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

X-ray diffraction microtomography using synchrotron radiation

CERN Document Server

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

2001-01-01

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

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

International Nuclear Information System (INIS)

Balyan, M.K.

2014-01-01

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

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

Bismuth on copper (110): analysis of the c(2x2) and p(4x1) structures by surface x-ray diffraction

DEFF Research Database (Denmark)

Lottermoser, L.; Buslaps, T.; Johnson, R.L.

1997-01-01

Surface X-ray diffraction has been used to analyze the atomic structures of the Cu(110)-c(2 x 2)-Bi and Cu(110)-p(4 x 1)-Bi reconstructions with submonolayer coverages. A quasi-hexagonal c(2 x 2) adlayer structure is formed when half a monolayer of bismuth is deposited; the coverage corresponds...... to 1.08 x 10(-15) atoms cm(-2). There is one Bi atom per c(2 x 2) surface unit cell, and the nearest-neighbor distance on the planar overlayer was found to be 4.43 Angstrom. In the case of the p(4 x 1) reconstruction formed at a coverage of 0.75 monolayers, both the in-plane and out-of-plane data...

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 ...

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)

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)

Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

International Nuclear Information System (INIS)

Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

2016-01-01

Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in Roman

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)

Evaluated Plan Stress Of Weld In Pressure Tube Using X Ray Diffraction Technique

International Nuclear Information System (INIS)

Phan Trong Phuc; Nguyen Duc Thanh; Luu Anh Tuyen

2011-01-01

X ray diffraction is a fundamental technique measuring stress, this technique has determined crystal strain in materials, from that determined stress in materials. This paper presents study of evaluating plane stress of weld in pressure tube, using modern XRD apparatus: X Pert Pro. (author)

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

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)

Diffraction Plane Dependence of Micro Residual Stresses in Uniaxially Extended Carbon Steels

Directory of Open Access Journals (Sweden)

T. Hanabusa

2010-12-01

Full Text Available In the stress measurement using X-ray or neutron diffraction, an elastic anisotropy as well as a plastic anisotropy of crystal must be carefully considered. In the X-ray and neutron diffraction stress measurement for polycrystalline materials, a particular {hkl} plane is used in measuring lattice strains. The dependence of an X-ray elastic constant on a diffraction plane is a typical example caused by an elastic anisotropy of the crystal. The yield strength and the work hardening rate of a single crystal depend on a crystallographic direction of the crystal. The difference in the yield strength and the work hardening rate relating to the crystallographic direction develops different residual stresses measured on each {hkl} diffraction after plastic deformation of a polycrystalline material. The present paper describes the result of the neutron stress measurement on uniaxially extended low and middle carbon steels. A tri-axial residual stress state developed in the extended specimens was measured on different kind of {hkl} diffraction plane. The measurement on the {110}, {200} and {211} diffraction showed that residual stresses increased with increasing the plastic elongation and the residual stresses on {110} were compressive, {200} were tensile and those on {211} were the middle of the former two planes.

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

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 ...

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-05-06

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

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

International Nuclear Information System (INIS)

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

1993-09-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-04-20

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

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

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

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

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

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

Simulating X-ray diffraction of textured films

DEFF Research Database (Denmark)

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

2008-01-01

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

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

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

Effects of out-of-plane disorder on the superconductivity of Bi{sub 2}Sr{sub 2-x}La{sub x}CuO{sub 6+{delta}}

Energy Technology Data Exchange (ETDEWEB)

Roehler, Juergen; Trabant, Christoph; Frielingsdorf, Johanna; Djemour, Rabia [Universitaet Koeln, 50937 Koeln (Germany); Martovitsky, Victor [Lebedev-Institute, 119991 Moscow (Russian Federation); Dudy, Lenart; Dwelk, Helmut; Krapf, Alica [Humboldt Universitaet Berlin, 12489 Berlin (Germany)

2008-07-01

The effects of out-of-plane substitutional order/disorder on cuprate superconductivity remains to a large extent an unresolved issue. We have investigated the connection between superconductivity and the lattice effects arising from the heterovalent doping of Bi{sub 2}Sr{sub 2-x}La{sub x}CuO{sub 6+{delta}}, x = 0.8-0.1. Decreasing lanthanum content tunes the compound through the entire underdoped and overdoped regimes. Cu-K and La- K EXAFS served as local structural probes, and single crystal X-ray diffraction for the determination of the basic unit cell, and the symmetry of the supercell. The oxygen atoms in the CuO{sub 2} planes were found significantly disordered, dependent on doping, and to exhibit minimum disorder around x{sub opt}=0.33. But the degree of substitutional disorder in the out-of-plane La environment turned out independent on the concentration of the La dopants, the superstructure symmetry, and the crystal growth parameters, whereas T{sub c} depends sensitively on them. No evidence was found for possible concentration dependent site changes of the La dopant from the nominal Sr to the Bi sites. We discuss the probably crucial role of the interstitial oxygen atoms for the superconducting properties of the Bi{sub 2}Sr{sub 2-x}La{sub x}CuO{sub 6+{delta}} system.

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.

High pressure Raman and single crystal X-ray diffraction of the alkali/calcium carbonate, shortite

Science.gov (United States)

Williams, Q. C.; Vennari, C.; O'Bannon, E. F., III

2015-12-01

Raman and synchrotron-based single crystal x-ray diffraction data have been collected on shortite (Na2Ca2(CO3)3) up to 10 GPa at 300 K. Shortite is of geological importance due to its presence in the ground-mass of kimberlites, and the alkaline-/carbon-rich character of kimberlitic eruptions. This investigation focuses on shortite's high pressure behavior and is relevant to the behavior of alkali-carbonate systems within Earth's upper mantle. X-ray data demonstrate that shortite's symmetry remains stable at high pressures—retaining orthorhombic C crystal system (Amm2) up to 10 GPa; diffraction data show a 12% volume decrease from room pressure, and a bulk modulus of 71.0(3) GPa. These also demonstrate that the c-axis is twice as compressible as the a- and b-axes. This anisotropic compression is likely due to the orientation of the relatively stiff carbonate groups, a third of which are oriented close to the plane of the a- and b-axes, c axis compression primarily involves the compaction of the 9-fold coordinate sodium and calcium polyhedral. The two distinct carbonate sites within the unit cell give rise to two Raman symmetric stretching modes of the symmetric stretch; the carbonate group stretching vibration which is close to in plane with the a- and b-axes shifts at 3.75 cm-1/GPa as opposed to the carbonate groups which is closer to in plane with the b- and c-axes which shift at 4.25 cm-1/GPa. This furthers evidence for anisotropic compression observed using x-ray diffraction--as the carbonate in plane with the a- and b-axes is compressed, the strength of oxygen bonds along the c-axis with the cations increases, thus decreasing the pressure shift of the mode. The out of plane bending vibration shifts at -0.48 cm-1/GPa, indicating an enhanced interaction of the oxygens with the cations. The multiple in plane bending modes all shift positively, as do at the low frequency lattice modes, indicating that major changes in bonding do not occur up to 10 GPa. The data

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

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.)

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.)

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...

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-10-15

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

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.

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.

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

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...

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)

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....

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)

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)

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

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)

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

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.

In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

Energy Technology Data Exchange (ETDEWEB)

Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

2017-04-15

The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

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 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 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)

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.

Synchrotron X-ray diffraction investigations on strains in the oxide layer of an irradiated Zircaloy fuel cladding

Energy Technology Data Exchange (ETDEWEB)

Chollet, Mélanie, E-mail: melanie.chollet@psi.ch [Paul Scherrer Institute, NES, 5232 Villigen (Switzerland); Valance, Stéphane; Abolhassani, Sousan; Stein, Gene [Paul Scherrer Institute, NES, 5232 Villigen (Switzerland); Grolimund, Daniel [Paul Scherrer Institute, SLS, 5232 Villigen (Switzerland); Martin, Matthias; Bertsch, Johannes [Paul Scherrer Institute, NES, 5232 Villigen (Switzerland)

2017-05-15

For the first time the microstructure of the oxide layer of a Zircaloy-2 cladding after 9 cycles of irradiation in a boiling water reactor has been analyzed with synchrotron micro-X-ray diffraction. Crystallographic strains of the monoclinic and to some extent of the tetragonal ZrO{sub 2} are depicted through the thick oxide layer. Thin layers of sub-oxide at the oxide-metal interface as found for autoclave-tested samples and described in the literature, have not been observed in this material maybe resulting from irradiation damage. Shifts of selected diffraction peaks of the monoclinic oxide show that the uniform strain produced during oxidation is orientated in the lattice and displays variations along the oxide layer. Diffraction peaks and their shifts from families of diffracting planes could be translated into a virtual tensor. This virtual tensor exhibits changes through the oxide layer passing by tensile or compressive components. - Highlights: •A Zircaloy-2 cladding irradiated 9 cycles was investigated thanks to synchrotron X-ray diffraction. •Microstructure and uniform strain through the oxide layer is revealed. •The m-ZrO{sub 2} uniform strain is oriented presenting compression along the (−111) plane. •Virtual tensor is built based on reflecting planes of families of grains. •Tensor components vary from tensile to compressive along the oxide layer.

Synchrotron X-ray diffraction investigations on strains in the oxide layer of an irradiated Zircaloy fuel cladding

International Nuclear Information System (INIS)

Chollet, Mélanie; Valance, Stéphane; Abolhassani, Sousan; Stein, Gene; Grolimund, Daniel; Martin, Matthias; Bertsch, Johannes

2017-01-01

For the first time the microstructure of the oxide layer of a Zircaloy-2 cladding after 9 cycles of irradiation in a boiling water reactor has been analyzed with synchrotron micro-X-ray diffraction. Crystallographic strains of the monoclinic and to some extent of the tetragonal ZrO 2 are depicted through the thick oxide layer. Thin layers of sub-oxide at the oxide-metal interface as found for autoclave-tested samples and described in the literature, have not been observed in this material maybe resulting from irradiation damage. Shifts of selected diffraction peaks of the monoclinic oxide show that the uniform strain produced during oxidation is orientated in the lattice and displays variations along the oxide layer. Diffraction peaks and their shifts from families of diffracting planes could be translated into a virtual tensor. This virtual tensor exhibits changes through the oxide layer passing by tensile or compressive components. - Highlights: •A Zircaloy-2 cladding irradiated 9 cycles was investigated thanks to synchrotron X-ray diffraction. •Microstructure and uniform strain through the oxide layer is revealed. •The m-ZrO 2 uniform strain is oriented presenting compression along the (−111) plane. •Virtual tensor is built based on reflecting planes of families of grains. •Tensor components vary from tensile to compressive along the oxide layer.

X-ray diffraction study of KTP (KTiOPO4) crystals under a static electric field

International Nuclear Information System (INIS)

Sebastian, M.T.; Klapper, H.; Bolt, R.J.

1992-01-01

X-ray diffraction studies are made on ion-conducting potassium titanyl phosphate (KTP) crystals with in situ DC electric field along different crystallographic directions. The X-ray rocking curves recorded with an electric field along the polar b axis (which is the direction of ion conduction) show a strong enhancement of the 040 reflection intensity (reflecting planes normal to the b axis) whereas the h0l reflections (reflecting planes parallel to the polar axis) do not show any intensity change. For an electric field normal to the polar axis no intensity change, either in 040 or in h0l reflections occurs. This observation is supplemented by X-ray topography. The 040 X-ray topographs recorded with in situ electric field along b exhibit strong extinction contrast in the form of striations parallel to the polar (ion-conduction) axis. The 040 intensity increase and the striation contrast are attributed to lattice deformation by the space-charge polarization due to the movement of the K + ions under the influence of the electric field. (orig.)

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

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)

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

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....

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...

X-ray diffraction study of A- plane non-polar InN epilayer grown by MOCVD

Science.gov (United States)

Moret, Matthieu; Briot, Olivier; Gil, Bernard

2015-03-01

Strong polarisation-induced electric fields in C-plane oriented nitrides semiconductor layers reduce the performance of devices. Eliminating the polarization fields can be achieved by growing nitrides along non polar direction. We have grown non polar A-plane oriented InN on R-plane (1‾102) nitridated sapphire substrate by MOCVD. We have studied the structural anisotropy observed in these layers by analyzing High Resolution XRay Diffraction rocking curve (RC) experiments as a function of the in-plane beam orientation. A-plane InN epilayer have a unique epitaxial relationship on R-Plane sapphire and show a strong structural anisotropy. Full width at half maximum (FWHM) of the InN(11‾20) XRD RC values are contained between 44 and 81 Arcmin. FWHM is smaller when the diffraction occurs along the [0001] and the largest FWHM values, of the (11‾20) RC, are obtained when the diffraction occurs along the [1‾100] in-plane direction. Atomic Force Microscopy imaging revealed morphologies with well organized crystallites. The grains are structured along a unique crystallographic orientation of InN, leading to larger domains in this direction. This structural anisotropy can be, in first approximation, attributed to the difference in the domain sizes observed. XRD reciprocal space mappings (RSM) were performed in asymmetrical configuration on (13‾40) and (2‾202) diffraction plane. RSM are measured with a beam orientation corresponding to a maximal and a minimal width of the (11‾20) Rocking curves, respectively. A simple theoretical model is exposed to interpret the RSM. We concluded that the dominant contribution to the anisotropy is due to the scattering coherence length anisotropy present in our samples.

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.

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...

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

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)

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

International Nuclear Information System (INIS)

Freyer, Benjamin

2013-01-01

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

Measurement of 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)

Determination of lattice parameters, strain state and composition in semipolar III-nitrides using high resolution X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Frentrup, Martin, E-mail: frentrup@physik.tu-berlin.de; Wernicke, Tim; Stellmach, Joachim; Kneissl, Michael [Institute of Solid State Physics, Technische Universität Berlin, Hardenbergstr. 36, 10623 Berlin (Germany); Hatui, Nirupam; Bhattacharya, Arnab [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Homi Bhabha Road, Mumbai 400005 (India)

2013-12-07

In group-III-nitride heterostructures with semipolar or nonpolar crystal orientation, anisotropic lattice and thermal mismatch with the buffer or substrate lead to a complex distortion of the unit cells, e.g., by shearing of the lattice. This makes an accurate determination of lattice parameters, composition, and strain state under assumption of the hexagonal symmetry impossible. In this work, we present a procedure to accurately determine the lattice constants, strain state, and composition of semipolar heterostructures using high resolution X-ray diffraction. An analysis of the unit cell distortion shows that four independent lattice parameters are sufficient to describe this distortion. Assuming only small deviations from an ideal hexagonal structure, a linear expression for the interplanar distances d{sub hkl} is derived. It is used to determine the lattice parameters from high resolution X-ray diffraction 2ϑ-ω-scans of multiple on- and off-axis reflections via a weighted least-square fit. The strain and composition of ternary alloys are then evaluated by transforming the elastic parameters (using Hooke's law) from the natural crystal-fixed coordinate system to a layer-based system, given by the in-plane directions and the growth direction. We illustrate our procedure taking an example of (112{sup ¯}2) Al{sub κ}Ga{sub 1−κ}N epilayers with Al-contents over the entire composition range. We separately identify the in-plane and out-of-plane strains and discuss origins for the observed anisotropy.

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

Ultrafast lattice dynamics in photoexcited nanostructures. Femtosecond X-ray diffraction with optimized evaluation schemes

International Nuclear Information System (INIS)

Schick, Daniel

2013-01-01

resulting X-ray diffraction response in photoexcited one-dimensional crystalline structures was developed in this thesis work. With the powerful experimental and theoretical framework at hand, I have studied the excitation and propagation of coherent phonons in more complex material systems. In particular, I have revealed strongly localized charge carriers after above-bandgap femtosecond photoexcitation of the prototypical multiferroic BiFeO 3 , which are the origin of a quasi-instantaneous and spatially inhomogeneous stress that drives coherent phonons in a thin film of the multiferroic. In a structurally imperfect thin film of the ferroelectric Pb(Zr 0.2 Ti 0.8 )O 3 , the ultrafast reciprocal-space mapping technique was applied to follow a purely strain-induced change of mosaicity on a picosecond time scale. These results point to a strong coupling of in- and out-of-plane atomic motion exclusively mediated by structural defects.

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

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

Science.gov (United States)

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

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

Directory of Open Access Journals (Sweden)

Hongjia Zhang

2018-03-01

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

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...

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

International Nuclear Information System (INIS)

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

1981-10-01

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

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

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

DEFF Research Database (Denmark)

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

1996-01-01

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

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

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.

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

Energy Technology Data Exchange (ETDEWEB)

Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-15

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

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.

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)

Calculated efficiencies of three-material low stress coatings for diffractive x-ray transmission optics

International Nuclear Information System (INIS)

Kubec, Adam; Braun, Stefan; Gawlitza, Peter; Menzel, Maik; Leson, Andreas

2016-01-01

Diffractive X-ray optical elements made by thin film coating techniques such as multilayer Laue lenses (MLL) and multilayer zone plates (MZP) are promising approaches to achieve resolutions in hard X-ray microscopy applications of less than 10 nm. The challenge is to make a lens with a large numerical aperture on the one hand and a decent working distance on the other hand. One of the limiting factors with the coated structures is the internal stress in the films, which can lead to significant bending of the substrate and various types of unwanted diffraction effects. Several approaches have been discussed to overcome this challenge. One of these is a three-material combination such as Mo/MoSi_2/Si, where four single layers per period are deposited. Mo and Si represent the absorber and spacer in this case while MoSi_2 forms a diffusion barrier; in addition the thicknesses of absorber and spacer are chosen to minimize residual stress of the overall coating. Here the diffraction efficiency as well as the profile of the beam in the focal plane are discussed in order to find a tradeoff between lowest residual stress and best diffraction properties.

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.

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)

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.

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)

Inspection of single CdSe nanowires by use of micro-focused X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Kurtulus, Oezguel [Dogus University, Istanbul (Turkey); Li, Zhen [University of Queensland, Brisbane (Australia); Arezki, Bahia; Biermanns, Andreas; Pietsch, Ullrich [University of Siegen (Germany)

2010-07-01

The morphology of CdSe nanowires (NW) can easily be controlled by various growth methods. In this study, CdSe NWs are prepared by solution-liquid-solid (SLS) approach providing needle-shaped wires of about 60nm in diameter and several microns in length. To make X-ray single NW inspection possible, the NWs were dispersed in toluene and hexadecylamine, homogenized by centrifugation and finally spin-coated on silicon substrate. SEM images revealed that the NWs are randomly oriented with length axis parallel to the substrate. However, at selected areas, the distance between neighboured NWs is in the order of one micron. These samples were investigated by X-ray diffraction using a 300 nm x 600 nm micro-focus at beamline ID1 of ESRF. Diffraction from 110W/2-20ZB basal plane was selected for single nanowire inspection. In order to measure various single objects subsequently, the sample was laterally scanned through the beam keeping the diffraction angle fixed. It was observed that the individual NWs differ slightly in peak position and peak width. From powder diffraction, it is known that NWs consist of an admixture of a wurtzite (W) and zinc-blende (ZB) structure units and the coherent illumination of sample by the micro-focus enables to visualize these zinc-blende and wurzite units separated by stacking faults.

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

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

Evaluation of material properties of SiC particle reinforced aluminum alloy composite using neutron and X-ray diffraction

International Nuclear Information System (INIS)

Akiniwa, Yoshiaki; Machiya, Shutaro; Kimura, Hidehiko; Tanaka, Keisuke; Minakawa, Nobuaki; Morii, Yukio; Kamiyama, Takashi

2006-01-01

The phase stresses under loading in a monolithic aluminum alloy and an aluminum alloy reinforced with silicon carbide particles were measured by the neutron diffraction method. Under uniaxial loading, the longitudinal and transverse strains in each constituent phase were measured. The diffraction elastic constants for each diffraction plane were investigated as a function of the diffraction intensity by TOF. Single peak analysis was carried out for each diffraction profile. The measured results were compared with the theoretical micromechanical models such as the self-consistent and Mori-Tanaka method using the Eshelby theory (MTE). The accuracy of the elastic constant strongly depends on the diffraction intensity. In order to confirm the rule of mixture, the phase stress was measured by the X-ray method. The macrostress calculated by the rule of mixture agreed very well with the applied stress. Finally, fatigue damage was evaluated by the neutron method. The change of the full width at half maximum in the aluminum phase during fatigue is small. On the other hand, the value in the SiC phase increased steeply just before fracture

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-03-15

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

Magnetic hysteresis of an artificial square ice studied by in-plane Bragg x-ray resonant magnetic scattering

Directory of Open Access Journals (Sweden)

J. P. Morgan

2012-06-01

Full Text Available We report X-ray resonant magnetic scattering studies of a Permalloy artificial square ice nanomagnet array, focussing on the field-driven evolution of the sum Σ and difference Δ signals of left and right handed circularly polarized synchrotron X-rays at different lateral positions in reciprocal space Qx. We used X-rays tuned to the Fe L3 resonance energy, with the scattering plane aligned along a principal symmetry axis of the array. Details of the specular Δ hysteresis curve are discussed, following the system magnetization from an initial demagnetized state. The periodic structure gives rise to distinct peaks at in-plane reciprocal Bragg positions, as shown by fitting Σ(Qx to a model based on a simple unit cell structure. Diffraction order-dependent hysteresis in Δ is observed, indicative of the reordering of magnetization on the system's two interpenetrating sublattices, which markedly deviates from an ideal Ising picture under strong applied fields.

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

Sagittal x-ray beam deviation at asymmetric inclined diffractors

Czech Academy of Sciences Publication Activity Database

Korytár, D.; Hrdý, Jaromír; Artemiev, Nikolai; Ferrari, C.; Freund, A.

2001-01-01

Roč. 8, - (2001), s. 1136-1139 ISSN 0909-0495 R&D Projects: GA MŠk OK 305; GA MPO PZ-CH/22 Institutional research plan: CEZ:AV0Z1010914 Keywords : x-ray optics * Si(111) W/grooved crystals * inclined diffraction * out-of-diffraction-plane beams * sagittal focusing Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.519, year: 2001

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…

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.

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 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

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

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

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.

Residual stress measurements by X-ray and neutron diffractions in heat-treated SiCw/A2014 composites

International Nuclear Information System (INIS)

Ohnuki, Takahisa; Fujita, Motoo; Tomota, Yo; Ono, Masayoshi

1998-01-01

Residual stresses due to various heat treatments in a 22 volume percent SiC whisker/A2014 metal matrix composite (MMC) were measured by using X-ray and neutron diffractions. Micro residual stresses generated from the differences in thermal expansion coefficients of the constituents and macro residual stresses associated with different cooling rates in the outer and inner regions of an MMC specimen must be distinguished in X-ray stress measurements. The conventional sin 2 ψ method under an assumption of plane stress condition has been found not to be applicable to the present MMC, because interactions among whiskers in the X-ray penetrating area yields σ 33 where the x 3 -axis is normal with respect to specimen's surface. An average value of σ 33 can be measured by X-ray diffraction technique, but does not seem enough to evaluate micro residual stresses. It is found that neutron diffraction is the most powerful method to measure micro residual stresses in the constituents. Elastic residual strains obtained by neutron diffraction in solution treated or T6 heat treated samples show good agreements with predictions calculated by using Eshelby inclusion theory coupled with the Mori-Tanaka mean field concept, indicating that the influence of stress relaxation is negligible. In addition, internal stresses relaxations during holding at room temperature, slow cooling from solution treatment temperature, or subzero cooling are discussed. (author)

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/

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...

Anisotropically biaxial strain in non-polar (112-0) plane In x Ga1-x N/GaN layers investigated by X-ray reciprocal space mapping.

Science.gov (United States)

Zhao, Guijuan; Li, Huijie; Wang, Lianshan; Meng, Yulin; Ji, Zesheng; Li, Fangzheng; Wei, Hongyuan; Yang, Shaoyan; Wang, Zhanguo

2017-07-03

In this study, the indium composition x as well as the anisotropically biaxial strain in non-polar a-plane In x Ga 1-x N on GaN is studied by X-ray diffraction (XRD) analysis. In accordance with XRD reciprocal lattice space mapping, with increasing indium composition, the maximum of the In x Ga 1-x N reciprocal lattice points progressively shifts from a fully compressive strained to a fully relaxed position, then to reversed tensile strained. To fully understand the strain in the ternary alloy layers, it is helpful to grow high-quality device structures using a-plane nitrides. As the layer thickness increases, the strain of In x Ga 1-x N layer releases through surface roughening and the 3D growth-mode.

Texture of poled tetragonal PZT detected by synchrotron X-ray diffraction and micromechanics analysis

International Nuclear Information System (INIS)

Hall, D.A.; Steuwer, A.; Cherdhirunkorn, B.; Withers, P.J.; Mori, T.

2005-01-01

The texture and lattice elastic strain due to electrical poling of tetragonal PZT (lead zirconate titanate) ceramics have been measured using high energy synchrotron X-ray diffraction. It is shown that XRD peak intensity ratios associated with crystal planes of the form {002}, {112} and {202} exhibit a linear dependence on cos-bar 2 Ψ, where Ψ represents the orientation angle between the plane normal and the macroscopic poling axis. The observed dependence of texture and lattice strain on the grain orientation can be understood on the basis that the macroscopic strain due to poling is the average of the poling strains of all the individual grains

Fabrication of Transition Edge Sensor Microcalorimeters for X-Ray Focal Planes

Science.gov (United States)

Chervenak, James A.; Adams, Joseph S.; Audley, Heather; Bandler, Simon R.; Betancourt-Martinez, Gabriele; Eckart, Megan E.; Finkbeiner, Fred M.; Kelley, Richard L.; Kilbourne, Caroline; Lee, Sang Jun;

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.

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.

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

International Nuclear Information System (INIS)

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

1981-01-01

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

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

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.

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

Science.gov (United States)

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

2015-05-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Spalling stress in oxidized thermal barrier coatings evaluated by X-ray diffraction method

Energy Technology Data Exchange (ETDEWEB)

Suzuki, K. [Faculty of Education and Human Sciences, Niigata Univ., Niigata (Japan); Tanaka, K. [Dept. of Mechanical Engineering, Nagoya Univ., Furoh-cho, Chikusa-ku, Nagoya (Japan)

2005-07-01

The spallation of thermal barrier coatings (TBCs) is promoted by thermally grown oxide (TGO). To improve TBCs, it is very important to understand the influence of TGO on the spalling stress. In this study 'the TBCs were oxidized at 1373 K for four different periods: 0, 500,1000 and 2000 h. The distribution of the in-plane stress in oxidized TBCs, {sigma}{sub 1}, was obtained by repeating the X-ray stress measurement with low energy X-rays after successive removal of the surface layer. The distribution of the out-of-plane stress, {sigma}{sub 1} - {sigma}{sub 3}, was measured with hard synchrotron X-rays, because high energy X-rays have a large penetration depth. From the results by the low and high energy X-rays, the spalling stress in the oxidized TBCs, {sigma}{sub 3}, was evaluated. The evaluated value of the spalling stress for the oxidized TBC was a small tension beneath the surface, but steeply increased near the interface between the top and bond coating. This large tensile stress near the interface is responsible for the spalling of the top coating. (orig.)

Influence of preferred orientation of minerals in the mineralogical identification process by X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Silva, Amanda Luzia da; Oliveira, Arno H. de [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear; Fernandes, Maria Lourdes Souza, E-mail: lourdesfernandes@ufmg.b [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Inst. de GeoCiencias. Centro de Pesquisa Professor Manoel Teixeira da Costa

2011-07-01

The X-ray diffraction corresponds to one of the main techniques for characterization of microstructures in crystalline materials, widely used in the identification of minerals in samples of geological materials. Some minerals have a property called preferred orientation which corresponds to the orientation tendency of the crystals of ground minerals to orient themselves in certain directions according to a preferred crystallographic plane. This property affects the analysis by X-ray diffraction and this fact can generates erroneous results in the characterization. The purpose of this study is to identify the negative influence of the preferred orientation of a mineral in the generation of diffraction patterns obtained in the X-ray diffraction analysis. For this, a sample of muscovite, a mineral of mica group, was prepared by two different methods: the frontal method and the back loading method. In the analysis using the frontal method there was displacement of the XRD pattern in the abscissa axis, where it was observed changes in interplanar distance and angle 2{theta} values, which are essential information for characterization and identification of a mineral. In the analysis using the back loading method, the generated XRD pattern showed no displacement in the axis of abscissas and showed interplanar distance and angle 2{theta} values closer to the real values for the muscovite. The results showed that one can only make improvements to the process of sample preparation minimizing the effect of preferred orientation in the analysis. There is no need to change conditions of diffractometer measurements. (author)

Influence of preferred orientation of minerals in the mineralogical identification process by X-ray diffraction

International Nuclear Information System (INIS)

Silva, Amanda Luzia da; Oliveira, Arno H. de; Fernandes, Maria Lourdes Souza

2011-01-01

The X-ray diffraction corresponds to one of the main techniques for characterization of microstructures in crystalline materials, widely used in the identification of minerals in samples of geological materials. Some minerals have a property called preferred orientation which corresponds to the orientation tendency of the crystals of ground minerals to orient themselves in certain directions according to a preferred crystallographic plane. This property affects the analysis by X-ray diffraction and this fact can generates erroneous results in the characterization. The purpose of this study is to identify the negative influence of the preferred orientation of a mineral in the generation of diffraction patterns obtained in the X-ray diffraction analysis. For this, a sample of muscovite, a mineral of mica group, was prepared by two different methods: the frontal method and the back loading method. In the analysis using the frontal method there was displacement of the XRD pattern in the abscissa axis, where it was observed changes in interplanar distance and angle 2θ values, which are essential information for characterization and identification of a mineral. In the analysis using the back loading method, the generated XRD pattern showed no displacement in the axis of abscissas and showed interplanar distance and angle 2θ values closer to the real values for the muscovite. The results showed that one can only make improvements to the process of sample preparation minimizing the effect of preferred orientation in the analysis. There is no need to change conditions of diffractometer measurements. (author)

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

Space resolved x-ray diffraction measurements of the supercooled state of polymers

International Nuclear Information System (INIS)

Asano, Tsutomu; Yoshida, Shinya; Nishida, Akira; Mina, M.F.

2002-01-01

In order to measure an ordering process of polymers, the supercooled state near the crystallizing surface was observed by a space resolved X-ray diffraction method at Photon Factory (PF). Using temperature slope crystallization, low density polyethylene and even-number paraffins were examined during crystallization from the melt state. The results indicate that polyethylene shows a sharp b-axis orientation where the lamellar normal and crystalline c-axis are perpendicular to the temperature slope. The crystalline lamellae are well-developed with lamellar thickness of 180 A. The supercooled melt state just above the crystallizing plane shows some diffraction in the small angle region without any crystalline reflection in the wide angle. This fact suggests that a long-range ordering (lamellar structure) appears prior to the short-range one (crystalline structure). The in-situ crystallizing surface was observed by an optical microscope connected to a TV system. The crystallizing surface of even-number paraffins moves to upwards in the temperature slope. In-situ X-ray measurements at PF revealed that the crystalline c-axis and lamellar normal of the even number paraffins are parallel to the temperature slope. From these results, the crystalline ordering and the surface movement of even number paraffins are explained using special nucleation mechanism including a screw dislocation. (author)

Characterization of individual stacking faults in a wurtzite GaAs nanowire by nanobeam X-ray diffraction.

Science.gov (United States)

Davtyan, Arman; Lehmann, Sebastian; Kriegner, Dominik; Zamani, Reza R; Dick, Kimberly A; Bahrami, Danial; Al-Hassan, Ali; Leake, Steven J; Pietsch, Ullrich; Holý, Václav

2017-09-01

Coherent X-ray diffraction was used to measure the type, quantity and the relative distances between stacking faults along the growth direction of two individual wurtzite GaAs nanowires grown by metalorganic vapour epitaxy. The presented approach is based on the general property of the Patterson function, which is the autocorrelation of the electron density as well as the Fourier transformation of the diffracted intensity distribution of an object. Partial Patterson functions were extracted from the diffracted intensity measured along the [000\\bar{1}] direction in the vicinity of the wurtzite 00\\bar{1}\\bar{5} Bragg peak. The maxima of the Patterson function encode both the distances between the fault planes and the type of the fault planes with the sensitivity of a single atomic bilayer. The positions of the fault planes are deduced from the positions and shapes of the maxima of the Patterson function and they are in excellent agreement with the positions found with transmission electron microscopy of the same nanowire.

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...

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

Hard state neutron star and black hole X-ray binaries in the radio:X-ray luminosity plane

Science.gov (United States)

Gallo, Elena; Degenaar, Nathalie; van den Eijnden, Jakob

2018-05-01

Motivated by the large body of literature around the phenomenological properties of accreting black hole (BH) and neutron star (NS) X-ray binaries in the radio:X-ray luminosity plane, we carry out a comparative regression analysis on 36 BHs and 41 NSs in hard X-ray states, with data over 7 dex in X-ray luminosity for both. The BHs follow a radio to X-ray (logarithmic) luminosity relation with slope β = 0.59 ± 0.02, consistent with the NSs' slope (β =0.44^{+0.05}_{-0.04}) within 2.5σ. The best-fitting intercept for the BHs significantly exceeds that for the NSs, cementing BHs as more radio loud, by a factor ˜22. This discrepancy can not be fully accounted for by the mass or bolometric correction gap, nor by the NS boundary layer contribution to the X-rays, and is likely to reflect physical differences in the accretion flow efficiency, or the jet powering mechanism. Once importance sampling is implemented to account for the different luminosity distributions, the slopes of the non-pulsating and pulsating NS subsamples are formally inconsistent (>3σ), unless the transitional millisecond pulsars (whose incoherent radio emission mechanism is not firmly established) are excluded from the analysis. We confirm the lack of a robust partitioning of the BH data set into separate luminosity tracks.

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.

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

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....

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

International Nuclear Information System (INIS)

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

1992-01-01

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

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

Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

Science.gov (United States)

Vasilieva, A. V.; Grigoryeva, N. A.; Mistonov, A. A.; Sapoletova, N. A.; Napolskii, K. S.; Eliseev, A. A.; Lukashin, A. V.; Tretyakov, Yu D.; Petukhov, A. V.; Byelov, D.; Chernyshov, D.; Okorokov, A. I.; Bouwman, W. G.; Grigoriev, S. V.

2010-10-01

Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a0 = 650 ± 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length Ltran is 2.4 ± 0.1 μm, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length Llong is 3.4 ± 0.2 μm, and the structure mosaic is of order of 10°.

Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

International Nuclear Information System (INIS)

Vasilieva, A V; Okorokov, A I; Grigoriev, S V; Grigoryeva, N A; Mistonov, A A; Sapoletova, N A; Napolskii, K S; Eliseev, A A; Lukashin, A V; Tretyakov, Yu D; Petukhov, A V; Byelov, D; Chernyshov, D; Bouwman, W G

2010-01-01

Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a 0 = 650 ± 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length L tran is 2.4 ± 0.1 μm, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length L long is 3.4 ± 0.2 μm, and the structure mosaic is of order of 10 0 .

Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

Energy Technology Data Exchange (ETDEWEB)

Vasilieva, A V; Okorokov, A I; Grigoriev, S V [Petersburg Nuclear Physics Institute, Gatchina, 188350, St. Petersburg (Russian Federation); Grigoryeva, N A; Mistonov, A A [Department of Physics, St. Petersburg State University, 198504, St. Petersburg (Russian Federation); Sapoletova, N A; Napolskii, K S; Eliseev, A A; Lukashin, A V; Tretyakov, Yu D [Department of Materials Science, Moscow State University, 119899, Moscow (Russian Federation); Petukhov, A V; Byelov, D [Debye Institute, Utrecht University, 3584 CH Utrecht (Netherlands); Chernyshov, D [SNBL European Synchrotron Radiation Facility (ESRF), 38043 Grenoble (France); Bouwman, W G, E-mail: vasilieva@lns.pnpi.spb.r [Delft Technical University, 2629 JB Delft (Netherlands)

2010-10-01

Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a{sub 0} = 650 {+-} 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length L{sub tran} is 2.4 {+-} 0.1 {mu}m, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length L{sub long} is 3.4 {+-} 0.2 {mu}m, and the structure mosaic is of order of 10{sup 0}.

X-ray diffraction study of stress relaxation in cubic boron nitride films grown with simultaneous medium-energy ion bombardment

International Nuclear Information System (INIS)

Abendroth, B.; Gago, R.; Eichhorn, F.; Moeller, W.

2004-01-01

Relaxation of the intrinsic stress of cubic boron nitride (cBN) thin films has been studied by x-ray diffraction (XRD) using synchrotron light. The stress relaxation has been attained by simultaneous medium-energy ion bombardment (2-10 keV) during magnetron sputter deposition, and was confirmed macroscopically by substrate curvature measurements. In order to investigate the stress-release mechanisms, XRD measurements were performed in in-plane and out-of-plane geometry. The analysis shows a pronounced biaxial state of compressive stress in the cBN films grown without medium-energy ion bombardment. This stress is partially released during the medium-energy ion bombardment. It is suggested that the main path for stress relaxation is the elimination of strain within the cBN grains due to annealing of interstitials

Atomic structure of large angle grain boundaries determined by quantitative X-ray diffraction techniques

International Nuclear Information System (INIS)

Fitzsimmons, M.R.; Sass, S.L.

1988-01-01

Quantitative X-ray diffraction techniques have been used to determine the atomic structure of the Σ = 5 and 13 [001] twist boundaries in Au with a resolution of 0.09 Angstrom or better. The reciprocal lattices of these boundaries were mapped out using synchrotron radiation. The atomic structures were obtained by testing model structures against the intensity observations with a chi square analysis. The boundary structure were modeled using polyhedra, including octahedra, special configurations of tetrahedra and Archimedian anti-prisms, interwoven together by the boundary symmetry. The results of this work point to the possibility of obtaining general rules for grain boundary structure based on X-ray diffraction observations that give the atomic positions with high resolution

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)

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)

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

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...

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

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

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)

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.

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.

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.)

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

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

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 stress measurement by use of synchrotron radiation source

International Nuclear Information System (INIS)

Yoshioka, Yasuo; Matsui, Hisaaki; Moro-oka, Toshimasa; Hasegawa, Ken-ichi; Nakajima, Tetsuo.

1986-01-01

In the field of X-ray stress measurement of polycrystalline materials, a diffraction plane at higher Bragg angle has to be selected in order to obtain the precise value of stress. However, the stress measurement on an optional (hkl) plane desired is not always possible because the X-ray beam exited from a metal target has a dispersive wave length. Recently, we have been able to use the synchrotron radiation source (SR) as an excellent X-ray source. In Japan, the facility of synchrotron radiation (Photon Factory, PF) was constructed in the National Laboratory for High Energy Physics (KEK) at Tsukuba academic city. The use of this SR enables the stress measurements on many (hkl) planes with high accuracy in the higher Bragg angle region by providing an X-ray beam having an optional wave length. We have started the X-ray stress analysis by use of the synchrotron radiation source. This paper reports the system of measurement and some results of preliminaly experiments. Since a monochromatic X-ray beam is required for the stress measurement, we used a beam line which consists of a double crystal monochrometer and a focusing mirror. X-rays between 4 KeV (λ = 0.31 nm) and 10 KeV (λ = 0.12 nm) are available with this optical system. We adopted a constant Bragg angle of 2θ = 154 deg for all the diffraction planes. A PSPC having a carbon fiber anode is made and used as a detector with the use of a fast digital signal processor. We could observe the diffraction profiles from (200), (211), (220), (310) and (321) crystal plane of alpha iron, respectively, and the residual stresses in these planes except the (200) plane were measured with high accuracy in a short time. Such feature especially suits the stress analysis of the material which has preferred orientation or stress gradient. (author)

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)

Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

Science.gov (United States)

Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

2018-02-05

The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

Real-time out-of-plane artifact subtraction tomosynthesis imaging using prior CT for scanning beam digital x-ray system

Energy Technology Data Exchange (ETDEWEB)

Wu, Meng, E-mail: mengwu@stanford.edu [Department of Electrical Engineering, Stanford University, Stanford, California 94305 (United States); Fahrig, Rebecca [Department of Radiology, Stanford University, Stanford, California 94305 (United States)

2014-11-01

Purpose: The scanning beam digital x-ray system (SBDX) is an inverse geometry fluoroscopic system with high dose efficiency and the ability to perform continuous real-time tomosynthesis in multiple planes. This system could be used for image guidance during lung nodule biopsy. However, the reconstructed images suffer from strong out-of-plane artifact due to the small tomographic angle of the system. Methods: The authors propose an out-of-plane artifact subtraction tomosynthesis (OPAST) algorithm that utilizes a prior CT volume to augment the run-time image processing. A blur-and-add (BAA) analytical model, derived from the project-to-backproject physical model, permits the generation of tomosynthesis images that are a good approximation to the shift-and-add (SAA) reconstructed image. A computationally practical algorithm is proposed to simulate images and out-of-plane artifacts from patient-specific prior CT volumes using the BAA model. A 3D image registration algorithm to align the simulated and reconstructed images is described. The accuracy of the BAA analytical model and the OPAST algorithm was evaluated using three lung cancer patients’ CT data. The OPAST and image registration algorithms were also tested with added nonrigid respiratory motions. Results: Image similarity measurements, including the correlation coefficient, mean squared error, and structural similarity index, indicated that the BAA model is very accurate in simulating the SAA images from the prior CT for the SBDX system. The shift-variant effect of the BAA model can be ignored when the shifts between SBDX images and CT volumes are within ±10 mm in the x and y directions. The nodule visibility and depth resolution are improved by subtracting simulated artifacts from the reconstructions. The image registration and OPAST are robust in the presence of added respiratory motions. The dominant artifacts in the subtraction images are caused by the mismatches between the real object and the prior CT

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}).

In situ x-ray diffraction study on AgI nanowire arrays

International Nuclear Information System (INIS)

Wang Yinhai; Ye Changhui; Wang Guozhong; Zhang Lide; Liu Yanmei; Zhao Zhongyan

2003-01-01

The AgI nanowire arrays were prepared in the ordered porous alumina membrane by an electrochemical method. Transmission electron microscopy observation shows that the AgI nanowires are located in the channels of the alumina membrane. In situ x-ray diffractions show that the nanowire arrays possess hexagonal close-packed structure (β-AgI) at 293 K, orienting along the (002) plane, whereas at 473 K, the nanowire arrays possess a body-centered cubic structure (α-AgI), orienting along the (110) plane. The AgI nanowire arrays exhibit a negative thermal expansion property from 293 to 433 K, and a higher transition temperature from the β to α phase. We ascribe the negative thermal expansion behavior to the phase transition from the β to α phase, and the elevated transition temperature to the radial restriction by the channels of alumina membrane

X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

International Nuclear Information System (INIS)

MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I.

1999-01-01

Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it's main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

Energy Technology Data Exchange (ETDEWEB)

MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I. [Heriot-Watt University, Edinburgh, (United Kingdom). Department of Mechanical and Chemical Engineering, Centre for Molecular and Interface Engineering

1999-12-01

Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it`s main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

PIXE and X-ray diffraction studies in ceramics of the Cuitzeo basin

International Nuclear Information System (INIS)

Bucio, L.; Ruvalcaba, J.L.; Filini, A.

2005-01-01

The methodology used to carry out the characterization of the ceramic material is based on the employment of two analytical techniques. The first one, X-ray diffraction (XRD), it is used to determine the composition of the present minerals and the general composition of the pastes. The second, X-ray emission induced by protons (PIXE), it is used to determine the composition of trace elements and bigger elements. The combined use of these techniques even allows to differ among ceramic pastes of very similar compositions. Although these techniques can be used in a non destructive way, in the case of ceramic studies it is required of taking a small quantity of sample of the potsherd, this is pulverized to homogenize the material and to carry out the XRD analysis. The same powder can be used to prepare a pellet and to carry out the PIXE analysis. (Author)

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

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...

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

Analysis of synchrotron X-ray diffraction patterns from fluorotic enamel samples

Energy Technology Data Exchange (ETDEWEB)

Almeida, Ana P.G.; Braz, Delson, E-mail: anapaulagalmeida@gmail.co [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Lab. de Instrumentacao Nuclear; Colaco, Marcos V.; Barroso, Regina C., E-mail: cely@uerj.b [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica; Porto, Isabel M., E-mail: belporto@ig.com.b [Universidade Estadual de Campinas (UNICAMP), Piracicaba, SP (Brazil). Faculdade de Odontologia; Gerlach, Raquel F., E-mail: rfgerlach@forp.usp.b [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Odontologia; Droppa Junior, Roosevelt, E-mail: rdroppa@lnls.b [Associacao Brasileira de Tecnologia de Luz Sincrotron (ABTLuS), Campinas, SP (Brazil)

2009-07-01

With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basics physical-chemistry reactions of demineralisation and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The hexagonal symmetry seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using technique Synchrotron X-ray diffraction in order to determine the crystal structure and crystallinity of on fluoroapatite (FAp) crystal present in fluoritic enamel. All the scattering profile measurements was carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. (author)

Analysis of synchrotron X-ray diffraction patterns from fluorotic enamel samples

International Nuclear Information System (INIS)

Almeida, Ana P.G.; Braz, Delson

2009-01-01

With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basics physical-chemistry reactions of demineralisation and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The hexagonal symmetry seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using technique Synchrotron X-ray diffraction in order to determine the crystal structure and crystallinity of on fluoroapatite (FAp) crystal present in fluoritic enamel. All the scattering profile measurements was carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. (author)

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

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)

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.

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

International Nuclear Information System (INIS)

Farrahi, G.H.

1996-01-01

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

X-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

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 ...

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.

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.

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....

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

Science.gov (United States)

Chung, Frank H

2017-05-01

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

A synchrotron X-ray diffraction study of non-proportional strain-path effects

International Nuclear Information System (INIS)

Collins, D.M.; Erinosho, T.; Dunne, F.P.E.; Todd, R.I.; Connolley, T.; Mostafavi, M.; Kupfer, H.; Wilkinson, A.J.

2017-01-01

Common alloys used in sheet form can display a significant ductility benefit when they are subjected to certain multiaxial strain paths. This effect has been studied here for a polycrystalline ferritic steel using a combination of Nakajima bulge testing, X-ray diffraction during biaxial testing of cruciform samples and crystal plasticity finite element (CPFE) modelling. Greatest gains in strain to failure were found when subjecting sheets to uniaxial loading followed by balanced biaxial deformation, resulting in a total deformation close to plane-strain. A combined strain of approximately double that of proportional loading was achieved. The evolution of macrostrain, microstrain and texture during non-proportional loading were evaluated by in-situ high energy synchrotron diffraction. The results have demonstrated that the inhomogeneous strain accumulation from non-proportional deformation is strongly dependent on texture and the applied strain-ratio of the first deformation pass. Experimental diffraction evidence is supported by results produced by a novel method of CPFE-derived diffraction simulation. Using constitutive laws selected on the basis of good agreement with measured lattice strain development, the CPFE model demonstrated the capability to replicate ductility gains measured experimentally.

Qualitative and quantitative determination of sediments phases in Chillon River by x-ray diffraction

International Nuclear Information System (INIS)

Miramira Tipula, Biviano; Zeballos Velasquez, Elvira; Chui Betancur, Heber; Valencia Salazar, Edilberto; Huaypar Vasquez, Yesena; Olivera de Lescano, Paula

2008-01-01

With this paper, we pretend to contribute with the recovery of Chillon River from a characterization of sediments. The objectives are the identification of pollution places along the bed of the Chillon River, from the Canta Province to Lima Province (Comas) and the determination of the preponderant factors of pollution. The qualitative and semi-quantitative determination of the sediments components have been carried out using the x-ray diffraction and x-ray fluorescence techniques, both of them will allow us to identify the pollute elements, for example the lead level in the Chillon River. (author)

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

Stress measurement by x-ray diffractometry

Energy Technology Data Exchange (ETDEWEB)

Mitchell, C M

1985-10-22

This invention relates to x-ray diffractometry and more particularly to apparatus and methods for the measurement of residual stress in polycrystalline, e.g. metallic, specimens. The procedure is based on measurement of the lattice strain of crystals by x-ray diffraction, in which change in the interplanar spacing of a set of crystal lattice planes due to strain causes a change in the diffraction angle of the scattered x-ray beam, from which latter change the magnitude of the strain can be determined. In a polycrystalline specimen, from well know relations for elastic behaviour in isotropic materials, the stress on a plane normal to a given direction in the surface has a component in the given direction which can be calculated from measurement of lattice strain in two directions in a plane containing the given direction and the normal to the specimen surface. In general three such stress components in three directions in the surface are required to determine the principal stresses and thus express the state of stress in the surface. (author). 2 tabs., 9 figs.

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-11-01

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

The measurement of stress and phase fraction distributions in pre and post-transition Zircaloy oxides using nano-beam synchrotron X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Swan, H., E-mail: helen.swan@nnl.co.uk [National Nuclear Laboratory, Building D5, Culham Science Centre, Abingdon, Oxfordshire, OX14 3DB (United Kingdom); Blackmur, M.S., E-mail: matthew.s.blackmur@nnl.co.uk [National Nuclear Laboratory, Building D5, Culham Science Centre, Abingdon, Oxfordshire, OX14 3DB (United Kingdom); Hyde, J.M., E-mail: jonathan.m.hyde@nnl.co.uk [National Nuclear Laboratory, Building D5, Culham Science Centre, Abingdon, Oxfordshire, OX14 3DB (United Kingdom); Laferrere, A., E-mail: alice.laferrere@atkinsglobal.com [W.S.Atkins, The Hub, Aztec West, 500 Park Ave, Almondsbury, Bristol BS32 4RZ (United Kingdom); Ortner, S.R., E-mail: susan.r.ortner@nnl.co.uk [National Nuclear Laboratory, Building D5, Culham Science Centre, Abingdon, Oxfordshire, OX14 3DB (United Kingdom); Styman, P.D., E-mail: paul.d.styman@nnl.co.uk [National Nuclear Laboratory, Building D5, Culham Science Centre, Abingdon, Oxfordshire, OX14 3DB (United Kingdom); Staines, C., E-mail: cassie.staines@nnl.co.uk [National Nuclear Laboratory, 102B, Stonehouse Park, Stonehouse, Gloucestershire, GL10 3UT (United Kingdom); Gass, M., E-mail: mhairi.gass@amecfw.com [Amec Foster Wheeler Clean Energy Europe, Walton House, Birchwood, WA3 6GA (United Kingdom); Hulme, H., E-mail: helen.hulme@amecfw.com [Amec Foster Wheeler Clean Energy Europe, Walton House, Birchwood, WA3 6GA (United Kingdom); Cole-Baker, A., E-mail: aidan.cole-baker@rolls-royce.com [Rolls-Royce plc, PO Box 2000, Derby, DE21 7XX (United Kingdom); Frankel, P., E-mail: philipp.frankel@manchester.ac.uk [Materials Performance Centre, School of Materials, The University of Manchester, Manchester, M13 9PL (United Kingdom)

2016-10-15

Zircaloy-4 oxide stress profiles and tetragonal:monoclinic oxide phase fraction distributions were studied using nano-beam transmission X-ray diffraction. Continuous stress relief and phase transformation during the first cycle of oxide growth was observed. The in-plane monoclinic stress was shown to relax strongly up to each transition, whereas in-plane tetragonal stress-relief (near the metal-oxide interface) was only observed post transition. The research demonstrates that plasticity in the metal and the development of a band of in-plane cracking both relax the monoclinic in-plane stress. The observations are consistent with a model of transition in which in-plane cracking becomes interlinked prior to transition. These cracks, combined with the development of cracks with a through-thickness component (driven primarily by plasticity in the metal) and/or a porous network of fine cracks (associated with phase transformation), form a percolation path through the oxide layer. The oxidising species can then percolate from the oxide surface to the metal/oxide interface, at which stage transition then ensues. - Highlights: • Measurement of stress in Zr-4 oxides using nano-beam transmission X-ray diffraction. • In-plane monoclinic stress relaxes strongly up to each transition. • In-plane tetragonal stress relaxation is only observed post transition. • Development of band of cracking is related to monoclinic in-plane stress relaxation. • Linking of in-plane cracking with through-plane crack/porosity leads to transition.

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.

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.)

Room temperature femtosecond X-ray diffraction of photosystem II microcrystals

Science.gov (United States)

Kern, Jan; Alonso-Mori, Roberto; Hellmich, Julia; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Sellberg, Jonas; Lassalle-Kaiser, Benedikt; Gildea, Richard J.; Glatzel, Pieter; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; McQueen, Trevor A.; DiFiore, Dörte; Fry, Alan R.; Messerschmidt, Marc; Miahnahri, Alan; Schafer, Donald W.; Seibert, M. Marvin; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Messinger, Johannes; Sauter, Nicholas K.; Zouni, Athina; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K.

2012-01-01

Most of the dioxygen on earth is generated by the oxidation of water by photosystem II (PS II) using light from the sun. This light-driven, four-photon reaction is catalyzed by the Mn4CaO5 cluster located at the lumenal side of PS II. Various X-ray studies have been carried out at cryogenic temperatures to understand the intermediate steps involved in the water oxidation mechanism. However, the necessity for collecting data at room temperature, especially for studying the transient steps during the O–O bond formation, requires the development of new methodologies. In this paper we report room temperature X-ray diffraction data of PS II microcrystals obtained using ultrashort (< 50 fs) 9 keV X-ray pulses from a hard X-ray free electron laser, namely the Linac Coherent Light Source. The results presented here demonstrate that the ”probe before destroy” approach using an X-ray free electron laser works even for the highly-sensitive Mn4CaO5 cluster in PS II at room temperature. We show that these data are comparable to those obtained in synchrotron radiation studies as seen by the similarities in the overall structure of the helices, the protein subunits and the location of the various cofactors. This work is, therefore, an important step toward future studies for resolving the structure of the Mn4CaO5 cluster without any damage at room temperature, and of the reaction intermediates of PS II during O–O bond formation. PMID:22665786

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].

Synchrotron x-ray-diffraction study of the structure and growth of Xe films adsorbed on the Ag(111) surface

International Nuclear Information System (INIS)

Dai, P.; Wu, Z.; Angot, T.; Wang, S.; Taub, H.; Ehrlich, S.N.

1999-01-01

Synchrotron x-ray scattering has been used to investigate the structure and growth of perhaps the simplest of all films: xenon physisorbed on the Ag(111) surface. High-resolution x-ray scans of the in-plane structure and lower-resolution scans (specular and nonspecular) of the out-of-plane order were performed. The Xe films were prepared under both quasiequilibrium and kinetic growth conditions, and have fewer structural defects than those investigated previously by others on graphite substrates. Under quasiequilibrium conditions, the bulk Xe-Xe spacing is reached at monolayer completion, and the monolayer and bilayer lattice constants at coexistence are inferred equal to within 0.005 Angstrom, consistent with theoretical calculations. The Xe/vacuum interface profile for a complete monolayer and bilayer grown at quasiequilibrium is found to be sharper than for kinetically grown films. At coverages above two layers, diffraction scans along the Xe(01l) rod for quasiequilibrated films are consistent with the presence of two domains having predominantly an ABC stacking sequence and rotated 60 degree with respect to each other about the surface normal. Annealing of these films alters neither the population of the two domains nor the fraction of ABA stacking faults. The thickest film grown under quasiequilibrium conditions exceeds 220 Angstrom (resolution limited). Under kinetic growth conditions, x-ray intensity oscillations at the Xe anti-Bragg position of the specular rod are observed as a function of time, indicating nearly layer-by-layer growth. Up to four complete oscillations corresponding to a film of eight layers have been observed before the intensity is damped out; the number of oscillations is found to depend on the substrate temperature, the growth rate, and the quality of the Ag(111) substrate. The specular reflectivity from kinetically grown films at nominal coverages of three and four layers has been analyzed using a Gaussian model which gives a film

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

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, ...

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.

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

Non-destructive analysis of micro texture and grain boundary character from X-ray diffraction contrast tomography

DEFF Research Database (Denmark)

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

2010-01-01

Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting new possibilities for mapping 3D grain shapes and crystallographic orientations in different classes of polycrystalline materials. X-ray diffraction contrast tomography (DCT) is a monochromatic beam...... imaging technique combining the principles of X-ray micro-tomography and three-dimensional X-ray diffraction microscopy (3DXRD). DCT provides simultaneous access to 3D grain shape, crystallographic orientation and attenuation coefficient distribution at the micrometer length scale. The microtexture...

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

International Nuclear Information System (INIS)

Kaehle, Stephan

2009-01-01

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

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

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

Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

Science.gov (United States)

Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, Il Woong; Walko, Donald A.; Dufresne, Eric M.; Jeong, Jaewoo; Samant, Mahesh G.; Parkin, Stuart S. P.; Freeland, John W.; Evans, Paul G.; Wen, Haidan

2016-02-01

Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase separated regions. The ability to simultaneously track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of-the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiated at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, and is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. The direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems.

Diffraction of a plane electromagnetic wave on a dielectric plate of variable density. [Field equatios, diffracted-wave angular distributions

Energy Technology Data Exchange (ETDEWEB)

Aivazyan, Yu M; Mergelyan, O S; Poulatov, M P

1974-01-01

Aproblem for the diffraction of a plane electromagnetic wave on a dielectric plate between two other dielectrics is solved. The dielectric constant of the plate depends periodically on three coordinates. From this solution it is possible to obtain the equations for fields and the angular distribution of diffracted waves for the particular cases of a crystal plate and a dielectric surface fluted in all directions. If the expansion is made in the variable of the electron density in crystals, the results will correspond to the problem for the X-ray diffraction on a crystal lattice, the values of the coefficient ..cap alpha -->..sub(tau) being determined by the lattice parameters.

X-ray nano-diffraction study of Sr intermetallic phase during solidification of Al-Si hypoeutectic alloy

Energy Technology Data Exchange (ETDEWEB)

Manickaraj, Jeyakumar; Gorny, Anton; Shankar, Sumanth, E-mail: shankar@mcmaster.ca [Light Metal Casting Research Centre (LMCRC), Department of Mechanical Engineering, McMaster University, 1280 Main Street W, Hamilton, Ontario L8S 4L7 (Canada); Cai, Zhonghou [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States)

2014-02-17

The evolution of strontium (Sr) containing intermetallic phase in the eutectic reaction of Sr-modified Al-Si hypoeutectic alloy was studied with high energy synchrotron beam source for nano-diffraction experiments and x-ray fluorescence elemental mapping. Contrary to popular belief, Sr does not seem to interfere with the Twin Plane Re-entrant Edge (TPRE) growth mechanism of eutectic Si, but evolves as the Al{sub 2}Si{sub 2}Sr phase during the eutectic reaction at the boundary between the eutectic Si and Al grains.

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

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.

X-ray structural studies of epitaxial yttrium silicide on Si(111)

International Nuclear Information System (INIS)

Martinez-Miranda, L.J.; Santiago-Aviles, J.J.; Graham, W.R.; Heiney, P.A.; Siegal, M.P.

1994-01-01

We performed a series of glancing angle and reflection x-ray diffraction experiments to study both the in-plane and out-of-plane structure of epitaxial YSi 2-x films grown on Si(111), with thicknesses ranging from 85 A to 510 A. These measurements allowed us to characterize the mean film lattice constants, the position correlation lengths of the film, and the presence and extent of strain as a function of film thickness. We find that the strain along the basal plane increases as a function of increasing thickness to approximately 1% in the 510 A film; the corresponding out-of-plane strain is such that the film unit cell volume increases as a function of thickness. The corresponding in-plane microscopic strain varies from 0.5% for the 85 A film to 0.3% for the 510 A film. We relate our results to the mode of film growth and the presence of pinholes in the films

Application of powder X-ray diffraction in studying the compaction behavior of bulk pharmaceutical powders.

Science.gov (United States)

Bandyopadhyay, Rebanta; Selbo, Jon; Amidon, Gregory E; Hawley, Michael

2005-11-01

This study investigates the effects of crystal lattice deformation on the powder X-ray diffraction (PXRD) patterns of compressed polycrystalline specimen (compacts/tablets) made from molecular, crystalline powders. The displacement of molecules and the corresponding adjustment of interplanar distances (d-spacings) between diffracting planes of PNU-288034 and PNU-177553, which have crystal habits with a high aspect ratio favoring preferred orientation during tableting, are demonstrated by shifts in the diffracted peak positions. The direction of shift in diffracted peak positions suggests a reduction of interplanar d-spacing in the crystals of PNU-288034 and PNU-177553 following compaction. There is also a general reduction of peak intensities following compression at the different compressive loads. The lattice strain representing the reduction in d-spacing is proportional to the original d-spacing of the uncompressed sample suggesting that, as with systems that obey a simple Hooke's law relationship, the further apart the planes of atoms/molecules within the lattice are, the easier it is for them to approach each other under compressive stresses. For a third model compound comprising more equant-shaped crystals of PNU-141659, the shift in diffracted peak positions are consistent with an expansion of lattice spacing after compression. This apparent anomaly is supported by the PXRD studies of the bulk powder consisting of fractured crystals where also, the shift in peak position suggests expansion of the lattice planes. Thus the crystals of PNU-141659 may be fracturing under the compressive loads used to produce the compacts. Additional studies are underway to relate the PXRD observations with the bulk tableting properties of these model compounds.

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

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)

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

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

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

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 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)

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}.

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

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

International Nuclear Information System (INIS)

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

2003-01-01

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

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.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

Science.gov (United States)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

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)

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.

About some practical aspects of X-ray diffraction : From powder to thin film

Energy Technology Data Exchange (ETDEWEB)

Valvoda, V [Charles Univ. Prague (Czech Republic). Faculty of Mathematics and Physics

1996-09-01

Structure of thin films can be amorphous, polycrystalline or epitaxial, and the films can be prepared as a single layer films, multilayers or as graded films. A complete structure analysis of thin films by means of X-ray diffraction (XRD) usually needs more than one diffraction geometry to be used. Their principles, advantages and disadvantages will be shortly described, especially with respect to their different sampling depth and different response to orientation of diffracting crystallographic planes. Main differences in structure of thin films with respect to powder samples are given by a singular direction of their growth, by their adhesion to a substrate and often also by a simultaneous bombardment by atomic species during the growth. It means that a thermodynamically unstable atomic structures can be found too. These special features of growth of thin polycrystalline films are reflected in often found strong preferred orientation of grains and in residual stresses conserved in the films. The methods of structure analysis of thin films by XRD will be compared with other techniques which can supply structure images on different scales.

Computer simulation on spatial resolution of X-ray bright-field imaging by dynamical diffraction theory for a Laue-case crystal analyzer

International Nuclear Information System (INIS)

Suzuki, Yoshifumi; Chikaura, Yoshinori; Ando, Masami

2011-01-01

Recently, dark-field imaging (DFI) and bright-field imaging (BFI) have been proposed and applied to visualize X-ray refraction effects yielded in biomedical objects. In order to clarify the spatial resolution due to a crystal analyzer in Laue geometry, a program based on the Takagi-Taupin equation was modified to be used for carrying out simulations to evaluate the spatial resolution of images coming into a Laue angular analyzer (LAA). The calculation was done with a perfect plane wave for diffraction wave-fields, which corresponded to BFI, under the conditions of 35 keV and a diffraction index 440 for a 2100 μm thick LAA. As a result, the spatial resolution along the g-vector direction showed approximately 37.5 μm. 126 μm-thick LAA showed a spatial resolution better than 3.1 μm under the conditions of 13.7 keV and a diffraction index 220.

Reproducibility of temporomandibular joint tomography. Influence of shifted X-ray beam and tomographic focal plane on reproducibility

International Nuclear Information System (INIS)

Saito, Masashi

1999-01-01

Proper tomographic focal plane and x-ray beam direction are the most important factors to obtain accurate images of the temporomandibular joint (TMJ). In this study, to clarify the magnitude of effect of these two factors on the image quality. We evaluated the reproducibility of tomograms by measuring the distortion when the x-ray beam was shifted from the correct center of the object. The effects of the deviation of the tomographic focal plane on image quality were evaluated by the MTF (Modulation Transfer Function). Two types of tomograms, one the plane type, the other the rotational type were used in this study. A TMJ model was made from Teflon for the purpose of evaluation by shifting the x-ray beam. The x-ray images were obtained by tilting the model from 0 to 10 degrees 2-degree increments. These x-ray images were processed for computer image analysis, and then the distance between condyle and the joint space was measured. To evaluate the influence of the shifted tomographic focal plane on image sharpness, the x-ray images from each setting were analyzed by MTF. To obtain the MTF, ''knife-edge'' made from Pb was used. The images were scanned with a microdensitometer at the central focal plane, and 0, 0.5, 1 mm away respectively. The density curves were analyzed by Fourier analysis and the MTF was calculated. The reproducibility of images became worse by shifting the x-ray beam. This tendency was similar for both tomograms. Object characteristics such as anterior and posterior portion of the joint space affected the deterioration of reproducibility of the tomography. The deviation of the tomographic focal plane also decreased the reproducibility of the x-ray images. The rotational type showed a better MTF, but it became seriously unfavorable with slight changes of the tomographic focal plane. Contrarily, the plane type showed a lower MTF, but the image was stable with shifting of the tomographic focal plane. (author)

Classification of glutinous rice (Oryza sativa L.) starches based on X-ray diffraction pattern

Energy Technology Data Exchange (ETDEWEB)

Zhang, Q.; Abe, T.; Ando, H.; Sasahara, T.

1993-07-01

This study was carried out to analyse the cultivar variability of the X-ray diffraction pattern of glutinous rice starches. Four peaks in the X-ray diffractograms were identified, i.e. 3b, 4a, 4b and 6a. The four peaks were measured from the base line for 71 cultivars and three M{sub 3} lines which were irradiated by γ-rays at the rates of 10, 20 and 30 kr, respectively. Glutinous rice starches were classified into two types by discriminant analysis based on the values of 3b/4b, 4a/4b and 6a/4b. The X-ray diffraction type of the three cultivars did not change with the cultivation areas of different latitude, while that of eleven cultivars varied. Degree of crystallinity was estimated using the formula, (I{sub max} — I{sub i})/I{sub max} where I{sub max} is the maximum height from background intensity line among cultivars, and I{sub i} represents the four peaks. These ratios indicated that the changes in the order of crystallinity were similar to those with the water content and/or hydration and temperature for gelatinization among and/or within cultivars. (author)

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.)

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

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

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....

Nanox: a miniature mechanical stress rig designed for near-field X-ray diffraction imaging techniques.

Science.gov (United States)

Gueninchault, N; Proudhon, H; Ludwig, W

2016-11-01

Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al-Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment.

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.)

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

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

Synthesis of hydroxyapatite and structural refinement by X-ray diffraction

International Nuclear Information System (INIS)

Araujo, Jorge Correa de

2007-01-01

A sample of hydroxyapatite was synthesized and its crystalline structure was analyzed by X-ray diffraction by means of the Rietveld method. Two functions were used to fit the peak profiles, modified Voigt (TCHZ) and Pearson VII. The occupational factors and lattice parameters obtained by both models show that the sample does not contain relevant cationic substitutions. The interatomic distances from Ca1 to oxygens O1, O2 and O3 were adequate for a pure hydroxyapatite without defect at site Ca1. Besides, the use of multiple lines in planes (300) and (002) associated with the model Pearson VII resulted in good agreement with the TCHZ model with respect to the size-strain effects with an ellipsoidal shape of crystallites. In conclusion, the procedures adopted in the synthesis of hydroxyapatite produced a pure and crystalline material. The experimental results of transmission electron microscopy confirmed the predicted shape of crystals. (author)

Axial and focal-plane diffraction catastrophe integrals

International Nuclear Information System (INIS)

Berry, M V; Howls, C J

2010-01-01

Exact expressions in terms of Bessel functions are found for some of the diffraction catastrophe integrals that decorate caustics in optics and mechanics. These are the axial and focal-plane sections of the elliptic and hyperbolic umbilic diffraction catastrophes, and symmetric elliptic and hyperbolic unfoldings of the X 9 diffraction catastrophes. These representations reveal unexpected relations between the integrals.

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.

Safety code 19: recommended safety procedures for the selection, installation and use of x-ray diffraction equipment

International Nuclear Information System (INIS)

1984-01-01

This document is one of a series of Safety Codes prepared by the Radiation Protection Bureau to set out requirements for the safe use of radiation emitting devices. The equipment and installation guidelines and safety procedures detailed in this Code are primarily for the instruction and guidance of persons employed in Federal Public Service Departments and Agencies, as well as those coming under the jurisdiction of the Canada Labour Code. This Safety Code is also intended to assist other users of X-ray diffraction equipment to select safe equipment and to install and use it so that the radiation hazard to the operator and other persons in its vicinity is negligible. It should be noted that facilities under provincial jurisdiction may be subject to requirements specified under provincial statutes. This Code supersedes Safety Code RPD-SC-7, entitled 'Requirements For Non-Medical X-Ray Equipment, Use and Installation', insofar as X-ray diffraction equipment is concerned, and it is intended to complement X-ray equipment design, construction and performance standards promulgated under the Radiation Emitting Devices Act

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.

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

X-ray diffraction microstructural analysis of bimodal size distribution MgO nano powder

International Nuclear Information System (INIS)

Suminar Pratapa; Budi Hartono

2009-01-01

Investigation on the characteristics of x-ray diffraction data for MgO powdered mixture of nano and sub-nano particles has been carried out to reveal the crystallite-size-related microstructural information. The MgO powders were prepared by co-precipitation method followed by heat treatment at 500 degree Celsius and 1200 degree Celsius for 1 hour, being the difference in the temperature was to obtain two powders with distinct crystallite size and size-distribution. The powders were then blended in air to give the presumably bimodal-size- distribution MgO nano powder. High-quality laboratory X-ray diffraction data for the powders were collected and then analysed using Rietveld-based MAUD software using the lognormal size distribution. Results show that the single-mode powders exhibit spherical crystallite size (R) of 20(1) nm and 160(1) nm for the 500 degree Celsius and 1200 degree Celsius data respectively with the nano metric powder displays narrower crystallite size distribution character, indicated by lognormal dispersion parameter of 0.21 as compared to 0.01 for the sub-nano metric powder. The mixture exhibits relatively more asymmetric peak broadening. Analysing the x-ray diffraction data for the latter specimen using single phase approach give unrealistic results. Introducing two phase models for the double-phase mixture to accommodate the bimodal-size-distribution characteristics give R = 100(6) and σ = 0.62 for the nano metric phase and R = 170(5) and σ= 0.12 for the σ sub-nano metric phase. (author)

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

International Nuclear Information System (INIS)

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

1995-01-01

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

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 ...

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

X-ray diffraction study of rare earth epitaxial structures grown by MBE onto (111) GaAs

International Nuclear Information System (INIS)

Bennett, W.R.; Farrow, R.F.C.; Parkin, S.S.P.; Marinero, E.E.; Segmuller, A.P.

1989-01-01

The authors report on the new epitaxial system LaF 3 /Er/Dy/Er/LaF 3 /GaAs(111) grown by molecular beam epitaxy. X-ray diffraction studies have been used to determine the epitaxial relationships between the rare earths, the LaF 3 and the substrate. Further studies of symmetric and asymmetric reflections yielded the in-plane and perpendicular strain components of the rare earth layers. Such systems may be used to probe the effects of magnetoelastic interactions and dimensionality on magnetic ordering in rare earth metal films