconstruction technique algorithm. Features of the test object were resolved to ∼100 nm in transverse and longitudinal extent in three-dimensional images rendered from the volumetric set

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.

Soft x-ray scanning microtomography with submicrometer resolution

International Nuclear Information System (INIS)

McNulty, I.; Haddad, W.S.; Trebes, J.E.; Anderson, E.H.

1995-01-01

Scanning soft x-ray microtomography was used to obtain high-resolution three-dimensional images of a microfabricated test object. Using a special rotation stage mounted on the scanning transmission x-ray microscope at the X1A beamline at the National Synchrotron Light Source, we recorded nine two-dimensional projections of the 3D test object over an angular range of -50 degree to +55 degree. The x-ray wavelength was 3.6 nm and the radiation dose to the object per projection was approximately 2x10 6 Gy. The object consisted of two gold patterns supported on transparent silicon nitride membranes, separated by 4.75 μm, with 100- to 300-nm-wide and 65-nm-thick features. We reconstructed a volumetric data set of the test object from the two-dimensional projections using an algebraic reconstruction technique algorithm. Features of the test object were resolved to ∼100 nm in transverse and longitudinal extent with low artifact in three-dimensional images rendered from the volumetric set

Quantitative X-ray microtomography with synchrotron radiation

Energy Technology Data Exchange (ETDEWEB)

Donath, T. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Materialforschung

2007-07-01

Synchrotron-radiation-based computed microtomography (SR{sub {mu}}CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR{sub {mu}}CT measurements have been further improved by enhancements that were made to the SR{sub {mu}}CT apparatus and to the reconstruction chain. For high-resolution SR{sub {mu}}CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR{sub {mu}}CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

Quantitative X-ray microtomography with synchrotron radiation

International Nuclear Information System (INIS)

Donath, T.

2007-01-01

Synchrotron-radiation-based computed microtomography (SR μ CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR μ CT measurements have been further improved by enhancements that were made to the SR μ CT apparatus and to the reconstruction chain. For high-resolution SR μ CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR μ CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

High temperature x-ray micro-tomography

Energy Technology Data Exchange (ETDEWEB)

MacDowell, Alastair A., E-mail: aamacdowell@lbl.gov; Barnard, Harold; Parkinson, Dilworth Y.; Gludovatz, Bernd [Lawrence Berkeley National Lab., Berkeley, CA 94720 (United States); Haboub, Abdel [Lawrence Berkeley National Lab., Berkeley, CA 94720 (United States); current –Lincoln Univ., Jefferson City, Missouri, 65101 (United States); Larson, Natalie; Zok, Frank [University California Santa Barbara, Santa Barbara CA 93106 (United States); Panerai, Francesco; Mansour, Nagi N. [NASA Ames Research Centre, Moffett Field, CA, 94035 (United States); Bale, Hrishikesh [University California Berkeley, Berkeley, CA 94720 (United States); current - Carl Zeiss X-ray Microscopy, 4385 Hopyard Rd #100, Pleasanton, CA 94588 (United States); Acevedo, Claire [Lawrence Berkeley National Lab., Berkeley, CA 94720 (United States); University California San Francisco, San Francisco, CA 94143 (United States); Liu, Dong [University of Bristol, Bristol BS8 1TH (United Kingdom); Ritchie, Robert O. [Lawrence Berkeley National Lab., Berkeley, CA 94720 (United States); University California Berkeley, Berkeley, CA 94720 (United States)

2016-07-27

There is increasing demand for 3D micro-scale time-resolved imaging of samples in realistic - and in many cases extreme environments. The data is used to understand material response, validate and refine computational models which, in turn, can be used to reduce development time for new materials and processes. Here we present the results of high temperature experiments carried out at the x-ray micro-tomography beamline 8.3.2 at the Advanced Light Source. The themes involve material failure and processing at temperatures up to 1750°C. The experimental configurations required to achieve the requisite conditions for imaging are described, with examples of ceramic matrix composites, spacecraft ablative heat shields and nuclear reactor core Gilsocarbon graphite.

Investigation of elemental distribution in lung samples by X-ray fluorescence microtomography

International Nuclear Information System (INIS)

Pereira, Gabriela R.; Rocha, Henrique S.; Lopes, Ricardo T.

2007-01-01

X-Ray Fluorescence Microtomography (XRFCT) is a suitable technique to find elemental distributions in heterogeneous samples. While x-ray transmission microtomography provides information about the linear attenuation coefficient distribution, XRFCT allows one to map the most important elements in the sample. The x-ray fluorescence tomography is based on the use of the X-ray fluorescence emitted from the elements contained in a sample so as to give additional information to characterize the object under study. In this work a rat lung and two human lung tissue samples have been investigated in order to verify the efficiency of the system in determination of the internal distribution of detected elements in these kinds of samples and to compare the elemental distribution in the lung tissue of an old human and a fetus. The experiments were performed at the X-Ray Fluorescence beamline (XRF) of the Brazilian Synchrotron Light Source (LNLS), Campinas, Brazil. A white beam was used for the excitation of the elements and the fluorescence photons have been detected by a HPGe detector. All the tomographies have been reconstructed using a filtered-back projection algorithm. It was possible to visualize the distribution of high atomic number elements on both, artificial and tissues samples. It was compared the quantity of Zn, Cu and Fe for the lung human tissue samples and verify that these elements have a higher concentration on the fetus tissue sample than the adult tissue sample. (author)

Microstructural characterization of industrial foams by gamma ray transmission and X-ray microtomography

International Nuclear Information System (INIS)

Rodrigues, Luiz Eduardo

2004-01-01

This work presents the total porosity measurements of the aluminum and silicon carbide (SiC) foams samples. For porosity determination the gamma ray transmission and X-ray microtomography with conic beam techniques were used. These methods have more advantage than conventional ones, because they are non destructive and provide more details of the analyzed material porous structure. The aluminum foam samples with 10, 20, 30, 40 and 45 ppi (pores per inch) and SiC ceramic foam samples with 20, 30, 45, 60, 75, 80 and 90 ppi were analysed by gamma transmission. The SiC 60, 75 and 90 ppi samples were also analyzed by X-ray microtomography. For the gamma ray transmission measurements it was used an 241 Am source (59.53 keV), a NaI(Tl) scintillation detector, collimators, a XYZ micrometric table and standard gamma spectrometry electronics connected to a multichannel analyzer, at the LFNA/UEL. For the X-ray microtomographic measurements, the Fein Focus X-ray system of the Nuclear Instrumentation Laboratory of the COPPE, located at the Universidade Federal do Rio de Janeiro, Rio de Janeiro, RJ, was used. This equipment provide us images with micrometric resolution (53.48 μm) using a conic X-ray beam and bidimensional detection. The microtomographic images were pre-processed and analyzed by the Imago software, developed at Porous Media and Materials Thermophysical Properties Laboratory (LMPT) of the Mechanical Engineering Department, located at Universidade Federal de Santa Catarina, Florianopolis, SC. Employing the The Imago software it was calculated the total porosity, pore size distribution and autocorrelation function C(u) of the binarized microtomographic images of the each sample. The microtomographic 3-D image of each sample was compared with 3-D image reconstructed by the Gaussian truncated method. This method generates a periodic 3-D porous structure by using of the autocorrelation function of one 2-D cross sectional image of the sample. (author)

Characterization of ceramic archaeological by high resolution X ray microtomography

International Nuclear Information System (INIS)

Machado, Alessandra C.; Freitas, Renato; Calza, Cristiane F.; Lopes, Ricardo T.; Lima, Inaya; Carvalho, Daniele D.; Gaspar, Maria D.

2013-01-01

Characterization of ceramic fragments is a very important area of research in art and archeometry area because it enables a greater understanding of how ancient civilizations behave and what were their traditions and customs. Petrography and chemical analyses are commonly used, but these techniques are destructive, which is not interesting for this type of sample. Through the exchange of multidisciplinary scientific knowledge and new partnerships, high resolution X-ray microtomography has been introduced in archaeological area as a great possibility of 3D inspection in a non-destructive way. The goal of this work is to investigate the internal microstructures of four samples of archeological ceramic, from the Archaeological Site of Macacu - RJ. The X-ray microtomography were performed in a high resolution setup, and can be used to infer the nature of organic temper even with all plant remains completely burnt out during the firing process and also to ensure the homogeneity of samples envisaged for geochemical analyses, especially with respect to the distribution of chemically diverse fabric compounds. In this way this study intends to contribute to our understanding of the archaeological and historical formations of this region. (author)

Characterization of ceramic archaeological by high resolution X ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Machado, Alessandra C.; Freitas, Renato; Calza, Cristiane F.; Lopes, Ricardo T.; Lima, Inaya, E-mail: alecastro@lin.ufrj.br [Coordenacao dos Programas de Pos-Graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Lab. de Instrumentacao Nuclear; Carvalho, Daniele D.; Gaspar, Maria D. [Museu Nacional (MN/UFRJ), RJ (Brazil). Centro de Tecnologia

2013-07-01

Characterization of ceramic fragments is a very important area of research in art and archeometry area because it enables a greater understanding of how ancient civilizations behave and what were their traditions and customs. Petrography and chemical analyses are commonly used, but these techniques are destructive, which is not interesting for this type of sample. Through the exchange of multidisciplinary scientific knowledge and new partnerships, high resolution X-ray microtomography has been introduced in archaeological area as a great possibility of 3D inspection in a non-destructive way. The goal of this work is to investigate the internal microstructures of four samples of archeological ceramic, from the Archaeological Site of Macacu - RJ. The X-ray microtomography were performed in a high resolution setup, and can be used to infer the nature of organic temper even with all plant remains completely burnt out during the firing process and also to ensure the homogeneity of samples envisaged for geochemical analyses, especially with respect to the distribution of chemically diverse fabric compounds. In this way this study intends to contribute to our understanding of the archaeological and historical formations of this region. (author)

X-Ray Micro-Tomography Applied to Nasa's Materials Research: Heat Shields, Parachutes and Asteroids

Science.gov (United States)

Panerai, Francesco; Borner, Arnaud; Ferguson, Joseph C.; Mansour, Nagi N.; Stern, Eric C.; Barnard, Harold S.; Macdowell, Alastair A.; Parkinson, Dilworth Y.

2017-01-01

X-ray micro-tomography is used to support the research on materials carried out at NASA Ames Research Center. The technique is applied to a variety of applications, including the ability to characterize heat shield materials for planetary entry, to study the Earth- impacting asteroids, and to improve broadcloths of spacecraft parachutes. From micro-tomography images, relevant morphological and transport properties are determined and validated against experimental data.

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

Geoscience Applications of Synchrotron X-ray Computed Microtomography

Science.gov (United States)

Rivers, M. L.

2009-05-01

Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution approaching one micron - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa - High speed radiography, with 100 microsecond temporal resolution - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x- ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The formation of frost flowers on Arctic sea-ice, which is important in controlling the atmospheric chemistry of mercury. - The distribution of

X-ray microtomography scanner using time-delay integration for elimination of ring artefacts in the reconstructed image

International Nuclear Information System (INIS)

Davis, G.R.; London Univ.; Elliott, J.C.; London Univ.

1997-01-01

Most X-ray microtomography scanners work on the same principle as third-generation medical CT scanners, that is, the same point in each projection is measured by the same detector element. This leads to ring artefacts in the reconstructed image if the X-ray sensitivities of the individual detector elements, after any analytical correction, are not all identical. We have developed an X-ray microtomography scanner which uses the time-delay integration method of imaging with a CCD detector to average the characteristics of all the detector elements in each linear projection together. This has the added advantage of allowing specimens which are larger than the detector and X-ray field to be scanned. The device also uses a novel mechanical stage to ''average out'' inhomogeneities in the X-ray field. The results show that ring artefacts in microtomographic images are eliminated using this technique. (orig.)

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.

Microstructural characterization of porous materials by X-ray microtomography and gamma ray transmission techniques

International Nuclear Information System (INIS)

Moreira, Anderson Camargo

2006-01-01

This work presents the application of the X-ray microtomography and gamma ray transmission techniques for the microstructure characterization of different kinds of materials. Total porosity, pore size distribution and the two point correlation functions were measured. The two point correlation function, which allows the reconstruction of 3D models, was carried out for two samples. Seven ceramic tablets of Alumina (Al 2 O 3 ), seven tablets of Boron Carbide (B 4 C), three samples of sedimentary rocks and one sample of Titanium foam were analyzed. The experimental set up for the Gamma Ray Transmission technique consisted of: a 2'' x 2'' crystal NaI(Tl) detector, an 241 Am radioactive source (59,53 keV, 100 mCi), an automatic micrometric table for the sample XZ movement and standard gamma spectrometry electronics. Two microtomography systems were used: a Fein Focus system, constituted by an X-ray tube, operated at 160 kV and 0.3 to 1.1 mA, a CCD camera and the movement sample system, and a Skyscan system, model 1072, with a X-ray tube operated at 100 kV and 100μA, and a CCD camera. The ceramic tablets, analyzed by the gamma ray transmission technique presented results for most of the porosities data with smaller confidence intervals and inside the intervals supplied by the tablets manufacturer. The Titanium porous sample was analyzed by the two techniques, its microtomography images achieved a resolution of 17μm, obtained employing the Fein Focus system. For both techniques, this sample showed high porosity, which allows its application for this purpose. The sandstones samples were analyzed by the Skyscan system, achieving resolutions of 19μm, 11μm and 3.8μm for each sample, respectively. The resolutions of 11μm and 3.8μm were the ones that generated better 2D sections for the respective samples and, consequently, more reliable porosities. The 3.8μm resolution was the one that best quantified the pore size distribution data, showing information not shown by

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 microtomography application in pore space reservoir rock.

Science.gov (United States)

Oliveira, M F S; Lima, I; Borghi, L; Lopes, R T

2012-07-01

Characterization of porosity in carbonate rocks is important in the oil and gas industry since a major hydrocarbons field is formed by this lithology and they have a complex media porous. In this context, this research presents a study of the pore space in limestones rocks by x-ray microtomography. Total porosity, type of porosity and pore size distribution were evaluated from 3D high resolution images. Results show that carbonate rocks has a complex pore space system with different pores types at the same facies. Copyright © 2011 Elsevier Ltd. All rights reserved.

High resolution x-ray microtomography of biological samples: Requirements and strategies for satisfying them

Energy Technology Data Exchange (ETDEWEB)

Loo, B.W. Jr. [Univ. of California, San Francisco, CA (United States)]|[Univ. of California, Davis, CA (United States)]|[Lawrence Berkeley National Lab., CA (United States); Rothman, S.S. [Univ. of California, San Francisco, CA (United States)]|[Lawrence Berkeley National Lab., CA (United States)

1997-02-01

High resolution x-ray microscopy has been made possible in recent years primarily by two new technologies: microfabricated diffractive lenses for soft x-rays with about 30-50 nm resolution, and high brightness synchrotron x-ray sources. X-ray microscopy occupies a special niche in the array of biological microscopic imaging methods. It extends the capabilities of existing techniques mainly in two areas: a previously unachievable combination of sub-visible resolution and multi-micrometer sample size, and new contrast mechanisms. Because of the soft x-ray wavelengths used in biological imaging (about 1-4 nm), XM is intermediate in resolution between visible light and electron microscopies. Similarly, the penetration depth of soft x-rays in biological materials is such that the ideal sample thickness for XM falls in the range of 0.25 - 10 {mu}m, between that of VLM and EM. XM is therefore valuable for imaging of intermediate level ultrastructure, requiring sub-visible resolutions, in intact cells and subcellular organelles, without artifacts produced by thin sectioning. Many of the contrast producing and sample preparation techniques developed for VLM and EM also work well with XM. These include, for example, molecule specific staining by antibodies with heavy metal or fluorescent labels attached, and sectioning of both frozen and plastic embedded tissue. However, there is also a contrast mechanism unique to XM that exists naturally because a number of elemental absorption edges lie in the wavelength range used. In particular, between the oxygen and carbon absorption edges (2.3 and 4.4 nm wavelength), organic molecules absorb photons much more strongly than does water, permitting element-specific imaging of cellular structure in aqueous media, with no artifically introduced contrast agents. For three-dimensional imaging applications requiring the capabilities of XM, an obvious extension of the technique would therefore be computerized x-ray microtomography (XMT).

Strain analysis of trabecular bone using time-resolved X-ray microtomography

Czech Academy of Sciences Publication Activity Database

Jiroušek, Ondřej; Zlámal, Petr; Kytýř, Daniel; Kroupa, M.

2011-01-01

Roč. 633, Suppl. 1 (2011), s. 148-151 ISSN 0168-9002. [International Workshop on Radiation Imaging Detectors /11./. Praha, 28.06.2009-02.07.2009] R&D Projects: GA ČR(CZ) GP103/07/P483 Institutional research plan: CEZ:AV0Z20710524 Keywords : trabecular bone * X-ray microtomography * strain analysis * intrinsic material properties Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.207, year: 2011

Magnified hard x-ray microtomography: toward tomography with submicron resolution

Science.gov (United States)

Schroer, Christian G.; Benner, Boris; Guenzler, Til F.; Kuhlmann, Marion; Lengeler, Bruno; Rau, Christoph; Weitkamp, Timm; Snigirev, Anatoly A.; Snigireva, Irina

2002-01-01

Parabolic compound refractive lenses (PCRLs) are high quality imaging optics for hard x-rays that can be used as an objective lens in a new type of hard x-ray full field microscope. Using an aluminium PCRL, this new type of microscope has been shown to have a resolution of 350 nm. Further improvement of the resolution down to 50 nm can be expected using beryllium as a lens material. The large depth of field (several mm) of the microscope results in sharp projection images for samples that fit into the field of view of about 300 micrometers. This allows to combine magnified imaging with tomographic techniques. First results of magnified microtomography are shown. Contrast formation in the microscope and the consequences for tomographic reconstruction are discussed. An outlook on further developments is given.

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

Advances in x-ray computed microtomography at the NSLS

International Nuclear Information System (INIS)

Dowd, B.A.; Andrews, A.B.; Marr, R.B.; Siddons, D.P.; Jones, K.W.; Peskin, A.M.

1998-08-01

The X-Ray Computed Microtomography workstation at beamline X27A at the NSLS has been utilized by scientists from a broad range of disciplines from industrial materials processing to environmental science. The most recent applications are presented here as well as a description of the facility that has evolved to accommodate a wide variety of materials and sample sizes. One of the most exciting new developments reported here resulted from a pursuit of faster reconstruction techniques. A Fast Filtered Back Transform (FFBT) reconstruction program has been developed and implemented, that is based on a refinement of the gridding algorithm first developed for use with radio astronomical data. This program has reduced the reconstruction time to 8.5 sec for a 929 x 929 pixel 2 slice on an R10,000 CPU, more than 8x reduction compared with the Filtered Back-Projection method

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

Determination of structural geometric parameters of industrial ceramic foams by gamma rays transmission and X-rays microtomography

International Nuclear Information System (INIS)

Rocha, Wilson Roberto Dejato da

2005-01-01

In this work, the gamma rays transmission and X-rays microtomography techniques are used for the evaluation of the porosity and the pore size distribution of SiC ceramic foams. It was also accomplished the three-dimensional images after the determination of samples geometric parameters. The geometric parameters were obtained by two-dimensional images analyses, generated by a Microfocus system, with a CCD camera, an images intensifier, a X-rays tube and an automatic system for rotation of the sample. The spatial resolution of the images was about 32 μm. In the gamma rays transmission methodology, a Nal(Tl) scintillation detector, an 241 Am (59.53 keV, 100 mCi) radioactive source and an automatic X-Z micrometric table was used. The analyzed samples had pores density of 30, 45, 60, 80 and 100 ppi (pores per inch). The gamma rays transmission technique was accurate to supply the porosity of the samples, which ranged about 90% and was in agreement with the values supplied by manufacturer of the foams. The 30 and 45 ppi samples analyzed by X-rays microtomography showed porosity results that agree with the average porosity supplied by the manufacturer. In other hand, the 60, 80 and 100 ppi samples systematically showed average porosity about 4%, lower than the average of the manufacturer. The pore size distributions found through the software IMAGO show the presence of smaller pores than those nominated by the manufacturer. The 30 ppi samples had voids inside the solid material of the ceramic foams structure. Gaussian truncated method, used in the three-dimensional reconstruction, was not able to take into the account the voids inside the solid matrix. (author)

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

Nano particle fluidisation in model 2-D and 3-D beds using high speed X-ray imaging and microtomography

International Nuclear Information System (INIS)

Gundogdu, O.; Jenneson, P. M.; Tuzun, U.

2007-01-01

Nanoparticles and nanocomposites have become a major focus of interest in science and technology due to exceptional properties they provide. However, handling and processing of ultra-fine powders is very challenging because they are extremely cohesive. Fluidization is one of techniques available to process powders. It has become increasingly important to understand how these nanoparticles can be handled and processed to benefit from their favourable properties. A high spatial (down to 400 nm) and temporal resolution (down to 1 ms) X-ray imaging apparatus has been designed to study nanoparticles in fluidized beds under different gas flow velocities. The mean volume distribution of the nanoparticle agglomerates was determined with X-ray microtomography. The X-ray microtomography technique provides valuable in situ, non-destructive structural information on the morphological changes that take place during fluidisation of powder samples

Nano particle fluidisation in model 2-D and 3-D beds using high speed X-ray imaging and microtomography

Energy Technology Data Exchange (ETDEWEB)

Gundogdu, O. [University of Surrey, Chemical and Process Engineering, School of Engineering (United Kingdom)], E-mail: o.gundogdu@surrey.ac.uk; Jenneson, P. M. [University of Surrey, Department of Physics, School of Electronics and Physical Sciences (United Kingdom); Tuzun, U. [University of Surrey, Chemical and Process Engineering, School of Engineering (United Kingdom)

2007-04-15

Nanoparticles and nanocomposites have become a major focus of interest in science and technology due to exceptional properties they provide. However, handling and processing of ultra-fine powders is very challenging because they are extremely cohesive. Fluidization is one of techniques available to process powders. It has become increasingly important to understand how these nanoparticles can be handled and processed to benefit from their favourable properties. A high spatial (down to 400 nm) and temporal resolution (down to 1 ms) X-ray imaging apparatus has been designed to study nanoparticles in fluidized beds under different gas flow velocities. The mean volume distribution of the nanoparticle agglomerates was determined with X-ray microtomography. The X-ray microtomography technique provides valuable in situ, non-destructive structural information on the morphological changes that take place during fluidisation of powder samples.

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

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)

Computer simulation for synchrotron radiation based X-ray fluorescent microtomography

International Nuclear Information System (INIS)

Deng Biao; Yu Xiaohan; Xu Hongjie

2007-01-01

Synchrotron radiation based fluorescent microtomography (SR-XFMT) is a nondestructive technique for detecting elemental composition and distribution inside a specimen with high spatial resolution and sensitivity, and will be an optional experimental technique at SSRF hard X-ray micro-focusing beamline now under construction. In this paper, the principles and developments of SR-XFMT are briefly introduced. Computer simulation of SR-XFMT experiment is performed. The image of the simulated sample is reconstructed using Filtered Back Projection (FBP), Algebraic Reconstruction Techniques (ART) and modified FBP with absorption correction. The qualities of the reconstructed images are analyzed and compared. The validity of these reconstruction techniques is discussed. (authors)

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

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

X-ray microtomography of damage in particle-reinforced metal matrix composites

International Nuclear Information System (INIS)

Mummery, P.M.; Derby, B.; Anderson, P.; Davis, G.; Elliott, J.C.

1993-01-01

The damage which occurs on plastic straining of silicon carbide particle-reinforced aluminium alloys has been characterised using x-ray microtomography. The technique is used to provide density measurements as a function of strain in addition to imaging the internal structure with a resolution of ∼15μm. This allows a much more accurate determination of microstructural damage in terms of void growth than is available from measurements of density using buoyancy methods or from elastic modulus decrease. These data can be combined with acoustic emission measurements during straining to allow damage nucleation and growth contributions to be separated. (orig.)

X-ray Computed Microtomography technique applied for cementitious materials: A review.

Science.gov (United States)

da Silva, Ítalo Batista

2018-04-01

The main objective of this article is to present a bibliographical review about the use of the X-ray microtomography method in 3D images processing of cementitious materials microstructure, analyzing the pores microstructure and connectivity network, enabling tthe possibility of building a relationship between permeability and porosity. The use of this technique enables the understanding of physical, chemical and mechanical properties of cementitious materials by publishing good results, considering that the quality and quantity of accessible information were significant and may contribute to the study of cementitious materials development. Copyright © 2018 Elsevier Ltd. All rights reserved.

Recent progress of hard x-ray imaging microscopy and microtomography at BL37XU of SPring-8

Energy Technology Data Exchange (ETDEWEB)

Suzuki, Yoshio, E-mail: yoshio@spring8.or.jp; Takeuchi, Akihisa; Terada, Yasuko; Uesugi, Kentaro [Japan Synchrotron Radiation Research Institute (JASRI/SPring-8), Sayo, Hyogo 679-5198 (Japan); Mizutani, Ryuta [Department of Applied Biochemistry, Tokai University, Hiratsuka, Kanagawa 259-1292 (Japan)

2016-01-28

A hard x-ray imaging microscopy and microtomography system is now being developed at the beamline 37XU of SPring-8. In the latest improvement, a spatial resolution of about 50 nm is achieved in two-dimensional imaging at 6 keV x-ray energy using a Fresnel zone plate objective with an outermost zone width of 35 nm. In the tomographic measurement, a spatial resolution of about 100 nm is achieved at 8 keV using an x-ray guide tube condenser optic and a Fresnel zone plate objective with an outermost zone width of 50 nm.

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

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.

Particle tracking during Ostwald ripening using time-resolved laboratory X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Werz, T., E-mail: thomas.werz@uni-ulm.de [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany); Baumann, M. [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany); Wolfram, U. [Ulm University, Institute of Orthopaedic Research and Biomechanics, Helmholtzstrasse 14, 89081 (Germany); Krill, C.E. [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany)

2014-04-01

Laboratory X-ray microtomography is investigated as a method for obtaining time-resolved images of microstructural coarsening of the semisolid state of Al–5 wt.% Cu samples during Ostwald ripening. Owing to the 3D imaging capability of tomography, this technique uniquely provides access to the growth rates of individual particles, thereby not only allowing a statistical characterization of coarsening—as has long been possible by conventional metallography—but also enabling quantification of the influence of local environment on particle boundary migration. The latter information is crucial to understanding growth kinetics during Ostwald ripening at high volume fractions of the coarsening phase. Automated image processing and segmentation routines were developed to close gaps in the network of particle boundaries and to track individual particles from one annealing step to the next. The particle tracking success rate places an upper bound of only a few percent on the likelihood of segmentation errors for any given particle. The accuracy of particle size trajectories extracted from the time-resolved tomographic reconstructions is correspondingly high. Statistically averaged coarsening data and individual particle growth rates are in excellent agreement with the results of prior experimental studies and with computer simulations of Ostwald ripening. - Highlights: • Ostwald ripening in Al–5 wt.% Cu measured by laboratory X-ray microtomography • Time-resolved measurement of individual particle growth • Automated segmentation routines developed to close gaps in particle boundary network • Particle growth/shrinkage rates deviate from LSW model prediction.

The ICTP-Elettra X-ray laboratory for cultural heritage and archaeology

International Nuclear Information System (INIS)

Tuniz, C.; Bernardini, F.; Cicuttin, A.; Crespo, M.L.; Dreossi, D.; Gianoncelli, A.; Mancini, L.; Mendoza Cuevas, A.

2013-01-01

A set of portable/transportable X-ray analytical instruments based on radiography, microtomography, fluorescence and diffraction have been built and are being operated at the Multidisciplinary Laboratory (MLAB) of the ‘Abdus Salam’ International Centre for Theoretical Physics (ICTP) in collaboration with Elettra-Sincrotrone Trieste. This is part of a project funded by the Region Friuli Venezia Giulia (Italy) and the ICTP, which aims to develop innovative X-ray analytical tools for noninvasive studies of cultural heritage objects and palaeontological remains. The X-ray instruments at MLAB are also used for hands-on training activities involving students and scientists from developing countries. The MLAB analytical tools complement the microtomography instruments available at Elettra-Sincrotrone Trieste. Examples of our first studies in archaeological and palaeontological applications are presented here

The ICTP-Elettra X-ray laboratory for cultural heritage and archaeology

Energy Technology Data Exchange (ETDEWEB)

Tuniz, C., E-mail: ctuniz@ictp.it [The ‘Abdus Salam’ International Centre for Theoretical Physics (UNESCO), Multidisciplinary Laboratory, via Beirut 31, 34014 Trieste (Italy); University La Sapienza, Dipartimento di Biologia Ambientale, P.le A. Moro 5, 00185 Rome (Italy); Centre for Archaeological Science, University of Wollongong, NSW 2522 (Australia); Bernardini, F., E-mail: fbernard@ictp.it [The ‘Abdus Salam’ International Centre for Theoretical Physics (UNESCO), Multidisciplinary Laboratory, via Beirut 31, 34014 Trieste (Italy); Cicuttin, A., E-mail: cicuttin@ictp.it [The ‘Abdus Salam’ International Centre for Theoretical Physics (UNESCO), Multidisciplinary Laboratory, via Beirut 31, 34014 Trieste (Italy); Crespo, M.L., E-mail: mcrespo@ictp.it [The ‘Abdus Salam’ International Centre for Theoretical Physics (UNESCO), Multidisciplinary Laboratory, via Beirut 31, 34014 Trieste (Italy); Dreossi, D., E-mail: diego.dreossi@elettra.trieste.it [Elettra-Sincrotrone Trieste S.C.p.A., SYRMEP Group, Strada Statale 14, AREA Science Park, 34149 Basovizza, Trieste (Italy); Gianoncelli, A., E-mail: alessandra.gianoncelli@elettra.trieste.it [Elettra-Sincrotrone Trieste S.C.p.A., SYRMEP Group, Strada Statale 14, AREA Science Park, 34149 Basovizza, Trieste (Italy); Mancini, L., E-mail: lucia.mancini@elettra.trieste.it [Elettra-Sincrotrone Trieste S.C.p.A., SYRMEP Group, Strada Statale 14, AREA Science Park, 34149 Basovizza, Trieste (Italy); Mendoza Cuevas, A., E-mail: amendoz0@ictp.it [The ‘Abdus Salam’ International Centre for Theoretical Physics (UNESCO), Multidisciplinary Laboratory, via Beirut 31, 34014 Trieste (Italy); Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana (Cuba); and others

2013-05-21

A set of portable/transportable X-ray analytical instruments based on radiography, microtomography, fluorescence and diffraction have been built and are being operated at the Multidisciplinary Laboratory (MLAB) of the ‘Abdus Salam’ International Centre for Theoretical Physics (ICTP) in collaboration with Elettra-Sincrotrone Trieste. This is part of a project funded by the Region Friuli Venezia Giulia (Italy) and the ICTP, which aims to develop innovative X-ray analytical tools for noninvasive studies of cultural heritage objects and palaeontological remains. The X-ray instruments at MLAB are also used for hands-on training activities involving students and scientists from developing countries. The MLAB analytical tools complement the microtomography instruments available at Elettra-Sincrotrone Trieste. Examples of our first studies in archaeological and palaeontological applications are presented here.

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)

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

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.)

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)

High-energy X-ray diffraction studies of disordered materials

International Nuclear Information System (INIS)

Kohara, Shinji; Suzuya, Kentaro

2003-01-01

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

Application of Image And X-Ray Microtomography Technique To Quantify Filler Distribution In Thermoplastic-Natural Rubber Blend Composites

International Nuclear Information System (INIS)

Ahmad, Sahrim; Rasid, Rozaidi; Mouad, A. T.; Aziz Mohamed, A.; Abdullah, Jaafar; Dahlan, M.; Mohamad, Mahathir; Jamro, Rafhayudi; Hamzah Harun, M.; Yazid, Hafizal; Abdullah, W. Saffiey W.

2010-01-01

X-ray microtomography and ImageJ 1.39 u is used as a tool to quantify volume percentage of B 4 C as fillers in thermoplastic-natural rubber blend composites. The use of percentage of area occupied by fillers as obtain from ImageJ from the microtomography sliced images enables the proposed technique to easily obtain the amount volume percentage of B 4 C in the composite non-destructively. Comparison with other technique such as density measurement and chemical analysis proves the proposed technique as one of the promising approach.

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...

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].

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.

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...

Reservoir core porosity in the Resende formation using 3D high-resolution X-ray computed microtomography

International Nuclear Information System (INIS)

Oliveira, Milena F.S.; Lima, Inaya; Lopes, Ricardo T.; Rocha, Paula Lucia F. da

2009-01-01

The storage capacity and production of oil are influenced, among other things, by rocks and fluids characteristics. Porosity is one of the most important characteristics to be analyzed in oil industry, mainly in oil prospection because it represents the direct capacity of storage fluids in the rocks. By definition, porosity is the ratio of pore volume to the total bulk volume of the formation, expressed in percentage, being able to be absolute or effective. The aim of this study was to calculate porosity by 3D High-Resolution X-ray Computed Microtomography using core plugs from Resende Formation which were collected in Porto Real, Rio de Janeiro State. This formation is characterized by sandstones and fine conglomerates with associated fine siliciclastic sediments, and the paleoenviroment is interpreted as a braided fluvial system. For acquisitions data, it was used a 3D high resolution microtomography system which has a microfocus X-ray tube (spot size < 5μm) and a 12-bit cooled X-ray camera (CCD fiber-optically coupled to a scintillator) operated at 100 kV and 100 μA. Twenty-two samples taken at different depths from two boreholes were analyzed. A total of 961 slices were performed with a resolution of 14.9 μm. The results demonstrated that μ-CT is a reliable and effective technique. Through the images and data it was possible to quantify the porosity and to view the size and shape of porous. (author)

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)

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)

Optimization of image quality and acquisition time for lab-based X-ray microtomography using an iterative reconstruction algorithm

Science.gov (United States)

Lin, Qingyang; Andrew, Matthew; Thompson, William; Blunt, Martin J.; Bijeljic, Branko

2018-05-01

Non-invasive laboratory-based X-ray microtomography has been widely applied in many industrial and research disciplines. However, the main barrier to the use of laboratory systems compared to a synchrotron beamline is its much longer image acquisition time (hours per scan compared to seconds to minutes at a synchrotron), which results in limited application for dynamic in situ processes. Therefore, the majority of existing laboratory X-ray microtomography is limited to static imaging; relatively fast imaging (tens of minutes per scan) can only be achieved by sacrificing imaging quality, e.g. reducing exposure time or number of projections. To alleviate this barrier, we introduce an optimized implementation of a well-known iterative reconstruction algorithm that allows users to reconstruct tomographic images with reasonable image quality, but requires lower X-ray signal counts and fewer projections than conventional methods. Quantitative analysis and comparison between the iterative and the conventional filtered back-projection reconstruction algorithm was performed using a sandstone rock sample with and without liquid phases in the pore space. Overall, by implementing the iterative reconstruction algorithm, the required image acquisition time for samples such as this, with sparse object structure, can be reduced by a factor of up to 4 without measurable loss of sharpness or signal to noise ratio.

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....

Three dimensional characterization of soil macroporosity by X-ray microtomography

International Nuclear Information System (INIS)

Passoni, Sabrina; Pires, Luiz Fernando; Rosa, Jadir Aparecido

2015-01-01

Analysis of the soil pore system represents an important way of characterizing soil structure. Properties such as the shape and number of pores can be determined through soil pore evaluations. This study presents a three-dimensional (3D) characterization of the shape and number of pores of a sub-tropical soil. To do so, a second generation X-ray microtomography equipped with a plain type detector was employed. A voltage of 120 kV and current of 80 mA was applied to the X-ray tube. The soil samples analyzed were collected at three different depths (0-10, 10-20, and 20-30 cm). The results obtained allowed qualitative (images) and quantitative (3D) analyses of the soil structure, revealing the potential of the microtomographic technique, as well as the study of differences in soil macroporosity at different depths. Macroporosity was 5.14 % in the 0-10 cm layer, 5.10 % in the 10-20 cm layer, and 6.64 % in the 20-30 cm layer. The macroporosity of unclassified pores (UN) was 0.30 % (0-10 and 10-20 cm) and 0.40 % (20-30 cm), while equant pores (EQ) had values of 0.01 % at the three depths under analysis. (author)

Three dimensional characterization of soil macroporosity by X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Passoni, Sabrina [Centro de Ensino Superior dos Campos Gerais, Ponta Grossa, PR (Brazil); Pires, Luiz Fernando, E-mail: lfpires@uepg.br [Universidade Estadual de Ponta Grossa (UFPG), Ponta Grossa, PR (Brazil). Departamento de Fisica; Heck, Richard [University of Guelph, School of Environmental Sciences, Guelph, Ontario (Canada); Rosa, Jadir Aparecido [Instituto Agronomico do Parana, Polo Regional de Pesquisa de Ponta Grossa, Ponta Grossa, PR (Brazil)

2015-03-15

Analysis of the soil pore system represents an important way of characterizing soil structure. Properties such as the shape and number of pores can be determined through soil pore evaluations. This study presents a three-dimensional (3D) characterization of the shape and number of pores of a sub-tropical soil. To do so, a second generation X-ray microtomography equipped with a plain type detector was employed. A voltage of 120 kV and current of 80 mA was applied to the X-ray tube. The soil samples analyzed were collected at three different depths (0-10, 10-20, and 20-30 cm). The results obtained allowed qualitative (images) and quantitative (3D) analyses of the soil structure, revealing the potential of the microtomographic technique, as well as the study of differences in soil macroporosity at different depths. Macroporosity was 5.14 % in the 0-10 cm layer, 5.10 % in the 10-20 cm layer, and 6.64 % in the 20-30 cm layer. The macroporosity of unclassified pores (UN) was 0.30 % (0-10 and 10-20 cm) and 0.40 % (20-30 cm), while equant pores (EQ) had values of 0.01 % at the three depths under analysis. (author)

3D synchrotron x-ray microtomography of paint samples

Science.gov (United States)

Ferreira, Ester S. B.; Boon, Jaap J.; van der Horst, Jerre; Scherrer, Nadim C.; Marone, Federica; Stampanoni, Marco

2009-07-01

Synchrotron based X-ray microtomography is a novel way to examine paint samples. The three dimensional distribution of pigment particles, binding media and their deterioration products as well as other features such as voids, are made visible in their original context through a computing environment without the need of physical sectioning. This avoids manipulation related artefacts. Experiments on paint chips (approximately 500 micron wide) were done on the TOMCAT beam line (TOmographic Microscopy and Coherent rAdiology experimenTs) at the Paul Scherrer Institute in Villigen, CH, using an x-ray energy of up to 40 keV. The x-ray absorption images are obtained at a resolution of 350 nm. The 3D dataset was analysed using the commercial 3D imaging software Avizo 5.1. Through this process, virtual sections of the paint sample can be obtained in any orientation. One of the topics currently under research are the ground layers of paintings by Cuno Amiet (1868- 1961), one of the most important Swiss painters of classical modernism, whose early work is currently the focus of research at the Swiss Institute for Art Research (SIK-ISEA). This technique gives access to information such as sample surface morphology, porosity, particle size distribution and even particle identification. In the case of calcium carbonate grounds for example, features like microfossils present in natural chalks, can be reconstructed and their species identified, thus potentially providing information towards the mineral origin. One further elegant feature of this technique is that a target section can be selected within the 3D data set, before exposing it to obtain chemical data. Virtual sections can then be compared with cross sections of the same samples made in the traditional way.

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

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

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

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

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.

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

Imaging biofilm in porous media using X-ray computed microtomography.

Science.gov (United States)

Davit, Y; Iltis, G; Debenest, G; Veran-Tissoires, S; Wildenschild, D; Gerino, M; Quintard, M

2011-04-01

In this study, a new technique for three-dimensional imaging of biofilm within porous media using X-ray computed microtomography is presented. Due to the similarity in X-ray absorption coefficients for the porous media (plastic), biofilm and aqueous phase, an X-ray contrast agent is required to image biofilm within the experimental matrix using X-ray computed tomography. The presented technique utilizes a medical suspension of barium sulphate to differentiate between the aqueous phase and the biofilm. Potassium iodide is added to the suspension to aid in delineation between the biofilm and the experimental porous medium. The iodide readily diffuses into the biofilm while the barium sulphate suspension remains in the aqueous phase. This allows for effective differentiation of the three phases within the experimental systems utilized in this study. The behaviour of the two contrast agents, in particular of the barium sulphate, is addressed by comparing two-dimensional images of biofilm within a pore network obtained by (1) optical visualization and (2) X-ray absorption radiography. We show that the contrast mixture provides contrast between the biofilm, the aqueous-phase and the solid-phase (beads). The imaging method is then applied to two three-dimensional packed-bead columns within which biofilm was grown. Examples of reconstructed images are provided to illustrate the effectiveness of the method. Limitations and applications of the technique are discussed. A key benefit, associated with the presented method, is that it captures a substantial amount of information regarding the topology of the pore-scale transport processes. For example, the quantification of changes in porous media effective parameters, such as dispersion or permeability, induced by biofilm growth, is possible using specific upscaling techniques and numerical analysis. We emphasize that the results presented here serve as a first test of this novel approach; issues with accurate segmentation of

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

International Nuclear Information System (INIS)

Yao, Shengkun; Fan, Jiadong; Zong, Yunbing; Sun, Zhibin; Zhang, Jianhua; Jiang, Huaidong; He, You; Zhou, Guangzhao; Xiao, Tiqiao; Huang, Qingjie

2016-01-01

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique over conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ∼1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

Science.gov (United States)

Yao, Shengkun; Fan, Jiadong; Zong, Yunbing; He, You; Zhou, Guangzhao; Sun, Zhibin; Zhang, Jianhua; Huang, Qingjie; Xiao, Tiqiao; Jiang, Huaidong

2016-03-01

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique over conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ˜1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.

Equally sloped X-ray microtomography of living insects with low radiation dose and improved resolution capability

Energy Technology Data Exchange (ETDEWEB)

Yao, Shengkun; Fan, Jiadong; Zong, Yunbing; Sun, Zhibin; Zhang, Jianhua; Jiang, Huaidong, E-mail: hdjiang@sdu.edu.cn [State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100 (China); He, You; Zhou, Guangzhao; Xiao, Tiqiao [Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Huang, Qingjie [School of Information Science and Engineering, Shandong University, Jinan 250100 (China)

2016-03-21

Three-dimensional X-ray imaging of living specimens is challenging due to the limited resolution of conventional absorption contrast X-ray imaging and potential irradiation damage of biological specimens. In this letter, we present microtomography of a living specimen combining phase-contrast imaging and a Fourier-based iterative algorithm termed equally sloped tomography. Non-destructive 3D imaging of an anesthetized living yellow mealworm Tenebrio molitor was demonstrated with a relatively low dose using synchrotron generated X-rays. Based on the high-quality 3D images, branching tracheoles and different tissues of the insect in a natural state were identified and analyzed, demonstrating a significant advantage of the technique over conventional X-ray radiography or histotomy. Additionally, the insect survived without problem after a 1.92-s X-ray exposure and subsequent absorbed radiation dose of ∼1.2 Gy. No notable physiological effects were observed after reviving the insect from anesthesia. The improved static tomographic method demonstrated in this letter shows advantage in the non-destructive structural investigation of living insects in three dimensions due to the low radiation dose and high resolution capability, and offers many potential applications in biological science.

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

Single photon energy dispersive x-ray diffraction

International Nuclear Information System (INIS)

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

2014-01-01

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored

Single photon energy dispersive x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

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

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.

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)

A quasi-realtime x-ray microtomography system at the Advanced Photon Source

International Nuclear Information System (INIS)

DeCarlo, F.; Foster, I.; Insley, J.; Kesselman, C.; Lane, P.; Mancini, D.; McNulty, I.; Su, M.; Tieman, B.; Wang, Y.; Laszewski, G. von

1999-01-01

The combination of high-brilliance x-ray sources, fast detector systems, wide-bandwidth networks, and parallel computers can substantially reduce the time required to acquire, reconstruct, and visualize high-resolution three-dimensional tomographic datasets. A quasi-realtime computed x-ray microtomography system has been implemented at the 2-BM beamline at the Advanced Photon Source at Argonne National Laboratory. With this system, a complete tomographic data set can be collected in about 15 minutes. Immediately after each projection is obtained, it is rapidly transferred to the Mathematics and Computing Sciences Division where preprocessing and reconstruction calculations are performed concurrently with the data acquisition by a SGI parallel computer. The reconstruction results, once completed, are transferred to a visualization computer that performs the volume rendering calculations. Rendered images of the reconstructed data are available for viewing back at the beamline experiment station minutes after the data acquisition was complete. The fully pipelined data acquisition and reconstruction system also gives us the option to acquire the tomographic data set in several cycles, initially with coarse then with fine angular steps. At present the projections are acquired with a straight-ray projection imaging scheme using 5-20 keV hard x rays in either phase or amplitude contrast mode at a 1-10 pm resolution. In the future, we expect to increase the resolution of the projections to below 100 nm by using a focused x-ray beam at the 2-ID-B beamline and to reduce the combined acquisition and computation time to the 1 min scale with improvements in the detectors, network links, software pipeline, and computation algorithms

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)

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)

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.

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)

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....

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

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...

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

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

High-resolution X-ray diffraction studies of multilayers

DEFF Research Database (Denmark)

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

1988-01-01

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

Microstructural characterization of industrial foams by gamma ray transmission and X-ray microtomography; Caracterizacao microestrutural de espumas industriais por transmissao de raios gama e microtomografia de raios X

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, Luiz Eduardo

2004-07-01

This work presents the total porosity measurements of the aluminum and silicon carbide (SiC) foams samples. For porosity determination the gamma ray transmission and X-ray microtomography with conic beam techniques were used. These methods have more advantage than conventional ones, because they are non destructive and provide more details of the analyzed material porous structure. The aluminum foam samples with 10, 20, 30, 40 and 45 ppi (pores per inch) and SiC ceramic foam samples with 20, 30, 45, 60, 75, 80 and 90 ppi were analysed by gamma transmission. The SiC 60, 75 and 90 ppi samples were also analyzed by X-ray microtomography. For the gamma ray transmission measurements it was used an {sup 241} Am source (59.53 keV), a NaI(Tl) scintillation detector, collimators, a XYZ micrometric table and standard gamma spectrometry electronics connected to a multichannel analyzer, at the LFNA/UEL. For the X-ray microtomographic measurements, the Fein Focus X-ray system of the Nuclear Instrumentation Laboratory of the COPPE, located at the Universidade Federal do Rio de Janeiro, Rio de Janeiro, RJ, was used. This equipment provide us images with micrometric resolution (53.48 {mu}m) using a conic X-ray beam and bidimensional detection. The microtomographic images were pre-processed and analyzed by the Imago software, developed at Porous Media and Materials Thermophysical Properties Laboratory (LMPT) of the Mechanical Engineering Department, located at Universidade Federal de Santa Catarina, Florianopolis, SC. Employing the The Imago software it was calculated the total porosity, pore size distribution and autocorrelation function C(u) of the binarized microtomographic images of the each sample. The microtomographic 3-D image of each sample was compared with 3-D image reconstructed by the Gaussian truncated method. This method generates a periodic 3-D porous structure by using of the autocorrelation function of one 2-D cross sectional image of the sample. (author)

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.

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging.

Science.gov (United States)

Warren, Anna J; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R; Horrell, Sam; McAuley, Katherine E; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-07-01

The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required.

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 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

Microstructure parameters evaluation of Botucatu formation sandstone by X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Fernandes, Jaquiel S.; Appoloni, Carlos R.; Marques, Leonardo C., E-mail: jaquielfernandes@yahoo.com.b, E-mail: appoloni@uel.b, E-mail: leocarma@yahoo.com.b [Universidade Estadual de Londrina (UEL), PR (Brazil). Dept. de Fisica. Lab. de Fisica Nuclear Aplicada; Fernandes, Celso P., E-mail: celso@lmpt.ufsc.b [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Dept. de Engenharia Mecanica. Lab. de Meios Porosos e Propriedades TermoFisicas (LMPT)

2009-07-01

Microstructural parameters evaluation of reservoir rocks are very important to petroleum industry. This work presents total porosity and pore size distribution measurement of a silicified sandstone sample from the Botucatu formation, collected at municipal district of Faxinal, Parana, Brazil. Porosity and pores size distribution were determined using X-Ray microtomography and imaging techniques. Acquired images had 2.9 mum spatial resolution. 800 2-D images where reconstructed for the microstructure analysis. The determined average porosity was 6.1 +- 2.1 %. 95 % of the porous phase refers to pores with radius ranging from 2.9 to 167.4 mum, presenting the larger frequency (6 %) at 5.9 mum radius. The 3-D volume of the sample was reconstructed and compared with the 3-D model obtained through the autocorrelation functions from the 2-D images analysis. (author)

Quantitative comparison of X-ray fluorescence microtomography setups: Standard and confocal collimator apparatus

Energy Technology Data Exchange (ETDEWEB)

Chukalina, M. [Institute of Microelectronics Technology RAS, 142432, Chernogolovka, Moscow District (Russian Federation)], E-mail: marina@ipmt-hpm.ac.ru; Simionovici, A. [Laboratoire de Geophysique Interne et Tectonophysique, University of Grenoble, BP 53, 38041, Grenoble (France)], E-mail: alexandre.simionovici@ujf-grenoble.fr; Zaitsev, S. [Institute of Microelectronics Technology RAS, 142432, Chernogolovka, Moscow District (Russian Federation)], E-mail: zaitsev@ipmt-hpm.ac.ru; Vanegas, C.J. [Institute of Microelectronics Technology RAS, 142432, Chernogolovka, Moscow District (Russian Federation)], E-mail: vanegas@ipmt-hpm.ac.ru

2007-07-15

Recently, there has been a renewed interest for fluorescence spectroscopy, as provided by modern setups which allow 2D and 3D imaging of elemental distributions. Two directions are currently under development: the SR-based fluorescence tomography in polar scanning geometry, provided by the new generation of X-ray microprobes and the confocal scanning geometry, which can be fielded in both SR and laboratory environments. The new probes bring forth a new age in fluorescence spectrometry: high resolution, high intensity and high sensitivity which allow 3D elemental mapping of volumes. The major task now is the development of these complex tools into fully quantitative probes, reproducible and straightforward for general use. In this work we analyze two X-ray fluorescence microtomography techniques: an apparatus tomography using a confocal collimator for the data collection and a standard first generation Computed Tomography (CT) in the parallel scanning scheme. We calculate the deposited dose (amount of energy deposited and distributed in the sample during the data collection time) and find the conditions for the choice of the tomography scheme.

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...

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)

X-ray microtomography

International Nuclear Information System (INIS)

Dunsmuir, J.H.; Ferguson, S.R.; D'Amico, K.L.; Stokes, J.P.

1991-01-01

In this paper the authors describe the application of a new high-resolution X-ray tomographic microscope to the study of porous media. The microscope was designed to exploit the properties of a synchrotron X-ray source to perform three dimensional tomography on millimeter sized objects with micron resolution and has been used in materials science studies with both synchrotron and conventional and synchrotron sources will be compared. In this work the authors have applied the microscope to measure the three dimensional structure of fused bead packs and berea sandstones with micron resolution and have performed preliminary studies of flow in these media with the microscope operated in a digital subtraction radiography mode. Computer graphics techniques have been applied to the data to visually display the structure of the pore body system. Tomographic imaging after flow experiments should detect the structure of the oil-water interface in the pore network and this work is ongoing

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

International Nuclear Information System (INIS)

Warren, Anna J.; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R.; Horrell, Sam; McAuley, Katherine E.; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-01-01

A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material. The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

Energy Technology Data Exchange (ETDEWEB)

Warren, Anna J. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); Armour, Wes [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); Oxford e-Research Centre, 7 Keble Road, Oxford OX1 3QG (United Kingdom); Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); Horrell, Sam [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); University of Liverpool, Liverpool L69 3BX (United Kingdom); McAuley, Katherine E.; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf, E-mail: gwyndaf.evans@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

2013-07-01

A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material. The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required.

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...

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)

Illicit drug detection using energy dispersive x-ray diffraction

Science.gov (United States)

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

2009-05-01

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

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

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

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

Development of a 3-D x-ray micro-tomography system and its application to trabecular bone/cement interface

International Nuclear Information System (INIS)

Chi, Yong Ki; Cho, Gyuseong

2004-01-01

In recent years, the interface analysis of micro-structure based objects is an important research in osteoporosis, vascular imaging since a 3-D X-ray micro-tomography system was developed. However, the micro-tomographic image shows the white-out appearance in case of imaging of similar density objects with low energy X-ray. Therefore these images must be analyzed about the interface between microstructure based objects for its application to biomechanical study. Many published studies suggested approximately assumed model of interface and predicted mechanical failure by means of Finite Element Method (FEM) but these FEM analysis has not used for modeling the real structure and interface between objects such as roughness, voids and pores of objects. We developed micro-tomography system and suggest the application of micro-tomographic image for predicting mechanical failure at the interface. The micro-tomography system consists of a 5 μm micro-focus X-ray tube, a CMOS-based image sensor and a rotating sample holder controlled by a precision motor. CMOS image sensor has 62x62 mm 2 sensing area and uses optical lenses system for increasing resolution. The sample which was manufactured by implanting cement in a pig hip bone was used and its fracture is considered to be an important cause of loosening of hip joint replacement in orthopedic implants. A Feldkamp's cone-beam reconstruction algorithm on the equispatial detector case was used for bone/cement 3D volume data and the analysis of a trabecular bone/cement interface containing white-out appearance was performed by using multiple criterion segmentation of region and volume. Finally, the segmented data can be used for fracture prediction of FEM by determining node of hexahedron meshing. In this paper, we present development of a 3-D cone beam micro-tomographic system with CMOS image sensor and its application to a complex structure of a trabecular bone and implanted cement for predicting the failure mechanism of

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

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.

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.

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 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 ...

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)

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...

Structural characterization of titanium porous foams by gamma rays transmission and X ray microtomography

International Nuclear Information System (INIS)

Moreira, Anderson C.; Appoloni, Carlos R.

2007-01-01

The advance in porous media studies and the consequent progresses of their applications in medicine, petroleum industry, metallurgy and others, rises the prominence of the area among scientists. This fact increases the research on different characterization techniques of porous materials. In this work three Titanium foams were analyzed by gamma rays transmission (GRT), and one of these was also analyzed by X-ray microtomography (μ-CT). The GRT experimental set consisted by a 2'' x 2''. NaI(Tl) detector, a 241-Am radioactive source (59,53 keV, 100 mCi) and a standard gamma spectrometry electronic chain. In the μ-CT technique it was used a SKYSCAN 1172 scanner consisting of an X-ray tube (20-100 kV and 0-250 μA), a CCD detector and a proper mechanic system for sample and detector movement. The system may reach ∼0.8 μm image resolution. Images of 815 slices of the sample were generated and analyzed by the IMAGO software. It permitted the determination of geometrical parameters like pore size distribution, total porosity and autocorrelation function. The analysis of data, obtained by both techniques, showed that porous media are homogeneous in the reached resolutions (1 mm to GRT and 5 μm to μ-CT). The average total porosities determined by GRT for each sample were φ 1 =53,47±0,36%, φ 2 =55,95±0,23% and φ 3 =56,80±0,56%, and the determined by μ-CT was φ 1 =53,47±0,36%. The porosity data of the Ti-1 sample shows good agreement from both techniques. The pore size distribution, from μ-CT technique of the Ti-1 sample, showed that 57% of porous phase have porous with radius in 20 to 80 μm range. (author)

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.

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)

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

X-ray microtomography study of the spallation response in Ta-W

Science.gov (United States)

McDonald, Samuel; Cotton, Matthew; Millett, Jeremy; Bourne, Neil; Withers, Philip

2013-06-01

The response of metallic materials to high strain-rate (impact) loading is of interest to a number of communities. Traditionally, the largest driver has been the military, in its need to understand armour and resistance to ballistic attack. More recently, industries such as aerospace (foreign object damage, bird strike, etc.), automotive (crash-worthiness) and satellite protection (orbital debris) have all appreciated the necessity of such information. It is therefore important to understand the dynamic tensile or spallation response, and in particular to be able to observe in three-dimensions, and in a non-invasive manner, the physical damage present in the spalled region post-impact. The current study presents plate impact experiments investigating the spallation damage response of recovered targets of the tantalum alloy Ta-2.5%W. Using X-ray microtomography the damage resulting from differing impact conditions (impact velocity/stress, pulse duration) is compared and characterised in 3-D. Combined with free surface velocity measurements, the tensile failure mechanisms during dynamic loading have been identified.

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.)

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.

X-ray micro-tomography investigation of the foaming process in the system of waste glass–silica mud–MnO{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Ducman, V., E-mail: vilma.ducman@zag.si [ZAG Ljubljana, Dimičeva 12, 1000 Ljubljana (Slovenia); Korat, L.; Legat, A. [ZAG Ljubljana, Dimičeva 12, 1000 Ljubljana (Slovenia); Mirtič, B. [NTF, Aškerčeva 12, 1000 Ljubljana (Slovenia)

2013-12-15

In case of foamed lightweight aggregates (LWAs), porosity is introduced by the addition of a foaming agent to the glassy matrix, which degasses at an elevated temperature, so that the resulting gases remain trapped inside the glassy structure. The efficiency of action of MnO{sub 2} as a foaming agent in waste glass and waste glass/silica mud systems was studied. Samples were fired at different temperatures and with different dwelling times at a certain temperature, and the development of porosity was investigated by means of X-ray micro-tomography. It was found that, with the prolongation in dwelling times, the number of pores decreased, while, on the other hand, the volume of these pores increased, and that the addition of silica mud increases the foaming temperature and slows down the foaming process. - Highlights: • Preparation of lightweight aggregate from waste glass, silica sludge, and MnO{sub 2} • DTA/TG investigation of MnO{sub 2} • Characterization of pore-forming process by means of X-ray micro-tomography (μcT)

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

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...

Software tools for quantification of X-ray microtomography at the UGCT

Energy Technology Data Exchange (ETDEWEB)

Vlassenbroeck, J. [Department of Subatomic and Radiation Physics, Ghent University, Proeftuinstraat 86, B-9000 Gent (Belgium)], E-mail: jelle.vlassenbroeck@ugent.be; Dierick, M.; Masschaele, B. [Department of Subatomic and Radiation Physics, Ghent University, Proeftuinstraat 86, B-9000 Gent (Belgium); Cnudde, V. [Department of Geology and Soil Science, Ghent University, Krijgslaan 281/S8, B-9000 Gent (Belgium); Van Hoorebeke, L. [Department of Subatomic and Radiation Physics, Ghent University, Proeftuinstraat 86, B-9000 Gent (Belgium); Jacobs, P. [Department of Geology and Soil Science, Ghent University, Krijgslaan 281/S8, B-9000 Gent (Belgium)

2007-09-21

The technique of X-ray microtomography using X-ray tube radiation offers an interesting tool for the non-destructive investigation of a wide range of materials. A major challenge lies in the analysis and quantification of the resulting data, allowing for a full characterization of the sample under investigation. In this paper, we discuss the software tools for reconstruction and analysis of tomographic data that are being developed at the UGCT. The tomographic reconstruction is performed using Octopus, a high-performance and user-friendly software package. The reconstruction process transforms the raw acquisition data into a stack of 2D cross-sections through the sample, resulting in a 3D data set. A number of artifact and noise reduction algorithms are integrated to reduce ring artifacts, beam hardening artifacts, COR misalignment, detector or stage tilt, pixel non-linearities, etc. These corrections are very important to facilitate the analysis of the 3D data. The analysis of the 3D data focuses primarily on the characterization of pore structures, but will be extended to other applications. A first package for the analysis of pore structures in three dimensions was developed under Matlab. A new package, called Morpho+, is being developed in a C++ environment, with optimizations and extensions of the previously used algorithms. The current status of this project will be discussed. Examples of pore analysis can be found in pharmaceuticals, material science, geology and numerous other fields.

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.

Synchrotron radiation X-ray microfluorescence techniques

Indian Academy of Sciences (India)

Synchrotron X-ray imaging systems with fluorescence techniques was developed for biomedical researches in Brazilian Synchrotron Laboratory. An X-ray fluorescence microtomography system was implemented to analyse human prostate and breast samples and an X-ray microfluorescence system was implemented to ...

Microstructural characterization of porous materials by X-ray microtomography and gamma ray transmission techniques; Caracterizacao da microestrutura de materiais porosos por microtomografia de raios X e transmissao de raios gama

Energy Technology Data Exchange (ETDEWEB)

Moreira, Anderson Camargo

2006-07-01

This work presents the application of the X-ray microtomography and gamma ray transmission techniques for the microstructure characterization of different kinds of materials. Total porosity, pore size distribution and the two point correlation functions were measured. The two point correlation function, which allows the reconstruction of 3D models, was carried out for two samples. Seven ceramic tablets of Alumina (Al{sub 2}O{sub 3}), seven tablets of Boron Carbide (B{sub 4}C), three samples of sedimentary rocks and one sample of Titanium foam were analyzed. The experimental set up for the Gamma Ray Transmission technique consisted of: a 2'' x 2'' crystal NaI(Tl) detector, an {sup 241} Am radioactive source (59,53 keV, 100 mCi), an automatic micrometric table for the sample XZ movement and standard gamma spectrometry electronics. Two microtomography systems were used: a Fein Focus system, constituted by an X-ray tube, operated at 160 kV and 0.3 to 1.1 mA, a CCD camera and the movement sample system, and a Skyscan system, model 1072, with a X-ray tube operated at 100 kV and 100{mu}A, and a CCD camera. The ceramic tablets, analyzed by the gamma ray transmission technique presented results for most of the porosities data with smaller confidence intervals and inside the intervals supplied by the tablets manufacturer. The Titanium porous sample was analyzed by the two techniques, its microtomography images achieved a resolution of 17{mu}m, obtained employing the Fein Focus system. For both techniques, this sample showed high porosity, which allows its application for this purpose. The sandstones samples were analyzed by the Skyscan system, achieving resolutions of 19{mu}m, 11{mu}m and 3.8{mu}m for each sample, respectively. The resolutions of 11{mu}m and 3.8{mu}m were the ones that generated better 2D sections for the respective samples and, consequently, more reliable porosities. The 3.8{mu}m resolution was the one that best quantified the pore size

Evaluation of Microstructural Parameters of Reservoir Rocks of the Guarani Aquifer by Analysis of Images Obtained by X- Ray Microtomography

Science.gov (United States)

Fernandes, J. S.; Lima, F. A.; Vieira, S. F.; Reis, P. J.; Appoloni, C. R.

2015-07-01

Microstructural parameters evaluation of porous materials, such as, rocks reservoir (water, petroleum, gas...), it is of great importance for several knowledge areas. In this context, the X-ray microtomography (μ-CT) has been showing a technical one quite useful for the analysis of such rocks (sandstone, limestone and carbonate), object of great interest of the petroleum and water industries, because it facilitates the characterization of important parameters, among them, porosity, permeability, grains or pore size distribution. The X-ray microtomography is a non-destructive method, that besides already facilitating the reuse of the samples analyzed, it also supplies images 2-D and 3-D of the sample. In this work samples of reservoir rock of the Guarani aquifer will be analyzed, given by the company of perforation of wells artesian Blue Water, in the municipal district of Videira, Santa Catarina, Brazil. The acquisition of the microtomographys data of the reservoir rocks was accomplished in a Skyscan 1172 μ-CT scanner, installed in Applied Nuclear Physics Laboratory (LFNA) in the State University of Londrina (UEL), Paraná, Brazil. In this context, this work presents the microstructural characterization of reservoir rock sample of the Guarani aquifer, analyzed for two space resolutions, 2.8 μm and 4.8 μm, where determined average porosity was 28.5% and 21.9%, respectively. Besides, we also determined the pore size distribution for both resolutions. Two 3-D images were generated of this sample, one for each space resolution, in which it is possible to visualize the internal structure of the same ones.

Evaluation of Microstructural Parameters of Reservoir Rocks of the Guarani Aquifer by Analysis of Images Obtained by X- Ray Microtomography

International Nuclear Information System (INIS)

Fernandes, J S; Lima, F A; Vieira, S F; Reis, P J; Appoloni, C R

2015-01-01

Microstructural parameters evaluation of porous materials, such as, rocks reservoir (water, petroleum, gas...), it is of great importance for several knowledge areas. In this context, the X-ray microtomography (μ-CT) has been showing a technical one quite useful for the analysis of such rocks (sandstone, limestone and carbonate), object of great interest of the petroleum and water industries, because it facilitates the characterization of important parameters, among them, porosity, permeability, grains or pore size distribution. The X-ray microtomography is a non-destructive method, that besides already facilitating the reuse of the samples analyzed, it also supplies images 2-D and 3-D of the sample. In this work samples of reservoir rock of the Guarani aquifer will be analyzed, given by the company of perforation of wells artesian Blue Water, in the municipal district of Videira, Santa Catarina, Brazil. The acquisition of the microtomographys data of the reservoir rocks was accomplished in a Skyscan 1172 μ-CT scanner, installed in Applied Nuclear Physics Laboratory (LFNA) in the State University of Londrina (UEL), Paraná, Brazil. In this context, this work presents the microstructural characterization of reservoir rock sample of the Guarani aquifer, analyzed for two space resolutions, 2.8 μm and 4.8 μm, where determined average porosity was 28.5% and 21.9%, respectively. Besides, we also determined the pore size distribution for both resolutions. Two 3-D images were generated of this sample, one for each space resolution, in which it is possible to visualize the internal structure of the same ones. (paper)

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

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 ...

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.

Micro-structural characterization of materials using synchrotron hard X-ray imaging techniques

International Nuclear Information System (INIS)

Agrawal, Ashish; Singh, Balwant; Kashyap, Yogesh; Sarkar, P. S.; Shukla, Mayank; Sinha, Amar

2015-01-01

X-ray imaging has been an important tool to study the materials microstructure with the laboratory based sources however the advent of third generation synchrotron sources has introduced new concepts in X-ray imaging such as phase contrast imaging, micro-tomography, fluorescence imaging and diffraction enhance imaging. These techniques are being used to provide information of materials about their density distribution, porosity, geometrical and morphological characteristics at sub-micron scalewith improved contrast. This paper discusses the development of various imaging techniques at synchrotron based imaging beamline Indus-2 and few recent experiments carried out at this facility

X-ray diffraction analysis of InAs nanowires

International Nuclear Information System (INIS)

Davydok, Anton

2013-01-01

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

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...

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....

Application of X-ray computed micro-tomography to the study of damage and oxidation kinetics of thermostructural composites

Energy Technology Data Exchange (ETDEWEB)

Caty, Olivier, E-mail: caty@lcts.u-bordeaux1.fr [Laboratory of Thermostructural Composites (LCTS), Université de Bordeaux, CNRS, SAFRAN, CEA, 3 Allée La Boétie, 33600 Pessac (France); Ibarroule, Philippe; Herbreteau, Mathieu; Rebillat, Francis [Laboratory of Thermostructural Composites (LCTS), Université de Bordeaux, CNRS, SAFRAN, CEA, 3 Allée La Boétie, 33600 Pessac (France); Maire, Eric [MATEIS Laboratory, INSA Lyon, 7 Avenue Jean Capelle, 69621 Villeurbanne Cedex (France); Vignoles, Gérard L. [Laboratory of Thermostructural Composites (LCTS), Université de Bordeaux, CNRS, SAFRAN, CEA, 3 Allée La Boétie, 33600 Pessac (France)

2014-04-01

Thermostructural composites are three-dimensionally (3D) structured materials. Weakening phenomena (mechanical and chemical) take place inside the material following its 3D structure and are thus hard to describe accurately. X-ray computed micro-tomography (μCT) is a recent solution that allows their experimental investigation. The technique is applied here to the study of failure under tensile loading and to the self healing processes during oxidation. Results are useful data to verify or invalidate hypotheses or estimations made in current models.

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.

HIGH-PERFORMANCE COMPUTING FOR THE STUDY OF EARTH AND ENVIRONMENTAL SCIENCE MATERIALS USING SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY

International Nuclear Information System (INIS)

FENG, H.; JONES, K.W.; MCGUIGAN, M.; SMITH, G.J.; SPILETIC, J.

2001-01-01

Synchrotron x-ray computed microtomography (CMT) is a non-destructive method for examination of rock, soil, and other types of samples studied in the earth and environmental sciences. The high x-ray intensities of the synchrotron source make possible the acquisition of tomographic volumes at a high rate that requires the application of high-performance computing techniques for data reconstruction to produce the three-dimensional volumes, for their visualization, and for data analysis. These problems are exacerbated by the need to share information between collaborators at widely separated locations over both local and tide-area networks. A summary of the CMT technique and examples of applications are given here together with a discussion of the applications of high-performance computing methods to improve the experimental techniques and analysis of the data

HIGH-PERFORMANCE COMPUTING FOR THE STUDY OF EARTH AND ENVIRONMENTAL SCIENCE MATERIALS USING SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY.

Energy Technology Data Exchange (ETDEWEB)

FENG,H.; JONES,K.W.; MCGUIGAN,M.; SMITH,G.J.; SPILETIC,J.

2001-10-12

Synchrotron x-ray computed microtomography (CMT) is a non-destructive method for examination of rock, soil, and other types of samples studied in the earth and environmental sciences. The high x-ray intensities of the synchrotron source make possible the acquisition of tomographic volumes at a high rate that requires the application of high-performance computing techniques for data reconstruction to produce the three-dimensional volumes, for their visualization, and for data analysis. These problems are exacerbated by the need to share information between collaborators at widely separated locations over both local and tide-area networks. A summary of the CMT technique and examples of applications are given here together with a discussion of the applications of high-performance computing methods to improve the experimental techniques and analysis of the data.

Quantitative measurements of localized density variations in cylindrical tablets using X-ray microtomography.

Science.gov (United States)

Busignies, Virginie; Leclerc, Bernard; Porion, Patrice; Evesque, Pierre; Couarraze, Guy; Tchoreloff, Pierre

2006-08-01

Direct compaction is a complex process that results in a density distribution inside the tablets which is often heterogeneous. Therefore, the density variations may affect the compact properties. A quantitative analysis of this phenomenon is still lacking. Recently, X-ray microtomography has been successfully used in pharmaceutical development to study qualitatively the impact of tablet shape and break-line in the density of pharmaceutical tablets. In this study, we evaluate the density profile in microcrystalline cellulose (Vivapur 12) compacts obtained at different mean porosity (ranging from 7.7% to 33.5%) using X-ray tomography technique. First, the validity of the Beer-Lambert law is studied. Then, density calibration is performed and density maps of cylindrical tablets are obtained and visualized using a process with colour-scale calibration plot which is explained. As expected, important heterogeneity in density is observed and quantified. The higher densities in peripheral region were particularly investigated and appraised in regard to the lower densities observed in the middle of the tablet. The results also underlined that in the case of pharmaceutical tablets, it is important to differentiate the mechanical properties representative of the total volume tablet and the mechanical properties that only characterize the tablet surface like the Brinell hardness measurements.

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

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

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

Directory of Open Access Journals (Sweden)

Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

2009-01-01

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

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, ...

X-ray microtomography study of the spallation response in Ta-W

International Nuclear Information System (INIS)

McDonald, S A; Withers, P J; Cotton, M; Millett, J C F; Bourne, N K

2014-01-01

Measurement of the damage field resulting from spallation due to shock induced loading is an important aspect of understanding the mechanisms controlling the dynamic tensile failure process. Furthermore, the ability to observe in three-dimensions, and in a non-invasive manner, the physical damage present in a spalled sample post-impact can provide important data for predictive damage models. In the current study, the influence of peak shock stress and pulse duration on the spallation damage response in the tantalum alloy Ta-2.5% W is presented. Rear surface velocimetry (HetV) measurements from plate impact experiments have been combined with 3-D characterisation and quantification of the resulting damage evolution in the recovered targets using X-ray microtomography. Small differences in spall strength are observed - an increase in the pulse duration results in a decrease in spall strength, while spall strength increases with increase in peak shock stress. The level of damaged induced (void coalescence) is more significant for an increase in pulse duration, with a local damage volume fraction double that of the case for an increase in peak shock stress.

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

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.

Computed microtomography and X-ray fluorescence analysis for comprehensive analysis of structural changes in bone.

Science.gov (United States)

Buzmakov, Alexey; Chukalina, Marina; Nikolaev, Dmitry; Schaefer, Gerald; Gulimova, Victoria; Saveliev, Sergey; Tereschenko, Elena; Seregin, Alexey; Senin, Roman; Prun, Victor; Zolotov, Denis; Asadchikov, Victor

2013-01-01

This paper presents the results of a comprehensive analysis of structural changes in the caudal vertebrae of Turner's thick-toed geckos by computer microtomography and X-ray fluorescence analysis. We present algorithms used for the reconstruction of tomographic images which allow to work with high noise level projections that represent typical conditions dictated by the nature of the samples. Reptiles, due to their ruggedness, small size, belonging to the amniote and a number of other valuable features, are an attractive model object for long-orbital experiments on unmanned spacecraft. Issues of possible changes in their bone tissue under the influence of spaceflight are the subject of discussions between biologists from different laboratories around the world.

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

Structural investigation of spherical hollow excipient Mannit Q by X-ray microtomography.

Science.gov (United States)

Kajihara, Ryusuke; Noguchi, Shuji; Iwao, Yasunori; Yasuda, Yuki; Segawa, Megumi; Itai, Shigeru

2015-11-10

The structure of Mannit Q particles, an excipient made by spray-drying a d-mannitol solution, and Mannit Q tablets were investigated by synchrotron X-ray microtomography. The Mannit Q particles had a spherical shape with a hollow core. The shells of the particles consisted of fine needle-shaped crystals, and columnar crystals were present in the hollows. These structural features suggested the following formation mechanism for the hollow particles:during the spray-drying process, the solvent rapidly evaporated from the droplet surface, resulting in the formation of shells made of fine needle-shaped crystals.Solvent remaining inside the shells then evaporated slowly and larger columnar crystals grew as the hollows formed. Although most of the Mannit Q particles were crushed on tableting, some of the particles retained their hollow structures, probably because the columnar crystals inside the hollows functioned as props. This demonstrated that the tablets with porous void spaces may be readily manufactured using Mannit Q. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

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

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

High-energy X-ray diffraction studies of short- and intermediate-range structure in oxide glasses

International Nuclear Information System (INIS)

Suzuya, Kentaro

2002-01-01

The feature of high-energy X-ray diffraction method is explained. The oxide glasses studies by using BL04B2, high-energy X-ray diffraction beam line of SPring-8, and the random system materials by high-energy monochromatic X-ray diffraction are introduced. An advantage of third generation synchrotron radiation is summarized. On SPring-8, the high-energy X-ray diffraction experiments of random system are carried out by BL04B2 and BL14B1 beam line. BL04B2 can select Si (111)(E=37.8 keV, λ=0.033 nm) and Si(220)(E=61.7 keV, λ=0.020 nm) as Si monochromator. The intermediate-range structure of (MgO) x (P 2 O 5 ) 1-x glass ,MgP 2 O 6 glass, B 2 O 3 glass, SiO 2 and GeO 2 are explained in detail. The future and application of high-energy X-ray diffraction are stated. (S.Y.)

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 ...

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 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}).

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

SYNCHROTRON X-RAY MICROTOMOGRAPHY, ELECTRON PROBE MICROANALYSIS, AND NMR OF TOLUENE WASTE IN CEMENT

International Nuclear Information System (INIS)

Butler, L.G.

1999-01-01

Synchrotron X-ray microtomography shows vesicular structures for toluene/cement mixtures, prepared with 1.22 to 3.58 wt% toluene. Three-dimensional imaging of the cured samples shows spherical vesicles, with diameters ranging from 20 to 250 microm; a search with EPMA for vesicles in the range of 1-20 microm proved negative. However, the total vesicle volume, as computed from the microtomography images, accounts for less than 10% of initial toluene. Since the cements were cured in sealed bottles, the larger portion of toluene must be dispersed within the cement matrix. Evidence for toluene in the cement matrix comes from 29 Si MAS NMR spectroscopy, which shows a reduction in chain silicates with added toluene. Also, 2 H NMR of d 8 -toluene/cement samples shows high mobility for all, toluene and thus no toluene/cement binding. A model that accounts for all observations follows: For loadings below about 3 wt%, most toluene is dispersed in the cement matrix, with a small fraction of the initial toluene phase separating from the cement paste and forming vesicular structures that are preserved in the cured cement. Furthermore, at loadings above 3 wt%, the abundance of vesicles formed during toluene/cement paste mixing leads to macroscopic phase separation (most toluene floats to the surface of the cement paste)

Quantitative analysis of flow processes in a sand using synchrotron-based X-ray microtomography

DEFF Research Database (Denmark)

Wildenschild, Dorthe; Hopmans, J.W.; Rivers, M.L.

2005-01-01

been of a mostly qualitative nature and no experiments have been presented in the existing literature where a truly quantitative approach to investigating the multiphase flow process has been taken, including a thorough image-processing scheme. The tomographic images presented here show, both......Pore-scale multiphase flow experiments were developed to nondestructively visualize water flow in a sample of porous material using X-ray microtomography. The samples were exposed to similar boundary conditions as in a previous investigation, which examined the effect of initial flow rate...... by qualitative comparison and quantitative analysis in the form of a nearest neighbor analysis, that the dynamic effects seen in previous experiments are likely due to the fast and preferential drainage of large pores in the sample. Once a continuous drained path has been established through the sample, further...

Determination of structural geometric parameters of industrial ceramic foams by gamma rays transmission and X-rays microtomography; Determinacao de parametros geometricos estruturais de espumas ceramicas industriais por transmissao de raios gama e microtomografia de raios X

Energy Technology Data Exchange (ETDEWEB)

Rocha, Wilson Roberto Dejato da

2005-07-01

In this work, the gamma rays transmission and X-rays microtomography techniques are used for the evaluation of the porosity and the pore size distribution of SiC ceramic foams. It was also accomplished the three-dimensional images after the determination of samples geometric parameters. The geometric parameters were obtained by two-dimensional images analyses, generated by a Microfocus system, with a CCD camera, an images intensifier, a X-rays tube and an automatic system for rotation of the sample. The spatial resolution of the images was about 32 {mu}m. In the gamma rays transmission methodology, a Nal(Tl) scintillation detector, an {sup 241}Am (59.53 keV, 100 mCi) radioactive source and an automatic X-Z micrometric table was used. The analyzed samples had pores density of 30, 45, 60, 80 and 100 ppi (pores per inch). The gamma rays transmission technique was accurate to supply the porosity of the samples, which ranged about 90% and was in agreement with the values supplied by manufacturer of the foams. The 30 and 45 ppi samples analyzed by X-rays microtomography showed porosity results that agree with the average porosity supplied by the manufacturer. In other hand, the 60, 80 and 100 ppi samples systematically showed average porosity about 4%, lower than the average of the manufacturer. The pore size distributions found through the software IMAGO show the presence of smaller pores than those nominated by the manufacturer. The 30 ppi samples had voids inside the solid material of the ceramic foams structure. Gaussian truncated method, used in the three-dimensional reconstruction, was not able to take into the account the voids inside the solid matrix. (author)

High-contrast x-ray microtomography in dental research

Science.gov (United States)

Davis, Graham; Mills, David

2017-09-01

X-ray microtomography (XMT) is a well-established technique in dental research. The technique has been used extensively to explore the complex morphology of the root canal system, and to qualitatively and quantitatively evaluate root canal instrumentation and filling efficacy in extracted teeth; enabling different techniques to be compared. Densitometric information can be used to identify and map demineralized tissue resulting from tooth decay (caries) and, in extracted teeth, the method can be used to evaluate different methods of excavation. More recently, high contrast XMT is being used to investigate the relationship between external insults to teeth and the pulpal reaction. When such insults occur, fluid may flow through dentinal tubules as a result of cracking or porosity in enamel. Over time, there is an increase in mineralization along the paths of the tubules from the pulp to the damaged region in enamel and this can be visualized using high contrast XMT. The scanner used for this employs time-delay integration to minimize the effects of detector inhomogeneity in order to greatly increase the upper limit on signal-to-noise ratio that can be achieved with long exposure times. When enamel cracks are present in extracted teeth, the presence of these pathways indicates that the cracking occurred prior to extraction. At high contrast, growth lines are occasionally seen in deciduous teeth which may have resulted from periods of maternal illness. Various other anomalies in mineralization resulting from trauma or genetic abnormalities can also be investigated using this technique.

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.

X-ray cone beam microtomography for quantitative assessment of tracheal and pharyngeal volumes of Rhodnius prolixus

International Nuclear Information System (INIS)

Souza, Izabella Soares de

2017-01-01

In the past decade microcomputerized tomography imaging using synchrotron radiation has become a powerful technique to generate high resolution images of Rhodinus prolixus. Images of soft tissues (protocerebrum and muscles) and dense structures (pharynx, trachea and esophagus) of R. prolixus head have been obtained using synchrotron radiation microtomography in mono and polychromatic configuration, respectively. Advancements in conventional microtomography have increased the achievable resolution and contrast, making this relatively inexpensive and widely available technology potentially useful for studies of insect internal morphology. The main goal of this work was to provide a new set of high quality microtomographic images of R. prolixus achieved by means of a desktop X-ray microtomograph. It allows the three-dimensional visualization of important chitinized structures: pharynx and tracheae. Pharyngeal and tracheal volumes were quantitatively evaluated at different days (1, 4, 10, 15 and 20) after feeding. The results suggest that variation of average volumes could be attributed to insect hormone 20-hydroxy-ecdysone (20-OH-Ec) pulse at 11 days after feeding. Pharyngeal volumes decrease 3.80 times. On the other hand, tracheal volumes increase 1.78 times. Head total volume showed similar trends than trachea. (author)

3D images of paper obtained by phase-contrast X-ray microtomography: image quality and binarisation

International Nuclear Information System (INIS)

Antoine, Christine; Nygaard, Per; Gregersen, O.W.; Holmstad, Rune; Weitkamp, Timm; Rau, Christoph

2002-01-01

A series of paper samples was investigated using high-resolution phase-contrast microtomography at the beamline ID 22 of the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. It was shown that X-ray microtomography is a non-destructive method suitable for high resolution depicting real 3D-paper structures. The method detects highly localised changes in the refractive index of the sample, such as fibre-pore interfaces. The resulting tomograms represented an outlined image of the fibre structure with an image resolution of 1 μm. Analyses were performed in dry state, but in addition some were done in wet state. The raw data obtained were transformed into 3D images. The reconstructed slices were in general of rather good quality, even if both noise and ring-like artifacts were observed. These required special filtering efforts before a segmented binary volume could be obtained for further use of the data. This approach was made up of semi-automatic routines to convert the structure into a binary format. The resulting binary volumes can be used for further characterisation of the 3D-paper structure

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

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

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)

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 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}.

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.

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.)

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

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.

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.)

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.

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....

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

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 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....

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

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.

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1991-05-16

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

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

International Nuclear Information System (INIS)

Trubin, V.A.; Szasz, A.

1991-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Shymanovich, U.

2007-11-13

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

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

International Nuclear Information System (INIS)

Shymanovich, U.

2007-01-01

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

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 ...

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].

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.

Fast x-ray fluorescence microtomography of hydrated biological samples.

Directory of Open Access Journals (Sweden)

Enzo Lombi

Full Text Available Metals and metalloids play a key role in plant and other biological systems as some of them are essential to living organisms and all can be toxic at high concentrations. It is therefore important to understand how they are accumulated, complexed and transported within plants. In situ imaging of metal distribution at physiological relevant concentrations in highly hydrated biological systems is technically challenging. In the case of roots, this is mainly due to the possibility of artifacts arising during sample preparation such as cross sectioning. Synchrotron x-ray fluorescence microtomography has been used to obtain virtual cross sections of elemental distributions. However, traditionally this technique requires long data acquisition times. This has prohibited its application to highly hydrated biological samples which suffer both radiation damage and dehydration during extended analysis. However, recent advances in fast detectors coupled with powerful data acquisition approaches and suitable sample preparation methods can circumvent this problem. We demonstrate the heightened potential of this technique by imaging the distribution of nickel and zinc in hydrated plant roots. Although 3D tomography was still impeded by radiation damage, we successfully collected 2D tomograms of hydrated plant roots exposed to environmentally relevant metal concentrations for short periods of time. To our knowledge, this is the first published example of the possibilities offered by a new generation of fast fluorescence detectors to investigate metal and metalloid distribution in radiation-sensitive, biological samples.

Quantitative analysis of minerals by X-ray diffraction

International Nuclear Information System (INIS)

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

1982-01-01

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

Reflectivity and diffraction of X rays applied to organic thin films

International Nuclear Information System (INIS)

Rieutord, Francois

1987-01-01

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

X-ray microtomography study of the compaction process of rods under tapping.

Science.gov (United States)

Fu, Yang; Xi, Yan; Cao, Yixin; Wang, Yujie

2012-05-01

We present an x-ray microtomography study of the compaction process of cylindrical rods under tapping. The process is monitored by measuring the evolution of the orientational order parameter, local, and overall packing densities as a function of the tapping number for different tapping intensities. The slow relaxation dynamics of the orientational order parameter can be well fitted with a stretched-exponential law with stretching exponents ranging from 0.9 to 1.6. The corresponding relaxation time versus tapping intensity follows an Arrhenius behavior which is reminiscent of the slow dynamics in thermal glassy systems. We also investigated the boundary effect on the ordering process and found that boundary rods order faster than interior ones. In searching for the underlying mechanism of the slow dynamics, we estimated the initial random velocities of the rods under tapping and found that the ordering process is compatible with a diffusion mechanism. The average coordination number as a function of the tapping number at different tapping intensities has also been measured, which spans a range from 6 to 8.

Granule-by-granule reconstruction of a sandpile from x-ray microtomography data

International Nuclear Information System (INIS)

Seidler, G. T.; Martinez, G.; Seeley, L. H.; Kim, K. H.; Behne, E. A.; Zaranek, S.; Chapman, B. D.; Heald, S. M.; Brewe, D. L.

2000-01-01

Mesoscale disordered materials are ubiquitous in industry and in the environment. Any fundamental understanding of the transport and mechanical properties of such materials must follow from a thorough understanding of their structure. However, in the overwhelming majority of cases, experimental characterization of such materials has been limited to first- and second-order structural correlation functions, i.e., the mean filling fraction and the structural autocorrelation function. We report here the successful combination of synchrotron x-ray microtomography and image processing to determine the full three-dimensional real-space structure of a model disordered material, a granular bed of relatively monodisperse glass spheres. Specifically, we determine the center location and the local connectivity of each granule. This complete knowledge of structure can be used to calculate otherwise inaccessible high-order correlation functions. We analyze nematic order parameters for contact bonds to characterize the geometric anisotropy or fabric induced by the sample boundary conditions. Away from the boundaries we find short-range bond orientational order exhibiting characteristics of the underlying polytetrahedral structure

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

International Nuclear Information System (INIS)

Fernandes, P.

2007-04-01

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

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

Science.gov (United States)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

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

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

International Nuclear Information System (INIS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-01-01

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

X-ray micro-tomography for investigations of brain tissues on cellular level

Science.gov (United States)

Khimchenko, Anna; Schulz, Georg; Deyhle, Hans; Thalmann, Peter; Zanette, Irene; Zdora, Marie-Christine; Bikis, Christos; Hipp, Alexander; Hieber, Simone E.; Schweighauser, Gabriel; Hench, Jürgen; Müller, Bert

2016-10-01

X-ray imaging in absorption contrast mode is well established for hard tissue visualization. However, performance for lower density materials is limited due to a reduced contrast. Our aim is three-dimensional (3D) characterization of micro-morphology of human brain tissues down to (sub-)cellular resolution within a laboratory environment. Using the laboratory-based microtomography (μCT) system nanotom m (GE Sensing and Inspection Technologies GmbH, Wunstorf, Germany) and synchrotron radiation at the Diamond-Manchester Imaging Branchline I13-2 (Diamond Light Source, Didcot, UK), we have acquired 3D data with a resolution down to 0.45 μm for visualization of a human cerebellum specimen down to cellular level. We have shown that all selected modalities, namely laboratory-based absorption contrast micro-tomography (LBμCT), synchrotron radiation based in-line single distance phase contrast tomography (SDPR) and synchrotron radiation based single-grating interferometry (GI), can reach cellular resolution for tissue samples with a size in the mm-range. The results are discussed qualitatively in comparison to optical microscopy of haematoxylin and eosin (HE) stained sections. As phase contrast yields to a better data quality for soft tissues and in order to overcome restrictions of limited beamline access for phase contrast measurements, we have equipped the μCT system nanotom m with a double-grating phase contrast set-up. Preliminary experimental results of a knee sample consisting of a bony part and a cartilage demonstrate that phase contrast data exhibits better quality compared to absorption contrast. Currently, the set-up is under adjustment. It is expected that cellular resolution would also be achieved. The questions arise (1) what would be the quality gain of laboratory-based phase contrast in comparison to laboratory-based absorption contrast tomography and (2) could laboratory-based phase contrast data provide comparable results to synchrotron radiation based

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

International Nuclear Information System (INIS)

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

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

Diffractive X-Ray Telescopes

International Nuclear Information System (INIS)

Skinner, G.K.; Skinner, G.K

2010-01-01

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

Thin film characterisation by advanced X-ray diffraction techniques

Energy Technology Data Exchange (ETDEWEB)

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

1996-09-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Barbosa, Caroline M., E-mail: carolmattosb@yahoo.com.br [Instituto de Arqueologia Brasileira (IAB), Belford Roxo, RJ (Brazil); Azeredo, Soraia R.; Lopes, Ricardo T., E-mail: soraia@lin.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/LIN/UFRJ), Rio de Janeiro, RJ (Brazil). Laboratorio de Instrumentacao Nuclear; Souza, Sheila M.F.M de, E-mail: sferraz@ensp.fiocruz.br [Fundacao Oswaldo Cruz (ENSP/FIOCRUZ), Rio de Janeiro, RJ (Brazil). Escola Nacional de Saude Publica Sergio Arouca

2013-07-01

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

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

Science.gov (United States)

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

2007-06-26

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

Assessment of the Structural Integrity of a Prototypical Instrumented IFMIF High Flux Test Module Rig by Fully 3D X-Ray Microtomography

International Nuclear Information System (INIS)

Tiseanu, I.; Craciunescu, T.; Mandache, B.N.; Simon, M.; Heinzel, V.; Stratmanns, E.; Simakov, S.P.; Leichtle, D.

2006-01-01

An inspection procedure to asses the mechanical integrity of IFMIF (International Fusion Materials Irradiation Facility) capsules and rigs during the irradiation campaign is necessary. Due to its penetration ability and contrast mechanism, the X-ray micro-tomography is the only known tool that could meet these requirements. In the High Flux Test Module (HFTM) of IFMIF miniaturized specimens are densely packed in capsules. The capsules which wear electric heaters and thermocouples are housed in rigs. To assure a well defined thermal contact the heater wires have to be attached to the capsules by brazing them into grooves. The examination of the quality of the braze material layer is of crucial interest in order to assure the best heat coupling of the heater wires to the capsule. A high density of the heaters is necessary to maintain the required temperature and, in addition NaK filling of narrow channels is employed for improving the 3D-heat transfer between the irradiation specimens and the capsule wall. Fully 3D tomographic inspections of a prototypical HFTM instrumented capsule, developed and manufactures at FZK, were conducted. In order to identify the optimum irradiation parameters and scanning configuration we carried out a comparative NDT analysis on two micro-tomography facilities, our compact, high magnification installation at NILPRP and two high-end industrial tomography facilities with higher X-ray energy and intensity at HWM. At optimum inspection parameters of a microfocus X-ray source (U=220 kV and I=300 μA) the geometry resolution was about 30-50 microns for characteristic dimension of the sample of 50 mm. Voids of 30 microns diameter and cracks of about 20 microns width can be detected. The absolute error of geometrical measurements should be sufficient for the assessment of the structural integrity of the irradiation capsule and for the geometry description within the thermal-hydraulic modeling. Space resolution could be further improved if one

Analyzing the compressive behavior of porous Ti6Al4V by X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Farias, Iván; Jimenez, Omar; Flores, Martín [Departamento de Ingeniería de Proyectos, Universidad de Guadalajara, Jalisco (Mexico); Olmos, Luís, E-mail: luisra24@gmail.com [Instituto de Investigaciones en Ciencias de la Tierra (INICIT), Universidad Michoacana de San Nicolás de Hidalgo, Michoacán (Mexico); Vergara-Hernández, Héctor Javier; Gárnica, Pedro [Instituto Tecnológico de Morelia, Michoacán (Mexico); Bouvard, Didier [Science et Ingénierie des Matériaux et Procédés (SIMaP), Université Grenoble Alpes (France)

2017-11-15

Samples with 40% vol. of pores and a pore size distribution between 100 and 500 μm were produced by powder metallurgy from Ti6Al4V alloy powders. Sintering was performed at 1300 °C during one hour in an inert Argon atmosphere in a vertical dilatometer. The compressive strength and the porosity of these samples was investigated before and after compression tests through X-ray microtomography. The values of the elastic modulus (8GPa) and yield strength (80MPa) are within the range of those used in bone implants. Porosity leads to greater deformation whereas fracture of compacts occurs perpendicularly to the applied load. It was determined that the origin of the failure is generated by rupture of interparticle necks and, large pores enhance the propagation of cracks. (author)

Analyzing the compressive behavior of porous Ti6Al4V by X-ray microtomography

International Nuclear Information System (INIS)

Farias, Iván; Jimenez, Omar; Flores, Martín; Olmos, Luís; Vergara-Hernández, Héctor Javier; Gárnica, Pedro; Bouvard, Didier

2017-01-01

Samples with 40% vol. of pores and a pore size distribution between 100 and 500 μm were produced by powder metallurgy from Ti6Al4V alloy powders. Sintering was performed at 1300 °C during one hour in an inert Argon atmosphere in a vertical dilatometer. The compressive strength and the porosity of these samples was investigated before and after compression tests through X-ray microtomography. The values of the elastic modulus (8GPa) and yield strength (80MPa) are within the range of those used in bone implants. Porosity leads to greater deformation whereas fracture of compacts occurs perpendicularly to the applied load. It was determined that the origin of the failure is generated by rupture of interparticle necks and, large pores enhance the propagation of cracks. (author)

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

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

Science.gov (United States)

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

2018-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2018-04-24

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

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

International Nuclear Information System (INIS)

Mai Zhenhong

2012-01-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

The application of X-ray, γ-ray and neutron diffraction to the characterization of single crystal perfection

International Nuclear Information System (INIS)

Freund, A.; Schneider, J.R.

1976-01-01

The work is divided into the following three chapters: 1) diffraction by perfect and imperfect crystals, 2) experimental apparatus (describing gamma ray, X-ray and neutron diffractometers), 3) application of diffraction methods to the development of neutron monochromators. (WBU) [de

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

DEFF Research Database (Denmark)

Küpper, Jochen; Stern, Stephan; Holmegaard, Lotte

2014-01-01

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

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)

Qualitative and quantitative analysis of different fluid phase in samples of glass beads by X-ray microtomography

International Nuclear Information System (INIS)

Marques, Leonardo C.; Nagata, Rodrigo; Appoloni, Carlos R.; Moreira, Anderson C.; Fernanades, Celso P.

2011-01-01

The X-ray microtomography has showed to be a useful tool for studies of inner structure of reservoir rocks. Moreover recent works have used this methodology to visualize different fluid phases present in these microstructures. In this paper X-ray microtomography has been applied to visualize three fluid phases, separately or simultaneously, in addition to a solid phase (glass beads). Two glass beads samples were manufactured and scanned, one with 0.8 mm (GB1) and other with 0.6 mm (GB2) diameter, respectively. The three fluid phases used were air, oil and a water-salt-potassium iodine solution. Two Skyscan scanners were used, both a 1172 model, which employs X-ray tube with W anode and cone beam. This laboratory based equipment is able to provide images of until 1 μm spatial resolution. One microtomograph is located at CENPES/PETROBRAS and has a CCD camera of 10 mega pixels resolution. It was used to measure the GB1 sample at 4.84 μm spatial resolution. The other one is located at LAMIR/UFPR and has a CCD camera of 11 mega pixels resolution. It was used to measure the GB2 sample at 4.99 μm spatial resolution. GB1 sample was set up with three fluid phases and presented 38.0 (2.7) % of total porosity before fluid presence and 3.5 % and 19.8 %, as lower and higher average porosity values, respectively, after to be filled with them. GB2 sample was set up with oil and water-salt-potassium iodine solution separated. It presented 36.7 (1.9) % of total porosity when dried, 18.7 (2.0) % when filled with oil and 0 % when filled with the solution. The 2D images clearly show the presence of the solution in addition to the air and solid phases. They also show that the presence of oil phase is less clear than the solution. When all the phases are present together in the sample it is possible to differentiate all of them. Individual 3D images are shown for each phase present in the sample. The 3D image containing all the phases is also shown. (author)

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

Diffraction enhanced X-ray imaging of mammals crystalline lens

International Nuclear Information System (INIS)

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

2005-01-01

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

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.

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

International Nuclear Information System (INIS)

Eberhart, J.-P.

1976-01-01

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

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.

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)

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...

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)

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....

Development of real-time x-ray microtomography system

International Nuclear Information System (INIS)

Takano, H; Morikawa, M; Konishi, S; Azuma, H; Shimomura, S; Tsusaka, Y; Kagoshima, Y; Nakano, S; Kosaka, N; Yamamoto, K

2013-01-01

We have developed a four-dimensional (4D) x-ray microcomputed tomography (CT) system that can obtain time-lapse CT volumes in real time. The system consists of a high-speed sample rotation system and a high-frame-rate x-ray imager, which are installed at a synchrotron radiation x-ray beamline. As a result of system optimization and introduction of a 'zoom resolution' procedure, a real-time 4D CT movie with a frame rate of 30 was obtained with a voxel size of 2.5 μm using 10 keV x-rays

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

International Nuclear Information System (INIS)

Riella, H.G.

1984-01-01

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

Method for obtaining silver nanoparticle concentrations within a porous medium via synchrotron X-ray computed microtomography.

Science.gov (United States)

Molnar, Ian L; Willson, Clinton S; O'Carroll, Denis M; Rivers, Mark L; Gerhard, Jason I

2014-01-21

Attempts at understanding nanoparticle fate and transport in the subsurface environment are currently hindered by an inability to quantify nanoparticle behavior at the pore scale (within and between pores) within realistic pore networks. This paper is the first to present a method for high resolution quantification of silver nanoparticle (nAg) concentrations within porous media under controlled experimental conditions. This method makes it possible to extract silver nanoparticle concentrations within individual pores in static and quasi-dynamic (i.e., transport) systems. Quantification is achieved by employing absorption-edge synchrotron X-ray computed microtomography (SXCMT) and an extension of the Beer-Lambert law. Three-dimensional maps of X-ray mass linear attenuation are converted to SXCMT-determined nAg concentration and are found to closely match the concentrations determined by ICP analysis. In addition, factors affecting the quality of the SXCMT-determined results are investigated: 1) The acquisition of an additional above-edge data set reduced the standard deviation of SXCMT-determined concentrations; 2) X-ray refraction at the grain/water interface artificially depresses the SXCMT-determined concentrations within 18.1 μm of a grain surface; 3) By treating the approximately 20 × 10(6) voxels within each data set statistically (i.e., averaging), a high level of confidence in the SXCMT-determined mean concentrations can be obtained. This novel method provides the means to examine a wide range of properties related to nanoparticle transport in controlled laboratory porous medium experiments.

Residual cold-work determination by X-ray diffraction

International Nuclear Information System (INIS)

Pireau, A.; Vanderborck, Y.

1990-01-01

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

Analysis of 3D Prints by X-ray Computed Microtomography and Terahertz Pulsed Imaging

DEFF Research Database (Denmark)

Markl, Daniel; Zeitler, J Axel; Rasch, Cecilie

2017-01-01

PURPOSE: A 3D printer was used to realise compartmental dosage forms containing multiple active pharmaceutical ingredient (API) formulations. This work demonstrates the microstructural characterisation of 3D printed solid dosage forms using X-ray computed microtomography (XμCT) and terahertz pulsed...... imaging (TPI). METHODS: Printing was performed with either polyvinyl alcohol (PVA) or polylactic acid (PLA). The structures were examined by XμCT and TPI. Liquid self-nanoemulsifying drug delivery system (SNEDDS) formulations containing saquinavir and halofantrine were incorporated into the 3D printed...... was characterised by XμCT and TPI on the basis of the computer-aided design (CAD) models of the dosage form (compartmentalised PVA structures were 7.5 ± 0.75% larger than designed; n = 3). CONCLUSIONS: The 3D printer can reproduce specific structures very accurately, whereas the 3D prints can deviate from...

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

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.

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)

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)

Small angle X ray diffraction investigation of twinned opal_like structures

NARCIS (Netherlands)

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

2012-01-01

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

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.)

Peculiarities of section topograms for the multiple diffraction of X rays

Energy Technology Data Exchange (ETDEWEB)

Kohn, V. G., E-mail: kohnvict@yandex.ru [National Research Centre “Kurchatov Institute” (Russian Federation); Smirnova, I. A. [Russian Academy of Sciences, Institute of Solid State Physics (Russian Federation)

2016-07-15

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

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.

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

International Nuclear Information System (INIS)

Zingaro, W.P.; Sicignano, A.

1980-01-01

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

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

Magnetic resonance imaging and X-ray microtomography studies of a gel-forming tablet formulation.

Science.gov (United States)

Laity, P R; Mantle, M D; Gladden, L F; Cameron, R E

2010-01-01

The capabilities of two methods for investigating tablet swelling are investigated, based on a study of a model gel-forming system. Results from magnetic resonance imaging (MRI) were compared with results from a novel application of X-ray microtomography (XmicroT) to track the movements of embedded glass microsphere tracers as the model tablets swelled. MRI provided information concerning the movement of hydration fronts into the tablets and the composition of the swollen gel layer, which formed at the tablet surface and progressively thickened with time. Conversely, XmicroT revealed significant axial expansion within the tablet core, at short times and ahead of the hydration fronts, where there was insufficient water to be observed by MRI (estimated to be around 15% by weight for the system used here). Thus, MRI and XmicroT may be regarded as complementary methods for studying the hydration and swelling behaviour of tablets. Copyright 2009 Elsevier B.V. All rights reserved.

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

NARCIS (Netherlands)

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

2011-01-01

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

Nano structured materials studied by coherent X-ray diffraction

International Nuclear Information System (INIS)

Gulden, Johannes

2013-03-01

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

Nano structured materials studied by coherent X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Gulden, Johannes

2013-03-15

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

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

Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry.

Science.gov (United States)

Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

2017-04-01

X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La 3 Ga 5 SiO 14 ) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space-time modulation of an X-ray beam.

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

Science.gov (United States)

Pinilla, Samuel; Poveda, Juan; Arguello, Henry

2018-03-01

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

Modern X-ray difraction. X-ray diffractometry for material scientists, physicists, and chemicists

International Nuclear Information System (INIS)

Spiess, L.; Schwarzer, R.; Behnken, H.; Teichert, G.

2005-01-01

The book yields a comprehensive survey over the applications of X-ray diffraction in fields like material techniques, metallurgy, electrotechniques, machine engineering, as well as micro- and nanotechniques. The necessary fundamental knowledge on X-ray diffraction are mediated foundedly and illustratively. Thereby new techniques and evaluation procedures are presented as well as well known methods. The content: Production and properties of X radiation, diffraction of X radiation, hardware for X-ray diffraction, methods of X-ray diffraction, lattice-constant determination, phase analysis, X-ray profile analysis, crystal structure analysis, X-ray radiographic stress analysis, X-ray radiographic texture analysis, crystal orientation determination, pecularities at thin films, small angle scattering

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)....

Diamond-anvil cell for radial x-ray diffraction

International Nuclear Information System (INIS)

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

2006-01-01

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

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.

Structural studies of disordered materials using high-energy x-ray diffraction from ambient to extreme conditions

Energy Technology Data Exchange (ETDEWEB)

Kohara, Shinji [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Itou, Masayoshi [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Suzuya, Kentaro [Japan Atomic Energy Agency (J-PARC/JAEA), Tokai, Naka, Ibaraki 319-1195 (Japan); Inamura, Yasuhiro [Japan Atomic Energy Agency (J-PARC/JAEA), Tokai, Naka, Ibaraki 319-1195 (Japan); Sakurai, Yoshiharu [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Ohishi, Yasuo [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Takata, Masaki [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

2007-12-19

High-energy x-rays from a synchrotron radiation source allow us to obtain high-quality diffraction data for disordered materials from ambient to extreme conditions, which is necessary for revealing the detailed structures of glass, liquid and amorphous materials. We introduced high-energy x-ray diffraction beamlines and a dedicated diffractometer for glass, liquid and amorphous materials at SPring-8 and report the recent developments of ancillary equipment. Furthermore, the structures of liquid and amorphous materials determined from the high-energy x-ray diffraction data obtained at SPring-8 are discussed.

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.

X-Ray Microtomography (μCT as a Useful Tool for Visualization and Interpretation of Shear Strength Test Results

Directory of Open Access Journals (Sweden)

Stefaniuk Damian

2015-02-01

Full Text Available The paper demonstrates the applicability of X-ray microtomography (ìCT to analysis of the results of shear strength examinations of clayey soils. The method of X-ray three-dimensional imaging offers new possibilities in soil testing. The work focuses on a non-destructive method of evaluation of specimen quality used in shear tests and mechanical behavior of soil. The paper presents the results of examination of 4 selected clayey soils. Specimens prepared for the triaxial test have been scanned using ìCT before and after the triaxial compression tests. The shear strength parameters of the soils have been estimated. Changes in soil structure caused by compression and shear failure have been presented as visualizations of the samples tested. This allowed for improved interpretation and evaluation of soil strength parameters and recognition of pre-existing fissures and the exact mode of failure. Basic geometrical parameters have been determined for selected cross-sections of specimens after failure. The test results indicate the utility of the method applied in soil testing.

Thermogravimetric and x-ray diffraction analyses of Luna-24 regolith samples

International Nuclear Information System (INIS)

Deshpande, V.V.; Dharwadkar, S.R.; Jakkal, V.S.

1979-01-01

Two samples of Luna-24 were analysed by X-ray diffraction and thermogravimetric (TG) techniques. The sample 24123.12 shows a weight loss of nearly 0.85 percent between 23O-440deg C and followed by 1.16 percent weight gain from 500 to 800deg C. The sample 23190.13 showed only a weight gain of about 1.5 percent from 5O0deg C to 900deg C. X-ray diffraction analyses show the presence of olivine, plagioclase, pigeonite, enstatite, and native iron in both the virgin samples. The heated samples, however, show that only the native iron got oxidized to iron oxide. The other constituents remain unaltered. (auth.)

Investigation of electronic order using resonant soft X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Schlappa, J.

2006-12-01

The aim of this PhD work was the application of resonant soft X-ray diffraction technique for the investigation of electronic order in transition metal oxides at the TM L{sub 2,3}-edge, trying to obtain a quantitative understanding of the data. The method was first systematically explored through application to a model system in order to test the feasibility of the technique and to understand of how X-ray optical effects have to be taken into account. Two more complex systems were investigated; stripe order in La{sub 1.8}Sr{sub 0.2}NiO{sub 4} and charge and orbital order in Fe{sub 3}O{sub 4}. The main focus of the work was on the spectroscopic potential of the technique, trying to obtain a level of quantitative description of the data. For X-ray absorption spectroscopy (XAS) from transition metal oxides, cluster configuration interaction calculation provides a powerful and realistic microscopic theory. In the frame work of this thesis cluster theory, considering explicit hybridization effects between the TM-ion and the surrounding oxygen ligands, has been applied for the first time to describe resonant diffraction data. (orig.)

Investigation of electronic order using resonant soft X-ray diffraction

International Nuclear Information System (INIS)

Schlappa, J.

2006-01-01

The aim of this PhD work was the application of resonant soft X-ray diffraction technique for the investigation of electronic order in transition metal oxides at the TM L 2,3 -edge, trying to obtain a quantitative understanding of the data. The method was first systematically explored through application to a model system in order to test the feasibility of the technique and to understand of how X-ray optical effects have to be taken into account. Two more complex systems were investigated; stripe order in La 1.8 Sr 0.2 NiO 4 and charge and orbital order in Fe 3 O 4 . The main focus of the work was on the spectroscopic potential of the technique, trying to obtain a level of quantitative description of the data. For X-ray absorption spectroscopy (XAS) from transition metal oxides, cluster configuration interaction calculation provides a powerful and realistic microscopic theory. In the frame work of this thesis cluster theory, considering explicit hybridization effects between the TM-ion and the surrounding oxygen ligands, has been applied for the first time to describe resonant diffraction data. (orig.)

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

Non-Destructive Quantification of Plastic Deformation in Steel: Employing X-Ray Diffraction Peak Broadening Analysis

Science.gov (United States)

2013-09-01

justifier l’élaboration d’une nouvelle analyse des pics de DRX dans les installations de RDDC Atlantique. Résultats : Plusieurs auteurs se sont penchés...2 3 X-Ray Diffraction Theory ...3 X-Ray Diffraction Theory The manifestation of desirable physical and chemical material properties may be readily discerned through investigation

X-ray Synchrotron Microtomography of a silicified Jurassic Cheirolepidiaceae (Conifer cone: histology and morphology of Pararaucaria collinsonae sp. nov.

Directory of Open Access Journals (Sweden)

David C. Steart

2014-10-01

Full Text Available We document a new species of ovulate cone (Pararaucaria collinsonae on the basis of silicified fossils from the Late Jurassic Purbeck Limestone Group of southern England (Tithonian Stage: ca. 145 million years. Our description principally relies on the anatomy of the ovuliferous scales, revealed through X-ray synchrotron microtomography (SRXMT performed at the Diamond Light Source (UK. This study represents the first application of SRXMT to macro-scale silicified plant fossils, and demonstrates the significant advantages of this approach, which can resolve cellular structure over lab-based X-ray computed microtomography (XMT. The method enabled us to characterize tissues and precisely demarcate their boundaries, elucidating organ shape, and thus allowing an accurate assessment of affinities. The cones are broadly spherical (ca. 1.3 cm diameter, and are structured around a central axis with helically arranged bract/scale complexes, each of which bares a single ovule. A three-lobed ovuliferous scale and ovules enclosed within pocket-forming tissue, demonstrate an affinity with Cheirolepidiaceae. Details of vascular sclerenchyma bundles, integument structure, and the number and attachment of the ovules indicate greatest similarity to P. patagonica and P. carrii. This fossil develops our understanding of the dominant tree element of the Purbeck Fossil Forest, providing the first evidence for ovulate cheirolepidiaceous cones in Europe. Alongside recent discoveries in North America, this significantly extends the known palaeogeographic range of Pararaucaria, supporting a mid-palaeolatitudinal distribution in both Gondwana and Laurasia during the Late Jurassic. Palaeoclimatic interpretations derived from contemporaneous floras, climate sensitive sediments, and general circulation climate models indicate that Pararaucaria was a constituent of low diversity floras in semi-arid Mediterranean-type environments.

X-ray Synchrotron Microtomography of a silicified Jurassic Cheirolepidiaceae (Conifer) cone: histology and morphology of Pararaucaria collinsonae sp. nov.

Science.gov (United States)

Steart, David C; Spencer, Alan R T; Garwood, Russell J; Hilton, Jason; Munt, Martin C; Needham, John; Kenrick, Paul

2014-01-01

We document a new species of ovulate cone (Pararaucaria collinsonae) on the basis of silicified fossils from the Late Jurassic Purbeck Limestone Group of southern England (Tithonian Stage: ca. 145 million years). Our description principally relies on the anatomy of the ovuliferous scales, revealed through X-ray synchrotron microtomography (SRXMT) performed at the Diamond Light Source (UK). This study represents the first application of SRXMT to macro-scale silicified plant fossils, and demonstrates the significant advantages of this approach, which can resolve cellular structure over lab-based X-ray computed microtomography (XMT). The method enabled us to characterize tissues and precisely demarcate their boundaries, elucidating organ shape, and thus allowing an accurate assessment of affinities. The cones are broadly spherical (ca. 1.3 cm diameter), and are structured around a central axis with helically arranged bract/scale complexes, each of which bares a single ovule. A three-lobed ovuliferous scale and ovules enclosed within pocket-forming tissue, demonstrate an affinity with Cheirolepidiaceae. Details of vascular sclerenchyma bundles, integument structure, and the number and attachment of the ovules indicate greatest similarity to P. patagonica and P. carrii. This fossil develops our understanding of the dominant tree element of the Purbeck Fossil Forest, providing the first evidence for ovulate cheirolepidiaceous cones in Europe. Alongside recent discoveries in North America, this significantly extends the known palaeogeographic range of Pararaucaria, supporting a mid-palaeolatitudinal distribution in both Gondwana and Laurasia during the Late Jurassic. Palaeoclimatic interpretations derived from contemporaneous floras, climate sensitive sediments, and general circulation climate models indicate that Pararaucaria was a constituent of low diversity floras in semi-arid Mediterranean-type environments.

Characterization of test specimens produced in reduced size for X-ray microtomography (µ-CT tests

Directory of Open Access Journals (Sweden)

E. E. BERNARDES

Full Text Available Abstract The need to use reduced sample sizes, in order to attain improved spatial resolution in (µ-CT tests applied in Portland cement composites, makes researchers perform the fractionation of materials to obtain samples with dimensions compatible with the capacity of the scanning equipment, which might cause alterations in the microstructure under analysis. Therefore, a test specimen (TS with dimensions compatible with the scanning capacity of a microtomography system that operates with an X-ray tube and voltage ranging from 20 to 100 kV was proposed. Axial compression strength tests were made and their total porosity was assessed by an apparent density and solid fraction density ratio, which were obtained by means of mercury and helium pycnometry and µ-CT technique, respectively. The adoption of that TS has shown to be viable for providing a sample with a higher level of representation.

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-08-31

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

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

International Nuclear Information System (INIS)

Cadalbert, Robert

1977-01-01

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

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.)

Apparatus development for high-pressure X-ray diffraction using synchrotron radiation

International Nuclear Information System (INIS)

Martinez, L.G.; Orlando, M.T.D.; Rossi, J.L.; Passamai Junior, J.L.; Melo, F.C.L.; Ferreira, F.F.

2006-01-01

Some phenomena in the field of condensed matter physics can be studied when the matter is submitted to extreme conditions of pressure, magnetic fields or temperatures. Once submitted to these conditions it is generally necessary to measure the properties of the matter in situ. The existence of a synchrotron light laboratory in Brazil opens up the chance of studying materials in extreme conditions by techniques like X-ray diffraction and absorption. However, when compared to high-energy synchrotrons accelerators, the Brazilian source offers a narrower energy range and lower flux. These facts impose limitation to perform diffraction experiments by energy dispersion and, consequently, the use of pressure cells with denser anvils like diamond. However, for a lower-pressure range, preliminary studies showed the viability of measurements in an angular dispersion configuration. This allows the use of silicon carbide anvils B 4C . In this work it is described the development of a hydrostatic pressure cell suitable for X-rays diffraction measurements in the Brazilian Synchrotron Light Laboratory using materials and technologies developed by the institutions and researchers involved in this project (IPEN, UFES, CTA and LNLS). This development can provide the scientific community with the possibility of performing X-ray diffraction measurements under hydrostatic pressure, initially up to 2 GPa, with possibilities of increasing the maximum pressure to higher values, with or without application of magnetic fields and high or low temperatures. (author)

Characterization of nanophase materials by x-ray diffraction and computer simulation

International Nuclear Information System (INIS)

Eastman, J.A.; Thompson, L.J.

1989-06-01

X-ray diffraction experiments on nanophase Pd have been performed with the primary goal of determining the nature of grain boundary structures in nanophase materials. A kinematical diffraction analysis has been developed to interpret x-ray θ--2θ data by comparing actual scans with scans produced by computer simulation. This simulation program has been used to explore the effects on diffracted intensity of a variety of microstructural and grain boundary structural parameters such as void concentration, grain size, grain boundary width, and changes in interplanar spacing and density in grain boundary regions. It has been found that a reasonable match to experimental data is produced by at least two model structures; in one, the material contains randomly positioned voids or vacancies, while in the other, the interplanar spacings in grain boundary regions are varied with respect to the spacings found in the grain interiors. 7 refs., 4 figs

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

Science.gov (United States)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction; Nouvelles etudes structurales de cristaux liquides par reflectivite et diffraction resonante des rayons X

Energy Technology Data Exchange (ETDEWEB)

Fernandes, P

2007-04-15

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

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.

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).

Measurements of transient electron density distributions by femtosecond X-ray diffraction; Messungen transienter Elektronendichteverteilungen durch Femtosekunden-Roentgenbeugung

Energy Technology Data Exchange (ETDEWEB)

Freyer, Benjamin

2013-05-02

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.

Search for Fluid Inclusions in a Carbonaceous Chondrite Using a New X-Ray Micro-Tomography Technique Combined with FIB Sampling

Science.gov (United States)

Tsuchiyama, A.; Miyake, A.; Zolensky, M. E.; Uesugi, K.; Nakano, T.; Takeuchi, A.; Suzuki, Y.; Yoshida, K.

2014-01-01

Early solar system aqueous fluids are preserved in some H chondrites as aqueous fluid inclusions in halite (e.g., [1]). Although potential fluid inclusions are also expected in carbonaceous chondrites [2], they have not been surely confirmed. In order to search for these fluid inclusions, we have developped a new X-ray micro-tomography technique combined with FIB sampling and applied this techniqu to a carbanaceous chondrite. Experimental: A polished thin section of Sutter's Mill meteorite (CM) was observed with an optical microscope and FE-SEM (JEOL 7001F) for chosing mineral grains of carbonates (mainly calcite) and sulfides (FeS and ZnS) 20-50 microns in typical size, which may have aqueous fluid inclusions. Then, a "house" similar to a cube with a roof (20-30 microns in size) is sampled from the mineral grain by using FIB (FEI Quanta 200 3DS). Then, the house was atached to a thin W-needle by FIB and imaged by a SR-based imaging microtomography system with a Fresnel zone plate at beamline BL47XU, SPring-8, Japan. One sample was imaged at two X-ray energies, 7 and 8 keV, to identify mineral phases (dual-enegy microtomography: [3]). The size of voxel (pixel in 3D) was 50-80 nm, which gave the effective spatial resolution of approx. 200 nm. A terrestrial quartz sample with an aqueous fluid inclusion with a bubble was also examined as a test sample by the same method. Results and discussion: A fluid inclusion of 5-8 microns in quartz was clearly identified in a CT image. A bubble of approx. 4 microns was also identified as refraction contrast although the X-ray absorption difference between fluid and bubble is small. Volumes of the fluid and bubble were obtained from the 3D CT images. Fourteen grains of calcite, two grains of iron sulfide and one grain of (Zn,Fe)S were examined. Ten calcite, one iron sulfide and one (Zn,Fe)S grains have inclusions >1 micron in size (the maximum: approx. 5 microns). The shapes are spherical or irregular. Tiny inclusions (tiny solid

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

International Nuclear Information System (INIS)

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

2008-01-01

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

Nondestructive strain depth profiling with high energy X-ray diffraction: System capabilities and limitations

Science.gov (United States)

Zhang, Zhan; Wendt, Scott; Cosentino, Nicholas; Bond, Leonard J.

2018-04-01

Limited by photon energy, and penetration capability, traditional X-ray diffraction (XRD) strain measurements are only capable of achieving a few microns depth due to the use of copper (Cu Kα1) or molybdenum (Mo Kα1) characteristic radiation. For deeper strain depth profiling, destructive methods are commonly necessary to access layers of interest by removing material. To investigate deeper depth profiles nondestructively, a laboratory bench-top high-energy X-ray diffraction (HEXRD) system was previously developed. This HEXRD method uses an industrial 320 kVp X-Ray tube and the Kα1 characteristic peak of tungsten, to produces a higher intensity X-ray beam which enables depth profiling measurement of lattice strain. An aluminum sample was investigated with deformation/load provided using a bending rig. It was shown that the HEXRD method is capable of strain depth profiling to 2.5 mm. The method was validated using an aluminum sample where both the HEXRD method and the traditional X-ray diffraction method gave data compared with that obtained using destructive etching layer removal, performed by a commercial provider. The results demonstrate comparable accuracy up to 0.8 mm depth. Nevertheless, higher attenuation capabilities in heavier metals limit the applications in other materials. Simulations predict that HEXRD works for steel and nickel in material up to 200 µm, but experiment results indicate that the HEXRD strain profile is not practical for steel and nickel material, and the measured diffraction signals are undetectable when compared to the noise.

Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

Science.gov (United States)

Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

2017-11-01

The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

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

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

Science.gov (United States)

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

2013-01-01

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

X-ray diffraction investigation of self-annealing in nanocrystalline copper electrodeposits

DEFF Research Database (Denmark)

Pantleon, Karen; Somers, Marcel A. J.

2006-01-01

X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multip...... twinning during self-annealing. The kinetics of self-annealing depends on the layer thickness as well as on the orientation and/or the size of the as-deposited crystallites. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.......X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multiple...

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.

X-ray diffraction and measurement of residual stresses

International Nuclear Information System (INIS)

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

1977-01-01

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

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...

Simultaneous X-ray diffraction from multiple single crystals of macromolecules

DEFF Research Database (Denmark)

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

2011-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-06-29

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

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.

A CMOS active pixel sensor system for laboratory- based x-ray diffraction studies of biological tissue

International Nuclear Information System (INIS)

Bohndiek, Sarah E; Cook, Emily J; Arvanitis, Costas D; Olivo, Alessandro; Royle, Gary J; Clark, Andy T; Prydderch, Mark L; Turchetta, Renato; Speller, Robert D

2008-01-01

X-ray diffraction studies give material-specific information about biological tissue. Ideally, a large area, low noise, wide dynamic range digital x-ray detector is required for laboratory-based x-ray diffraction studies. The goal of this work is to introduce a novel imaging technology, the CMOS active pixel sensor (APS) that has the potential to fulfil all these requirements, and demonstrate its feasibility for coherent scatter imaging. A prototype CMOS APS has been included in an x-ray diffraction demonstration system. An industrial x-ray source with appropriate beam filtration is used to perform angle dispersive x-ray diffraction (ADXRD). Optimization of the experimental set-up is detailed including collimator options and detector operating parameters. Scatter signatures are measured for 11 different materials, covering three medical applications: breast cancer diagnosis, kidney stone identification and bone mineral density calculations. Scatter signatures are also recorded for three mixed samples of known composition. Results are verified using two independent models for predicting the APS scatter signature: (1) a linear systems model of the APS and (2) a linear superposition integral combining known monochromatic scatter signatures with the input polychromatic spectrum used in this case. Cross validation of experimental, modelled and literature results proves that APS are able to record biologically relevant scatter signatures. Coherent scatter signatures are sensitive to multiple materials present in a sample and provide a means to quantify composition. In the future, production of a bespoke APS imager for x-ray diffraction studies could enable simultaneous collection of the transmitted beam and scattered radiation in a laboratory-based coherent scatter system, making clinical transfer of the technique attainable

Formation mechanism of channel segregation in carbon steels by inclusion flotation: X-ray microtomography characterization and multi-phase flow modeling

International Nuclear Information System (INIS)

Cao, Yan Fei; Chen, Yun; Li, Dian Zhong

2016-01-01

Recent experimental dissections of steel ingots and multi-scale simulations have led to the discovery of a potential driving force for channel segregation: the flotation of oxide-based inclusion (D. Li et al., Nat. Commun. 5:5572 (2014)). Further experimental analysis and numerical modeling are necessary to clarify this mechanism in detail. In this work, the inclusions in a carbon steel ingot that exhibits severe channel segregations were characterized by the 3D X-ray microtomography, which revealed a significant enrichment and growth of inclusions in the channels. Based on above microtomography characterization, a 2D macrosegregation model encompassing the inclusion flotation was established. In the model, the motions of solid inclusions and liquid were described using the multi-phase flow scheme within the Euler-Lagrange framework. The benchmark simulations showed that sufficient inclusion populations with appropriate sizes are capable of altering the local flow patterns and destabilize the mushy zone, initiating the subsequent channel segregation. The continuous interplay between melt convection, inclusion flotation and solidification eventually causes the formation of macroscale channel. The predicted sizes and volume fraction of inclusions that are able to trigger the channel segregation effectively are consistent with the data obtained via microtomography characterization. The macrosegregation model was then applied to predict the channel segregations in an industrial carbon steel ingot. A rather good agreement of A-segregates was achieved between the simulation and the dissected ingot.

Noninvasive Measurement of Vulnerability to Drought-Induced Embolism by X-Ray Microtomography.

Science.gov (United States)

Choat, Brendan; Badel, Eric; Burlett, Regis; Delzon, Sylvain; Cochard, Herve; Jansen, Steven

2016-01-01

Hydraulic failure induced by xylem embolism is one of the primary mechanisms of plant dieback during drought. However, many of the methods used to evaluate the vulnerability of different species to drought-induced embolism are indirect and invasive, increasing the possibility that measurement artifacts may occur. Here, we utilize x-ray computed microtomography (microCT) to directly visualize embolism formation in the xylem of living, intact plants with contrasting wood anatomy (Quercus robur, Populus tremula × Populus alba, and Pinus pinaster). These observations were compared with widely used centrifuge techniques that require destructive sampling. MicroCT imaging provided detailed spatial information regarding the dimensions and functional status of xylem conduits during dehydration. Vulnerability curves based on microCT observations of intact plants closely matched curves based on the centrifuge technique for species with short vessels (P. tremula × P. alba) or tracheids (P. pinaster). For ring porous Q. robur, the centrifuge technique significantly overestimated vulnerability to embolism, indicating that caution should be used when applying this technique to species with long vessels. These findings confirm that microCT can be used to assess the vulnerability to embolism on intact plants by direct visualization. © 2016 American Society of Plant Biologists. All Rights Reserved.

Determination of SiC ceramic foams microstructure properties by X-rays microtomography

International Nuclear Information System (INIS)

Nagata, Rodrigo; Appoloni, Carlos Roberto; Fernandes, Jaquiel Salvi

2009-01-01

Silicon carbide ceramic foams (SiC) can operate at high temperatures, which allow them to be used as heat exchangers, liquid metal filters, composite of rocket nozzles, etc. For many of these applications it is very important to know the foams' porosity. In this work the porosity of SiC ceramic foams was determined by X-rays microtomography, a powerful non-destructive technique that allows the analysis of the sample's internal structure. The samples have pore densities of 30, 45, 60, 80 and 100 pores per inch (ppi). The spatial resolution obtained was 24.8 μm. The cross sections' reconstruction was performed with a cone beam filtered backprojection algorithm. In the analyses, micropores were observed in the foam's lattice wire of the 30 ppi and 45 ppi samples. Micropores were present in few cross sections of 60 ppi sample too, but it was not found in the 80 ppi and 100 ppi samples. The total porosities obtained were Φ = (88.8 ± 4.3) %, Φ = (85.2 ± 1.4) %, Φ = (82.3 ± 1.8) %, Φ (79.9 ± 1.3) % and Φ = (80.4 ± 1.5) %, for the 30, 45, 60, 80 and 100 ppi samples, respectively. (author)

Single order soft X-ray diffraction with quasi-random radius pinhole array spectroscopic photon sieves

International Nuclear Information System (INIS)

Zhang Qiang-Qiang; Wei Lai; Yang Zu-Hua; Qian Feng; Fan Quan-Ping; Zhang Bo; Gu Yu-Qiu; Cao Lei-Feng

2014-01-01

A novel single order diffraction grating in the soft X-ray region, called quasi-random radius pinhole array spectroscopic photon sieves (QRSPS), is proposed in this paper. This new grating is composed of pinholes on a substrate, whose radii are quasi-random, while their centers are regular. Analysis proves that its transmittance function across the grating bar is similar to that of sinusoidal transmission gratings. Simulation results show that the QRSPS can suppress higher-order diffraction effectively. And the QRSPS would still retain its characteristic of single order diffraction when we take the effect of X-ray penetration into account. These properties indicate that the QRSPS can be used in the soft X-ray spectra measurement. (electromagnetism, optics, acoustics, heat transfer, classical mechanics, and fluid dynamics)

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)

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.

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.

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

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

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

Data.gov (United States)

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

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

Data.gov (United States)

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

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

International Nuclear Information System (INIS)

Czuba, J.; Dziedzic, A.

1978-01-01

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

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.

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)

Fusion bonding of Si wafers investigated by x ray diffraction

DEFF Research Database (Denmark)

Weichel, Steen; Grey, Francois; Rasmussen, Kurt

2000-01-01

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

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

Indian Academy of Sciences (India)

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

Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

Directory of Open Access Journals (Sweden)

M. S. Conconi

2014-12-01

Full Text Available The firing transformations of traditional (clay based ceramics are of technological and archeological interest, and are usually reported qualitatively or semiquantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite, the low crystalline (metakaolinite and/or spinel type pre-mullite and glassy phases evolution of a triaxial (clay-quartz-feldspar ceramic fired in a wide temperature range between 900 and 1300 ºC. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 ºC spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and

Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

International Nuclear Information System (INIS)

Conconi, M.S.; Gauna, M.R.; Serra, M.F.; Suarez, G.; Aglietti, E.F.; Rendtorff, N.M.

2014-01-01

The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

Energy Technology Data Exchange (ETDEWEB)

Conconi, M.S.; Gauna, M.R.; Serra, M.F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC), Buenos Aires (Argentina); Suarez, G.; Aglietti, E.F.; Rendtorff, N.M., E-mail: rendtorff@cetmic.unlp.edu.ar [Universidad Nacional de La Plata (UNLP), Buenos Aires (Argentina). Fac. de Ciencias Exactas. Dept. de Quimica

2014-10-15

The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

A novel technique for investigation of complete and partial anisotropic wetting on structured surface by X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Santini, M., E-mail: maurizio.santini@unibg.it [Department of Engineering and Applied Sciences, University of Bergamo, Bergamo (Italy); Guilizzoni, M. [Department of Energy, Politecnico di Milano, Milano (Italy); Fest-Santini, S. [Department of Engineering, University of Bergamo, Bergamo (Italy); Lorenzi, M. [School of Engineering and Mathematical Sciences, City University London, London (United Kingdom)

2015-02-15

An experimental study about the anisotropic wetting behavior of a surface patterned with parallel grooves is presented as an application example of a novel technique for investigation of complete and partial anisotropic wetting on structured surface by X-ray microtomography. Shape of glycerin droplets on such surface is investigated by X-ray micro computed tomography (microCT) acting as a non-intrusive, full volume 3D microscope with micrometric spatial resolution. The reconstructed drop volumes enable to estimate the exact volumes of the drops, their base contours, and 3D static contact angles, based on true cross-sections of the drop-surface couple. Droplet base contours are compared to approximate geometrical contour shapes proposed in the literature. Contact angles along slices parallel and perpendicular to the grooves direction are compared with each other. The effect of the sessile drop volume on the wetting behavior is discussed. The proposed technique, which is applicable for any structured surface, enables the direct measure of Wenzel ratio based on the microCT scan in the wetted region usually inapproachable by any others. Comparisons with simplified models are presented and congruence of results with respect to the minimum resolution needed is evaluated and commented.

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

DEFF Research Database (Denmark)

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

1998-01-01

within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

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)

Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

International Nuclear Information System (INIS)

Haboub, Abdel; Nasiatka, James R.; MacDowell, Alastair A.; Bale, Hrishikesh A.; Cox, Brian N.; Marshall, David B.; Ritchie, Robert O.

2014-01-01

A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C

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.

X-ray diffraction study of pure plutonium under pressure

Energy Technology Data Exchange (ETDEWEB)

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

2009-03-15

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

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

International Nuclear Information System (INIS)

Wieteska, K.

1998-01-01

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

Micro-CTvlab: A web based virtual gallery of biological specimens using X-ray microtomography (micro-CT).

Science.gov (United States)

Keklikoglou, Kleoniki; Faulwetter, Sarah; Chatzinikolaou, Eva; Michalakis, Nikitas; Filiopoulou, Irene; Minadakis, Nikos; Panteri, Emmanouela; Perantinos, George; Gougousis, Alexandros; Arvanitidis, Christos

2016-01-01

During recent years, X-ray microtomography (micro-CT) has seen an increasing use in biological research areas, such as functional morphology, taxonomy, evolutionary biology and developmental research. Micro-CT is a technology which uses X-rays to create sub-micron resolution images of external and internal features of specimens. These images can then be rendered in a three-dimensional space and used for qualitative and quantitative 3D analyses. However, the online exploration and dissemination of micro-CT datasets are rarely made available to the public due to their large size and a lack of dedicated online platforms for the interactive manipulation of 3D data. Here, the development of a virtual micro-CT laboratory (Micro-CT vlab ) is described, which can be used by everyone who is interested in digitisation methods and biological collections and aims at making the micro-CT data exploration of natural history specimens freely available over the internet. The Micro-CT vlab offers to the user virtual image galleries of various taxa which can be displayed and downloaded through a web application. With a few clicks, accurate, detailed and three-dimensional models of species can be studied and virtually dissected without destroying the actual specimen. The data and functions of the Micro-CT vlab can be accessed either on a normal computer or through a dedicated version for mobile devices.

Identification of strain fields in pure Al and hybrid Ni/Al metal foams using X-ray micro-tomography under loading

International Nuclear Information System (INIS)

Fíla, T.; Jiroušek, O.; Jung, A.; Kumpová, I.

2016-01-01

Hybrid foams are materials formed by a core from a standard open cell metal foam that is during the process of electrodeposition coated by a thin layer of different nanocrystalline metals. The material properties of the base metal foam are in this way modified resulting in higher plateau stress and, more importantly, by introduction of strain-rate dependence to its deformation response. In this paper, we used time-lapse X-ray micro-tomography for the mechanical characterization of Ni/Al hybrid foams (aluminium open cell foams with nickel coating layer). To fully understand the effects of the coating layer on the material's effective properties, we compared the compressive response of the base uncoated foam to the response of the material with coating thickness of 50 and 75 μm. Digital volume correlation (DVC) was applied to obtain volumetric strain fields of the deforming micro-structure up to the densification region of the deforming cellular structure. The analysis was performed as a compressive mechanical test with simultaneous observation using X-ray radiography and tomography. A custom design experimental device was used for compression of the foam specimens in several deformation states directly in the X-ray setup. Planar X-ray images were taken during the loading phases and a X-ray tomography was performed at the end of each loading phase (up to engineering strain 22%). The samples were irradiated using micro-focus reflection type X-ray tube and images were taken using a large area flat panel detector. Tomography reconstructions were used for an identification of a strain distribution in the foam using digital volumetric correlation. A comparison of the deformation response of the coated and the uncoated foam in uniaxial quasi-static compression is summarized in the paper.

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.

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

Indian Academy of Sciences (India)

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

Synchrotron-Radiation Induced X-Ray Emission (SRIXE)

Energy Technology Data Exchange (ETDEWEB)

Jones, Keith W.

1999-09-01

and increase in scientific use can be maintained for the synchrotron x-ray source. A short summary of the present state of the synchrotron radiation-induced x-ray emission (SRIXE) method is presented here. Basically, SRIXE experiments can include any that depend on the detection. of characteristic x-rays produced by the incident x-ray beam born the synchrotron source as they interact with a sample. Thus, experiments done to measure elemental composition, chemical state, crystal, structure, and other sample parameters can be considered in a discussion of SRIXE. It is also clear that the experimentalist may well wish to use a variety of complementary techniques for study of a given sample. For this reason, discussion of computed microtomography (CMT) and x-ray diffraction is included here. It is hoped that this present discussion will serve as a succinct introduction to the basic ideas of SRIXE for those not working in the field and possibly help to stimulate new types of work by those starting in the field as well as by experienced practitioners of the art. The topics covered include short descriptions of (1) the properties of synchrotron radiation, (2) a description of facilities used for its production, (3) collimated microprobe, (4) focused microprobes, (5) continuum and monoenergetic excitation, (6) detection limits, (7) quantitation, (8) applications of SRIXE, (9) computed microtomography (CMT), and (10)chemical speciation using x-ray absorption near-edge structure (XANES) and extended x-ray absorption fine structure (EXAFS). An effort has been made to cite a wide variety of work from different laboratories to show the vital nature of the field.

Synchrotron-Radiation Induced X-Ray Emission (SRIXE)

International Nuclear Information System (INIS)

Jones, Keith W.

1999-01-01

and increase in scientific use can be maintained for the synchrotron x-ray source. A short summary of the present state of the synchrotron radiation-induced x-ray emission (SRIXE) method is presented here. Basically, SRIXE experiments can include any that depend on the detection. of characteristic x-rays produced by the incident x-ray beam born the synchrotron source as they interact with a sample. Thus, experiments done to measure elemental composition, chemical state, crystal, structure, and other sample parameters can be considered in a discussion of SRIXE. It is also clear that the experimentalist may well wish to use a variety of complementary techniques for study of a given sample. For this reason, discussion of computed microtomography (CMT) and x-ray diffraction is included here. It is hoped that this present discussion will serve as a succinct introduction to the basic ideas of SRIXE for those not working in the field and possibly help to stimulate new types of work by those starting in the field as well as by experienced practitioners of the art. The topics covered include short descriptions of (1) the properties of synchrotron radiation, (2) a description of facilities used for its production, (3) collimated microprobe, (4) focused microprobes, (5) continuum and monoenergetic excitation, (6) detection limits, (7) quantitation, (8) applications of SRIXE, (9) computed microtomography (CMT), and (10)chemical speciation using x-ray absorption near-edge structure (XANES) and extended x-ray absorption fine structure (EXAFS). An effort has been made to cite a wide variety of work from different laboratories to show the vital nature of the field

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Science.gov (United States)

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

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

International Nuclear Information System (INIS)

Rehbein, S.

2002-01-01

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

Assessment of the structural integrity of a prototypical instrumented IFMIF high flux test module rig by fully 3D X-ray microtomography

Energy Technology Data Exchange (ETDEWEB)

Tiseanu, Ion [National Institute for Laser, Plasma and Radiation Physics, Plasma Physics and Nuclear Fusion Laboratory NILPRP, P.O. Box MG-36, R-77125 Bucharest-Magurele (Romania)], E-mail: tiseanu@infim.ro; Simon, Martin [Hans Waelischmiller GmbH (HWM), Schiessstattweg 16, D-88677 Markdorf (Germany); Craciunescu, Teddy; Mandache, Bogdan N. [National Institute for Laser, Plasma and Radiation Physics, Plasma Physics and Nuclear Fusion Laboratory NILPRP, P.O. Box MG-36, R-77125 Bucharest-Magurele (Romania); Heinzel, Volker; Stratmanns, Erwin; Simakov, Stanislaw P.; Leichtle, Dieter [Forschungszentrum Karlsruhe (FZK), Institut fuer Reaktorsicherheit IRS, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

2007-10-15

An inspection procedure to assess the mechanical integrity of the International Fusion Materials Irradiation Facility (IFMIF) capsules and rigs during the irradiation campaign is necessary. Due to its penetration ability and contrast mechanism, the X-ray microtomography is the only known tool that could meet these requirements. In the high flux test module (HFTM) of IFMIF miniaturized specimens are densely packed in capsules. The capsules, which wear electric heaters and thermocouples, are housed in rigs. To assure a well-defined thermal contact the heater wires have to be attached to the capsules by brazing them into grooves. The examination of the quality of the braze material layer is of crucial interest in order to assure the best heat coupling of the heater wires to the capsule. A high density of the heaters is necessary to maintain the required temperature and, in addition NaK filling of narrow channels is employed for improving the 3D-heat transfer between the irradiation specimens and the capsule wall. Fully 3D tomographic inspections of a prototypical HFTM instrumented capsule, developed and manufactured at FZK, were conducted. In order to identify the optimum irradiation parameters and scanning configuration we carried out a comparative NDT analysis on two microtomography facilities: a compact, high magnification installation at NILPRP and a high-end industrial tomography facility with higher X-ray energy and intensity at HWM. At optimum inspection parameters of a directional microfocus X-ray source (U = 220 kV and I = 300 {mu}A) the geometry resolution was about 30 microns for characteristic dimension of the sample of 50 mm. Voids of 30 microns diameter and cracks of about 20 microns width can be detected. The absolute error of geometrical measurements is sufficient for the assessment of the structural integrity of the irradiation capsule and for the geometry description within the thermal-hydraulic modeling. The space resolution and the overall

Assessment of the structural integrity of a prototypical instrumented IFMIF high flux test module rig by fully 3D X-ray microtomography

International Nuclear Information System (INIS)

Tiseanu, Ion; Simon, Martin; Craciunescu, Teddy; Mandache, Bogdan N.; Heinzel, Volker; Stratmanns, Erwin; Simakov, Stanislaw P.; Leichtle, Dieter

2007-01-01

An inspection procedure to assess the mechanical integrity of the International Fusion Materials Irradiation Facility (IFMIF) capsules and rigs during the irradiation campaign is necessary. Due to its penetration ability and contrast mechanism, the X-ray microtomography is the only known tool that could meet these requirements. In the high flux test module (HFTM) of IFMIF miniaturized specimens are densely packed in capsules. The capsules, which wear electric heaters and thermocouples, are housed in rigs. To assure a well-defined thermal contact the heater wires have to be attached to the capsules by brazing them into grooves. The examination of the quality of the braze material layer is of crucial interest in order to assure the best heat coupling of the heater wires to the capsule. A high density of the heaters is necessary to maintain the required temperature and, in addition NaK filling of narrow channels is employed for improving the 3D-heat transfer between the irradiation specimens and the capsule wall. Fully 3D tomographic inspections of a prototypical HFTM instrumented capsule, developed and manufactured at FZK, were conducted. In order to identify the optimum irradiation parameters and scanning configuration we carried out a comparative NDT analysis on two microtomography facilities: a compact, high magnification installation at NILPRP and a high-end industrial tomography facility with higher X-ray energy and intensity at HWM. At optimum inspection parameters of a directional microfocus X-ray source (U = 220 kV and I = 300 μA) the geometry resolution was about 30 microns for characteristic dimension of the sample of 50 mm. Voids of 30 microns diameter and cracks of about 20 microns width can be detected. The absolute error of geometrical measurements is sufficient for the assessment of the structural integrity of the irradiation capsule and for the geometry description within the thermal-hydraulic modeling. The space resolution and the overall

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-08-01

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

Real-time observation of epitaxial crystal growth in gaseous environment using x-ray diffraction and x-ray reflectometry

International Nuclear Information System (INIS)

Kawamura, Tomoaki; Bhunia, Satyaban; Watanabe, Yoshio; Fujikawa, Seiji

2008-01-01

We made the x-ray diffractometer combined with the MOCVD growth system for the real-time observation of epitaxial growth in gaseous environment, and investigated the growth mechanism of InP crystals. Changes of the (-5/2 O) Bragg diffraction during the growth revealed that the growth starts immediately after the In source has been supplied and gradually stopped, owing to the migrating In atoms on the surface. Additionally, one can easily determine the growth modes, including 3-dimensional mode, layer-by-layer mode, and step-flow mode, by observing the change of x-ray reflectivity with various growth conditions. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Kiyota, Eduardo [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Sousa, Sylvia Morais de [Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP (Brazil); Santos, Marcelo Leite dos; Costa Lima, Aline da [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil); Menossi, Marcelo [Departamento de Genética e Evolução, Instituto de Biologia, Universidade Estadual de Campinas, Campinas-SP (Brazil); Yunes, José Andrés [Laboratório de Biologia Molecular, Centro Infantil Boldrini, Campinas-SP (Brazil); Aparicio, Ricardo, E-mail: aparicio@iqm.unicamp.br [Laboratório de Biologia Estrutural, Instituto de Química, Universidade Estadual de Campinas, CP 6154, 13083-970 Campinas-SP (Brazil)

2007-11-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

KAUST Repository

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

2012-01-01

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

A Monte Carlo error simulation applied to calibration-free X-ray diffraction phase analysis

International Nuclear Information System (INIS)

Braun, G.E.

1986-01-01

Quantitative phase analysis of a system of n phases can be effected without the need for calibration standards provided at least n different mixtures of these phases are available. A series of linear equations relating diffracted X-ray intensities, weight fractions and quantitation factors coupled with mass balance relationships can be solved for the unknown weight fractions and factors. Uncertainties associated with the measured X-ray intensities, owing to counting of random X-ray quanta, are used to estimate the errors in the calculated parameters utilizing a Monte Carlo simulation. The Monte Carlo approach can be generalized and applied to any quantitative X-ray diffraction phase analysis method. Two examples utilizing mixtures of CaCO 3 , Fe 2 O 3 and CaF 2 with an α-SiO 2 (quartz) internal standard illustrate the quantitative method and corresponding error analysis. One example is well conditioned; the other is poorly conditioned and, therefore, very sensitive to errors in the measured intensities. (orig.)

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

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

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.

Reconstruction of Stress and Composition Profiles from X-ray Diffraction Experiments - How to Avoid Ghost Stresses?

DEFF Research Database (Denmark)

Christiansen, Thomas; Somers, Marcel A.J.

2004-01-01

On evaluating lattice strain-depth or stress-depth profiles with X-ray diffraction, the variation of the information depth while combining various tilt angles,psi, in combination with lattice spacing gradients leads to artefacts,so-called ghost or fictitious stresses. X-ray diffraction lattice...... method for the evaluation of stress/strain and composition profiles, while minimising the risk for ghost stresses....

Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders

Directory of Open Access Journals (Sweden)

Yifeng Yun

2015-03-01

Full Text Available Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED data collection, namely automated diffraction tomography (ADT and rotation electron diffraction (RED, have been developed. Compared with X-ray diffraction (XRD and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni–Se–O–Cl crystals, zeolites, germanates, metal–organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three

Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

Science.gov (United States)

Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

2015-03-01

Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods

Computer simulation tools for X-ray analysis scattering and diffraction methods

CERN Document Server

Morelhão, Sérgio Luiz

2016-01-01

The main goal of this book is to break down the huge barrier of difficulties faced by beginners from many fields (Engineering, Physics, Chemistry, Biology, Medicine, Material Science, etc.) in using X-rays as an analytical tool in their research. Besides fundamental concepts, MatLab routines are provided, showing how to test and implement the concepts. The major difficult in analyzing materials by X-ray techniques is that it strongly depends on simulation software. This book teaches the users on how to construct a library of routines to simulate scattering and diffraction by almost any kind of samples. It provides to a young student the knowledge that would take more than 20 years to acquire by working on X-rays and relying on the available textbooks. In this book, fundamental concepts in applied X-ray physics are demonstrated through available computer simulation tools. Using MatLab, more than eighty routines are developed for solving the proposed exercises, most of which can be directly used in experimental...

IL 12: Femtosecond x-ray powder diffraction

International Nuclear Information System (INIS)

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

2010-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Wu, M.; Loisel, G. P. [Sandia National Laboratories, Albuquerque, New Mexico 87123 (United States)

2014-11-15

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

Mineral identification in Colombian coals using Moessbauer spectroscopy and X-ray diffraction

International Nuclear Information System (INIS)

Fajardo, M.; Mojica, J.; Barraza, J.; Perez Alcazar, G.A.; Tabares, J.A.

1999-01-01

Minerals were identified in three Colombian coal samples from the Southwest of the country using Moessbauer spectroscopy and X-ray diffraction. Original and sink separated coal fractions of specific gravity 1.40 and 1.60 with particle size less than 600 μm were used in the study. Using Moessbauer spectroscopy, the minerals identified in the original coal samples were pyrite jarosite, ankerite, illite and ferrous sulfate, whereas by means of X-ray diffraction, minerals identified were kaolinite, quartz, pyrite, and jarosite. Differences in mineral composition were found in the original and sink separated fractions using both techniques. Moessbauer spectra show that the mineral phases in low concentrations such as illite, ankerite and ferrous sulfate do not always appear in the spectra of sink coals, despite of those minerals occurring in the original coal, due to the fact that they are associated with the organic matter and not liberated in the grinding process. X-ray results show that the peak intensity grows as the specific gravity is increased indicating that the density separation method could be an effective process to clean coal

X-ray diffraction measurements in KCl shocked along [100

International Nuclear Information System (INIS)

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

2000-01-01

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

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.

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 computed microtomography integrated to petrography for the three-dimensional study of rock porosity; A microtomografia computadorizada de raios x integrada a petrografia no estudo tridimensional de porosidade em rochas

Energy Technology Data Exchange (ETDEWEB)

Reis Neto, Joss Manoel dos; Fiori, Alberto Pio; Lopes, Angela Pacheco; Pinto-Coelho, Cristina Valle; Vasconcellos, Eleonora Maria Gouvea; Silva, Gabriel Fischer da [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Geologia; Marchese, Clarice; Secchi, Rodrigo, E-mail: jmreis@ufpr.br, E-mail: fiori@ufpr.br, E-mail: angelalopes@ufpr.br, E-mail: cristinavpc@ufpr.br, E-mail: eleonora@ufpr.br, E-mail: fischergab@hotmail.com, E-mail: clamarchese@hotmail.com, E-mail: rosecchi@yahoo.com.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Geologia. Lab. de Analise de Minerais e Rochas

2011-09-15

The porosity contained in rocks is object of study by geoscientists due to the various genetic implications of these features. However, what have been motivating the search for new analytical techniques to study pores are the petrophysical analyses. The experimental techniques for porosity analysis, such as mercury or gas injection, allow a quantitative approach, but do not allow the visualization of the porous framework. Petrographic analysis by optical microscopy allows the visualization and quantification of intergranular pores, but it is restricted to the two-dimensional space and quantifications are less representative. Technological advances in X-ray computed microtomography (micro-CT) allowed three-dimensional analysis of pore geometry in microscale, in addition to automated volume measurements. The analyses of marble, quartzite, sandstone and dolomite breccia represented in this work and performed under the Project Falhas/ PETROBRAS/UFPR, show the shape, size, connectivity, tortuosity, pore volume and distribution in these rocks, demonstrating the differences in the rocks' porous frameworks. The integration of micro-CT to petrography allows the identification of mineral phases with attenuation of contrasting X-rays, placing the incidence of porosity in the mineralogical context in three dimensions, in addition to the contribution to the consistency of the method. Although the resolution is limited in the X-ray microtomography that was used (the Skyscan model 1172), which does not reach the smallest pore size of some rocks, the integration of both techniques provides new information, of extreme importance for the research about micro-features related to the pores in rocks, helping in genetic interpretations and significantly contributing for the analyses of reservoirs. (author)

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

DEFF Research Database (Denmark)

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

2005-01-01

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

Characterization of low density carbon foams by x-ray computed tomography (CT) and ion microtomography (IMF)

International Nuclear Information System (INIS)

Moddeman, W.E.; Kramer, D.P.; Firsich, D.W.; Trainer, P.D.; Yancy, R.N.; Weirup, D.L.; Logan, C.M.; Pontau, A.E.; Antolak, A.J.; Morse, D.H.

1990-01-01

Two NDT techniques were used to characterize low-density, microcellular, carbon foams fabricated from a salt replica process. In this paper the two techniques are x-ray computed tomography (CT) and ion microtomography (IMT); data are presented on carbon foams that contain high-density regions. The data show that densities which differ by 3 ) materials. The data reveal that the carbon foams produced by this replica process have small density variations; the density being ∼30% greater at the outer edges than when compared to the interior of the foam. In addition, the density gradient is found to be rather sharp, that is the density drops-off rapidly from the outer edges to a uniform one in the interior of the foam. This edge build-up in carbon density was explained in terms of polymer concentrating on the foam exterior during drying which immediately followed a polymer infusion processing step. Supporting analytical data from other techniques show the foam material to be >88.8% carbon

Micromanipulation and pick-up system for X-Ray diffraction characterization of micrometer-sized single particles

International Nuclear Information System (INIS)

Takeichi, Y; Inami, N; Saito, K; Otori, H; Sagayama, R; Kumai, R; Ono, K; Ueno, T

2014-01-01

We describe a micromanipulation and pick-up system for preparing a micrometer-sized single particle for X-ray diffraction characterization. Combining a microgripper based on microelectromechanical systems, piezo-motor-driven linear stages, and a gamepad, the system provides precise and intuitive handling of the object. Single-crystal X-ray diffraction measurements of Sm-Fe-N permanent magnet were performed using this system. We also describe a method to distinguish crystallographically homogeneous particles found in powder-form samples.

The structural analysis of zinc borate glass by laboratory EXAFS and X-ray diffraction measurements

International Nuclear Information System (INIS)

Kajinami, Akihiko; Harada, Yasushi; Inoue, Shinsuke; Deki, Shigehito; Umesaki, Norimasa

1999-01-01

The structure of zinc borate glass has been investigated by laboratory EXAFS and X-ray diffraction measurement as preliminary investigations for the detailed study in SPring-8. The zinc borate glass was prepared in the range from 40 to 65 mol% of zinc oxide content. The X-ray diffraction was measured by horizontal θ-θ goniometer with 60 kV and 300 mA output of Mo target. The EXAFS of zinc borate glass was measured by laboratory EXAFS system with 20 kV, 100 mA output of Mo target for the K absorption edge of zinc atom. From the X-ray diffraction and the EXAFS measurements, it is found that the zinc ion is surrounded by four oxygen atoms and formed a tetrahedral structure whose (Zn-O) distance is about 2 A and that the structure is unchanged with the zinc oxide content. The diffraction data show that the neighboring structure of boron atom transforms from BO 4 tetrahedra to BO 3 tetragonal planar structure with increasing of the zinc oxide content. (author)

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.)

A study of the reactivity of elemental Cr/Se/Te thin multilayers using X-ray reflectometry, in situ X-ray diffraction and X-ray absorption spectroscopy

International Nuclear Information System (INIS)

Behrens, Malte; Tomforde, Jan; May, Enno; Kiebach, Ragnar; Bensch, Wolfgang; Haeussler, Dietrich; Jaeger, Wolfgang

2006-01-01

The reactivity of [Cr/Se/Te] multilayers under annealing was investigated using X-ray reflectometry, in situ X-ray diffraction, X-ray absorption fine structure (XAFS) measurements and transmission electron microscopy. For all samples, interdiffusion was complete at temperatures between 100 and 300 deg. C, depending on the repeating tri-layer thickness. A crystalline phase nucleated approximately 20 deg. C above the temperature where interdiffusion was finished. The first crystalline phase in a binary Cr/Te sample was layered CrTe 3 nucleating at 230 deg. C. In ternary samples (Se:Te=0.6-1.2), the low-temperature nucleation of such a layered CrQ 3 (Q=Se, Te) phase is suppressed and instead the phase Cr 2 Q 3 nucleates first. Interestingly, this phase decomposes around 500 deg. C into layered CrQ 3 . In contrast, binary Cr/Se samples form stable amorphous alloys after interdiffusion and Cr 3 Se 4 nucleates around 500 deg. C as the only crystalline phase. Evaluation of the XAFS data of annealed samples yield Se-Cr distances of 2.568(1) and 2.552(1) A for Cr 2 Q 3 and CrQ 3 , respectively. In the latter sample, higher coordination shells around Se are seen accounting for the Se-Te contacts in the structure. - Graphical abstract: The first step of the reaction of elemental Cr/Te/Se-multilayers is the interdiffusion of the elements as evidenced by the decay of the modulation peaks in the low-angle region of the X-ray diffraction patterns. The subsequent growth of Bragg peaks at higher scattering angles indicates crystallization of chromium chalcogenide Cr 2 Te 3- x Se x

X-ray diffraction, Raman and photoacoustic studies of InSb nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Ersching, K., E-mail: kleb85@hotmail.com [Departamento de Fisica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Campos, C.E.M.; Lima, J.C. de; Grandi, T.A. [Departamento de Fisica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Souza, S.M. [Departamento de Engenharia Mecanica, Universidade Federal de Santa Catarina, Campus Universitario Trindade, 88040-900 Florianopolis, Santa Catarina (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, 13 565-905 Sao Carlos, SP (Brazil)

2010-08-01

Zinc blend InSb nanocrystals were generated by mechanical alloying and X-ray diffraction, Raman spectroscopy and photoacoustic absorption spectroscopy techniques were used to study its structural, optical and thermal properties. Annealed nanocrystals were also studied. Residual amorphous and minority crystalline (Sb and In{sub 2}O{sub 3}) phases were also observed for mechanical alloyed and thermal annealed samples, respectively. The structural parameters, phase fractions, average crystallite sizes and microstrains of all crystalline phases found in the samples were obtained from Rietveld analyses of their X-ray diffraction patterns. Raman results for both as-milled and annealed samples show the Raman active LO and TO modes of the zinc blend InSb phase and Sb-rich regions. The photoacoustic results of both samples were satisfactorily explained by thermal bending heat transfer mechanism and an increase on effective thermal diffusivity coefficient was observed after annealing.

Sample cell for in-field X-ray diffraction experiments

Directory of Open Access Journals (Sweden)

Viktor Höglin

2015-01-01

Full Text Available A sample cell making it possible to perform synchrotron radiation X-ray powder diffraction experiments in a magnetic field of 0.35 T has been constructed. The device is an add-on to an existing sample cell and contains a strong permanent magnet of NdFeB-type. Experiments have shown that the setup is working satisfactory making it possible to perform in-field measurements.

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...

Quantitative analysis of crystalline pharmaceuticals in tablets by pattern-fitting procedure using X-ray diffraction pattern.

Science.gov (United States)

Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

2010-10-15

A pattern-fitting procedure using an X-ray diffraction pattern was applied to the quantitative analysis of binary system of crystalline pharmaceuticals in tablets. Orthorhombic crystals of isoniazid (INH) and mannitol (MAN) were used for the analysis. Tablets were prepared under various compression pressures using a direct compression method with various compositions of INH and MAN. Assuming that X-ray diffraction pattern of INH-MAN system consists of diffraction intensities from respective crystals, observed diffraction intensities were fitted to analytic expression based on X-ray diffraction theory and separated into two intensities from INH and MAN crystals by a nonlinear least-squares procedure. After separation, the contents of INH were determined by using the optimized normalization constants for INH and MAN. The correction parameter including all the factors that are beyond experimental control was required for quantitative analysis without calibration curve. The pattern-fitting procedure made it possible to determine crystalline phases in the range of 10-90% (w/w) of the INH contents. Further, certain characteristics of the crystals in the tablets, such as the preferred orientation, size of crystallite, and lattice disorder were determined simultaneously. This method can be adopted to analyze compounds whose crystal structures are known. It is a potentially powerful tool for the quantitative phase analysis and characterization of crystals in tablets and powders using X-ray diffraction patterns. Copyright 2010 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-08-27

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

Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

International Nuclear Information System (INIS)

Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

2013-01-01

Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

Heterogeneous vesiculation of 2011 El Hierro xeno-pumice revealed by X-ray computed microtomography

Science.gov (United States)

Berg, S. E.; Troll, V. R.; Deegan, F. M.; Burchardt, S.; Krumbholz, M.; Mancini, L.; Polacci, M.; Carracedo, J. C.; Soler, V.; Arzilli, F.; Brun, F.

2016-12-01

During the first week of the 2011 El Hierro submarine eruption, abundant light-coloured pumiceous, high-silica volcanic bombs coated in dark basanite were found floating on the sea. The composition of the light-coloured frothy material (`xeno-pumice') is akin to that of sedimentary rocks from the region, but the textures resemble felsic magmatic pumice, leaving their exact mode of formation unclear. To help decipher their origin, we investigated representative El Hierro xeno-pumice samples using X-ray computed microtomography for their internal vesicle shapes, volumes, and bulk porosity, as well as for the spatial arrangement and size distributions of vesicles in three dimensions (3D). We find a wide range of vesicle morphologies, which are especially variable around small fragments of rock contained in the xeno-pumice samples. Notably, these rock fragments are almost exclusively of sedimentary origin, and we therefore interpret them as relicts an the original sedimentary ocean crust protolith(s). The irregular vesiculation textures observed probably resulted from pulsatory release of volatiles from multiple sources during xeno-pumice formation, most likely by successive release of pore water and mineral water during incremental heating and decompression of the sedimentary protoliths.

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

Catalysts at work: From integral to spatially resolved X-ray absorption spectroscopy

DEFF Research Database (Denmark)

Grunwaldt, Jan-Dierk; Kimmerle, B.; Baiker, A.

2009-01-01

available techniques, X-ray absorption spectroscopy (XAS) is a well-suited tool for this purpose as the different selected examples highlight. Two different techniques, scanning and full-field X-ray microscopy/tomography, are described and compared. At first, the tomographic structure of impregnated alumina...... pellets is presented using full-field transmission microtomography and compared to the results obtained with a scanning X-ray microbeam technique to analyse the catalyst bed inside a catalytic quartz glass reactor. On the other hand, by using XAS in scanning microtomography, the structure...... metal-based catalysts. In order to obtain spectroscopic information on the spatial variation of the oxidation state of the catalyst inside the reactor XAS spectra were recorded by scanning with a micro-focussed beam along the catalyst bed. Alternatively, full-field transmission imaging was used...

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

International Nuclear Information System (INIS)

Yoshimura, Jun-ichi

2015-01-01

A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory, where the effect of the Pendellösung intensity oscillation on the moiré pattern is explained in detail. A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general

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.

Quasi-kinoform type multilayer zone plate with high diffraction efficiency for high-energy X-rays

International Nuclear Information System (INIS)

Tamura, S; Yasumoto, M; Kamijo, N; Uesugi, K; Takeuchi, A; Terada, Y; Suzuki, Y

2009-01-01

Fresnel zone plate (FZP) with high diffraction efficiency leads to high performance X-ray microscopy with the reduction of the radiation damage to biological specimens. In order to attain high diffraction efficiency in high energy X-ray region, we have developed multilevel-type (6-step) multilayer FZPs with the diameter of 70 micron. The efficiencies of two FZPs were evaluated at the BL20XU beamline of SPring-8. For one FZP, the peak efficiency for the 1st-order diffraction of 51% has been obtained at 70 keV. The efficiencies higher than 40% have been achieved in the wide energy range of 70-90 keV. That for the 2nd-order diffraction of 46% has been obtained at 37.5 keV.

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.

Quantification of rutile in anatase by X-ray diffraction

International Nuclear Information System (INIS)

Chavez R, A.

2001-01-01

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

X-Ray diffraction studies of silicon implanted with high energy ions

International Nuclear Information System (INIS)

Wieteska, K.; Wierzchowski, W.; Graeff, W.

1998-01-01

The character of lattice deformation in silicon implanted with high energy alpha-particles and protons was studied using a number of X-ray methods. The experiments included double-crystal spectrometer method as well as single crystal section and projection topography realised both with conventional and synchrotron X-ray sources. All observed diffraction patterns were reasonably explainable assuming the lattice parameter distribution proportional to the vacancy-interstitial distribution coming from the Biersack-ziegler theory. The theoretical rocking curves and distribution in back-reflection double-crystal and section topographs well corresponding to the experimental results were calculated using numerical integration of the takagi-taupin equations

Quantitative strain analysis of surfaces and interfaces using extremely asymmetric x-ray diffraction

International Nuclear Information System (INIS)

Akimoto, Koichi; Emoto, Takashi

2010-01-01

Strain can reduce carrier mobility and the reliability of electronic devices and affect the growth mode of thin films and the stability of nanometer-scale crystals. To control lattice strain, a technique for measuring the minute lattice strain at surfaces and interfaces is needed. Recently, an extremely asymmetric x-ray diffraction method has been developed for this purpose. By employing Darwin's dynamical x-ray diffraction theory, quantitative evaluation of strain at surfaces and interfaces becomes possible. In this paper, we review our quantitative strain analysis studies on native SiO 2 /Si interfaces, reconstructed Si surfaces, Ni/Si(111)-H interfaces, sputtered III-V compound semiconductor surfaces, high-k/Si interfaces, and Au ion-implanted Si. (topical review)