X-ray powder diffraction analysis of liquid-phase-sintered silicon carbide ceramics

Energy Technology Data Exchange (ETDEWEB)

Ortiz, A.L.; Sanchez-Bajo, F. [Universidad de Extremadura, Badajoz (Spain). Dept. de Electronica e Ingenieria Electromecanica; Cumbrera, F.L. [Universidad de Extremadura, Badajoz (Spain). Dept. de Fisica

2002-07-01

In an attempt to gain a comprehensive understanding of the microstructural evolution in liquid-phase-sintered silicon carbide ceramics, the effect of the starting {beta}-SiC powder has been studied. Pellets of two different {beta}-SiC starting powders were sintered with simultaneous additions of Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3} at 1950 C for 1 hour in flowing argon atmosphere. Here we have used X-ray diffraction to obtain the relative abundance of the resulting SiC polytypes after sintering. The significant influence of the defects concentration on the {beta} to {alpha} transformation rate has been determined using the Rietveld method. (orig.)

Fundamentals of powder x-ray diffraction practice

International Nuclear Information System (INIS)

Raftery, T.

2002-01-01

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

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 powder microdiffraction for routine analysis of paintings

Czech Academy of Sciences Publication Activity Database

Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Hradil, David; Grygar, Tomáš

2005-01-01

Roč. 20, č. 3 (2005), s. 224-229 ISSN 0885-7156 R&D Projects: GA MŠk(CZ) LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray microdiffraction * artwork analysis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.483, year: 2005

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.

Synchrotron hard X-ray imaging of shock-compressed metal powders

Science.gov (United States)

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

2015-06-01

This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

Determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities

International Nuclear Information System (INIS)

Rius, J.; Miravitlles, C.

1988-01-01

A strategy for the determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities is presented. It is based on the automated full-symmetry Patterson search method described by Rius and Miravitlles where the Fourier coefficients of the observed Patterson function are modified to allow the use of powder diffraction intensity data. Its application to two structures, one with simulated and one with experimental data, is shown. (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...

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

Homogeneity characterisation of (U,Gd)O2 sintered pellets by X-ray diffraction powder analysis applying Rietveld method

International Nuclear Information System (INIS)

Leyva, Ana G.; Vega, Daniel R.; Trimarco, Veronica G.; Marchi, Daniel E.

1999-01-01

The (U,Gd)O 2 sintered pellets are fabricated by different methods. The homogeneity characterisation of Gd content seems to be necessary as a production control to qualify the process and the final product. The micrographic technique is the most common method used to analyse the homogeneity of these samples, this method requires time and expertise to obtain good results. In this paper, we propose an analysis of the X-ray diffraction powder patterns through the Rietveld method, in which the differences between the experimental data and the calculated from a crystalline structure model proposed are evaluated. This result allows to determine the cell parameters, that can be correlated with the Gd concentration, and the existence of other phases with different Gd ratio. (author)

Powder X-ray diffraction study af alkali alanates

DEFF Research Database (Denmark)

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

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

Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source.

Energy Technology Data Exchange (ETDEWEB)

Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

2007-01-01

A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source

International Nuclear Information System (INIS)

Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

2007-01-01

A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

Acemetacin cocrystal structures by powder X-ray diffraction

Science.gov (United States)

Bolla, Geetha

2017-01-01

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

Acemetacin cocrystal structures by powder X-ray diffraction

Directory of Open Access Journals (Sweden)

Geetha Bolla

2017-05-01

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

Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals

Directory of Open Access Journals (Sweden)

Íris Duarte

2016-09-01

Full Text Available The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled “Green production of cocrystals using a new solvent-free approach by spray congealing” (Duarte et al., 2016 [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II produced using the cooling crystallization method reported in “Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile” (Yu et al., 2010 [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

Resolution of crystal structures by X-ray and neutrons powder diffraction using global optimisation methods; Resolution des structures cristallines par diffraction des rayons X et neutrons sur poudres en utilisant les methodes d'optimisation globale

Energy Technology Data Exchange (ETDEWEB)

Palin, L

2005-03-15

We have shown in this work that X-ray diffraction on powder is a powerful tool to analyze crystal structure. The purpose of this thesis is the resolution of crystal structures by X-ray and neutrons diffraction on powder using global optimisation methods. We have studied 3 different topics. The first one is the order-disorder phenomena observed in some globular organic molecular solids. The second is the opiate family of neuropeptides. These neurotransmitters regulate sensory functions including pain and control of respiration in the central nervous system. The aim of our study was to try to determine the crystal structure of Leu-enkephalin and some of its sub-fragments. The determination of the crystal structures has been done performing Monte Carlo simulations. The third one is the location of benzene in a sodium-X zeolite. The zeolite framework was already known and the benzene has been localized by simulated annealing and by the use of maximum entropy maps.

Development of x-ray laminography under an x-ray microscopic condition

International Nuclear Information System (INIS)

Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

2011-01-01

An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

Determination of Ni(II) crystal structure by powder x-ray diffraction ...

African Journals Online (AJOL)

X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

Computer x-ray powder diffraction patterns and densities for corundum, aluminium, zirconium, delta-UZr2 and the zirconium hydrides

International Nuclear Information System (INIS)

Ferguson, I.F.

1976-11-01

The computer-calculated X-ray powder diffraction patterns and theoretical densities of α-Al 2 O 3 ; Al; α-Zr; β-Zr; delta-UZr 2 ; γ, delta - and epsilon-zirconium hydrides are presented. Brief comments are given on some of the published X-ray powder diffraction data on these phases. (author)

Powder X-ray diffraction laboratory, Reston, Virginia

Science.gov (United States)

Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

2014-01-01

The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

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

CERN Document Server

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

2018-01-01

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

Absolute determination by X-ray diffraction of a binary or ternary mixture: nickel oxide and fluoride in a nickel powder (1960)

International Nuclear Information System (INIS)

Charpin, P.; Hauptman, A.

1960-01-01

The method employed is based upon the comparison between computed and measured intensities for conveniently selected X-Ray diffraction lines of each component of the powder. Care must be taken to allow for absorption, both inside each grain and in overall sample. This method has been applied to the determination of nickel oxide and fluoride in a nickel powder. (author) [fr

In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

Science.gov (United States)

Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

2006-12-01

We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

X-ray powder crystallography with vertex instrumentation

International Nuclear Information System (INIS)

Chatzisotiriou, V.; Christofis, I.; Dimitriou, N.; Karvelas, S.; Karydas, A.G.; Loukas, D.; Pavlidis, A.; Spirou, S.; Dre, C.; Haralabidis, N.; Misiakos, K.; Tsoi, E.; Perdikatsis, V.; Psycharis, V.; Terzis, A.; Turchetta, R.

1998-01-01

An X-ray Diffractometer for Powder Crystallography is described along with experimental results and future plans. This is an intermediate instrument toward a long linear array system. Three channels of a silicon microstrip detector, are the detecting elements in the present instrument. Each detector channel is followed by a VLSI readout chain, which consists of a charge preamplifier with pulse shaping circuitry, a discriminator, and a 16-bit counter. Control and data acquisition is performed with a custom made PC readout card. A motorized goniometer scans the angle range of interest. Calibration of the system is done with reference samples and data which are captured with a one-channel conventional NaI detector. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

Elemental investigation of talcum baby powder by X-Ray florescence and fast neutron activation Techniques

International Nuclear Information System (INIS)

Hassan, M. F.; Abd El Wahab, M.; Nada, A.

2008-01-01

Different samples of Egyptian and Hungarian talcum powders were studied, using X-ray florescence (XRF) and Fast Neutron Activation Analysis (FNAA) techniques to ensure the safety of its use. The K (X-rays) and the gamma-rays were measured, using Si(Li) and high-purity germanium (HPGe) spectrometers to detect and determine qualitatively and quantitatively the constituents of the studied samples. The concentrations of the elements (Mg, Si, Al, Fe, Zn, and Ba) were measured and their presence was confirmed by X-ray, lifetime and/or XRF measurements. One of these samples was also studied, using the Environmental Scanning Electron Microscope (ESEM)

Combining selective sequential extractions, X-Ray Absorption Spectroscopy, and X-Ray Powder Diffraction for Cu (II speciation in soil and mineral phases

Directory of Open Access Journals (Sweden)

Tatiana Minkina

2017-04-01

Full Text Available Interaction of Cu (II ions with the matrix of soil and mineral phases of layered silicates was assessed by the Miller method of selective sequential fractionation and a set of synchrotron X-ray methods, including X-ray powder diffraction (XRD and X-ray absorption spectroscopy (XANES. It was shown that the input of Cu into Calcic Chernozem in the form of monoxide (CuO and salt (Cu(NO32 affected the transformation of Cu compounds and their affinity for metal-bearing phases. It was found that the contamination of soil with a soluble Cu(II salt increased the bioavailability of the metal and the role of organic matter and Fe oxides in the fixation and retention of Cu. During the incubation of soil with Cu monoxide, the content of the metal in the residual fractions increased, which was related to the possible entry of Cu in the form of isomorphic impurities into silicates, as well as to the incomplete dissolution of exogenic compounds at the high level of their input into the soil. A mechanism for the structural transformation of minerals was revealed, which showed that ion exchange processes result in the sorption of Cu (II ions from the saturated solution by active sites on the internal surface of the lattice of dioctahedral aluminosilicates. Surface hydroxyls at the octahedral aluminum atom play the main role. X-ray diagnostics revealed that excess Cu(II ions are removed from the system due to the formation and precipitation of coarsely crystalline Cu(NO3(OH3.

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

DEFF Research Database (Denmark)

Amri, Mahrez; Fitch, Andy; Norby, Poul

2015-01-01

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

Phase transitions of Cu.sub.3+x./sub.Si observed by temperature-dependent x-ray powder diffraction

Czech Academy of Sciences Publication Activity Database

Correa, Cinthia Antunes; Poupon, Morgane; Kopeček, Jaromír; Král, Robert; Zemenová, Petra; Lecourt, J.; Barrier, N.; Brázda, Petr; Klementová, Mariana; Palatinus, Lukáš

2017-01-01

Roč. 91, Dec (2017), s. 129-139 ISSN 0966-9795 R&D Projects: GA ČR GC15-08842J Institutional support: RVO:68378271 Keywords : X-ray powder diffraction * differential scanning calorimetry * phase transitions * Cu3+xSi Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.140, year: 2016

Calculated powder x-ray diffraction data for three tantalum tungstates

International Nuclear Information System (INIS)

Holcombe, C.E. Jr.

1976-11-01

A study was made of computer-simulated powder x-ray diffraction data for Ta 22 W 4 O 67 , Ta 2 WO 8 , and Ta 16 W 18 O 94 --the three compounds in the Ta 2 O 5 --WO 3 system from 27 to 69 mole percent WO 3 . The crystal structures of Ta 2 WO 8 and one form of Ta 16 W 18 O 94 (Type B) were deduced from reported data. 8 tables

Efficiency of Lu2SiO5:Ce (LSO) powder phosphor as X-ray to light converter under mammographic imaging conditions

International Nuclear Information System (INIS)

David, S.; Michail, C.; Valais, I.; Nikolopoulos, D.; Liaparinos, P.; Kalivas, N.; Kalatzis, I.; Toutountzis, A.; Efthimiou, N.; Loudos, G.; Sianoudis, I.; Cavouras, D.; Dimitropoulos, N.; Nomicos, C.D.; Kandarakis, I.; Panayiotakis, G.S.

2007-01-01

The aim of the present study was to examine the light emission efficiency of Lu 2 SiO 5 :Ce (LSO) powder scintillator under X-ray mammographic imaging conditions. Powder LSO scintillator has never been used in X-ray imaging. For the purposes of the present study, a 25 mg/cm 2 thick scintillating screen was prepared in our laboratory, by sedimentation of Lu 2 SiO 5 :Ce powder. Absolute luminescence efficiency measurements were performed within the range of X-ray tube voltages (22-49 kVp) used in mammographic applications. Parameters related to X-ray detection, i.e. the energy absorption efficiency (EAE) and the quantum detection efficiency (QDE) were calculated. A theoretical model, describing radiation and light transfer, was employed to fit experimental data and to estimate values of the intrinsic conversion efficiency and the light attenuation coefficients of the screen. The spectral compatibility of the LSO powder scintillator to mammographic X-ray films and to various electronic optical detectors was determined by performing light emission spectrum measurements and by taking into account the spectral sensitivity of the optical detectors. Results in the voltage range used in mammography showed that Lu 2 SiO 5 :Ce powder scintillator has approximately 10% higher values of QDE and 4.5% higher values of EAE than Gd 2 O 2 S:Tb

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

Directory of Open Access Journals (Sweden)

Yifeng Yun

2015-03-01

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

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

Science.gov (United States)

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

2015-03-01

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

Final Report for X-ray Diffraction Sample Preparation Method Development

Energy Technology Data Exchange (ETDEWEB)

Ely, T. M. [Hanford Site (HNF), Richland, WA (United States); Meznarich, H. K. [Hanford Site (HNF), Richland, WA (United States); Valero, T. [Hanford Site (HNF), Richland, WA (United States)

2018-01-30

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture.

Science.gov (United States)

Padrela, Luis; de Azevedo, Edmundo Gomes; Velaga, Sitaram P

2012-08-01

The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product. The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods. Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550 mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0-100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG). The IND-SAC cocrystal calibration curve showed excellent linearity (R(2) = 0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R(2) = 0.9981). The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method. The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.

Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

Science.gov (United States)

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

2015-03-10

A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

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

International Nuclear Information System (INIS)

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

1977-01-01

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

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

DEFF Research Database (Denmark)

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

2015-01-01

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

X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Ray, N.B.

1977-01-01

The principle, instrument and procedure of X-ray fluorescence spectrometry are described. It is a rapid, simple and sensitive method for the trace analysis of elements from sodium to uranium in powder, liquid or metal samples. (M.G.B.)

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-07-01

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

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

International Nuclear Information System (INIS)

Tanaka, Masahiko; Katsuya, Yoshio; Sakata, Osami

2016-01-01

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe_2O_4 (inverse spinel structure) using X-rays near Fe K absorption edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe_2O_4 crystal structure.

Microstructural study of Ce1-xGdxO2-δ (x = 0.1 and 0.2) nano crystallized powders synthesized by the polymeric precursor method

International Nuclear Information System (INIS)

Cela, B.; Macedo, D.A.; Souza, G.L.; Paskocimas, C.A.; Martinelli, A.E.; Nascimento, R.M.

2009-01-01

Gadolinia-doped ceria powders (Ce 1-x Gd x O 2-δ ) were prepared with substitution of 10 and 20% of the dopant element by the polymeric precursor method. This method makes possible the attainment of homogeny powder in molecular level, ideal to application in Solid Oxide Fuel Cell (SOFC) component. In this work, the particulated materials were calcinated in a range from 500 °C to 900 °C and structurally characterized by X-Ray Diffraction (XRD). The sintering behaviors of the compact samples were determined by dilatometric analyses. The results showed the method efficiency to attain monophasic nanopowder with cubic crystalline structure starting at 700 °C. The crystallite average size and crystalline parameter were determined by the Rietveld refinement method. (author)

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

Validation of powder X-ray diffraction following EN ISO/IEC 17025.

Science.gov (United States)

Eckardt, Regina; Krupicka, Erik; Hofmeister, Wolfgang

2012-05-01

Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase identification. In case of the detection limit, a statistical evaluation of the signal-to-noise ratio showed that a peak criterion of three sigma is inadequate and recommendations for a more realistic peak criterion are given. Finally, the results of an international proficiency test showed the secure performance of PXRD. © 2012 American Academy of Forensic Sciences.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

Energy Technology Data Exchange (ETDEWEB)

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorption edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.

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

CERN Document Server

Takemura, K; Fujihisa, H; Kikegawa, T

2002-01-01

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

Determinations of silicon and phosphorus in Pepperbush standard reference material by neutron activation and x-ray fluorescence methods

International Nuclear Information System (INIS)

Mizumoto, Yoshihiko; Nishio, Hirofumi; Hayashi, Takeshi; Kusakabe, Toshio; Iwata, Shiro.

1987-01-01

Silicon and phosphorus contents in Pepperbush standard reference material were determined by neutron activation and X-ray fluorescence methods. In neutron activation analysis, β-ray spectra of 32 P produced by 31 P(n,γ) 32 P reaction on Pepperbush and standard samples were measured by a low background β-ray spectrometer. In X-ray fluorescence analysis, the standard samples were prepared by mixing the Pepperbush powder with silicon dioxide and diammonium hydrogenphosphate. Characteristic X-rays from the samples were analyzed by a wavelength dispersive X-ray fluorescence spectrometer. From the β and X-ray intensities, silicon and phosphorus contents in Pepperbush were determined to be 1840 ± 80 and 1200 ± 50 μg g -1 , respectively. (author)

Diffractometric method for obtaining of x-ray diffraction patterns of transplutonium element compounds

International Nuclear Information System (INIS)

Dubasov, Yu.V.; Aleksandrov, B.M.; Baranov, Yu.I.; Golubev, V.A.; Nikolaev, V.B.

1986-01-01

Method allowing to carry out X-ray radiographic investigations of powders of high radioactive α-sources (transuranium and transplutonium compounds) by the diffractometric method have been developed. The method is tested for three americium compounds crystallizing in different syngonies - dioxide, formiate, oxalate. The substance quantity necessary for analysis is 0.5-1 mg. The investigations can be carried out with diffractometers of general purpose of DRON-UMI and DRON-20 types

Preliminary study of determination of UO2 grain size using X-ray diffraction method

International Nuclear Information System (INIS)

Mulyana, T.; Sambodo, G. D.; Juanda, D.; Fatchatul, B.

1998-01-01

The determination of UO 2 grain size has accomplished using x-ray diffraction method. The UO 2 powder is obtained from sol-gel process. A copper target as radiation source in the x-ray diffractometer was used in this experiment with CμKα characteristic wavelength 1.54433 Angstrom. The result indicate that the UO 2 mean grain size on presintered (temperature 800 o C) has the value 456.8500 Angstrom and the UO 2 mean grain size on sintered (temperature 1700 o C) has value 651.4934 Angstrom

Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

International Nuclear Information System (INIS)

Roberts, G.A.; Stewart, K.D.

2004-01-01

The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

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

International Nuclear Information System (INIS)

Paszkowicz, W.

2002-01-01

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

Imaging properties of cerium doped Yttrium Aluminum Oxide (YAP:Ce) powder scintillating screens under X-ray excitation

Energy Technology Data Exchange (ETDEWEB)

Kalivas, N. [Greek Atomic Energy Commission, 15310 Ag. Paraskevi, P.O. Box 60092 (Greece); Valais, I. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece)]|[Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Salemis, G.; Karagiannis, C.; Konstantinidis, A.; Nikolopoulos, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Loudos, G.; Sakelios, N.; Karakatsanis, N.; Nikita, K. [Department of Electrical and Computer Engineering, National Technical University of Athens, 9 Iroon Polytechniou, 15780 Zografos (Greece); Gayshan, V.L.; Gektin, A.V. [Institute of Scintillation Materials, Lenin Avenue 60, 310072 Kharkov (Ukraine); Sianoudis, I. [Department of Physics, Chemistry and Materials Technology, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Giokaris, N. [Physics Department National Capodistrian University of Athens, Panepistimioupolis Ilisia, 15771 Athens (Greece)]|[Institute of Accelerating Systems and Applications, P.O. Box 17214, 10024 Athens (Greece); Nomicos, C.D. [Department of Electronics, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Dimitropoulos, N. [Department of Medical Imaging, ' Euromedica' Medical Center, Mesogeion 2-4, 11527 Athens (Greece); Cavouras, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Panayiotakis, G. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece); Kandarakis, I. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece)]. E-mail: kandarakis@teiath.gr

2006-12-20

The aim of the present study was to evaluate the imaging performance of YAP:Ce powder scintillating screens under exposure conditions employed in diagnostic radiology (50-140 kV). Various screens were prepared in our laboratory from YAP: Ce powder (Phosphor Technology, Ltd.), with coating thickness ranging from 53 to 110 mg/cm{sup 2}. The imaging performance of the screens was assessed by experimental determination of the modulation transfer function (MTF) and the noise transfer function (NTF). MTF was determined by the edge spread function (ESF) method while NTF was estimated by noise power spectrum (NPS) measurements after uniform screen irradiation. In addition, parameters related to overall image quality, such as the signal-to-noise ratio transfer (MTF/NTF), were estimated. MTF curves were affected by the beam hardening effects caused by the patient simulating 20 mm thick aluminum phantom. Under these conditions MTF values were found to increase with the mean X-ray photon energy. A similar effect was observed for NTF curves. Results were compared with data obtained on CsI:Tl scintillator. Taking into consideration the very fast response of YAP:Ce, these data may be of interest in designing X-ray imaging detectors.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Qualitative analysis of a powdered diamond sample by particle induced X-ray emission (PIXE)

International Nuclear Information System (INIS)

Mabida, C.; Annegarn, H.J.; Renan, M.J.; Sellschop, J.P.F.

The main purpose of this analysis was to determine whether nickel is present in diamond powder as a trace element. Particle induced X-ray emission (PIXE) showed unambiguously that nickel was present. Due to the convenience of PIXE in multielemental analysis, the investigations also include a number of other trace elements in the sample

Novel X-ray Communication Based XNAV Augmentation Method Using X-ray Detectors

Directory of Open Access Journals (Sweden)

Shibin Song

2015-09-01

Full Text Available The further development of X-ray pulsar-based NAVigation (XNAV is hindered by its lack of accuracy, so accuracy improvement has become a critical issue for XNAV. In this paper, an XNAV augmentation method which utilizes both pulsar observation and X-ray ranging observation for navigation filtering is proposed to deal with this issue. As a newly emerged concept, X-ray communication (XCOM shows great potential in space exploration. X-ray ranging, derived from XCOM, could achieve high accuracy in range measurement, which could provide accurate information for XNAV. For the proposed method, the measurement models of pulsar observation and range measurement observation are established, and a Kalman filtering algorithm based on the observations and orbit dynamics is proposed to estimate the position and velocity of a spacecraft. A performance comparison of the proposed method with the traditional pulsar observation method is conducted by numerical experiments. Besides, the parameters that influence the performance of the proposed method, such as the pulsar observation time, the SNR of the ranging signal, etc., are analyzed and evaluated by numerical experiments.

Fast X-ray powder diffraction on I11 at Diamond.

Science.gov (United States)

Thompson, Stephen P; Parker, Julia E; Marchal, Julien; Potter, Jonathan; Birt, Adrian; Yuan, Fajin; Fearn, Richard D; Lennie, Alistair R; Street, Steven R; Tang, Chiu C

2011-07-01

The commissioning and performance characterization of a position-sensitive detector designed for fast X-ray powder diffraction experiments on beamline I11 at Diamond Light Source are described. The detecting elements comprise 18 detector-readout modules of MYTHEN-II silicon strip technology tiled to provide 90° coverage in 2θ. The modules are located in a rigid housing custom designed at Diamond with control of the device fully integrated into the beamline data acquisition environment. The detector is mounted on the I11 three-circle powder diffractometer to provide an intrinsic resolution of Δ2θ approximately equal to 0.004°. The results of commissioning and performance measurements using reference samples (Si and AgI) are presented, along with new results from scientific experiments selected to demonstrate the suitability of this facility for powder diffraction experiments where conventional angle scanning is too slow to capture rapid structural changes. The real-time dehydrogenation of MgH(2), a potential hydrogen storage compound, is investigated along with ultrafast high-throughput measurements to determine the crystallite quality of different samples of the metastable carbonate phase vaterite (CaCO(3)) precipitated and stabilized in the presence of amino acid molecules in a biomimetic synthesis process.

Determination of Ti, Cr, Cu and Ta in niobium oxide by X-ray fluorescence method

International Nuclear Information System (INIS)

Dixit, R.M.; Deshpande, S.S.

1986-01-01

An x-ray fluorescence method for the determination of Ti, Cr, Cu and Ta in niobium oxide has been developed. Samples/standards in powder form are mixed with boric acid in the proportion of 1:1 (400 mg. each). Double layer pellets are prepared by pressing this mixture over a primary boric acid pellet. Philips PW-1220, a semiautomatic x-ray spectrometer with tungsten target x-ray tube for excitation and LiF (200) crystal for dispersion have been used. The determination range is from 0.005 to 0.1per cent for Ti and Cr, 0.01 to 0.1per cent for Cu and 0.05 to 1per cent for Ta. (author)

Standard test method for verifying the alignment of X-Ray diffraction instrumentation for residual stress measurement

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

1.1 This test method covers the preparation and use of a flat stress-free test specimen for the purpose of checking the systematic error caused by instrument misalignment or sample positioning in X-ray diffraction residual stress measurement, or both. 1.2 This test method is applicable to apparatus intended for X-ray diffraction macroscopic residual stress measurement in polycrystalline samples employing measurement of a diffraction peak position in the high-back reflection region, and in which the θ, 2θ, and ψ rotation axes can be made to coincide (see Fig. 1). 1.3 This test method describes the use of iron powder which has been investigated in round-robin studies for the purpose of verifying the alignment of instrumentation intended for stress measurement in ferritic or martensitic steels. To verify instrument alignment prior to stress measurement in other metallic alloys and ceramics, powder having the same or lower diffraction angle as the material to be measured should be prepared in similar fashion...

X-ray characterisation of nanostructured materials

DEFF Research Database (Denmark)

Oddershede, Jette

X-ray powder di®raction (XRPD) is an excellent tool for characterising the bulk structure of crystalline materials. Along with the growing interest in exploiting materials with decreasing particle sizes and increasing number of defects, factors that complicate the traditional interpretation...... of the experi- mental XRPD patterns, the need for new interpretation methods has arisen. The method described in the present thesis is by no means new, in fact it was developed by Debye in 1915. However, the Debye method it is rather computationally heavy, so in practise it is only applicable to the X-ray char...

X-ray fluorescence spectrometric and optical emission spectographic analysis of thoria in thoriated copper metal powder

International Nuclear Information System (INIS)

Chandola, L.C.; Khanna, P.P.

1984-01-01

Two methods, one using the X-ray fluorescence (XRF) spectrometric technique and another using optical emission spectrographic (OES) technique are described for the determination of thoria in the concentration range 0.5-10% in thoriated copper metal powder. The precision of XRF method is superior to OES method but when sample quantity is very small, the OES method is useful. For XRF method, 500 mg sample is mixed with boric acid binding material and converted to a tablet for analysis. For OES method, only 200 mg sample is needed which is glued to the flat ends of two graphite electrodes for excitation by AC arc. The precision obtained in XRF is better than +-1% and in OES it is +-23%. (author)

The X-ray powder diffraction pattern and lattice parameters of perovskite

International Nuclear Information System (INIS)

Ball, C.J.; Napier, J.G.

1988-02-01

The interplanar spacings and intensities of all lines appearing in the X-ray powder diffraction pattern of perovskite have been calculated. Many of the lines occur in groups with a large amount of overlap. As an aid to identifying the lines which are observed, the intensity profiles of the major groups have been plotted. Those lines which are relatively free of overlap and can be identified unambiguously have been used to calculate the lattice parameters, with the results a=5.4424 ± 0.0001 A, b=7.6417 ± 0.0002 A, c=5.3807 ± 0.0001 A

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

International Nuclear Information System (INIS)

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

1987-01-01

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

Characterization by X-ray tomography of granulated alumina powder during in situ die compaction

Energy Technology Data Exchange (ETDEWEB)

Cottrino, Sandrine; Jorand, Yves, E-mail: yves.jorand@insa-lyon.fr; Maire, Eric; Adrien, Jérôme

2013-07-15

Compaction process, the aim of which being to obtain green bodies with low porosity and small size, is often used before sintering treatment. Prior to die filling, the ceramic powder is generally granulated to improve flowability. However during compaction, density heterogeneity and critical size defects may appear due to intergranule and granule-die wall frictions. In this work, the influence of granule formulation on the compact morphology has been studied. To do so, a compaction setup was installed inside an X-ray tomography equipment so that the evolution of the compact morphology could be analysed during the whole compaction process. We have demonstrated that high humidity rate and the addition of binder in the granule formulation increase density heterogeneity and generate larger defects. - Highlights: • An original compaction set up was installed inside an X-Ray tomography equipment. • The compaction process of granulated ceramic powder is imaged. • The compact green microstructure is quantified and related to the compaction stages. • The most detrimental defects of dry-pressed parts are caused by hollow granules. • Formulations without binder allow a reduction of the number of large defects.

X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

Energy Technology Data Exchange (ETDEWEB)

Brown, Allan

1970-12-15

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

X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

International Nuclear Information System (INIS)

Brown, Allan

1970-12-01

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

Apparatus and method X-ray image processing

International Nuclear Information System (INIS)

1984-01-01

The invention relates to a method for X-ray image processing. The radiation passed through the object is transformed into an electric image signal from which the logarithmic value is determined and displayed by a display device. Its main objective is to provide a method and apparatus that renders X-ray images or X-ray subtraction images with strong reduction of stray radiation. (Auth.)

Two methods for studying the X-ray variability

NARCIS (Netherlands)

Yan, Shu-Ping; Ji, Li; Méndez, Mariano; Wang, Na; Liu, Siming; Li, Xiang-Dong

2016-01-01

The X-ray aperiodic variability and quasi-periodic oscillation (QPO) are the important tools to study the structure of the accretion flow of X-ray binaries. However, the origin of the complex X-ray variability from X-ray binaries remains yet unsolved. We proposed two methods for studying the X-ray

Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data

International Nuclear Information System (INIS)

Rybak, Jens-Christoph

2012-01-01

of this thesis. A method is presented, which allows, by indexing a diffractogram, intensity extraction and structure solution by charge flipping, to solve the structure of a material, ab initio, from X-ray powder diffraction data exclusively. Moreover it is shown how to refine structures with a high amount of weakly scattering atoms, using rigid body constraints. The structure solutions of 3 ∞ [Ga(Tz) 2 ], 3 ∞ [Sr(Im) 2 ]:Ce and 3 ∞ [Yb(Im) 3 ]ImH from X-ray powder diffraction data are further examples for the successful application of the method presented within this thesis.

An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

Science.gov (United States)

Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

2015-01-01

While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

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

A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

CERN Document Server

Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

1999-01-01

A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

X-ray fluorescence spectroscopic determination of heavy metals and ...

African Journals Online (AJOL)

Purpose: To determine the heavy metal and trace element composition of the powdered aerial parts of Origanum sipyleum L. and its water extract. Methods: The heavy metal and trace elements content of the powdered plant material and 2 % aqueous extract were evaluated by x-ray fluorescence spectroscopy with silicon ...

The analysis of powder diffraction data

International Nuclear Information System (INIS)

David, W.I.F.; Harrison, W.T.A.

1986-01-01

The paper reviews neutron powder diffraction data analysis, with emphasis on the structural aspects of powder diffraction and the future possibilities afforded by the latest generation of very high resolution neutron and x-ray powder diffractometers. Traditional x-ray powder diffraction techniques are outlined. Structural studies by powder diffraction are discussed with respect to the Rietveld method, and a case study in the Rietveld refinement method and developments of the Rietveld method are described. Finally studies using high resolution powder diffraction at the Spallation Neutron Source, ISIS at the Rutherford Appleton Laboratory are summarized. (U.K.)

Solving Crystal Structures from Powder Diffraction Data

DEFF Research Database (Denmark)

Christensen, A. Nørlund; Lehmann, M. S.; Nielsen, Mogens

1985-01-01

High resolution powder data from both neutron and X-ray (synchrotron) sources have been used to estimate the possibility of direct structure determination from powder data. Two known structures were resolved by direct methods with neutron and X-ray data. With synchrotron X-ray data, the measured ...

X-ray fluorescence method for trace analysis and imaging

International Nuclear Information System (INIS)

Hayakawa, Shinjiro

2000-01-01

X-ray fluorescence analysis has a long history as conventional bulk elemental analysis with medium sensitivity. However, with the use of synchrotron radiation x-ray fluorescence method has become a unique analytical technique which can provide tace elemental information with the spatial resolution. To obtain quantitative information of trace elemental distribution by using the x-ray fluorescence method, theoretical description of x-ray fluorescence yield is described. Moreover, methods and instruments for trace characterization with a scanning x-ray microprobe are described. (author)

Method for reducing x-ray background signals from insertion device x-ray beam position monitors

Directory of Open Access Journals (Sweden)

Glenn Decker

1999-11-01

Full Text Available A method is described that provides a solution to the long-standing problem of stray radiation-induced signals on photoemission-based x-ray beam position monitors (BPMs located on insertion device x-ray beam lines. The method involves the introduction of a chicane into the accelerator lattice that directs unwanted x radiation away from the photosensitive x-ray BPM blades. This technique has been implemented at the Advanced Photon Source, and experimental confirmation of the technique is provided.

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/

Solid-state structural properties of 2,4,6-trimethoxybenzene derivatives, determined directly from powder X-ray diffraction data in conjunction with other techniques

International Nuclear Information System (INIS)

Pan Zhigang; Xu Mingcan; Cheung, Eugene Y.; Platts, James A.; Harris, Kenneth D.M.; Constable, Edwin C.; Housecroft, Catherine E.

2006-01-01

Structural properties of 2,4,6-trimethoxybenzaldehyde, 2,4,6-trimethoxybenzyl alcohol and 2,4,6-trimethoxyacetophenone have been determined directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm (GA) technique for structure solution followed by Rietveld refinement. Structural similarities and contrasts within this family of materials are elucidated. The work illustrates the value of utilizing information from other sources, including spectroscopic data and computational techniques, as a means of augmenting the structural knowledge established from the powder X-ray diffraction data

An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer

DEFF Research Database (Denmark)

Shen, Yanbin; Pedersen, Erik Ejler; Christensen, Mogens

2014-01-01

An electrochemical cell has been designed for powder X-ray diffraction (PXRD) studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode...... to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li4Ti5O12 anode and LiMn2O4 cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na0.84Fe0.56Mn0.44O2)....

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.

Validation of the method of quantitative phase analysis by X-ray diffraction in API: case of Tibolone

International Nuclear Information System (INIS)

Silva, R P; Ambrósio, M F S; Epprecht, E K; Avillez, R R; Achete, C A; Kuznetsov, A; Visentin, L C

2016-01-01

In this study, different structural and microstructural models applied to X-ray analysis of powder diffraction data of polymorphic mixtures of known concentrations of Tibolone were investigated. The X-ray data obtained in different diffraction instruments were analysed via Rietveld method using the same analytical models. The results of quantitative phase analysis show that regardless of the instrument used, the values of the calculated concentrations follow the same systematics with respect to the final errors. The strategy to select a specific analytical model that leads to lower measurement errors is here presented. (paper)

Growth and Characterization of La1-x Mnx O3 (x=0.01 mol) Powder and Fibre

International Nuclear Information System (INIS)

Yin Yin Win; Pwint Yee Thein; Than Than Win; Yin Maung Maung; Ko Ko Kyaw Soe

2010-12-01

An improved method is proposed for the preparation of Ianthanum manganite (LaMaO3) powder by the calcinations of a composite carbonate of the respective metallic elements formed by mixing an aqueous solution of a water-soluble ammonium carbonate and an aqueous solution of inorganic salts, e.g, chlorides, of the respective metallic elements. The surface morphology of the LaMnO3 is studied by scanning electron microscopy (SEM), X-rays fluorescent (XRF) technique is used for chemical analysis. Structural properties are characterized by X-rays Diffraction (XRD). Chemical and physical reaction of LaMnO3 powder is investigated by Thermogravimetric Analysis-Differential Thermal Analysis (TGA-DTA). Electrospun LaMnO3 fibre is formed on Al-foil and their characteristic is examined by SEM and XRD.

1-(2-furoyl)-3,3-(diphenyl)thiourea: spectroscopic characterization and structural study from X-ray powder diffraction using simulated annealing

Energy Technology Data Exchange (ETDEWEB)

Estevez H, O.; Duque, J. [Universidad de La Habana, Instituto de Ciencia y Tecnologia de Materiales, 10400 La Habana (Cuba); Rodriguez H, J. [UNAM, Instituto de Investigaciones en Materiales, 04510 Mexico D. F. (Mexico); Yee M, H., E-mail: oestevezh@yahoo.com [Instituto Politecnico Nacional, Escuela Superior de Fisica y Matematicas, 07738 Mexico D. F. (Mexico)

2015-07-01

1-Furoyl-3,3-diphenylthiourea (FDFT) was synthesized, and characterized by Ftir, {sup 1}H and {sup 13}C NMR and ab initio X-ray powder structure analysis. FDFT crystallizes in the monoclinic space group P2{sub 1} with a = 12.691(1), b = 6.026(2), c = 11.861(1) A, β = 117.95(2) and V = 801.5(3) A{sup 3}. The crystal structure has been determined from laboratory X-ray powder diffraction data using direct space global optimization strategy (simulated annealing) followed by the Rietveld refinement. The thiourea group makes a dihedral angle of 73.8(6) with the furoyl group. In the crystal structure, molecules are linked by van der Waals interactions, forming one-dimensional chains along the a axis. (Author)

Preparation and characterisation of nanocrystalline IrxSn1-xO2 electrocatalytic powders

International Nuclear Information System (INIS)

Marshall, A.; Borresen, B.; Hagen, G.; Tsypkin, M.; Tunold, R.

2005-01-01

Nanocrystalline oxide powders of the type Ir x Sn 1-x O 2 (0.2-bar x-bar 1) have been produced and characterised. These oxides have been developed primarily as oxygen evolution electrocatalysts for proton exchange membrane (PEM) water electrolysers. Two methods were used to produce the oxide materials: the modified polyol method and the Adams fusion method. X-ray diffraction analysis suggests that an iridium-tin oxide solid solution with a rutile structure can be produced using the modified polyol method, with a linear relationship between the lattice parameters and composition. The crystal size of the solid solution phase is below 15-bar nm for all compositions. The Adams fusion method results in at least two separate oxide phases, namely a tin rich oxide and an iridium rich oxide. X-ray photoelectron spectroscopy (XPS) analysis revealed no significant difference between the bulk and surface compositions, and that the iridium was present in at least two valent states. The electrical resistivity of the powders was compared, and an exponential increase in resistivity with tin addition was found. Overall the resistivity measurements suggest that the limit for tin addition is around 50-60-bar mol% due to the high ohmic losses expected at higher tin contents in a PEM water electrolyser

Thermal expansion and phase transformation studies on some materials by high temperature x-ray powder diffractometry

International Nuclear Information System (INIS)

Rajagopalan, S.; Kutty, K.V.G.; Jajoo, H.K.; Ananthakrishnan, S.K.; Asurvatharaman, R.

1988-01-01

A high temperature chamber based on electrical resistance heating has been integrated to an existing x-ray powder diffractometer. The system is capable of going upto 2500degC at programmed rates of heating. Temperature measurement is carried out by means by Pt/Rh or W/Re thermocouples or by optical pyrometry depending upon the temperature range. Provision exists for performing high temperature x-ray diffractometry in vacuum or in a gaseous atmosphere of low x-ray absorption. The x-ray optical alignment has been ensured by accurately measuring the unit cell lengths of x-ray diffraction standards like silicon and tungsten. The thermocouples have been calibrated within the system by monitoring the melting points of gold and silver. The well characterized transformation of zirconia from the monoclinic to tetragonal structure occuring around 1100degC has been satisfactorily reproduced . The high temperature phase transitions in some rare earth oxides have been studi ed. lattice parameter measurements on a variety of materials as a function of temperature upto 1500degC have been carried out and the data found to be in agreement with the literature values. From the measured lattice parameter values, percentage thermal expansion and coefficients of thermal expansion have been calculated for many substances from room temperature to 15000degC. (author). 20 refs., 9 figs

Modified X-ray method of a study of duodenum

Energy Technology Data Exchange (ETDEWEB)

Korolyuk, I.P.; Bugakov, V.M.; Shinkin, V.M.

A modified X-ray examination of duodenum under hypotension conditions is described. In comparison with the existing method, the above-mentioned modification allows one to investigate the duodenum by using double contrast - the high-concentrated barium suspension and the gas, formed after the gasificated powder dose. 327 patients have been examined by the given method, 126 of them have been diagnosed to suffer from inflammatory diseases of the stomach and the duodenum, 22 of them suffering from the duodenum peptic ulcer, 107 of them - pancreatitis, 48-cholelithiasis, 24 - the tumor of the pancreatoduodenum zone. 65 patients have been operated on. Roentgenomorphologic comparisons have been carried out for 66 patients suffering from inflammatory deseases of the duodenum. Duodenum visualization of 283 patients is found to be good and satisfactory. The given method may be used under any conditions, including polyclinics, due to the sparing nature.

Measuring the black hole mass in ultraluminous X-ray sources with the X-ray scaling method

Science.gov (United States)

Jang, I.; Gliozzi, M.; Satyapal, S.; Titarchuk, L.

2018-01-01

In our recent work, we demonstrated that a novel X-ray scaling method, originally introduced for Galactic black holes (BH), could be reliably extended to estimate the mass of supermassive black holes accreting at moderate to high level. Here, we apply this X-ray scaling method to ultraluminous X-ray sources (ULXs) to constrain their MBH. Using 49 ULXs with multiple XMM-Newton observations, we infer that ULXs host both stellar mass BHs and intermediate mass BHs. The majority of the sources of our sample seem to be consistent with the hypothesis of highly accreting massive stellar BHs with MBH ∼ 100 M⊙. Our results are in general agreement with the MBH values obtained with alternative methods, including model-independent variability methods. This suggests that the X-ray scaling method is an actual scale-independent method that can be applied to all BH systems accreting at moderate-high rate.

Structure of La2Cu2O5 by high-resolution synchrotron X-ray powder diffraction

International Nuclear Information System (INIS)

La Placa, S.J.; Bringley, J.F.; Scott, B.A.; Cox, D.E.

1993-01-01

Dicopper(II) dilanthanum pentaoxide, La 2 Cu 2 O 5 , M r =484.90, orthorhombic, Pbam. At T=300 K: a=5.5490(1), b=10.4774(2), c=3.8796(1) A, V=225.557(8) A 3 , Z=2, D x =7.139 g cm -3 , λ=1.2000 A. Final R I =6.20, R p =14.6 and R wp =20.61%, 124 independent reflections observed. The structure has been refined from high-resolution synchrotron X-ray powder diffraction data using the Rietveld method. It is of the oxygen-defect perovskite type and is composed entirely of corner-shared CuO 5 square pyramids, which share oxygen vacancies forming vacancy tunnels along the c axis. The La atoms reside at a perovskite-like A-site and are tenfold coordinated by oxygen. (orig.)

Characterization of Beryllium Windows for Coherent X-ray Optics

International Nuclear Information System (INIS)

Goto, Shunji; Yabashi, Makina; Tamasaku, Kenji; Ishikawa, Tetsuya

2007-01-01

Beryllium foils fabricated by several processes were characterized using spatially coherent x rays at 1-km beamline of SPring-8. By thickness dependence of bright x-ray spot density due to Fresnel diffraction from several-micron deficiencies, we found that speckles (bright x-ray spots) were due to voids with densities 103-104 mm-3 in powder foils and ingot foils. Compared with powder and ingot foils, a polished physical-vapor-deposited (PVD) beryllium foil gave highly uniform beams with no speckles. The PVD process eliminates the internal voids in principle and the PVD foil is the best for coherent x-ray applications

Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

Directory of Open Access Journals (Sweden)

Yan Zilin

2017-01-01

Full Text Available The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM. Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.

[Particle size determination by radioisotope x-ray absorptiometry with sedimentation method].

Science.gov (United States)

Matsui, Y; Furuta, T; Miyagawa, S

1976-09-01

The possibility of radioisotope X-ray absorptiometry to determine the particle size of powder in conjunction with sedimentation was investigated. The experimental accuracy was primarily determined by Cow and X-ray intensity. where Co'=weight concentration of the particle in the suspension w'=(micron/rho)l/(mu/rho)s-rhol/rhos rho; density micron/rho; mass absorption coefficient, suffix l and s indicate dispersion and particle, respectively. The radiosiotopes, Fe-55, Pu-238 and Cd-109 have high w-values over the wide range of the atomic number. However, a source of high micron value such as Fe-55 is not suitable because the optimal X-ray transmission length, Lopt is decided by the expression, micronlLopt approximately 2/(1+C'ow') by using Cd-109 AgKX-ray source, the weight size distribution of particles from the heavy elements such as PbO2 to light elements such as Al2O3 or flyash was determined.

Large-scale synthesis of Pb1-xLa xTiO3 ceramic powders by molten salt method

International Nuclear Information System (INIS)

Cai Zongying; Xing Xianran; Yu Ranbo; Liu Guirong; Xing Qifeng

2006-01-01

The ferroelectric perovskite type lanthanum doped lead titanate (PLT) ceramic powders were synthesized in one step with the starting materials of PbC 2 O 4 , La 2 O 3 and TiO 2 in NaCl-KCl molten salts in the temperature range of 700-950 deg. C. It was found that molten salt method was a large scale and easy preparation way to produce PLT powders with high dispersity. Tetragonal phase Pb 1-x La x TiO 3 ceramic powders were identified by XRD in the composition range 0 ≤ x ≤ 0.3 and mono-dispersed particles with spheric shape and less than 100 nm size were observed by SEM. The grain sizes of Pb 1-x La x TiO 3 ceramic powders increased with the increase of La content and decreased with calcination temperature. The grain growth progress and the possible reaction mechanism in molten salts and its influencing factors were discussed in this work. The grain growth process was the main influencing factor of the grain size, which depended on the solubility in the flux

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

Science.gov (United States)

Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

2018-04-01

A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

X-Ray analysis and methods for nondestructive control (On the 100-anniversary of X-ray foundation)

International Nuclear Information System (INIS)

Sosnin, F.R.

1995-01-01

Brief consideration is given to the history of X-ray discovery, formation of domestic X-ray industry. Principles of operation and potentialities of X-ray diffraction analysis, gammagraphy, radioscopy, radiometric analysis are described briefly. Domestic and foreign scientists, institutes and companies who contributed much to development of methods for nondestructive control are listed

Feasibility study on X-ray source with pinhole imaging method

International Nuclear Information System (INIS)

Qiu Rui; Li Junli

2007-01-01

In order to verify the feasibility of study on X-ray source with pinhole imaging method, and optimize the design of X-ray pinhole imaging system, an X-ray pinhole imaging equipment was set up. The change of image due to the change of the position and intensity of X-ray source was estimated with mathematical method and validated with experiment. The results show that the change of the spot position and gray of the spot is linearly related with the change of the position and intensity of X-ray source, so it is feasible to study X-ray source with pinhole imaging method in this application. The results provide some references for the design of X-ray pinhole imaging system. (authors)

On the response of Y 3Al 5O 12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

Science.gov (United States)

Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

2005-02-01

The aim of this study was to examine Y 3Al 5O 12:Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166 mg/cm 2 were prepared in our laboratory by sedimentation of Y 3Al 5O 12: Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120 kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (η≈0.03-0.05) and light attenuation coefficients (σ≈26.5 cm/g) were derived through this fitting. Y 3Al 5O 12:Ce showed peak emission in the wavelength range 530-550 nm. The light emission efficiency was found to be maximum for the 107 mg/cm 2 layer. Due to its "green" emission spectrum, Y 3Al 5O 12:Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3Al 5O 12:Ce could be considered for application in X-ray imaging especially in various digital detectors.

On the response of Y3Al5O12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

International Nuclear Information System (INIS)

Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

2005-01-01

The aim of this study was to examine Y 3 Al 5 O 12 :Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166mg/cm 2 were prepared in our laboratory by sedimentation of Y 3 Al 5 O 12 : Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (ηC ∼0.03-0.05) and light attenuation coefficients (σ∼26.5cm 2 /g) were derived through this fitting. Y 3 Al 5 O 12 :Ce showed peak emission in the wavelength range 530-550nm. The light emission efficiency was found to be maximum for the 107mg/cm 2 layer. Due to its 'green' emission spectrum, Y 3 Al 5 O 12 :Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3 Al 5 O 12 :Ce could be considered for application in X-ray imaging especially in various digital detectors

Crystal structure and tautomerism of Pigment Yellow 138 determined by X-ray powder diffraction and solid-state NMR

DEFF Research Database (Denmark)

Gumbert, Silke D.; Körbitzer, Meike; Alig, Edith

2016-01-01

The crystal structure of C.I. Pigment Yellow 138 was determined from X-ray powder diffraction data using real-space methods with subsequent Rietveld refinements. The tautomeric state was investigated by solid-state 1D and 2D multinuclear NMR experiments. In the crystals, the compound exhibits...... the NH-tautomer with a hydrogen atom situated at the nitrogen of the quinoline moiety. Direct evidence of the presence of the NH-tautomer is provided by 1H–14N HMQC solid-state NMR at very fast MAS. Solid-state dispersion-corrected density functional theory calculations with BLYP-D3 confirm...

Dehydrogenation kinetics of pure and nickel-doped magnesium hydride investigated by in situ time-resolved powder X-ray diffraction

DEFF Research Database (Denmark)

Jensen, T.R.; Andreasen, A.; Vegge, Tejs

2006-01-01

The dehydrogenation kinetics of pure and nickel (Ni)-doped (2w/w%) magnesium hydride (MgH2) have been investigated by in situ time-resolved powder X-ray diffraction (PXD). Deactivated samples, i.e. air exposed, are investigated in order to focus on the effect of magnesium oxide (MgO) surface layers......, which might be unavoidable for magnesium (Mg)-based storage media for mobile applications. A curved position-sensitive detector covering 120 degrees in 20 and a rotating anode X-ray source provide a time resolution of 45 s and up to 90 powder pattems collected during an experiment under isothermal...... by the Johnson-Mehi-Avrami formalism in order to derive rate constants at different temperatures. The apparent activation energies for dehydrogenation of pure and Ni-doped magnesium hydride were E-A approximate to 300 and 250 kJ/mol, respectively. Differential scanning calorimetry gave, E-A = 270 k...

Analysis of the average poly-cyclic aromatic unit in a meta-anthracite coal using conventional x-ray powder diffraction and intensity separation methods

International Nuclear Information System (INIS)

Wertz, D.L.; Bissell, M.

1994-01-01

X-ray characterizations of coals and coal products have occurred for many years. Hirsch and Cartz measured the diffraction from several coals over the reciprocal space region from s = 0.12 angstrom -1 to 7.5 angstrom -1 where s = (4π/λ) sinΘ. In these studies, a 9 cm powder camera was used to study the high angle region, and a transmission type focusing camera equipped with a LiF monochromator was used for the low angle measurements. They reported that the height of the graphene peak measured for each coal is proportional to the % carbon in the coals. Hirsch also suggested that the ontyberem anthracite has a lamellar diameter of ca. 16 angstrom corresponding to an aromatic lamellae of ca. C 87 . For coals with lower carbon content, Hirsch proposed much smaller lamellae; C 19 for a coal with 80% carbon, and C 24 for a coal with 89% carbon. The subject coal for this study is a meta-anthracite which was derived from the Portsmouth, RI mine. The Narragansett Basin contains anthracite and meta-anthracite coals of Pennsylvanian Age. The Basin was a techtonically active non-marine coal-forming basin which has been impacted by several tectonic events. Because of the importance placed by coal scientists no correctly characterizing the nature of the micro-level structural cluster(s) in coals and because of improvements in both x-ray experimentation capabilities and computing power, we have measured the x-ray diffraction and scattering produced from irradiation of this meta-anthracite coal which contains about 94% aromatic carbon. The goal of our study is to determine the intra-planar, and where possible, inter-planar structural details of coals. To accomplish this goal we have utilized the methods normally used for the molecular analysis of non-crystalline condensed phases such as liquids, solutions, and amorphous solids. Reported herein are the results obtained from the high angle x-ray analysis of this coal

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

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.

Application of combined multivariate techniques for the description of time-resolved powder X-ray diffraction data

Czech Academy of Sciences Publication Activity Database

Taris, A.; Grosso, M.; Brundu, M.; Guida, V.; Viani, Alberto

2017-01-01

Roč. 50, č. 2 (2017), s. 451-461 ISSN 1600-5767 R&D Projects: GA MŠk(CZ) LO1219 Keywords : in situ X-ray powder diffraction * amorphous content * chemically bonded ceramic s * statistical total correlation spectroscopy * multivariate curve resolution Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 2.495, year: 2016 http://journals.iucr.org/j/issues/2017/02/00/ap5006/index.html

Development and directions of powder diffraction on proteins

Energy Technology Data Exchange (ETDEWEB)

Von Dreele, R B; Besnard, C; Basso, S; Camus, F; Pattison, P; Schiltz, M; Wright, J P; Margiolaki, R; Fitch, A N; Fox, G C; Prugoveeki, S; Beckers, D; Helliwell, J R; Helliwell, M; Jones, R H; Roberts, M A; Miura, K; Kahn, R; Giacovazzo, C; Altomare, A; Caliandro, R; Camalli, M; Cuocci, C; Moliterni, A G.G.; Rizzi, R; Hinrichsen, B; Kern, A; Coelho, A A; Degen, T; Kokkinidis, M; Fadouloglou, V; Gazi, A; Panopoulos, N; Pinotsis, N; Wilmanns, M; Norrman, M; Schluckebier, G; Prugoveeki, B; Dilovic, J; Matkovic-Calogovic, D; Bill, David; Markvardsen, A; Grosse-Kunstleve, R; Rius, J; Glykos Nicholas, M; Murshudov, G N

2007-07-01

X-ray diffraction is one of the most important method for obtaining information about the structure of proteins and thereby for gaining insight into fundamental biological and biochemical mechanisms. This seminar was dedicated to X-ray powder diffraction and was organized around 6 sessions: 1) what can powder diffraction do for proteins?, 2) adapting experimentally to proteins, 3) interpreting powder data, 4) the world of protein crystallography, 5) advancing methods for powder data analysis, and 6) transferable methods from single crystals. This document gathers the abstracts of the 23 papers presented. (A.C.)

Development and directions of powder diffraction on proteins

International Nuclear Information System (INIS)

Von Dreele, R.B.; Besnard, C.; Basso, S.; Camus, F.; Pattison, P.; Schiltz, M.; Wright, J.P.; Margiolaki, R.; Fitch, A.N.; Fox, G.C.; Prugoveeki, S.; Beckers, D.; Helliwell, J.R.; Helliwell, M.; Jones, R.H.; Roberts, M.A.; Miura, K.; Kahn, R.; Giacovazzo, C.; Altomare, A.; Caliandro, R.; Camalli, M.; Cuocci, C.; Moliterni, A.G.G.; Rizzi, R.; Hinrichsen, B.; Kern, A.; Coelho, A.A.; Degen, T.; Kokkinidis, M.; Fadouloglou, V.; Gazi, A.; Panopoulos, N.; Pinotsis, N.; Wilmanns, M.; Norrman, M.; Schluckebier, G.; Prugoveeki, B.; Dilovic, J.; Matkovic-Calogovic, D.; Bill, David; Markvardsen, A.; Grosse-Kunstleve, R.; Rius, J.; Glykos Nicholas, M.; Murshudov, G.N.

2007-01-01

X-ray diffraction is one of the most important method for obtaining information about the structure of proteins and thereby for gaining insight into fundamental biological and biochemical mechanisms. This seminar was dedicated to X-ray powder diffraction and was organized around 6 sessions: 1) what can powder diffraction do for proteins?, 2) adapting experimentally to proteins, 3) interpreting powder data, 4) the world of protein crystallography, 5) advancing methods for powder data analysis, and 6) transferable methods from single crystals. This document gathers the abstracts of the 23 papers presented. (A.C.)

Comparison of x-ray computed tomography, through-transmission ultrasound, and low-kV x-ray imaging for characterizing green-state ceramics

International Nuclear Information System (INIS)

Roberts, R.A.; Ellingson, W.A.; Vannier, M.W.

1985-06-01

Green-state MgAl 2 O 4 compact disk specimens have been studied by x-ray computed tomography (CT), through-transmission pulsed ultrasound, and low-kV x-ray imaging to compare the abilities of these nondestructive evaluation (NDE) methods to detect flaws and density variations. X-ray computed tomographic images were obtained from a 125-kV (peak) imaging system with a 512 x 512 matrix and a pixel size of 100 μm. A 3- to 10- MHz focused-beam ultrasonic transducer was used, together with special immersion techniques, to obtain topographical maps of acoustic attenuation and phase velocity; a 30 x 30 matrix was used in the ultrasonic scans. A 35-kV x-ray system with high-resolution type RR film was used to obtain conventional radiographs. Large-scale nonuniform density gradients were detected with CT and ultrasonics in supposedly uniform ceramic disks. In addition, inclusions in the green-state samples were detected by all three methods, with each method providing certain advantages. The influence of grain structure and other ceramic powder characteristics will be examined in the future. 5 refs., 9 figs

Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

Energy Technology Data Exchange (ETDEWEB)

Blagoev, K., E-mail: kblagoev@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Grozeva, M., E-mail: margo@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Malcheva, G., E-mail: bobcheva@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Neykova, S., E-mail: sevdalinaneikova@abv.bg [National Institute of Archaeology with Museum, Bulgarian Academy of Sciences, 2 Saborna, 1000 Sofia (Bulgaria)

2013-01-01

The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893–972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained.

Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

International Nuclear Information System (INIS)

Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

2013-01-01

The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893–972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained

New analytical method for asbestos determination in Syrian soils using X-ray diffraction

International Nuclear Information System (INIS)

Kassem, M.

2009-07-01

In this work, a standard samples have been prepared by mixing a definite quantity of soil with calculated concentration of asbestos; 1, 2, 4, 8, 10, 20, 40, 60, 80, 100% wt . The samples have been analyzed by x-ray powder diffraction using the same parameters ; 2θ between 5-90, detector step= 0.5 /30 sec. The diffraction peaks intensities have been chosen such a manner than no superposition with those of the soil. confidence levels has been used as accuracy method for error calculation of the peaks positions. (author)

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

Science.gov (United States)

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

Simulation study on unfolding methods for diagnostic X-rays and mixed gamma rays

International Nuclear Information System (INIS)

Hashimoto, Makoto; Ohtaka, Masahiko; Ara, Kuniaki; Kanno, Ikuo; Imamura, Ryo; Mikami, Kenta; Nomiya, Seiichiro; Onabe, Hideaki

2009-01-01

A photon detector operating in current mode that can sense X-ray energy distribution has been reported. This detector consists of a row of several segment detectors. The energy distribution is derived using an unfolding technique. In this paper, comparisons of the unfolding techniques among error reduction, spectrum surveillance, and neural network methods are discussed through simulation studies on the detection of diagnostic X-rays and gamma rays emitted by a mixture of 137 Cs and 60 Co. For diagnostic X-ray measurement, the spectrum surveillance and neural network methods appeared promising, while the error reduction method yielded poor results. However, in the case of measuring mixtures of gamma rays, the error reduction method was both sufficient and effective. (author)

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.

A comparison between the Structural Results obtained by X-ray Single Crystal Data and by Neutron Powder Data for BaVs/sb3/

International Nuclear Information System (INIS)

Marezio, M.

1986-01-01

The structure of BaVs/sb3/, as refined from X-ray single-crystal data to an R factor of 0.011, is compared to the structure of the same compound obtained from neutron powder data (Rsb(ro) = 6.82, Rsb(psilon) = 4.09). As expected, the X-ray standard deviations of the positional and thermal parameters are smaller than the corresponding neutron standard deviations. However, the dynamical disorder deduced from the anomalously large thermal vibrations of the vanadium atoms obtained from the X-ray data is also evidenced by the neutron refinement. On the other hand, the neutron standard deviations of the lattice parameters are smaller than the X-ray counterparts

Direct method of deconvolution. Application to the interpretation of X ray diffraction line profiles

International Nuclear Information System (INIS)

Louer, Daniel

1969-01-01

In the first parts of this research thesis, the author reports the development of an original method of correction of X ray profiles, and the comparison of the different correction schemes within the frame of the analysis of a specific aberration of the diffractometer: the receiver slot. Based on corrected profiles, the author applied the different methods leading to the calculation of the dimensions and shape of particles which form a hydroxide nickel powder. He reports the physical-chemical analysis of nickel and zinc basic nitrates. Although some basic salts lead to widened X diffraction profiles the interpretation of which remains to be made, this work remained limited to the application of the described methods to the nickel hydroxide sample resulting from an extended hydrolysis of nickel basic nitrates

X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

Science.gov (United States)

Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

2012-05-01

Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory.

A readout system for X-ray powder crystallography

CERN Document Server

Loukas, D; Pavlidis, A; Karvelas, E; Psycharis, K; Misiakos, V; Mousa, J; Dre, C

2000-01-01

A system for capturing and processing data, from radiation detectors, in the field of X-ray crystallography has been developed. The system includes a custom-made mixed analog-digital 16-channel VLSI circuit in 50 mu m pitch. Each channel comprises a charge amplifier, a shaper, a comparator and a 21-bit counter. The circuit can be scaled in a daisy chain configuration. Data acquisition is performed with a custom made PCI card while the control software is developed with Visual C++ under the MS Windows NT environment. Performance of a fully operational system, in terms of electronic noise, statistical variations and data capture speed is presented. The noise level permits counting of X-rays down to 8 keV while the counting capability is in excess of 200 kHz. The system is intended for X-ray crystallography with silicon detectors.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

Science.gov (United States)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science

Czech Academy of Sciences Publication Activity Database

Švarcová, Silvie; Kočí, Eva; Bezdička, Petr; Hradil, David; Hradilová, J.

2010-01-01

Roč. 398, č. 2 (2010), s. 1061-1076 ISSN 1618-2642 R&D Projects: GA AV ČR KJB200320901 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray micro-diffraction * quantitative phase analysis * forensic Subject RIV: CA - Inorganic Chemistry Impact factor: 3.841, year: 2010

Quasimonochromatic x-ray computed tomography by the balanced filter method using a conventional x-ray source

International Nuclear Information System (INIS)

Saito, Masatoshi

2004-01-01

A quasimonochromatic x-ray computed tomography (CT) system utilizing balanced filters has recently been developed for acquiring quantitative CT images. This system consisted of basic components such as a conventional x-ray generator for radiography, a stage for mounting and rotating objects, and an x-ray line sensor camera. Metallic sheets of Er and Yb were used as the balanced filters for obtaining quasimonochromatic incident x rays that include the characteristic lines of the W Kα doublet from a tungsten target. The mean energy and energy width of the quasimonochromatic x rays were determined to be 59.0 and 1.9 keV, respectively, from x-ray spectroscopic measurements using a high-purity Ge detector. The usefulness of the present x-ray CT system was demonstrated by obtaining spatial distributions of the linear attenuation coefficients of three selected samples--a 20 cm diameter cylindrical water phantom, a 3.5 cm diameter aluminum rod, and a human head phantom. The results clearly indicate that this apparatus is surprisingly effective for estimating the distribution of the linear attenuation coefficients without any correction of the beam-hardening effect. Thus, implementing the balanced filter method on an x-ray CT scanner has promise in producing highly quantitative CT images

Techniques for materials research with synchrotron radiation x-rays

International Nuclear Information System (INIS)

Bowen, D.K.

1983-01-01

A brief introductory survey is presented of the properties and generation of synchrotron radiation and the main techniques developed so far for its application to materials problems. Headings are:synchrotron radiation; X-ray techniques in synchrotron radiation (powder diffraction; X-ray scattering; EXAFS (Extended X-ray Absorption Fine Structure); X-ray fluorescent analysis; microradiography; white radiation topography; double crystal topography); future developments. (U.K.)

Characterization of Metal Powders Used for Additive Manufacturing.

Science.gov (United States)

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

Characterization of Metal Powders Used for Additive Manufacturing

Science.gov (United States)

Slotwinski, JA; Garboczi, EJ; Stutzman, PE; Ferraris, CF; Watson, SS; Peltz, MA

2014-01-01

Additive manufacturing (AM) techniques1 can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process. PMID:26601040

Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

Science.gov (United States)

Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

2003-10-01

The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

X-ray and gamma ray waveguide, cavity and method

International Nuclear Information System (INIS)

Vali, V.; Krogstad, R.S.; Willard, H.R.

1978-01-01

An x-ray and gamma ray waveguide, cavity, and method for directing electromagnetic radiation of the x-ray, gamma ray, and extreme ultraviolet wavelengths are described. A hollow fiber is used as the waveguide and is manufactured from a material having an index of refraction less than unity for these wavelengths. The internal diameter of the hollow fiber waveguide and the radius of curvature for the waveguide are selectively predetermined in light of the wavelength of the transmitted radiation to minimize losses. The electromagnetic radiation is obtained from any suitable source ad upon introduction into the waveguide is transmitted along a curvilinear path. The waveguide may be formed as a closed loop to create a cavity or may be used to direct the electromagnetic radiation to a utilization site

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.

Ray tracing method for simulation of laser beam interaction with random packings of powders

Science.gov (United States)

Kovalev, O. B.; Kovaleva, I. O.; Belyaev, V. V.

2018-03-01

Selective laser sintering is a technology of rapid manufacturing of a free form that is created as a solid object by selectively fusing successive layers of powder using a laser. The motivation of this study is due to the currently insufficient understanding of the processes and phenomena of selective laser melting of powders whose time scales differ by orders of magnitude. To construct random packings from mono- and polydispersed solid spheres, the algorithm of their generation based on the discrete element method is used. A numerical method of ray tracing is proposed that is used to simulate the interaction of laser radiation with a random bulk packing of spherical particles and to predict the optical properties of the granular layer, the extinction and absorption coefficients, depending on the optical properties of a powder material.

The Crystal Structure of the Malaria Pigment Hemozoin as Elucidated by X-ray Powder Diffraction

DEFF Research Database (Denmark)

Straasø, Tine

survival. Successful inhibition of hemozoin crystallization will lead to parasitic death and thus break the cycle. The aim of this thesis is to elucidate the structure of hemozoin by means of X-ray diffraction techniques. Knowledge of the structure will help facilitate intelligent drug design in the future....... As part of the project an all-in-vacuum powder diffractometer was developed, which provides data with a minimum background level and an improved signal-to-noise ratio. Moreover, the diffractometer is designed with the particular purpose of decreasing the number of parameters to be fitted. Installation...

X-ray Powder Diffraction for Characterization of Raw Materials in Banknotes.

Science.gov (United States)

Marabello, Domenica; Benzi, Paola; Lombardozzi, Antonietta; Strano, Morela

2017-07-01

We report about the X-ray powder diffraction characterization of crystalline materials used to produce genuine and counterfeit banknotes, performed with a single-crystal diffractometer that permits fast and nondestructive measurements in different 0.5-mm sized areas; 20-euro denomination genuine banknotes were analyzed, and results were compared with counterfeit banknotes. The analysis shows that the papers used to print real banknotes are composed, as expected, of cotton-based cellulose and titanium dioxide as crystalline additive, but different polymorphs of TiO 2 for different emission countries are evidenced. The counterfeit banknotes are composed of cellulose based on wood pulp; moreover, an unexpected significant quantity of TiO 2 was found to be mixed with calcite, indicating that the paper employed by forgers is not simply a common low-cost type. The crystalline index and intensity ratios between the peaks attributable to cellulose and fillers can provide additional information to trace back paper suppliers for forensic purposes. © 2017 American Academy of Forensic Sciences.

Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

Science.gov (United States)

Yamamura, Shigeo; Momose, Yasunori

2003-06-18

The purpose of this study is to characterize the monoclinic crystals in tablets by using X-ray powder diffraction data and to evaluate the deformation feature of crystals during compression. The monoclinic crystals of acetaminophen and benzoic acid were used as the samples. The observed X-ray diffraction intensities were fitted to the analytic expression, and the fitting parameters, such as the lattice parameters, the peak-width parameters, the preferred orientation parameter and peak asymmetric parameter were optimized by a non-linear least-squares procedure. The Gauss and March distribution functions were used to correct the preferred orientation of crystallites in the tablet. The March function performed better in correcting the modification of diffraction intensity by preferred orientation of crystallites, suggesting that the crystallites in the tablets had fiber texture with axial orientation. Although a broadening of diffraction peaks was observed in acetaminophen tablets with an increase of compression pressure, little broadening was observed in the benzoic tablets. These results suggest that "acetaminophen is a material consolidating by fragmentation of crystalline particles and benzoic acid is a material consolidating by plastic deformation then occurred rearrangement of molecules during compression". A pattern-fitting procedure is the superior method for characterizing the crystalline drugs of monoclinic crystals in the tablets, as well as orthorhombic isoniazid and mannitol crystals reported in the previous paper.

A program for the derivation of crystal unit cell parameters from X-ray powder diffraction measurements

International Nuclear Information System (INIS)

Ferguson, I.F.; Rogerson, A.H.

1984-01-01

The program, FIRESTAR, determines the dimensions of a crystallographic unit cell from a set of X-ray powder diffraction measurements corresponding to a set of Bragg reflections, provided that the crystal system applicable is known and the Bragg reflections have been indexed. The program includes a range of possible extrapolation functions, and the data may be weighted. Provision is made for detecting and rejecting a single 'bad' measurement, and then rejecting measurements which lie outside an error limit set in the input data. (orig.)

Geometric estimation method for x-ray digital intraoral tomosynthesis

Science.gov (United States)

Li, Liang; Yang, Yao; Chen, Zhiqiang

2016-06-01

It is essential for accurate image reconstruction to obtain a set of parameters that describes the x-ray scanning geometry. A geometric estimation method is presented for x-ray digital intraoral tomosynthesis (DIT) in which the detector remains stationary while the x-ray source rotates. The main idea is to estimate the three-dimensional (3-D) coordinates of each shot position using at least two small opaque balls adhering to the detector surface as the positioning markers. From the radiographs containing these balls, the position of each x-ray focal spot can be calculated independently relative to the detector center no matter what kind of scanning trajectory is used. A 3-D phantom which roughly simulates DIT was designed to evaluate the performance of this method both quantitatively and qualitatively in the sense of mean square error and structural similarity. Results are also presented for real data acquired with a DIT experimental system. These results prove the validity of this geometric estimation method.

A comparative study of the use of powder X-ray diffraction, Raman and near infrared spectroscopy for quantification of binary polymorphic mixtures of piracetam.

Science.gov (United States)

Croker, Denise M; Hennigan, Michelle C; Maher, Anthony; Hu, Yun; Ryder, Alan G; Hodnett, Benjamin K

2012-04-07

Diffraction and spectroscopic methods were evaluated for quantitative analysis of binary powder mixtures of FII(6.403) and FIII(6.525) piracetam. The two polymorphs of piracetam could be distinguished using powder X-ray diffraction (PXRD), Raman and near-infrared (NIR) spectroscopy. The results demonstrated that Raman and NIR spectroscopy are most suitable for quantitative analysis of this polymorphic mixture. When the spectra are treated with the combination of multiplicative scatter correction (MSC) and second derivative data pretreatments, the partial least squared (PLS) regression model gave a root mean square error of calibration (RMSEC) of 0.94 and 0.99%, respectively. FIII(6.525) demonstrated some preferred orientation in PXRD analysis, making PXRD the least preferred method of quantification. Copyright © 2012 Elsevier B.V. All rights reserved.

Electron Paramagnetic Resonance and X-ray Diffraction of Boron- and Phosphorus-Doped Nanodiamonds

Science.gov (United States)

Binh, Nguyen Thi Thanh; Dolmatov, V. Yu.; Lapchuk, N. M.; Shymanski, V. I.

2017-11-01

Powders of boron- and phosphorus-doped detonation nanodiamonds and sintered pellets of non-doped nanodiamond powders were studied using electron paramagnetic resonance and x-ray diffraction. Doping of detonation nanodiamond crystals with boron and phosphorus was demonstrated to be possible. These methods could be used to diagnose diamond nanocrystals doped during shock-wave synthesis.

FTIR spectroscopy and X-ray powder diffraction characterization of microcrystalline cellulose obtained from alfa fibers

Directory of Open Access Journals (Sweden)

Trache D.

2013-07-01

Full Text Available Many cereal straws have been used as raw materials for the preparation of microcrystalline cellulose (MCC. These raw materials were gradually replaced with wood products; nevertheless about 10% of the world overall pulp production is obtained from non-wood raw material. The main interest in pulp made from straw is that it provides excellent fibres for different industries with special properties, and that it is the major available source of fibrous raw material in some geographical areas. The aim of the present work was to characterize microcrystalline cellulose prepared from alfa fibers using the hydrolysis process. The products obtained are characterized with FTIR spectroscopy and X-ray powder diffraction. As a result, FTIR spectroscopy is an appropriate technique for studying changes occurred by any chemical treatment. The spectrum of alfa grass stems shows the presence of lignin and hemicelluloses. However, the cellulose spectrum indicates that the extraction of lignin and hemicellulose was effective. The X-ray analysis indicates that the microcrystalline cellulose is more crystalline than the source material.

Comparison between powder and slices diffraction methods in teeth samples

Energy Technology Data Exchange (ETDEWEB)

Colaco, Marcos V.; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (IF/UERJ), RJ (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada; Porto, Isabel M. [Universidade Estadual de Campinas (FOP/UNICAMP), Piracicaba, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia; Gerlach, Raquel F. [Universidade de Sao Paulo (FORP/USP), Rieirao Preto, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia, Estomatologia e Fisiologia; Costa, Fanny N. [Coordenacao dos Programas de Pos-Graduacao de Engenharia (LIN/COPPE/UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear

2011-07-01

Propose different methods to obtain crystallographic information about biological materials are important since powder method is a nondestructive method. Slices are an approximation of what would be an in vivo analysis. Effects of samples preparation cause differences in scattering profiles compared with powder method. The main inorganic component of bones and teeth is a calcium phosphate mineral whose structure closely resembles hydroxyapatite (HAp). The hexagonal symmetry, however, seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. Were analyzed ten third molar teeth. Five teeth were separated in enamel, detin and circumpulpal detin powder and five in slices. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. The LNLS synchrotron light source is composed of a 1.37 GeV electron storage ring, delivering approximately 4x10{sup -1}0 photons/s at 8 keV. A double-crystal Si(111) pre-monochromator, upstream of the beamline, was used to select a small energy bandwidth at 11 keV . Scattering signatures were obtained at intervals of 0.04 deg for angles from 24 deg to 52 deg. The human enamel experimental crystallite size obtained in this work were 30(3)nm (112 reflection) and 30(3)nm (300 reflection). These values were obtained from measurements of powdered enamel. When comparing the slice obtained 58(8)nm (112 reflection) and 37(7)nm (300 reflection) enamel diffraction patterns with those generated by the powder specimens, a few differences emerge. This work shows differences between powder and slices methods, separating characteristics of sample of the method's influence. (author)

Comparison between powder and slices diffraction methods in teeth samples

International Nuclear Information System (INIS)

Colaco, Marcos V.; Barroso, Regina C.; Porto, Isabel M.; Gerlach, Raquel F.; Costa, Fanny N.

2011-01-01

Propose different methods to obtain crystallographic information about biological materials are important since powder method is a nondestructive method. Slices are an approximation of what would be an in vivo analysis. Effects of samples preparation cause differences in scattering profiles compared with powder method. The main inorganic component of bones and teeth is a calcium phosphate mineral whose structure closely resembles hydroxyapatite (HAp). The hexagonal symmetry, however, seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. Were analyzed ten third molar teeth. Five teeth were separated in enamel, detin and circumpulpal detin powder and five in slices. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. The LNLS synchrotron light source is composed of a 1.37 GeV electron storage ring, delivering approximately 4x10 -1 0 photons/s at 8 keV. A double-crystal Si(111) pre-monochromator, upstream of the beamline, was used to select a small energy bandwidth at 11 keV . Scattering signatures were obtained at intervals of 0.04 deg for angles from 24 deg to 52 deg. The human enamel experimental crystallite size obtained in this work were 30(3)nm (112 reflection) and 30(3)nm (300 reflection). These values were obtained from measurements of powdered enamel. When comparing the slice obtained 58(8)nm (112 reflection) and 37(7)nm (300 reflection) enamel diffraction patterns with those generated by the powder specimens, a few differences emerge. This work shows differences between powder and slices methods, separating characteristics of sample of the method's influence. (author)

Model independent method to deconvolve hard X-ray spectra

Energy Technology Data Exchange (ETDEWEB)

Polcaro, V.F.; Bazzano, A.; Ubertini, P.; La Padula, C. (Consiglio Nazionale delle Ricerche, Frascati (Italy). Lab. di Astrofisica Spaziale); Manchanda, R.K. (Tata Inst. of Fundamental Research, Bombay (India))

1984-07-01

A general purpose method to deconvolve the energy spectra detected by means of the use of a hard X-ray telescope is described. The procedure does not assume any form of input spectrum and the observed energy loss spectrum is directly deconvolved into the incident photon spectrum, the form of which can be determined independently of physical interpretation of the data. Deconvolution of the hard X-ray spectrum of Her X-1, detected during the HXR 81M experiment, by the method independent method is presented.

X-ray chemical analyzer for field applications

International Nuclear Information System (INIS)

Gamba, O.O.M.

1977-01-01

A self-supporting portable field multichannel x-ray chemical analyzer system is claimed. It comprises a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an x-ray energy dispersive spectrometry technique

Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

International Nuclear Information System (INIS)

Rukiah, M.; Assaad, Th.

2012-06-01

The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

Sulfur content measurement in coal by X-ray fluorescence method

International Nuclear Information System (INIS)

Cechak, T.; Thinova, L.

2001-01-01

X-ray fluorescence, using backscattering, was employed in the determination of sulfur content and ash content measurement in coal. The results of the methods are given to illustrate the differences between the chemical analysis and X-ray fluorescence method.

Bulk synthesis of nanocrystalline urania powders by citrate gel-combustion method

International Nuclear Information System (INIS)

Sanjay Kumar, D.; Ananthasivan, K.; Venkata Krishnan, R.; Amirthapandian, S.; Dasgupta, Arup

2016-01-01

Bulk quantities (60 g) of nanocrystalline (nc) free flowing urania powders with crystallite size ranging from 38 to 252 nm have been synthesized for the first time by the citrate gel combustion method. A systematic study of the influence of the fuel (citric acid) to oxidant (nitrate) ratio (R) on the characteristics of the urania powders has been carried out for the first time. Mixture with an “R” value of 0.25 exhibited a vigorous auto-ignition reaction. This reaction was investigated with Differential Scanning Calorimetry (DSC) and in-situ thermogravimetry coupled with differential thermal analysis and mass spectrometry (TG-DTA-MS). The bulk density, specific surface area, X-ray crystallite size, residual carbon and size distribution of particles of this powder were unique. Microscopic and microstructural investigation of selected samples revealed the presence of nanocrystals with irregular exfoliated morphology; their Electron Energy Loss Spectra testified the covalency of the U–O bond. - Highlights: • Bulk quantities of nanocrystalline urania were prepared for the first time using citrate gel combustion method. • Volume combustion was observed in mixtures with fuel to nitrate ratio (R) 0.25. • The value of R was found to significantly influence the characteristics of the final product. • Typical exfoliated microstructure and nanopores were observed. • Established correlation between particle size distribution and bulk density, X-ray crystallite size and lattice strain. • Relationship between fuel to nitrate (R) mole ratio and physical characteristics of powders were also established.

Determination of chlorine in coal by X-ray fluorescence spectrometry method

Energy Technology Data Exchange (ETDEWEB)

Marek, S.; Bojarska, K. [Central Mining Institute, Katowice (Poland). Dept. of Environmental Monitoring

1997-12-31

Determination of chlorine contents in coal is essential for both environmental protection and its technological use. The existing method of chlorine determination in coal are titration methods which have considerable errors particularly in the low concentration range. The elaborated method with the use of X-ray fluorescence spectrometry in a comparison to the other methods is much faster and has better precision and accuracy. The principle of the method lies in the measurement of X-ray fluorescence radiation intensity which is emitted by chlorine in a sample and its comparison with standards. The calibration of the elaborated XRF method is based on natural coals having various concentrations of chlorine within the whole range of its occurrence in Polish coals. Concentrations for the calibration purpose were obtained by the determination of chlorine contents in selected coals by atomic absorption spectrometry method. The procedure of sample preparation for direct X-ray measurements, instrumental measuring conditions and the way of calibration curve preparation are described in the paper. All X-ray measurements were done with a Phillips sequential X-ray fluorescence spectrometer. A double anode Cr-Au X-ray tube with maximum power 3000 MW was used as the excitation source. 5 figs., 4 tabs.

Synthesis and characterization of lead zirconate titanate powders obtained by the oxidant peroxo method

International Nuclear Information System (INIS)

Camargo, Emerson R.; Leite, Edson R.; Longo, Elson

2009-01-01

Lead zirconate titanate (PbZr 1-x Ti x O 3 ) was synthesized by the 'oxidant peroxo method (OPM)' with 'x' between 0.25 and 0.50. Titanium metal was dissolved into a hydrogen peroxide/ammonia aqueous solution, followed by the addition of lead and zirconium nitrate solution. The amorphous precipitated precursor obtained was crystallized by heat treatment between 400 and 1000 deg. C. Images of transmission microscopy showed spherical particles with average diameter between 20 and 60 nm, and the presence of necks between particles treated at 700 deg. C. All of the unpressed powders were characterized by X-ray diffractometry and FT-Raman spectroscopy. Powder samples with 'x' up to 0.35 showed rhombohedral structure when treated at temperatures higher than 500 deg. C, and tetragonal structure when 'x' was higher than 0.40. Analysis of XRD and Raman spectroscopy of the precursor powders showed amorphous-like structures, however powders treated at 400 deg. C showed a structure identified as an intermediate pyrochlore phase, independently of the Zr and Ti mole ratio

X-Ray Diffraction Studies on the Thermal Stability of Calcium ...

African Journals Online (AJOL)

Calcium-Strontium hydroxyapatite (HAP) solid solutions in the presence and absence of diethylamine (DEA) were prepared by the method of co-precipitation from basic media. The samples were heated at 773.15K in a furnace. Characterization of the samples by x-ray powder diffractometry, atomic absorption spectroscopy ...

Powder X-ray diffraction studies of structural and kinetic aspects of polymorphism

International Nuclear Information System (INIS)

Chan, F.C.

1999-01-01

Polymorphism is a poorly understood phenomenon that is of considerable technological interest to the pharmaceutical industry. The polymorph selected can influence the bioavailability, processing and stability of the pharmaceutical dosage form. In this study structural, kinetic and thermodynamics aspects of polymorphism and polymorphic phase transformations have been examined using powder X-ray diffraction (PXRD). The compound sulphathiazole is a well-studied model in the investigation of polymorphism and crystal growth. There are five known polymorphic forms and the structure of form V was unknown until this study. The difficulty has been that it has not been possibly to prepare crystals of appropriate size and quality for single crystal diffraction. Furthermore, structure solution from powder data for organic molecules is almost impossible. Despite the challenge the structure of sulphathiazole form V have been solved ab initio from powder data using direct methods. With 16 non-hydrogen atoms in the molecule and two molecules in the asymmetric unit, this structure represents a significant advance in terms of the complexity of an organic structure solved from PXRD data. The structural data should be invaluable for rationalizing experimental observations and the development of theoretical ideas regarding polymorphism and crystal growth. The second part of the study, has examined kinetics of polymorphic phase transformations as a function of pressure combined with temperature using real-time synchrotron PXRD. The significance of pressure arises from the fact that phase transitions can be induced in pharmaceuticals during tabletting. The phase transformation behaviour of rubidium iodide (chosen as a simple test model) has been investigated as a function of isobaric pressure at ambient and elevated temperatures. The kinetics have been characterized by using the Johnson-Melil-Avrami equation. The effect of successive cycling across the transition pressure was also

Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

International Nuclear Information System (INIS)

Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

2004-01-01

The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out

Conformational analysis of an acyclic tetrapeptide: ab-initio structure determination from X-ray powder diffraction, Hirshfeld surface analysis and electronic structure.

Science.gov (United States)

Das, Uday; Naskar, Jishu; Mukherjee, Alok Kumar

2015-12-01

A terminally protected acyclic tetrapeptide has been synthesized, and the crystal structure of its hydrated form, Boc-Tyr-Aib-Tyr-Ile-OMe·2H2O (1), has been determined directly from powder X-ray diffraction data. The backbone conformation of tetrapeptide (1) exhibiting two consecutive β-turns is stabilized by two 4 → 1 intramolecular N-H · · · O hydrogen bonds. In the crystalline state, the tetrapeptide molecules are assembled through water-mediated O-H · · · O hydrogen bonds to form two-dimensional molecular sheets, which are further linked by intermolecular C-H · · · O hydrogen bonds into a three-dimensional supramolecular framework. The molecular electrostatic potential (MEP) surface of (1) has been used to supplement the crystallographic observations. The nature of intermolecular interactions in (1) has been analyzed quantitatively through the Hirshfeld surface and two-dimensional fingerprint plot. The DFT optimized molecular geometry of (1) agrees closely with that obtained from the X-ray structure analysis. The present structure analysis of Boc-Tyr-Aib-Tyr-Ile-OMe·2H2 O (1) represents a case where ab-initio crystal structure of an acyclic tetrapeptide with considerable molecular flexibility has been accomplished from laboratory X-ray powder diffraction data. Copyright © 2015 European Peptide Society and John Wiley & Sons, Ltd.

Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction

DEFF Research Database (Denmark)

Karjalainen, Milja; Airaksinen, Sari; Rantanen, Jukka

2005-01-01

The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form...... of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity...... to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting...

Titanium dioxide nanoparticles: synthesis, X-Ray line analysis and chemical composition study

Energy Technology Data Exchange (ETDEWEB)

Chenari, Hossein Mahmoudi, E-mail: mahmoudi_hossein@guilan.ac.ir, E-mail: h.mahmoudiph@gmail.com [University of Guilan, Rasht (Iran, Islamic Republic of); Seibel, Christoph; Hauschild, Dirk; Reinert, Friedrich [Karlsruhe Institute of Technology - KIT, Gemeinschaftslabor für Nanoanalytik, Karlsruhe (Germany); Abdollahian, Hossein [Nanotechnology Research Center of Urmia University, Urmia, (Iran, Islamic Republic of)

2016-11-15

TiO{sub 2} nanoparticles have been synthesized by the sol-gel method using titanium alkoxide and isopropanol as a precursor. The structural properties and chemical composition of the TiO{sub 2} nanoparticles were studied using X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy.The X-ray powder diffraction pattern confirms that the particles are mainly composed of the anatase phase with the preferential orientation along [101] direction. The physical parameters such as strain, stress and energy density were investigated from the Williamson- Hall (W-H) plot assuming a uniform deformation model (UDM), and uniform deformation energy density model (UDEDM). The W-H analysis shows an anisotropic nature of the strain in nano powders. The scanning electron microscopy image shows clear TiO{sub 2} nanoparticles with particle sizes varying from 60 to 80nm. The results of mean particle size of TiO{sub 2} nanoparticles show an inter correlation with the W-H analysis and SEM results. Our X-ray photoelectron spectroscopy spectra show that nearly a complete amount of titanium has reacted to TiO{sub 2}. (author)

Structural studies of carbon nanotubes by powder x-ray diffraction at SPring-8 and KEK PF

CERN Document Server

Maniwa, Y; Fujiwara, A

2003-01-01

Powder X-ray diffraction (XRD) studies on carbon nanotubes (CNTs) using synchrotron radiation are reported. In spite of the observed broad XRD peak profiles of two-dimensional triangular (hexagonal) lattice of single-wall carbon nanotubes (SWNTs), it was shown that useful structural information, such as the tube diameter and its distribution, can be deduced from detailed analysis of the characteristic XRD patterns. In particular, powder-XRD measurements were performed to study the phase transition of encapsulated materials inside SWNTs. In the C sub 7 sub 0 -one dimensional (1D) crystals formed inside SWNTs, importance of one-dimensionality in the C sub 7 sub 0 -molecular dynamics was suggested. It was also shown that water inside SWNTs undergoes a phase transition from liquid to an ice-nanotube structure below -38degC. Conversion process from SWNT to double-wall carbon nanotube (DWNT) was also studied by XRD.

Effect of powder sample granularity on fluorescent intensity and on thermal parameters in x-ray diffraction Rietveld analysis

International Nuclear Information System (INIS)

Sparks, C.J.; Specht, E.D.; Ice, G.E.; Kumar, R.; Zschack, P.; Shiraishi, T.; Hisatsune, K.

1991-01-01

The effect of sample granularity on diffracted x-ray intensity was evaluated by measuring the 2θ dependence of x-ray fluorescence from various samples. Measurements were made in the symmetric geometry on samples ranging from single crystals to highly absorbing coarse powders. A characteristic shape for the absorption correction was observed. A demonstration of the sensitivity of Rietveld refined site occupation parameters is made on CuAu and Cu 50 Au 44 Ni 6 alloys refined with and without granularity corrections. These alloys provide a good example of the effect of granularity due to their large linear x-ray absorption coefficients. Sample granularity and refined thermal parameters obtained from the Rietveld analysis were found to be correlated. Without a granularity correction, the refined thermal parameters are too low and can actually become negative in an attempt to compensate for granularity. A general shape for granularity correction can be included in refinement procedures. If no granularity correction is included, data should be restricted to above 30 degrees 2θ, and thermal parameters should be ignored unless extreme precautions are taken to produce >5 μm particles and high packing densities

Methods of X-ray examination of condylar knee replacement

International Nuclear Information System (INIS)

Vavrik, P.

1988-01-01

A detailed description is presented of the methodology of X-ray examination of patients with a condylar knee replacement. Preoperative examination includes standard anterio-posterior and lateral projections, axial projection of the patella in 30 deg flexion of the knee, examination of the mechanical axis of the extremity on a 90 x 30 format and the radioscopic assessment of the centre of the hip joint, essential for the correct centering of the knee implant. Immediately after surgery the position of the implant is checked in two standard projections. Another X-ray check is made after six weeks, before partial loading of the joint is permitted. A complete X-ray examination is made prior to the full loading of the knee joint. The methods are also discussed of the X-ray evaluation of complications such as aseptic loosening of the components, infection, instability, fractures. The general solution od these problems is described. The necessity is underlined of the deliberate and qualified indication of X-ray examinations. The basic prerequisites are listed for reducing the present considerable radiation burden of these patients in the course of the many X-ray examinations. (author). 7 figs., 3 tab., 6 refs

A wavelet transform algorithm for peak detection and application to powder x-ray diffraction data.

Science.gov (United States)

Gregoire, John M; Dale, Darren; van Dover, R Bruce

2011-01-01

Peak detection is ubiquitous in the analysis of spectral data. While many noise-filtering algorithms and peak identification algorithms have been developed, recent work [P. Du, W. Kibbe, and S. Lin, Bioinformatics 22, 2059 (2006); A. Wee, D. Grayden, Y. Zhu, K. Petkovic-Duran, and D. Smith, Electrophoresis 29, 4215 (2008)] has demonstrated that both of these tasks are efficiently performed through analysis of the wavelet transform of the data. In this paper, we present a wavelet-based peak detection algorithm with user-defined parameters that can be readily applied to the application of any spectral data. Particular attention is given to the algorithm's resolution of overlapping peaks. The algorithm is implemented for the analysis of powder diffraction data, and successful detection of Bragg peaks is demonstrated for both low signal-to-noise data from theta-theta diffraction of nanoparticles and combinatorial x-ray diffraction data from a composition spread thin film. These datasets have different types of background signals which are effectively removed in the wavelet-based method, and the results demonstrate that the algorithm provides a robust method for automated peak detection.

Sample cell for powder x-ray diffraction at up to 500 bars and 200 deg. C

International Nuclear Information System (INIS)

Jupe, Andrew C.; Wilkinson, Angus P.

2006-01-01

A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube

Standardized method for reproducing the sequential X-rays flap

International Nuclear Information System (INIS)

Brenes, Alejandra; Molina, Katherine; Gudino, Sylvia

2009-01-01

A method is validated to estandardize in the taking, developing and analysis of bite-wing radiographs taken in sequential way, in order to compare and evaluate detectable changes in the evolution of the interproximal lesions through time. A radiographic positioner called XCP® is modified by means of a rigid acrylic guide, to achieve proper of the X ray equipment core positioning relative to the XCP® ring and the reorientation during the sequential x-rays process. 16 subjects of 4 to 40 years old are studied for a total number of 32 registries. Two x-rays of the same block of teeth of each subject have been taken in sequential way, with a minimal difference of 30 minutes between each one, before the placement of radiographic attachment. The images have been digitized with a Super Cam® scanner and imported to a software. The measurements in X and Y-axis for both x-rays were performed to proceed to compare. The intraclass correlation index (ICI) has shown that the proposed method is statistically related to measurement (mm) obtained in the X and Y-axis for both sequential series of x-rays (p=0.01). The measures of central tendency and dispersion have shown that the usual occurrence is indifferent between the two measurements (Mode 0.000 and S = 0083 and 0.109) and that the probability of occurrence of different values is lower than expected. (author) [es

The determination of gold in activated charcoal by use of a loose-powder technique and x-ray-fluorescence spectrometry

International Nuclear Information System (INIS)

Balaes, A.M.E.

1984-01-01

The method of analysis described is applicable to samples of activated charcoal with a gold concentration of 15g/t and higher. The use of a loose-powder technique minimizes the time taken for the preparation of samples. A platinum internal standard is used for the correction for matrix effects and for differences that could be caused by the packing of the loose charcoal into liquid-sample cups. The precision of the method ranges from a relative standard deviation of 0,085 to 0,016 for concentrations of gold from 67 to 3800g/t respectively. The agreement between the recommended values for a set of reference samples and the values obtained by the X-ray-fluorescence method is better than 3 per cent. The overall time required for the analysis of ten samples and standards is approximately 1 hour. A detailed laboratory method and a computer programme for the calculations are given as appendices

Method and apparatus for scanning x-ray tomography

International Nuclear Information System (INIS)

Albert, R.D.

1988-01-01

In a method of producing a tomographic image of a subject that includes the steps of generating X-rays at a moving origin point by directing a charged particle beam to a target surface, deflecting the charged particle beam to travel the origin point through a predetermined raster scan at the surface, detecting variations of X-ray intensity during the course of the raster scan at spaced apart detection points situated at the opposite side of the subject from the origin point, generating a first sequence of data values that is indicative of variations of X-ray intensity at a first of the detection points at successive times during the course of the raster scan and generating at least a second sequence of data values that is indicative of variations of X-ray intensity at a second of the detection points at successive times during the course of the same raster scan, the improvement is described comprising: combining successive individual data values of the first sequence that are generated by X-rays from successive particular locations in the raster scan with at least individual data values of the second sequence that are generated by X-rays from predetermined successive different locations in the same raster scan in order to produce a composite sequence of data values, and producing an image corresponding to at least a portion of the raster scan which depicts variations of the magnitude of successive data values of the composite sequence

Twenty-seventh annual conference applications of x-ray analysis

International Nuclear Information System (INIS)

McCarthy, G.J.; Ruud, C.O.

1978-01-01

Abstracts are presented of papers given at the conference. Topics covered include: special techniques in powder diffraction; specimen handling; x-ray fluorescence applications; applications of XRD and x-ray imaging; progress in the reduction of matrix effects in XRF; evaluation of XRD patterns; XRF innovations; XRD stress analysis and mathematical data analysis

X-ray computed tomography imaging method which is immune to beam hardening effect

International Nuclear Information System (INIS)

Kanno, Ikuo; Uesaka, Akio; Nomiya, Seiichiro; Onabe, Hideaki

2009-01-01

For the easy treatment of cancers, early finding of them is an important theme of study. X-ray transmission measurement and computed tomography (CT) are powerful tools for finding cancers. The x-ray CT shows cross sectional view of human body and is able to detect small cancers such as 1 cm in diameter. The CT, however, gives very high dose exposure to human body: some 10 to 1000 times higher dose exposure than the chest radiography. It is not possible to have medical health check using CT frequently, in view of both individual and public accumulated dose exposures. The authors have been working on the reduction of dose exposure in x-ray transmission measurements in case of detecting iodine contrast media, which concentrates in cancers. In our method, energy information of x-rays is employed: in conventional x-ray transmission measurements, x-rays are measured as current and the energy of each x-ray is ignored. The numbers of x-ray events, φ 1 and φ 2 , of which energies are lower and higher than the one of iodine K-edge, respectively, are used for the estimation of iodine thickness in cancers. Moreover, high energy x-rays, which are not sensitive to the absorption by iodine, are cut by a filter made of higher atomic number material than iodine. We call this method filtered x-ray energy subtraction (FIX-ES) method. This FIX-ES method was shown twice as sensitive to iodine than current measurement method. With the choice of filter thickness, minimum dose exposure in FIX-ES is 30% of that when white x-rays are employed. In the study described above, we concentrated on the observation of cancer part. In this study, a cancer phantom in normal tissue is observed by FIX-ES method. The results are compared with the ones obtained by current measurement method. (author)

Synthesis and characterization of lead zirconate titanate powders obtained by the oxidant peroxo method

Energy Technology Data Exchange (ETDEWEB)

Camargo, Emerson R. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Department of Chemistry, UFSCar-Federal University of Sao Carlos, Rod. Washington Luis km 235, CP 676, Sao Carlos SP, 13565-905 (Brazil)], E-mail: camargo@ufscar.br; Leite, Edson R. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Department of Chemistry, UFSCar-Federal University of Sao Carlos, Rod. Washington Luis km 235, CP 676, Sao Carlos SP, 13565-905 (Brazil)], E-mail: derl@power.ufscar.br; Longo, Elson [Department of Biochemistry, Chemistry Institute of Araraquara, UNESP, Sao Paulo State University Rua Francisco Degni, CP 355 Araraquara SP, 14801-907 Brazil (Brazil)], E-mail: elson@iq.unesp.br

2009-02-05

Lead zirconate titanate (PbZr{sub 1-x}Ti{sub x}O{sub 3}) was synthesized by the 'oxidant peroxo method (OPM)' with 'x' between 0.25 and 0.50. Titanium metal was dissolved into a hydrogen peroxide/ammonia aqueous solution, followed by the addition of lead and zirconium nitrate solution. The amorphous precipitated precursor obtained was crystallized by heat treatment between 400 and 1000 deg. C. Images of transmission microscopy showed spherical particles with average diameter between 20 and 60 nm, and the presence of necks between particles treated at 700 deg. C. All of the unpressed powders were characterized by X-ray diffractometry and FT-Raman spectroscopy. Powder samples with 'x' up to 0.35 showed rhombohedral structure when treated at temperatures higher than 500 deg. C, and tetragonal structure when 'x' was higher than 0.40. Analysis of XRD and Raman spectroscopy of the precursor powders showed amorphous-like structures, however powders treated at 400 deg. C showed a structure identified as an intermediate pyrochlore phase, independently of the Zr and Ti mole ratio.

A model independent method to deconvolve hard X-ray spectra

International Nuclear Information System (INIS)

Polcaro, V.F.; Bazzano, A.; Ubertini, P.; La Padula, C.

1984-01-01

A general purpose method to deconvolve the energy spectra detected by means of the use of a hard X-ray telescope is described. The procedure does not assume any form of input spectrum and the observed energy loss spectrum is directly deconvolved into the incident photon spectrum, the form of which can be determined independently of physical interpretation of the data. Deconvolution of the hard X-ray spectrum of Her X-1, detected during the HXR 81M experiment, by the method independent method is presented. (orig.)

X-ray spectrum local method

International Nuclear Information System (INIS)

Avdonin, S.A.

1985-01-01

General characteristic and bases of X-ray spectrum local method used for qualitative and quantitative analyses of the mineral chemical composition with volumetric locality of several cubic micrometers. The method is based on the excitation in a sample of characteristic and bremsstrahlung spectra by means of a narrow electron beam at 5-50 keV accelerating voltage. Application of the method when studying uranium minerals and ores is considered. The method allows to determine the uranium presence forms in the ores, morphological features of the minerals, mineral microstructure, UO 2 and UO 3 ratios for unhydrous uraninites and pitchblendes and also to determine mineralization age

Coherent methods in X-ray scattering

International Nuclear Information System (INIS)

Gorobtsov, Oleg

2017-05-01

X-ray radiation has been used to study structural properties of materials for more than a hundred years. Construction of extremely coherent and bright X-ray radiation sources such as free electron lasers (FELs) and latest generationstorage rings led to rapid development of experimental methods relying on high radiation coherence. These methods allow to perform revolutionary studies in a wide range of fields from solid state physics to biology. In this thesis I focus on several important problems connected with the coherent methods. The first part considers applications of dynamical diffraction theory on crystals to studies with coherent X-ray radiation. It presents the design of a high-resolution spectrometer for free electron lasers that should allow to resolve spectral structure of individual FEL pulses. The spectrometer is based on the principle of dynamical diffraction focusing. The knowledge of individual FEL pulse spectra is necessary for understanding FEL longitudinal coherence. In the same part I present quasi-kinematical approximation to dynamical theory which allows to treat analytically phase effects observed in X-ray coherent imaging on nanocrystals. These effects may play a big role when methods such as ptychography are used to study crystalline samples. The second part deals with measurements of FEL coherence properties using intensity - intensity interferometry. Results of several experiments performed at FELs FLASH and LCLS are revealed in this section. I have developed models and theories to explain the behavior observed in experiments on FLASH. These models allowed to extract information about external positional jitter of FEL pulses and secondary beams present in FEL radiation. In the LCLS experiment the Hanbury Brown and Twiss type interferometry was performed on Bragg peaks from colloidal crystal. This did not require additional measurements without the sample and information was extracted directly from diffraction patterns. Therefore intensity

Coherent methods in X-ray scattering

Energy Technology Data Exchange (ETDEWEB)

Gorobtsov, Oleg

2017-05-15

X-ray radiation has been used to study structural properties of materials for more than a hundred years. Construction of extremely coherent and bright X-ray radiation sources such as free electron lasers (FELs) and latest generationstorage rings led to rapid development of experimental methods relying on high radiation coherence. These methods allow to perform revolutionary studies in a wide range of fields from solid state physics to biology. In this thesis I focus on several important problems connected with the coherent methods. The first part considers applications of dynamical diffraction theory on crystals to studies with coherent X-ray radiation. It presents the design of a high-resolution spectrometer for free electron lasers that should allow to resolve spectral structure of individual FEL pulses. The spectrometer is based on the principle of dynamical diffraction focusing. The knowledge of individual FEL pulse spectra is necessary for understanding FEL longitudinal coherence. In the same part I present quasi-kinematical approximation to dynamical theory which allows to treat analytically phase effects observed in X-ray coherent imaging on nanocrystals. These effects may play a big role when methods such as ptychography are used to study crystalline samples. The second part deals with measurements of FEL coherence properties using intensity - intensity interferometry. Results of several experiments performed at FELs FLASH and LCLS are revealed in this section. I have developed models and theories to explain the behavior observed in experiments on FLASH. These models allowed to extract information about external positional jitter of FEL pulses and secondary beams present in FEL radiation. In the LCLS experiment the Hanbury Brown and Twiss type interferometry was performed on Bragg peaks from colloidal crystal. This did not require additional measurements without the sample and information was extracted directly from diffraction patterns. Therefore intensity

Method for calculating required shielding in medical x-ray rooms

International Nuclear Information System (INIS)

Karppinen, J.

1997-10-01

The new annual radiation dose limits - 20 mSv (previously 50 mSv) for radiation workers and 1 mSv (previously 5 mSv) for other persons - implies that the adequacy of existing radiation shielding must be re-evaluated. In principle, one could assume that the thicknesses of old radiation shields should be increased by about one or two half-value layers in order to comply with the new dose limits. However, the assumptions made in the earlier shielding calculations are highly conservative; the required shielding was often determined by applying the maximum high-voltage of the x-ray tube for the whole workload. A more realistic calculation shows that increased shielding is typically not necessary if more practical x-ray tube voltages are used in the evaluation. We have developed a PC-based calculation method for calculating the x-ray shielding which is more realistic than the highly conservative method formerly used. The method may be used to evaluate an existing shield for compliance with new regulations. As examples of these calculations, typical x-ray rooms are considered. The lead and concrete thickness requirements as a function of x-ray tube voltage and workload are also given in tables. (author)

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.

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

Indian Academy of Sciences (India)

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

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

Energy Technology Data Exchange (ETDEWEB)

Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

2013-06-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

International Nuclear Information System (INIS)

Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

2013-01-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

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)

Studies of oxide-based thin-layered heterostructures by X-ray scattering methods

Energy Technology Data Exchange (ETDEWEB)

Durand, O. [Thales Research and Technology France, Route Departementale 128, F-91767 Palaiseau Cedex (France)]. E-mail: olivier.durand@thalesgroup.com; Rogers, D. [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Universite de Technologie de Troyes, 10-12 rue Marie Curie, 10010 (France); Teherani, F. Hosseini [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Andrieux, M. [LEMHE, ICMMOCNRS-UMR 8182, Universite d' Orsay, Batiment 410, 91410 Orsay (France); Modreanu, M. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland)

2007-06-04

Some X-ray scattering methods (X-ray reflectometry and Diffractometry) dedicated to the study of thin-layered heterostructures are presented with a particular focus, for practical purposes, on the description of fast, accurate and robust techniques. The use of X-ray scattering metrology as a routinely working non-destructive testing method, particularly by using procedures simplifying the data-evaluation, is emphasized. The model-independent Fourier-inversion method applied to a reflectivity curve allows a fast determination of the individual layer thicknesses. We demonstrate the capability of this method by reporting X-ray reflectometry study on multilayered oxide structures, even when the number of the layers constitutive of the stack is not known a-priori. Fast Fourier transform-based procedure has also been employed successfully on high resolution X-ray diffraction profiles. A study of the reliability of the integral-breadth methods in diffraction line-broadening analysis applied to thin layers, in order to determine coherent domain sizes, is also reported. Examples from studies of oxides-based thin-layers heterostructures will illustrate these methods. In particular, X-ray scattering studies performed on high-k HfO{sub 2} and SrZrO{sub 3} thin-layers, a (GaAs/AlOx) waveguide, and a ZnO thin-layer are reported.

JAX: a micro-computer based X-ray diffractometer controller

International Nuclear Information System (INIS)

Naval, P.C. Jr.

1987-05-01

This paper describes a micro-computer based X-ray diffractometer controller and explores its possibilities in simplifying acquisition and analysis of X-ray powder diffraction data. The interrupt-driven controller can operate in both present time and present count data acquisition modes and allows a data analysis program to execute concurrently with data collection. (Auth.). 16 figs.; 2 tabs

X-ray and synchrotron methods in studies of cultural heritage sites

Energy Technology Data Exchange (ETDEWEB)

Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu., E-mail: elenatereschenko@yandex.ru; Prosekov, P. A.; Dyakova, Yu. A. [National Research Centre “Kurchatov Institute” (Russian Federation)

2016-09-15

X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

X-ray and synchrotron methods in studies of cultural heritage sites

International Nuclear Information System (INIS)

Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu.; Prosekov, P. A.; Dyakova, Yu. A.

2016-01-01

X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

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

International Nuclear Information System (INIS)

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

2005-01-01

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

X-ray studies, spectral characterization and thermal behaviour of a ...

African Journals Online (AJOL)

HP04)3]. H20, I, was synthesized by reacting Zn2+ ions with tris-(2-aminoethyl) amine phosphate [C6H21N4][P04].5H20. The compound was characterized by powder x-ray diffraction analysis, energy dispersive analysis by x-ray and infrared ...

Ultrafast x-ray scattering on nanoparticle dynamics

International Nuclear Information System (INIS)

Plech, A; Ibrahimkutty, S; Issenmann, D; Kotaidis, V; Siems, A

2013-01-01

Pulsed X-ray scattering is used for the determination of structural dynamics of laser-irradiated gold particles. By combining several scattering methods such as powder scattering, small angle scattering and diffuse wide angle scattering it is possible to reconstruct the kinetics of structure evolution on several lengths scales and derive complementary information on the particles and their local environment. A generic structural phase diagram for the reaction as function of delay time after laser excitation and laser fluence can be constructed.

Ti₃SiC₂ Synthesis by Powder Metallurgical Methods

OpenAIRE

Kero, Ida; Antti, Marta-Lena; Odén, Magnus

2007-01-01

Titanium silicon carbide MAX phase was synthesised by a powder metallurgical method from ball milled TiC/Si powders of two different compositions, with TiC/Si ratios of 3:2 and 3:2.2 respectively. The cold pressed samples were analysed by dilatometry under flowing argon or sintered under vacuum for different times. The sintered samples were evaluated using x-ray diffraction (XRD). This study showed that titanium carbide was always present as a secondary phase and silicon carbide accompanied t...

Determination of iron and titanium in kaolins by the method of non-dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Bialy, N.; Kierzek, J.; Parus, J.

1976-01-01

The possibility of application of the radioactive source excited X-ray fluorescence analysis for titanium and iron determination in kaolins to the routine test of the refinement process has been studied. The iron content can be determined with a simple counting system using a single-channel pulse height analyser, argon filled proportional counter and 109 Cd source of 3 mCi for the excitation of K Fe rays. The samples were analyzed both as pellets and powders. The iron content ranged from 0.2-2.5% and titanium from 0.1-0.64%. The best values of precision and determination limit have been achieved for iron with 238 Pu and for titanium with 55 Fe. The precision and accuracy of the X-ray fluorescence method of iron and titanium determination in kaolins are comparable to those of the chemical method. For the simultaneous iron and titanium determination in the discussed region of concentration it is the most advantageous to use the plutonium source with the activity of several tens of mCi and Si(Li) detector with a moderate resolution (250-300 eV for 5.9 keV). The time of the analysis carried out by the described method is several times shorter than the chemical method. The apparatus used in this method is relatively simple, the sample preparation does not require any chemical treatment and the cost of labour of the sample preparation is minimal. (T.G.)

Characterization of powdered fish heads for bone graft biomaterial applications.

Science.gov (United States)

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

Science.gov (United States)

de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

2009-01-01

Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

Consolidation processing parameters and alternative processing methods for powder metallurgy Al-Cu-Mg-X-X alloys

Science.gov (United States)

Sankaran, K. K.

1987-01-01

The effects of varying the vacuum degassing parameters on the microstructure and properties of Al-4Cu-1Mg-X-X (X-X = 1.5Li-0.2Zr or 1.5Fe-0.75Ce) alloys processed from either prealloyed (PA) or mechanically alloyed (M) powder, and consolidated by either using sealed aluminum containers or containerless vacuum hot pressing were studied. The consolidated billets were hot extruded to evaluate microstructure and properties. The MA Li-containing alloy did not include Zr, and the MA Fe- and Ce-containing alloy was made from both elemental and partially prealloyed powder. The alloys were vacuum degassed both above and below the solution heat treatment temperature. While vacuum degassing lowered the hydrogen content of these alloys, the range over which the vacuum degassing parameters were varied was not large enough to cause significant changes in degassing efficiency, and the observed variations in the mechanical properties of the heat treated alloys were attributed to varying contributions to strengthening by the sub-structure and the dispersoids. Mechanical alloying increased the strength over that of alloys of similar composition made from PA powder. The inferior properties in the transverse orientation, especially in the Li-containing alloys, suggested deficiencies in degassing. Among all of the alloys processed for this study, the Fe- and Ce-containing alloys made from MA powder possessed better combinations of strength and toughness.

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.

The equation of state of PbTiO sub 3 up to 37 GPa: a synchrotron x-ray powder diffraction study

CERN Document Server

Sani, A; Levy, D

2002-01-01

High-pressure synchrotron x-ray powder diffraction patterns were collected using ID09 of ESRF (Grenoble, France) for a powder sample of PbTiO sub 3 , placed in a diamond anvil cell. The patterns were collected at room temperature using nitrogen (up to 37 GPa) and methanol-ethanol solution (up to 7 GPa) as pressure-transmitting media. The bulk moduli were calculated for the first time using the Vinet equation of state and they were compared to those of isostructural compounds. The trend of the spontaneous polarization as a function of pressure confirms that the ferroelectric-paraelectric phase transition at 11.2 GPa possesses a second-order character.

A novel x-ray circularly polarized ranging method

International Nuclear Information System (INIS)

Song Shi-Bin; Xu Lu-Ping; Zhang Hua; Shen Yang-He; Gao Na

2015-01-01

Range measurement has found multiple applications in deep space missions. With more and further deep space exploration activities happening now and in the future, the requirement for range measurement has risen. In view of the future ranging requirement, a novel x-ray polarized ranging method based on the circular polarization modulation is proposed, termed as x-ray circularly polarized ranging (XCPolR). XCPolR utilizes the circular polarization modulation to process x-ray signals and the ranging information is conveyed by the circular polarization states. As the circular polarization states present good stability in space propagation and x-ray detectors have light weight and low power consumption, XCPolR shows great potential in the long-distance range measurement and provides an option for future deep space ranging. In this paper, we present a detailed illustration of XCPolR. Firstly, the structure of the polarized ranging system is described and the signal models in the ranging process are established mathematically. Then, the main factors that affect the ranging accuracy, including the Doppler effect, the differential demodulation, and the correlation error, are analyzed theoretically. Finally, numerical simulation is carried out to evaluate the performance of XCPolR. (paper)

X-Ray powder diffractometry, crystallographic phase analysis and ...

African Journals Online (AJOL)

Computerized X-Ray diffraction system has been used to determine the composition and lattice parameters of raw and activated kaolinite. The universal diffractometry URD 63 was interfaced with computer via an APX 63 software package for rapid capturing of data on reflected intensity and other crystallographic ...

Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

DEFF Research Database (Denmark)

Johnsen, Rune; Krumeich, Frank; Norby, Poul

2010-01-01

Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

Study of Y{sub 1−x}Er{sub x}FeO{sub 3} (0≤x≤1) powder synthesized by sol–gel method and their magnetic properties

Energy Technology Data Exchange (ETDEWEB)

Cheng, Man; Jiang, Guojian, E-mail: guojianjiang@sit.edu.cn; Yang, Wenqian; Duan, Li; Peng, Wei; Chen, Jiang; Wang, Xiaojian

2016-11-01

A series of single phase Y{sub 1−x}Er{sub x}FeO{sub 3} (0≤x≤1) orthoferrite samples were synthesized by sol-gel method and their magnetic properties were studied in detail. The prepared samples were characterized by X-ray diffraction (XRD), vibrating sample magnetometer (VSM) and differential scanning calorimetry (DSC). The obviously weak ferromagnetic property, which caused by Dzialoshinski Moriya (DM) antisymmetric exchange mechanism, was observed in YFeO{sub 3} for the magnetization jump at H=0 Oe. The magnetization of YFeO{sub 3} was evidently changed by doping Er{sup 3+}. The increase of the Er{sup 3+} content in Y{sub 1−x}Er{sub x}FeO{sub 3} greatly enhanced the paramagnetic component and gradually decreased the ferromagnetic component. - Highlights: • We synthesized a series of single phase Y{sub 1−x}Er{sub x}FeO{sub 3} orthoferrite powder by sol–gel method. • We studied magnetic properties of Y{sub 1−x}Er{sub x}FeO{sub 3} (0≤x≤1) in detail. • The magnetization of YFeO{sub 3} was evidently changed by doping Er{sup 3+}.

Poly[μ-(1-azaniumylethane-1,1-diyl)- bis(hydrogen phosphonato)sodium]: A powder X-ray diffraction study

International Nuclear Information System (INIS)

Rukiah, M.; Assaad, T.

2015-01-01

The title two-dimensional coordination polymer, [Na(C2H8NO6P2)]n, was characterized using powder X-ray diffraction data and its structure refined using the Rietveld method. The asymmetric unit contains one Na(+) cation and one (1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonate) anion. The central Na(+) cation exhibits distorted octahedral coordination geometry involving two deprotonated O atoms, two hydroxy O atoms and two double-bonded O atoms of the bisphosphonate anion. Pairs of sodium-centred octahedra share edges and the pairs are in turn connected to each other by the biphosphonate anion to form a two-dimensional network parallel to the (001) plane. The polymeric layers are connected by strong O-H...O hydrogen bonding between the hydroxy group and one of the free O atoms of the bisphosphonate anion to generate a three-dimensional network. Further stabilization of the crystal structure is achived by N-H...O and O-H...O hydrogen bonding.(author)

The x-ray time of flight method for investigation of ghosting in amorphous selenium-based flat panel medical x-ray imagers

International Nuclear Information System (INIS)

Rau, A.W.; Bakueva, L.; Rowlands, J.A.

2005-01-01

Amorphous selenium (a-Se) based real-time flat-panel imagers (FPIs) are finding their way into the digital radiology department because they offer the practical advantages of digital x-ray imaging combined with an image quality that equals or outperforms that of conventional systems. The temporal imaging characteristics of FPIs can be affected by ghosting (i.e., radiation-induced changes of sensitivity) when the dose to the detector is high (e.g., portal imaging and mammography) or the images are acquired at a high frame rate (e.g., fluoroscopy). In this paper, the x-ray time-of-flight (TOF) method is introduced as a tool for the investigation of ghosting in a-Se photoconductor layers. The method consists of irradiating layers of a-Se with short x-ray pulses. From the current generated in the a-Se layer, ghosting is quantified and the ghosting parameters (charge carrier generation rate and carrier lifetimes and mobilities) are assessed. The x-ray TOF method is novel in that (1) x-ray sensitivity (S) and ghosting parameters can be measured simultaneously (2) the transport of both holes and electrons can be isolated, and (3) the method is applicable to the practical a-Se layer structure with blocking contacts used in FPIs. The x-ray TOF method was applied to an analysis of ghosting in a-Se photoconductor layers under portal imaging conditions, i.e., 1 mm thick a-Se layers, biased at 5 V/μm, were irradiated using a 6 MV LINAC x-ray beam to a total dose (ghosting dose) of 30 Gy. The initial sensitivity (S 0 ) of the a-Se layers was 63±2 nC cm -2 cGy -1 . It was found that S decreases to 30% of S 0 after a ghosting dose of 5 Gy and to 21% after 30 Gy at which point no further change in S occurs. At an x-ray intensity of 22 Gy/s (instantaneous dose rate during a LINAC x-ray pulse), the charge carrier generation rate was 1.25±0.1x10 22 ehp m -3 s -1 and, to a first approximation, independent of the ghosting dose. However, both hole and electron transport showed a

An automated x-ray stress measurement system using a microcomputer

International Nuclear Information System (INIS)

Kurita, Masanori; Miyagawa, Matsuo; Sato, Fumiyoshi; Sugiharai, Shigeru; Ishii, Masami; Sumiyoshi, Michio.

1985-01-01

An automated system for a rapid and precise X-ray stress measurement using a microcomputer has been developed. A block diagram of the system and a flowchart for the stress measurement method are shown. Of the various methods, the one most suitable for the material to be measured can be programmed in this system. The residual stress in a hardened steel having a broad diffraction profile (half-width of 7.2 deg ) could be measured in six minutes with a small standard deviation of 13 MPa by the Gaussian curve method using the sin 2 ψ method. Both the oscillation and the fixed ψ methods, using the Gaussian curve method, allow the X-ray stress measurement of coarse-grained steels; the sin 2 ψ diagram obtained by these methods had a good linearity. The residual stress measurement of an annealed chromium powder gave almost zero stress values, -3.2 to 2.9 MPa depending on the method used, showing a high accuracy of the system. (author)

NiTiO3 powders obtained by polymeric precursor method: Synthesis and characterization

International Nuclear Information System (INIS)

Lopes, K.P.; Cavalcante, L.S.; Simoes, A.Z.; Varela, J.A.; Longo, E.; Leite, E.R.

2009-01-01

Nickel titanate (NiTiO 3 ) powders were synthesized by the polymeric precursor method after thermal treatment at different temperatures for 2 h in air atmosphere. The decomposition of the precursors was monitored by differential scanning calorimetry and thermogravimetric analysis. The NiTiO 3 powders presented a reduction in the specific surface area and increase of the average particle size with the evolution of the temperature. The structural evolution of NiTiO 3 phase was accompanied by X-ray diffraction and Fourier transform Raman spectroscopy. By scanning electron microscopy was revealed the agglomerated nature of very fine particles of NiTiO 3 powders annealed from 600 to 1000 deg. C

The stoichiometry of synthetic alunite as a function of hydrothermal aging investigated by solid-state NMR spectroscopy, powder X-ray diffraction and infrared spectroscopy

DEFF Research Database (Denmark)

Grube, Elisabeth; Nielsen, Ulla Gro

2015-01-01

The stoichiometry of a series of synthetic alunite (nominally KAl3(SO4)2(OH)6) samples prepared by hydrothermal methods as a function of reaction time (1 – 31 days) has been investigated by powder X-ray diffraction, Fourier transform infrared spectroscopy as well as solid-state 1H and 27Al magic...... of potassium defects present, from 17.261(1) to 17.324(5) Å. Solid-state 27Al MAS NMR revealed a decrease in the defect concentration as a function of time and showed the presence of 7-10 % impurities in the samples....

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

Science.gov (United States)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

FIST - a suite of X-ray powder crystallography programs for use with a HP-65 calculator

International Nuclear Information System (INIS)

Ferguson, I.F.; Turek, M.

1977-12-01

Programs for X-ray powder crystallography are defined for use with a Hewlett Packard HP-65 (programmable) pocket calculator. These include the prediction of all Bragg reflections for defined P-, F-, I-cubic, tetragonal, hexagonal and orthorhombic cells; the calculation of the position of a specific Bragg reflection from defined unit cells with all symmetries except triclinic; interconversion of theta, 2theta, sin 2 theta and d, as well as the calculation of the Nelson-Riley function; the computation of crystal densities; the interconversion of rhombohedral and hexagonal unit cells, lsub(c) determinations for graphite, the calculation of a and c for boron carbide; and Miller index transformations between various unit cells. (author)

Material Discriminated X-Ray CT System by Using New X-Ray Imager with Energy Discriminate Function

Directory of Open Access Journals (Sweden)

Toru Aoki

2008-04-01

Full Text Available Material discriminated X-ray CT system has been constructed by using conventional X-ray tube (white X-ray source and photon-counting X-ray imager as an application with energy band detection. We have already reported material identify X-ray CT using K-shell edge method elsewhere. In this report the principle of material discrimination was adapted the separation of electron-density and atomic number from attenuation coefficient mapping in X-ray CT reconstructed image in two wavelength X-ray CT method using white X-ray source and energy discriminated X-ray imager by using two monochrome X-ray source method. The measurement phantom was prepared as four kinds material rods (Carbon(C, Iron(Fe, Copper(Cu, Titanium(Ti rods of 3mm-diameter inside an aluminum(Al rod of 20mm-diameter. We could observed material discriminated X-ray CT reconstructed image, however, the discrimination properties were not good than two monochrome X-ray CT method. This results was could be explained because X-ray scattering, beam-hardening and so on based on white X-ray source, which could not observe in two monochrome X-ray CT method. However, since our developed CdTe imager can be detect five energy-bands at the same time, we can use multi-band analysis to decrease the least square error margin. We will be able to obtain more high separation in atomic number mapping in X-ray CT reconstructed image by using this system.

Use of the maximum entropy method in X-ray astronomy

International Nuclear Information System (INIS)

Willingale, R.

1981-01-01

An algorithm used to apply the maximum entropy method in X-ray astronomy is described. It is easy to programme on a digital computer and fast enough to allow processing of two-dimensional images. The method gives good noise suppression without loss of instrumental resolution and has been successfully applied to several data analysis problems in X-ray astronomy. The restoration of a high-resolution image from the Einstein Observatory demonstrates the use of the algorithm. (author)

X-ray holography

International Nuclear Information System (INIS)

Faigel, G.; Tegze, M.; Belakhovsky, M.; Marchesini, S.; Bortel, G.

2003-01-01

In the last decade holographic methods using hard X-rays were developed. They are able to resolve atomic distances, and can give the 3D arrangement of atoms around a selected element. Therefore, hard X-ray holography has potential applications in chemistry, biology and physics. In this article we give a general description of these methods and discuss the developments in the experimental technique. The capabilities of hard X-ray holography are demonstrated by examples

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Characterization of ceramic powder compacts

International Nuclear Information System (INIS)

Yanai, K.; Ishimoto, S.; Kubo, T.; Ito, K.; Ishikawa, T.; Hayashi, H.

1995-01-01

UO 2 and Al 2 O 3 powder packing structures in cylindrical powder compacts are observed by scanning electron microscopy using polished cross sections of compacts fixed by low viscosity epoxy resin. Hard aggregates which are not destroyed during powder compaction are observed in some of the UO 2 powder compacts. A technique to measure local density in powder compacts is developed based on counting characteristic X-ray intensity by energy dispersive X-ray analysis (EDX). The local density of the corner portion of the powder compact fabricated by double-acting dry press is higher than that of the inner portion. ((orig.))

Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors

Energy Technology Data Exchange (ETDEWEB)

Katsuya, Yoshio; Tanaka, Masahiko [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Song, Chulho [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Ito, Kimihiko; Kubo, Yoshimi [Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan)

2016-01-15

An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a “one shot” measurement. We tested the performance of the diffractometer with reference CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.

Statistical analysis of x-ray stress measurement by centroid method

International Nuclear Information System (INIS)

Kurita, Masanori; Amano, Jun; Sakamoto, Isao

1982-01-01

The X-ray technique allows a nondestructive and rapid measurement of residual stresses in metallic materials. The centroid method has an advantage over other X-ray methods in that it can determine the angular position of a diffraction line, from which the stress is calculated, even with an asymmetrical line profile. An equation for the standard deviation of the angular position of a diffraction line, σsub(p), caused by statistical fluctuation was derived, which is a fundamental source of scatter in X-ray stress measurements. This equation shows that an increase of X-ray counts by a factor of k results in a decrease of σsub(p) by a factor of 1/√k. It also shows that σsub(p) increases rapidly as the angular range used in calculating the centroid increases. It is therefore important to calculate the centroid using the narrow angular range between the two ends of the diffraction line where it starts to deviate from the straight background line. By using quenched structural steels JIS S35C and S45C, the residual stresses and their standard deviations were calculated by the centroid, parabola, Gaussian curve, and half-width methods, and the results were compared. The centroid of a diffraction line was affected greatly by the background line used. The standard deviation of the stress measured by the centroid method was found to be the largest among the four methods. (author)

X-ray irradiation induced reduction and nanoclustering of lead in borosilicate glass

NARCIS (Netherlands)

Stanley, H.B.; Banerjee, D.; Breemen, van L.C.A.; Ciston, J.; Liebscher, C.H.; Martis, V.; Merino, D.H.; Longo, A.; Pattison, P.; Peters, G.W.M.; Portale, G.; Sen, Sabyasachi; Bras, W.

2014-01-01

We have studied the formation of nanoparticles in lead sulfide (PbS)-doped borosilicate glass subjected to a two-step nucleation and growth heat treatment using in situ small-angle X-ray scattering (SAXS). The microstructure produced was subsequently characterized using X-ray powder diffraction

Black powder in gas pipelines

Energy Technology Data Exchange (ETDEWEB)

Sherik, Abdelmounam [Saudi Aramco, Dhahran (Saudi Arabia)

2009-07-01

Despite its common occurrence in the gas industry, black powder is a problem that is not well understood across the industry, in terms of its chemical and physical properties, source, formation, prevention or management of its impacts. In order to prevent or effectively manage the impacts of black powder, it is essential to have knowledge of its chemical and physical properties, formation mechanisms and sources. The present paper is divided into three parts. The first part of this paper is a synopsis of published literature. The second part reviews the recent laboratory and field work conducted at Saudi Aramco Research and Development Center to determine the compositions, properties, sources and formation mechanisms of black powder in gas transmission systems. Microhardness, nano-indentation, X-ray Diffraction (XRD), X-ray Fluorescence (XRF) and Scanning Electron Microscopy (SEM) techniques were used to analyze a large number of black powder samples collected from the field. Our findings showed that black powder is generated inside pipelines due to internal corrosion and that the composition of black powder is dependent on the composition of transported gas. The final part presents a summary and brief discussion of various black powder management methods. (author)

Investigation of the human spleen by X-ray microanalysis

International Nuclear Information System (INIS)

Kopani, M.; Jakubovsky, J.; Polak, S.

2001-01-01

Qualitative and quantitative topographic analysis using X-ray fluorescence (XRF), X-ray powder diffraction (XRD) and scanning electron microscopy was performed in tissue samples of rat and human spleens. The presence of silico-aluminium and silico-calcareous particles of various sizes could be seen. The presence of the inorganic substances mentioned in the human red pulp cords is assumed to be a consequence of the purifying function of the spleen. (Authors)

X-ray coherent scattering tomography of textured material (Conference Presentation)

Science.gov (United States)

Zhu, Zheyuan; Pang, Shuo

2017-05-01

Small-angle X-ray scattering (SAXS) measures the signature of angular-dependent coherently scattered X-rays, which contains richer information in material composition and structure compared to conventional absorption-based computed tomography. SAXS image reconstruction method of a 2 or 3 dimensional object based on computed tomography, termed as coherent scattering computed tomography (CSCT), enables the detection of spatially-resolved, material-specific isotropic scattering signature inside an extended object, and provides improved contrast for medical diagnosis, security screening, and material characterization applications. However, traditional CSCT methods assumes materials are fine powders or amorphous, and possess isotropic scattering profiles, which is not generally true for all materials. Anisotropic scatters cannot be captured using conventional CSCT method and result in reconstruction errors. To obtain correct information from the sample, we designed new imaging strategy which incorporates extra degree of detector motion into X-ray scattering tomography for the detection of anisotropic scattered photons from a series of two-dimensional intensity measurements. Using a table-top, narrow-band X-ray source and a panel detector, we demonstrate the anisotropic scattering profile captured from an extended object and the reconstruction of a three-dimensional object. For materials possessing a well-organized crystalline structure with certain symmetry, the scatter texture is more predictable. We will also discuss the compressive schemes and implementation of data acquisition to improve the collection efficiency and accelerate the imaging process.

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

High-speed X-ray phase tomography with Talbot interferometer and fringe scanning method

International Nuclear Information System (INIS)

Kibayashi, Shunsuke; Harasse, Sébastien; Yashiro, Wataru; Momose, Atsushi

2012-01-01

High-speed X-ray phase tomography based on the Fourier-transform method has been demonstrated with an X-ray Talbot interferometer using white synchrotron radiation. We report the experimental results of high-speed X-ray phase tomography with fringe-scanning method instead of Fourier-transform method to improve spatial resolution without a considerable increase of scan time. To apply fringe-scanning method to high speed tomography, we tested a scan that is a synchronous combination of one-way continuous movements of the sample rotation and the grating displacement. When this scanning method was combined with X-ray phase tomography, we were able to obtain a scan time of 5 s. A comparison of the image quality derived with the conventional approach and with the proposed approach using the fringe-scanning method showed that the latter had better spatial resolution.

ASSESSMENT OF RESTORATION METHODS OF X-RAY IMAGES WITH EMPHASIS ON MEDICAL PHOTOGRAMMETRIC USAGE

Directory of Open Access Journals (Sweden)

S. Hosseinian

2016-06-01

Full Text Available Nowadays, various medical X-ray imaging methods such as digital radiography, computed tomography and fluoroscopy are used as important tools in diagnostic and operative processes especially in the computer and robotic assisted surgeries. The procedures of extracting information from these images require appropriate deblurring and denoising processes on the pre- and intra-operative images in order to obtain more accurate information. This issue becomes more considerable when the X-ray images are planned to be employed in the photogrammetric processes for 3D reconstruction from multi-view X-ray images since, accurate data should be extracted from images for 3D modelling and the quality of X-ray images affects directly on the results of the algorithms. For restoration of X-ray images, it is essential to consider the nature and characteristics of these kinds of images. X-ray images exhibit severe quantum noise due to limited X-ray photons involved. The assumptions of Gaussian modelling are not appropriate for photon-limited images such as X-ray images, because of the nature of signal-dependant quantum noise. These images are generally modelled by Poisson distribution which is the most common model for low-intensity imaging. In this paper, existing methods are evaluated. For this purpose, after demonstrating the properties of medical X-ray images, the more efficient and recommended methods for restoration of X-ray images would be described and assessed. After explaining these approaches, they are implemented on samples from different kinds of X-ray images. By considering the results, it is concluded that using PURE-LET, provides more effective and efficient denoising than other examined methods in this research.

X-Ray fluorescence determination of the mobile forms of toxic elements in meadow chernozems

International Nuclear Information System (INIS)

Belikov, K.N.; Blank, A.B.; Shevtsov, N.I.

1997-01-01

An X-ray fluorescence method for determining mobile forms of Mn, V, Cr, Co, Ni, Zn, and Pb in meadow chernozems was developed. It is based on the extraction of analytes with an acetate-ammonia buffer solution and the evaporation of the obtained filtrate with carbon powder followed by the X-ray fluorescence analysis of the dry residue. The effect of concomitants on the analytical signals of elements under determination was examined. It was suggested to spike samples with barium in order to decrease analytical errors. (author)

Diffuse scattering of neutrons and X-rays

International Nuclear Information System (INIS)

Novion, C.H. de

1978-01-01

Diffuse scattering is used to study defect concentrations of about 10 -4 in the case of X-rays and 10 -3 in the case of neutrons. The foundations of diffuse scattering formalism are given, some experimental devices described and a few applications discussed: study by diffraction on powders of defects in CeOsub(2-x); short-range order study by X-rays on Cusub(0.75) Ausub(0.25); short-range order study by neutrons on Cusub(0.435)Nisub(0.565); short-range order study by electrons TiOx; study of irradiation-induced self-interstitials in Al; study of holes created by neutrons in Al [fr

Method for detecting binding events using micro-X-ray fluorescence spectrometry

Science.gov (United States)

Warner, Benjamin P.; Havrilla, George J.; Mann, Grace

2010-12-28

Method for detecting binding events using micro-X-ray fluorescence spectrometry. Receptors are exposed to at least one potential binder and arrayed on a substrate support. Each member of the array is exposed to X-ray radiation. The magnitude of a detectable X-ray fluorescence signal for at least one element can be used to determine whether a binding event between a binder and a receptor has occurred, and can provide information related to the extent of binding between the binder and receptor.

Development of a methodology for low-energy X-ray absorption correction in biological samples using radiation scattering techniques

International Nuclear Information System (INIS)

Pereira, Marcelo O.; Anjos, Marcelino J.; Lopes, Ricardo T.

2009-01-01

Non-destructive techniques with X-ray, such as tomography, radiography and X-ray fluorescence are sensitive to the attenuation coefficient and have a large field of applications in medical as well as industrial area. In the case of X-ray fluorescence analysis the knowledge of photon X-ray attenuation coefficients provides important information to obtain the elemental concentration. On the other hand, the mass attenuation coefficient values are determined by transmission methods. So, the use of X-ray scattering can be considered as an alternative to transmission methods. This work proposes a new method for obtain the X-ray absorption curve through superposition peak Rayleigh and Compton scattering of the lines L a e L β of Tungsten (Tungsten L lines of an X-ray tube with W anode). The absorption curve was obtained using standard samples with effective atomic number in the range from 6 to 16. The method were applied in certified samples of bovine liver (NIST 1577B) , milk powder and V-10. The experimental measurements were obtained using the portable system EDXRF of the Nuclear Instrumentation Laboratory (LIN-COPPE/UFRJ) with Tungsten (W) anode. (author)

Non-contact micro mass evaluation method using an X-ray microscope

Energy Technology Data Exchange (ETDEWEB)

Kim, Jiseok; Sun, Gwang Min; Baek, Ha Ni; Hoang, Sy Minh Tuan; Park, Sun Ae [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2017-07-15

For the mass inspection of attached foils such as printed electrodes, mass should be measured by a non-contact method with the capacity to measure a small mass of micrograms. In this study, the masses of 1 mg to 10 mg electrodes were evaluated using an X-ray microscope. The results were compared with the masses determined by using a digital scale with a 0.005 mg error. The average of the relative error between the mass measurements using the X-ray microscope and those using the digital scale was less than 2.51%. The results show that X-ray mass evaluation method can be used for mass measurement of micro objects by replacing a digital scale.

Matching methods evaluation framework for stereoscopic breast x-ray images.

Science.gov (United States)

Rousson, Johanna; Naudin, Mathieu; Marchessoux, Cédric

2016-01-01

Three-dimensional (3-D) imaging has been intensively studied in the past few decades. Depth information is an important added value of 3-D systems over two-dimensional systems. Special focuses were devoted to the development of stereo matching methods for the generation of disparity maps (i.e., depth information within a 3-D scene). Dedicated frameworks were designed to evaluate and rank the performance of different stereo matching methods but never considering x-ray medical images. Yet, 3-D x-ray acquisition systems and 3-D medical displays have already been introduced into the diagnostic market. To access the depth information within x-ray stereoscopic images, computing accurate disparity maps is essential. We aimed at developing a framework dedicated to x-ray stereoscopic breast images used to evaluate and rank several stereo matching methods. A multiresolution pyramid optimization approach was integrated to the framework to increase the accuracy and the efficiency of the stereo matching techniques. Finally, a metric was designed to score the results of the stereo matching compared with the ground truth. Eight methods were evaluated and four of them [locally scaled sum of absolute differences (LSAD), zero mean sum of absolute differences, zero mean sum of squared differences, and locally scaled mean sum of squared differences] appeared to perform equally good with an average error score of 0.04 (0 is the perfect matching). LSAD was selected for generating the disparity maps.

Spiral chain structure of high pressure selenium-II' and sulfur-II from powder x-ray diffraction

International Nuclear Information System (INIS)

Fujihisa, Hiroshi; Yamawaki, Hiroshi; Sakashita, Mami; Yamada, Takahiro; Honda, Kazumasa; Akahama, Yuichi; Kawamura, Haruki; Le Bihan, Tristan

2004-01-01

The structure of high pressure phases, selenium-II ' (Se-II ' ) and sulfur-II (S-II), for α-Se 8 (monoclinic Se-I) and α-S 8 (orthorhombic S-I) was studied by powder x-ray diffraction experiments. Se-II ' and S-II were found to be isostructural and to belong to the tetragonal space group I4 1 /acd, which is made up of 16 atoms in the unit cell. The structure consisted of unique spiral chains with both 4 1 and 4 3 screws. The results confirmed that the structure sequence of the pressure-induced phase transitions for the group VIb elements depended on the initial molecular form. The chemical bonds of the phases are also discussed from the interatomic distances that were obtained

Precision test method by x-ray absorbent clay

International Nuclear Information System (INIS)

Nakadai, Toru; Matsukawa, Hideyuki; Sekita, Jun-ichiro; Murakoshi, Atsushi.

1982-01-01

In X-ray penetration photography of such as welds with reinforcing metal and castings of complex shape, the X-ray absorbent clay developed to eliminate various disadvantages of the conventional absorbents was further studied for better application. The results of the usage are as follows. Because the X-ray absorbent is clay, it is flexible in form, and gives good adhesion to test objects. In the welds and castings mentioned, it is effective for reducing the scattered ray, accordingly, it results in superior images. The following matters are described: contrast in radiographs, the required conditions for X-ray absorbents in general, the properties of the absorbent (absorption coefficient, consistency, density), improvement in radiographs by means of the X-ray absorbent clay (wall thickness compensation, masking, the application together with narrow-field irradiation photography). (Mori, K.)

Advances in X-ray powder diffraction profile analysis and its application in ceramic material studies

International Nuclear Information System (INIS)

Zhang, Y.

1988-01-01

This dissertation is concerned with the following major aspects: (1) the development of necessary computer codes to carry out X-ray powder diffraction profile analysis (XPDPA) calculations; (2) the establishment of a general reference material (GRM) which greatly extends the application of XPDPA and the study of the application of the GRM in profile analysis; (3) the determination of the coherent diffracting domain size and the lattice residual microstrain for some shock-modified and jet-milled materials. A computer code for diffraction profile refinement, XRAYL, fits a diffraction profile with any one of five mathematical functions, either as symmetric or asymmetric (split mode) forms. The resulting patterns meet the requirements for successful profile analysis of microstrain and crystallite size. Powder diffraction profile analysis requires an instrument calibration standard to correct data for instrumental profiles due to the system optics. A general reference material, LaB 6 , has been established. The pattern of this LaB 6 powder can be used to generate a reference pattern for any other substance. Through three applications, it has been shown that this LaB 6 sample can be used to remove the instrumental broadenings and gives reasonable size and strain estimates in the profile analysis of other materials. Many previous studies have shown that the solid state reactivity and physical properties of some ceramic materials can be substantially enhanced. XPDPA techniques have been used to study the plastic deformation and the reduction of crystallite size for eight shock-modified ceramic materials. The size and strain values of these materials are correlated with shock parameters

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

Parametric X-rays from a polycrystalline target

International Nuclear Information System (INIS)

Lobach, Ihar; Benediktovitch, Andrei; Feranchuk, Ilya; Lobko, Alexander

2015-01-01

Highlights: • X-ray radiation from relativistic electrons in a polycrystal is described. • Analytical results are found for two models of the polycrystal texture. • Characteristic number of emitted photons for real accelerator is 10 6 s −1 . • Intensity distribution at fixed frequency resembles a set of rings. • Radiation intensities in monocrystals and polycrystals are compared. - Abstract: A theoretical description of parametric X-ray radiation (PXR) from a nanocrystal powder target is presented in terms of the orientation distribution function (ODF). Two models of ODF resulting in the analytical solution for the PXR intensity distribution are used and the characteristic features of this distribution are considered. A promising estimate of the number of the emitted photons is obtained for the case of a nanodiamond powder target using the parameters of ASTA Facility at Fermilab. The PXR spectra from polycrystal and single crystal targets are compared. The application scenarios of PXR from nanocrystals are discussed.

Direct methods for surface X-ray diffraction

International Nuclear Information System (INIS)

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

2000-01-01

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

X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

Science.gov (United States)

Varberg, Thomas D.; Skakuj, Kacper

2015-01-01

Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

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

Energy Technology Data Exchange (ETDEWEB)

Kyaw-Soe,

1990-05-01

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

X-ray beam generator

International Nuclear Information System (INIS)

Koller, T.J.; Randmer, J.A.

1977-01-01

A method of minimizing the preferential angular absorption of the divergent beam from an X-ray generator is described. The generator consists of an X-ray shielded housing with an X-ray transmissive window symmetrically placed in radial alignment with a focal spot area on a sloped target surface of an X-ray tube in the housing. The X-ray tube may be of the stationary anode type or of the rotating anode type. (U.K.)

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

International Nuclear Information System (INIS)

Susini, J.

2004-01-01

Soon after the discovery of X-rays in 1895 by W. Roentgen, it became rapidly clear that the methods traditionally used in the visible light regime, namely refraction, diffraction and reflection were difficult to apply for X-ray optics. The physical origins of these difficulties are closely linked to the very nature of interaction of X-rays with matter. The small deviation δ of the refractive index of condensed matter from unity makes it difficult to extend refraction-based optics from the optical spectral region to the X-ray region because the refraction angle is proportional to δ. Similarly it is very challenging to extend diffraction-based focusing techniques to X-rays because the diffraction angle scales inversely with wavelength. Finally, the use of reflection-based optics is also limited by the very small critical angle for total reflection. All those fundamental limitations prevented for almost one century, the development of X-ray microscopy whereas electron microscopy became a standard tool. In the past twenty years, interests for X-ray microscopy revived, mainly because of several major advances in X-ray sources and X-ray optics. X-ray microscopy techniques are now emerging as powerful and complementary tools for submicron investigations. Soft X-ray microscopes offer traditionally the possibility to form direct images of thick hydrated biological material in near-native environment, at a spatial resolution well beyond that achievable with visible light microscopy. Natural contrast is available in the soft X-ray region, in the so-called ''water-window'', due to the presence of absorption edges of the major constituents (C,N,O). Recent advances in manufacturing techniques have enlarged the accessible energy range of micro-focussing optics and offer new applications in a broad range of disciplines. X-ray microscopy in the 1 - 30 keV energy range is better suited for fluorescence to map trace elements, tomography for 3D imaging and micro-diffraction. The

Phase-contrast X-ray imaging using an X-ray interferometer for biological imaging

Energy Technology Data Exchange (ETDEWEB)

Momose, Atsushi; Koyama, Ichiro [Tokyo Univ., Dept. of Applied Physics, Tokyo (Japan); Takeda, Tohoru; Itai, Yuji [Tsukuba Univ., Inst. of Clinical Medicine, Tsukuba, Ibaraki (Japan); Yoneyama, Akio [Hitachi Ltd., Advanced Research Laboratory, Saitama (Japan)

2002-04-01

The potential of phase-contrast X-ray imaging using an X-ray interferometer is discussed comparing with other phase-contrast X-ray imaging methods, and its principle of contrast generation is presented including the case of phase-contrast X-ray computed tomography. The status of current instrumentation is described and perspectives for practical applications are discussed. (author)

Absolute determination by X-ray diffraction of a binary or ternary mixture: nickel oxide and fluoride in a nickel powder (1960); Dosage absolu par diffraction X d'un melange binaire ou ternaire: oxyde et fluorure de nickel dans une poudre de nickel (1960)

Energy Technology Data Exchange (ETDEWEB)

Charpin, P; Hauptman, A [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1960-07-01

The method employed is based upon the comparison between computed and measured intensities for conveniently selected X-Ray diffraction lines of each component of the powder. Care must be taken to allow for absorption, both inside each grain and in overall sample. This method has been applied to the determination of nickel oxide and fluoride in a nickel powder. (author) [French] La methode utilisee, dite 'absolue' est basee sur le calcul des intensites theoriques de raies de diffraction convenablement choisies. Elle n'est applicable que si l'absorption est negligeable a travers chaque grain constituant l'echantillon et a travers l'echantillon total. Elle a ete employee pour doser, ensemble ou separement, de l'oxyde et du fluorure de nickel dans une poudre de nickel. (auteur)

A portable x-ray source and method for radiography

International Nuclear Information System (INIS)

Golovanivsky, K.S.

1996-01-01

A portable x-ray source that produces a sufficient x-ray flux to produce high quality x-ray images on x-ray films. The source includes a vacuum chamber filled with a heavy atomic weight gas at low pressure and an x-ray emitter. The chamber is in a magnetic field and an oscillating electric field and generates electron cyclotron resonance (ECR) plasma having a ring of energetic electrons inside the chamber. The electrons bombard the x-ray emitter which in turn produces x-ray. A pair of magnetic members generate an axisymmetric magnetic mirror trap inside the chamber. The chamber may be nested within a microwave resonant cavity and between the magnets or the chamber and the microwave cavity may be a single composite structure. (author)

Analysis of fresco paintings by X-ray fluorescence method

International Nuclear Information System (INIS)

Cechak, T.; Gerndt, J.; Musilek, L.; Kopecka, I.

2000-01-01

In this work we present the application of X-ray fluorescence analysis (XRFA) to examine fresco paintings from the Karlstejn castle. The X-ray fluorescence apparatus built and operated in the Laboratory of Quantitative Methods in Research of Ancient Monuments was used for the purpose of fresco paintings measurements. The X-ray sources (radionuclides) generate the characteristic X-ray photons from the sample. The Si(Li) detector measures numbers and energies of photons emitted from the specimen. The energy and number of photons detected can be converted into kind and amount of measured atoms. These results give data for qualitative and quantitative analysis of samples. XRFA is relatively simple and non-destructive method. Capability of in-situ measurement is one of big advantages of this method. The radionuclide sources of exciting radiation (e.g. 55 Fe enables the excitation of elements with Z up to 23, 238 Pu is used in interval of Z from 20 to 39 etc.) were used. An Si(Li) semiconductor detector with a 5 l Dewar vessel and portable spectroscopy system enable the in situ measurement. Narrow collimation of the exciting beam makes it possible to select the measured area of fresco painting. The valuable fresco paintings from the Karlstejn castle were investigated in this way. The measurements were carried out in collaboration with the Analytical Laboratory of the State Institute for the Preservation of Historic Monuments. A suitable analysis of paintings makes it possible to detect the kind of colours and evaluate changes in the surface colour of paintings and suggest useful and timely procedures for their conservation and restoration. (author)

Envelope method for background elimination from X-ray fluorescence spectra

International Nuclear Information System (INIS)

Monakhov, V.V.; Naumenko, P.A.; Chashinskaya, O.A.

2006-01-01

The influence of the background noise caused by Bremsstrahlung on the accuracy of the envelope method at x-ray fluorescence spectra processing is studied. This is carried out by the example of model spectra at different forms of Bremsstrahlung noise as well as at the presence of background noise in spectra. The interpolation by parabolic splines is used for the estimation of the error of the envelope method for the elimination of continuos background noise. It is found out that the error of the proposed method constitutes decimal parts of percent. It is shown that the envelope method is the effective technique for the elimination of the continuous Bremsstrahlung from x-ray fluorescence spectra of the first order [ru

Development of X-ray radiography examination technology by image processing method

Energy Technology Data Exchange (ETDEWEB)

Min, Duck Kee; Koo, Dae Seo; Kim, Eun Ka [Korea Atomic Energy Research Institute, Taejon (Korea)

1998-06-01

Because the dimension of nuclear fuel rods was measured with rapidity and accuracy by X-ray radiography examination, the set-up of image processing system which was composed of 979 CCD-L camera, image processing card and fluorescent lighting was carried out, and the image processing system enabled image processing to perform. The examination technology of X-ray radiography, which enabled dimension measurement of nuclear fuel rods to perform, was developed by image processing method. The result of dimension measurement of standard fuel rod by image processing method was 2% reduction in relative measuring error than that of X-ray radiography film, while the former was better by 100 {approx} 200 {mu}m in measuring accuracy than the latter. (author). 9 refs., 22 figs., 3 tabs.

Construction of x-ray Kβ filters to monochromatize the radiation of a conventional x-ray tube

International Nuclear Information System (INIS)

Moreira, M.V.B.; Oliveira, A.G.

1987-01-01

The construction of Zr and Nb Kβ filters to produce monochromatic radiation of a conventional X-ray Mo-tube (λK a = 0.7107 A) is described. Disks of NB and Zr, 6.4 mm in diameter and 0.03 to 0.06 mm thick, were prepared. The filters performance was tested by means of NaCl powder difraction patterns. (author) [pt

Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

Directory of Open Access Journals (Sweden)

Apinpus Rujiwatra

2011-01-01

Full Text Available A rapid synthesis of lead zirconate fine powders by microwave-assisted hydrothermal technique is reported. The influences of type of lead precursor, concentration of potassium hydroxide mineraliser, applied microwave power and irradiation time are described. The synthesised powders were characterised by powder X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopic microanalysis and light scattering technique. The merits of the microwave application in reducing reaction time and improving particle mono-dispersion and size uniformity as well as the drawbacks, viz. low purity of the desired phase and increasing demand of mineraliser, are discussed in relation to conventional heating method.

Portable X-ray fluorescence analyzer of high sensitivity using X-ray tube excitation

International Nuclear Information System (INIS)

Vatai, E.; Ando, L.

1982-01-01

A review of the three main methods of X-ray fluorescence analysis and their problems is given. The attainable accuracy and effectiveness of each method are discussed. The main properties of portable X-ray analyzers required by the industry are described. The results and experiences of R and D activities in ATOMKI (Debrecen, Hungary) for developing portable X-ray analyzers are presented. The only way for increasing the accuracy and decreasing the measuring time is the application of X-ray tube excitation instead of radioactive sources. The new ATOMKI equipment presently under construction and patenting uses X-ray tube excitation; it will increase the accuracy of concentration determination by one order of magnitude. (D.Gy.)

The study on the X-ray correction method of long fracture displacement

International Nuclear Information System (INIS)

Jia Bin; Huang Ailing; Chen Fuzhong; Men Chunyan; Sui Chengzong; Cui Yiming; Yang Yundong

2010-01-01

Objective: To explore the image correction of fracture displacement by conventional X-ray photography (ortho tropic and lateral) and test by computed tomography (CT). Methods: The correction method of fracture displacement was designed according to geometry of X-ray photography. Selected one midhumeral fracture specimen which designed with lateral shift and angular displacement, and scanned from anteroposterior and position respectively, and also volume scanned using CT, the data obtained from volume scan were processed using multiplanar reconstruction (MPR) and shaded surface display (SSD). The displacement data relied on X-ray image, CT with MPR and SSD processing, actual design of specimens were compared respectively. Results: The direction and degree of displacement among correction data of X-ray images and the data from MPR and SSD, actual design of specimen were little difference, location difference <1.5 mm, degree difference <1.5 degree. Conclusion: It is really reliable for fracture displacement by conventional X-ray photography with coordinate correction, and it is helpful to obviously improve the diagnostic accuracy of the degree of fracture displacement. (authors)

Surface characterization of selected polymer thin films by total-reflection x-ray fluorescence spectroscopy and x-ray reflectivity

International Nuclear Information System (INIS)

Innis, Vallerie Ann A.

2006-01-01

Development of available x-ray characterizations tools for grazing incidence techniques was done to be able to probe nano-size thin films. Alignment of a Philips x-ray powder diffractometer was improved to let it perform as an x-ray reflectometer. X-ray reflectometry was coupled with total-reflection x-ray fluorescence spectroscopy. Evaluation of the performance of this grazing incidence techniques was done by preparing polymer thin films of carboxymethylcellulose, carrageenan and polyvinylpyrrolidone (PVP). The thickness of the films were varied by varying the process parameters such as concentration, spin speed and spin time. Angle-dispersive total-reflection x-ray fluorescence spectroscopy profiles of three films showed film formation only in carrageenan and PVP. For both carrageenan and PVP, an increase in concentration yielded a corresponding increase in intensity of the fluorescent or scattered peaks. XRR profiles of carrageenan thin films yielded a mean value for the critical angle close to quartz substrate. Thickness measurements of the prepared carrageenan thin films showed that concentration was the main determinant for final film thickness over the other process parameters. Sulfur fluorescent intensity derived from the TXRF measurement showed a linear relationship with the measured thickness by XRR. For PVP, measured critical angle is lower than quartz. Poor adhesion of the polymer onto the substrate yielded a limited number of thickness measurements made from the XRR profiles. (Author)

Effects of X-ray tube parameters on thickness measure precision in X-ray profile gauge

International Nuclear Information System (INIS)

Miao Jichen; Wu Zhifang; Xing Guilai

2011-01-01

Instantaneous profile gauge technology has been widely used in metallurgy industry because it can on-line get the profile of steel strip. It has characters of high measure precision and wide measure range, but the X-ray tube parameters only can be set few different values during measurement. The relations of thickness measure precision and X-ray tube current, X-ray tube voltage were analyzed. The results show that the X-ray tube current affects the thickness measure precision and the X-ray tube voltage determines the thickness measure range. The method of estimating the X-ray current by thickness measure precision was provided in the end. This method is the base of X-ray source selection and X-ray source parameter's setting in the instantaneous profile gauge. (authors)

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

In-house characterization of protein powder

DEFF Research Database (Denmark)

Hartmann, Christian Grundahl; Nielsen, Ole Faurskov; Ståhl, Kenny

2010-01-01

X-ray powder diffraction patterns of lysozyme and insulin were recorded on a standard in-house powder diffractometer. The experimental powder diffraction patterns were compared with patterns calculated from Protein Data Bank coordinate data. Good agreement was obtained by including straightforward...... to include calculated H-atom positions did not improve the overall fit and was abandoned. The method devised was shown to be a quick and convenient tool for distinguishing precipitates and polymorphs of proteins....

Simulation of transmitted X-rays in a polycapillary X-ray lens

Energy Technology Data Exchange (ETDEWEB)

Peng, Shiqi [The Key Laboratory of Beam Technology and Material Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Liu, Zhiguo, E-mail: liuzhiguo512@126.com [The Key Laboratory of Beam Technology and Material 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; Wang, Kai; Yi, Longtao; Yang, Kui; Chen, Man; Wang, Jinbang [The Key Laboratory of Beam Technology and Material Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

2015-09-21

The geometrical description of capillary systems adjusted for the controlled guiding of X-rays and the basic theory of the transmission of X-rays are presented. A method of numerical calculation, based on Ray-Tracing theory, is developed to simulate the transmission efficiency of an X-ray parallel lens and the shape and size of the light spot gain from it. The simulation results for two half-lenses are in good agreement with the experimental results.

Application of radionuclide sources for excitation in energy-dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Hoffmann, P.

1986-01-01

X-ray fluorescence (XRF) analysis is in broad application in many fields of science where elemental determinations are necessary. Solid and liquid samples are analyzed by this method. Solids are introduced in thin or thick samples as melted glass, pellets, powders or as original specimen. The excitation of X-ray spectra can be performed by specific and polychromic radiation of X-ray tubes, by protons, deuterons, α-particles, heavy ions and synchrotron radiation from accelerators and by α-particles, X- and γ-rays and by bremsstrahlung generated by β - -particles from radionuclide sources. The radionuclides are devided into groups with respect to their decay mode and the energy of the emitted radiation. The broad application of radionuclides in XRF excitation is shown in examples as semi-quantitative analysis of glasses, as quantitative analysis of coarse ceramics and as quantitative determination of heavy elements (mainly actinides) in solutions. The advantages and disadvantages of radionuclide excitation in XRF analysis are discussed. (orig.) [de

Method of producing a pseudo-color photograph with X-rays

Energy Technology Data Exchange (ETDEWEB)

Tajima, M

1965-05-08

Conventional black and white X-ray photography cannot simultaneously produce an image on photographic film of a subject having regions of high and low X-ray absorption due to the limitation of photographic density range, gradation and exposure tolerance. This invention records both regions as images of different colors on the same color photographic film. According to a method of this invention for making an X-ray pseudo-color photograph, the subject is directly irradiated by an X-ray beam emergent from an X-ray beam generator, and an X-ray permeation image of the subject is converted into and displayed as a visible light image by means of a fluorescent screen. In one aspect of this invention, there is used a color photographic film which has at least two kinds of sensitive and coloring layers exhibiting the same sensitivity. During the period in which the visible image is displayed, the film is exposed to the visible light in such a way that at least two color filters differing in color and density are successively interposed between the film and the fluorescent screen. In another aspect, a color photographic film is employed having at least two kinds of sensitive and coloring layers exhibiting different sensitivities. During the period in which the visible image is displayed, the film is exposed to visible light by sequentially interposing at least two color filters of different color but of equal density. In this manner, regions comparatively low in X-ray absorption, such as the lungs, and regions comparatively high in absorption, such as the heart, appear as, for example, a blue image and a red image on the color photographic film, respectively.

Graphene oxide powders with different oxidation degree, prepared by synthesis variations of the Hummers method

International Nuclear Information System (INIS)

Guerrero-Contreras, Jesus; Caballero-Briones, F.

2015-01-01

Graphene oxide (GO) powders with different oxidation degree estimated through the relative intensity of the infrared absorption bands related to oxygen containing groups were prepared through variations of the Hummers method. The GO powders were analyzed by Transmission Electron Microscopy, Energy dispersive spectroscopy, X-ray Photoelectron Spectroscopy, Fourier Transform Infrared Spectroscopy, Raman spectroscopy, X-ray Diffraction, UV–VIS spectroscopy and Electrical Resistance measurements. Several square micron GO sheets with low wrinkling were obtained. Oxygen to carbon ratio is around 0.2 in all the samples although a strong variance in the relative intensity of the oxygen related infrared bands is evident. Thus, the oxidation degree was estimated from the FTIR measurements using the quotient between the C–O related bands area to the total area under the spectra. FTIR shows presence of hydroxyl (–OH), epoxy (C–O–C), carboxyl (–COOH) and carbonyl (C=O) moieties and evidence of intermolecular interactions between adjacent groups. These interactions influence the exfoliation degree, the absorbance of the GO suspensions, as well as the electrical resistance, while the crystalline domain sizes, estimated from XRD and Raman do not show a noticeable behavior related with the composition and molecular structure. The results indicate that the electrical resistance is influenced mainly by the surface chemistry of the GO powders and not only by the O/C ratio. The control of the surface chemistry of GO powders would allow their use as additives in organic bulk heterojunction solar cells with enhanced photoconversion efficiency. - Highlights: • Powders of graphene oxide with different oxidation degree were prepared through variations of the Hummers method. • Raman spectroscopy and XRD demonstrated similar crystallite domain size in the samples. • Electrical resistance, exfoliation degree and optical absorption depend on the molecular structure. �

Graphene oxide powders with different oxidation degree, prepared by synthesis variations of the Hummers method

Energy Technology Data Exchange (ETDEWEB)

Guerrero-Contreras, Jesus; Caballero-Briones, F., E-mail: fcaballero@ipn.mx

2015-03-01

Graphene oxide (GO) powders with different oxidation degree estimated through the relative intensity of the infrared absorption bands related to oxygen containing groups were prepared through variations of the Hummers method. The GO powders were analyzed by Transmission Electron Microscopy, Energy dispersive spectroscopy, X-ray Photoelectron Spectroscopy, Fourier Transform Infrared Spectroscopy, Raman spectroscopy, X-ray Diffraction, UV–VIS spectroscopy and Electrical Resistance measurements. Several square micron GO sheets with low wrinkling were obtained. Oxygen to carbon ratio is around 0.2 in all the samples although a strong variance in the relative intensity of the oxygen related infrared bands is evident. Thus, the oxidation degree was estimated from the FTIR measurements using the quotient between the C–O related bands area to the total area under the spectra. FTIR shows presence of hydroxyl (–OH), epoxy (C–O–C), carboxyl (–COOH) and carbonyl (C=O) moieties and evidence of intermolecular interactions between adjacent groups. These interactions influence the exfoliation degree, the absorbance of the GO suspensions, as well as the electrical resistance, while the crystalline domain sizes, estimated from XRD and Raman do not show a noticeable behavior related with the composition and molecular structure. The results indicate that the electrical resistance is influenced mainly by the surface chemistry of the GO powders and not only by the O/C ratio. The control of the surface chemistry of GO powders would allow their use as additives in organic bulk heterojunction solar cells with enhanced photoconversion efficiency. - Highlights: • Powders of graphene oxide with different oxidation degree were prepared through variations of the Hummers method. • Raman spectroscopy and XRD demonstrated similar crystallite domain size in the samples. • Electrical resistance, exfoliation degree and optical absorption depend on the molecular structure. �

Smoothed Particle Inference: A Kilo-Parametric Method for X-ray Galaxy Cluster Modeling

Energy Technology Data Exchange (ETDEWEB)

Peterson, John R.; Marshall, P.J.; /KIPAC, Menlo Park; Andersson, K.; /Stockholm U. /SLAC

2005-08-05

We propose an ambitious new method that models the intracluster medium in clusters of galaxies as a set of X-ray emitting smoothed particles of plasma. Each smoothed particle is described by a handful of parameters including temperature, location, size, and elemental abundances. Hundreds to thousands of these particles are used to construct a model cluster of galaxies, with the appropriate complexity estimated from the data quality. This model is then compared iteratively with X-ray data in the form of adaptively binned photon lists via a two-sample likelihood statistic and iterated via Markov Chain Monte Carlo. The complex cluster model is propagated through the X-ray instrument response using direct sampling Monte Carlo methods. Using this approach the method can reproduce many of the features observed in the X-ray emission in a less assumption-dependent way that traditional analyses, and it allows for a more detailed characterization of the density, temperature, and metal abundance structure of clusters. Multi-instrument X-ray analyses and simultaneous X-ray, Sunyaev-Zeldovich (SZ), and lensing analyses are a straight-forward extension of this methodology. Significant challenges still exist in understanding the degeneracy in these models and the statistical noise induced by the complexity of the models.

X-ray and nuclear methods for comparative analysis of environmental samples

International Nuclear Information System (INIS)

Kudryashov, V.I.; Gundorina, S.F.; Frontas'eva, M.V.; Saidmuradov, Zh.

1988-01-01

X-ray and instrumental neutron activation methods, and in some cases methods of photon activation (X-ray spectral analysis with proton activation and analysis on the basis of (p, n) reaction) were used to obtain elementary content of different water samples. The possibility of getting space-time dependences of trace elementary concentrations in water (and under certain conditions in atmosphere) is shown. These data are to be used at a complex investigation of sanitary norms of water systems. The advantages of abovementined methods are discussed for obtaining different elementary content in water in different ways

X-ray phase analysis in leucite systems

Czech Academy of Sciences Publication Activity Database

Maixner, J.; Kloužková, A.; Mrázová, M.; Kohoutková, Martina

2007-01-01

Roč. 26, č. 2 (2007), s. 531-536 ISSN 0044-2968 R&D Projects: GA MPO 2A-1TP1/063 Institutional research plan: CEZ:AV0Z40320502 Keywords : cubic leucite * phase transformation * X-ray powder diffraction Subject RIV: CA - Inorganic Chemistry Impact factor: 1.338, year: 2007

Synthesis of alumina powders by precipitation method and solvothermal treatment

International Nuclear Information System (INIS)

Politchuk, J.O.; Lima, N.B.; Lazar, D.R.R.; Ussui, V.; Yoshito, W.K.

2012-01-01

The improvement of alumina powders synthesis processes has been focused on the preparation of ceramic powders with well defined crystalline structure and with high specific surface area and nanometric particle size without formation of hard agglomerates. For this purpose the precipitation step should be studied and and also the temperature of alumina crystallization should be reduced. The aim of this study was to obtain alumina powders by hydroxide precipitation with ammonia in the presence of cationic surfactant, followed by solvothermal treatment and calcination. The powders were characterized by TG/DTA, X-ray diffraction, surface area measurements by gas adsorption (BET) and scanning electron microscopy. The results showed that powders produced by solvothermal treatment without surfactant have higher crystallinity. However the presence of CTAB enhances 240% the specific surface area compared with powders produced without this reagent (author)

X-ray diagnostic in gas discharge

International Nuclear Information System (INIS)

Chen Suhe; Wang Dalun; Cui Gaoxian; Wang Mei; Fu Yibei; Zhang Xinwei; Zhang Wushou

1995-01-01

X rays were observed when the anomalous phenomenon in the metal loaded with deuterium studied by the gas-discharge method. Therefore the X-ray energy spectra were measured by the absorption method, the specific X-ray approach and the NaI scintillation counter, while X-ray intensity was estimated by using 7 Li thermoluminescent foils. The X-ray average energy measured by the absorption method is 27.6 +- 2.1 keV, which is fitted within the error extent to 26.0 +-2.4 keV monoenergetic X rays measured by the NaI scintillation counter

Characterization of (1 1 1) surface tailored Pt nanoparticles by electrochemistry and X-ray powder diffraction

International Nuclear Information System (INIS)

Beyerlein, K.R.; Solla-Gullon, J.; Herrero, E.; Garnier, E.; Pailloux, F.; Leoni, M.; Scardi, P.; Snyder, R.L.; Aldaz, A.; Feliu, J.M.

2010-01-01

Platinum nanoparticles with a mean size of 8.7 nm were synthesized by a salt reduction reaction having polyhedron shapes with preferential (1 1 1) surfaces. In situ electrochemical characterization of nanoparticles was performed which confirmed the existence of mostly (1 1 1) surface sites in the sample. The effect of this surface in the electrooxidation of CO was measured. Debye Function Analysis (DFA) and Whole Powder Pattern Modelling (WPPM) of the measured X-ray diffraction pattern were carried out to obtain statistical information on the particle size and shape present in the sample. Both analyses determined that the octahedron particle shape was the most abundant which was also consistent with TEM observations. The existence of a small percentage of single twinned particles was determined by DFA, WPPM, as well as analysis of HRTEM images.

Cone Beam X-ray Luminescence Computed Tomography Based on Bayesian Method.

Science.gov (United States)

Zhang, Guanglei; Liu, Fei; Liu, Jie; Luo, Jianwen; Xie, Yaoqin; Bai, Jing; Xing, Lei

2017-01-01

X-ray luminescence computed tomography (XLCT), which aims to achieve molecular and functional imaging by X-rays, has recently been proposed as a new imaging modality. Combining the principles of X-ray excitation of luminescence-based probes and optical signal detection, XLCT naturally fuses functional and anatomical images and provides complementary information for a wide range of applications in biomedical research. In order to improve the data acquisition efficiency of previously developed narrow-beam XLCT, a cone beam XLCT (CB-XLCT) mode is adopted here to take advantage of the useful geometric features of cone beam excitation. Practically, a major hurdle in using cone beam X-ray for XLCT is that the inverse problem here is seriously ill-conditioned, hindering us to achieve good image quality. In this paper, we propose a novel Bayesian method to tackle the bottleneck in CB-XLCT reconstruction. The method utilizes a local regularization strategy based on Gaussian Markov random field to mitigate the ill-conditioness of CB-XLCT. An alternating optimization scheme is then used to automatically calculate all the unknown hyperparameters while an iterative coordinate descent algorithm is adopted to reconstruct the image with a voxel-based closed-form solution. Results of numerical simulations and mouse experiments show that the self-adaptive Bayesian method significantly improves the CB-XLCT image quality as compared with conventional methods.

Applications of the Basic programming language in X-ray spectrometry

International Nuclear Information System (INIS)

Diaz-Guerra, J.P.; Roca, M.

1981-01-01

An assembly of programs written in ''Basic'' language and related with the calculation needs at the X-ray spectrometry laboratory of the Spanish J.E.N. has been developed. The principal problems considered, concerning the X-ray fluorescence technique, are the following: selection of the instrumental parameters; correction of the effects due to the dead time, background and spectral interferences; fitting of polynomial functions, which relate the variables intensity-concentration; application of some empirical-mathematical methods (Lucas-Tooth, Beattie and Brissey and Tertian procedures) to the correction of the inter-element effects; addition method, and statistical treatment of the results (correlation coefficient and ''F'' and ''t'' tests). Likewise, programs for the computation of spacings from powder diffraction patterns (Debye-Scherrer and counter diffractometer procedures) have been written. The proposed programs run following conversational patterns, in which different possibilities and incidences have been foreseen. (author)

X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

International Nuclear Information System (INIS)

Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Dziadowicz, M.; Kopeć, E.; Majewska, U.; Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I.; Wudarczyk-Moćko, J.; Góźdź, S.

2015-01-01

A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

Energy Technology Data Exchange (ETDEWEB)

Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Dziadowicz, M.; Kopeć, E. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Majewska, U. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Wudarczyk-Moćko, J. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Góźdź, S. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Institute of Public Health, Jan Kochanowski University, IX Wieków Kielc 19, 25-317 Kielce (Poland)

2015-12-01

A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

X-ray spectroscopy and X-ray crystallography of metalloenzymes at XFELs

International Nuclear Information System (INIS)

Yano, Junko

2016-01-01

The ultra-bright femtosecond X-ray pulses provided by X-ray Free Electron Lasers (XFELs) open capabilities for studying the structure and dynamics of a wide variety of biological and inorganic systems beyond what is possible at synchrotron sources. Although the structure and chemistry at the catalytic sites have been studied intensively in both biological and inorganic systems, a full understanding of the atomic-scale chemistry requires new approaches beyond the steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure at ambient conditions, while overcoming X-ray damage to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by using the intense and ultra-short femtosecond X-ray pulses from an XFEL, where sample is probed before it is damaged. We have developed methodology for simultaneously collecting crystallography data and X-ray emission spectra, using an energy dispersive spectrometer at ambient conditions. In addition, we have developed a way to collect metal L-edge data of dilute samples using soft X-rays at XFELs. The advantages and challenges of these methods will be described in this review. (author)

Quantitative X-ray diffraction analysis of alumina, silicon carbide and zirconium carbide in ceramic composites

International Nuclear Information System (INIS)

Veiga, Sonia M.B.; Bressiani, Jose Carlos; Veiga, Marcello M.; Chaklader, Asoke C.D.

1995-01-01

The x-ray diffraction technique has been successfully applied to determine the phases formed in a carbo thermal synthesis of ceramic composites (Al 2 O 3 -Si C and Al 2 O 3 -Si C-Zr C) using kaolinite, cyanite and zircon as precursors. The powder method using fluorite as internal standard has shown reliable results to estimate accurately phases in composites (relative error as low as 5%). In addition, quantitative X-ray analysis allows an indirect evaluation of Si O (gas) losses from the system during the carbo thermal reaction. (author)

High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

Science.gov (United States)

Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

2015-06-01

High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

Powder diffraction

Energy Technology Data Exchange (ETDEWEB)

Hart, M.

1995-12-31

the importance of x-ray powder diffraction as an analytical tool for phase identification of materials was first pointed out by Debye and Scherrer in Germany and, quite independently, by Hull in the US. Three distinct periods of evolution lead to ubiquitous application in many fields of science and technology. In the first period, until the mid-1940`s, applications were and developed covering broad categories of materials including inorganic materials, minerals, ceramics, metals, alloys, organic materials and polymers. During this formative period, the concept of quantitative phase analysis was demonstrated. In the second period there followed the blossoming of technology and commercial instruments became widely used. The history is well summarized by Parrish and by Langford and Loueer. By 1980 there were probably 10,000 powder diffractometers in routine use, making it the most widely used of all x-ray crystallographic instruments. In the third, present, period data bases became firmly established and sophisticated pattern fitting and recognition software made many aspects of powder diffraction analysis routine. High resolution, tunable powder diffractometers were developed at sources of synchrotron radiation. The tunability of the spectrum made it possible to exploit all the subtleties of x-ray spectroscopy in diffraction experiments.

Powder diffraction

International Nuclear Information System (INIS)

Hart, M.

1995-01-01

The importance of x-ray powder diffraction as an analytical tool for phase identification of materials was first pointed out by Debye and Scherrer in Germany and, quite independently, by Hull in the US. Three distinct periods of evolution lead to ubiquitous application in many fields of science and technology. In the first period, until the mid-1940's, applications were and developed covering broad categories of materials including inorganic materials, minerals, ceramics, metals, alloys, organic materials and polymers. During this formative period, the concept of quantitative phase analysis was demonstrated. In the second period there followed the blossoming of technology and commercial instruments became widely used. The history is well summarized by Parrish and by Langford and Loueer. By 1980 there were probably 10,000 powder diffractometers in routine use, making it the most widely used of all x-ray crystallographic instruments. In the third, present, period data bases became firmly established and sophisticated pattern fitting and recognition software made many aspects of powder diffraction analysis routine. High resolution, tunable powder diffractometers were developed at sources of synchrotron radiation. The tunability of the spectrum made it possible to exploit all the subtleties of x-ray spectroscopy in diffraction experiments

Bulk synthesis of nanocrystalline urania powders by citrate gel-combustion method

Science.gov (United States)

Sanjay Kumar, D.; Ananthasivan, K.; Venkata Krishnan, R.; Amirthapandian, S.; Dasgupta, Arup

2016-01-01

Bulk quantities (60 g) of nanocrystalline (nc) free flowing urania powders with crystallite size ranging from 38 to 252 nm have been synthesized for the first time by the citrate gel combustion method. A systematic study of the influence of the fuel (citric acid) to oxidant (nitrate) ratio (R) on the characteristics of the urania powders has been carried out for the first time. Mixture with an "R" value of 0.25 exhibited a vigorous auto-ignition reaction. This reaction was investigated with Differential Scanning Calorimetry (DSC) and in-situ thermogravimetry coupled with differential thermal analysis and mass spectrometry (TG-DTA-MS). The bulk density, specific surface area, X-ray crystallite size, residual carbon and size distribution of particles of this powder were unique. Microscopic and microstructural investigation of selected samples revealed the presence of nanocrystals with irregular exfoliated morphology; their Electron Energy Loss Spectra testified the covalency of the U-O bond.

X-ray studies on electrochemical systems. Synchrotron methods for energy materials

Energy Technology Data Exchange (ETDEWEB)

Braun, Artur [Empa. Eidgenoessische Materialpruefungs- und Forschungsanstalt, Duebendorf (Switzerland)

2017-07-01

This book is your graduate level entrance into battery, fuel cell and solar cell research at synchrotron X-ray sources. Materials scientists find numerous examples for the combination of electrochemical experiments with simple and with highly complex X-ray scattering and spectroscopy methods. Physicists and chemists can link applied electrochemistry with fundamental concepts of condensed matter physics, physical chemistry and surface science.

Method of producing a pseudo-color photograph with X-rays

International Nuclear Information System (INIS)

Tajima, Mataichi.

1965-01-01

Conventional black and white X-ray photography cannot simultaneously produce an image on photographic film of a subject having regions of high and low X-ray absorption due to the limitation of photographic density range, gradation and exposure tolerance. This invention records both regions as images of different colors on the same color photographic film. According to a method of this invention for making an X-ray pseudo-color photograph, the subject is directly irradiated by an X-ray beam emergent from an X-ray beam generator, and an X-ray permeation image of the subject is converted into and displayed as a visible light image by means of a fluorescent screen. In one aspect of this invention, there is used a color photographic film which has at least two kinds of sensitive and coloring layers exhibiting the same sensitivity. During the period in which the visible image is displayed, the film is exposed to the visible light in such a way that at least two color filters differing in color and density are successively interposed between the film and the fluorescent screen. In another aspect, a color photographic film is employed having at least two kinds of sensitive and coloring layers exhibiting different sensitivities. During the period in which the visible image is displayed, the film is exposed to visible light by sequentially interposing at least two color filters of different color but of equal density. In this manner, regions comparatively low in X-ray absorption, such as the lungs, and regions comparatively high in absorption, such as the heart, appear as, for example, a blue image and a red image on the color photographic film, respectively. (Takasuka, S.)

Moving-Article X-Ray Imaging System and Method for 3-D Image Generation

Science.gov (United States)

Fernandez, Kenneth R. (Inventor)

2012-01-01

An x-ray imaging system and method for a moving article are provided for an article moved along a linear direction of travel while the article is exposed to non-overlapping x-ray beams. A plurality of parallel linear sensor arrays are disposed in the x-ray beams after they pass through the article. More specifically, a first half of the plurality are disposed in a first of the x-ray beams while a second half of the plurality are disposed in a second of the x-ray beams. Each of the parallel linear sensor arrays is oriented perpendicular to the linear direction of travel. Each of the parallel linear sensor arrays in the first half is matched to a corresponding one of the parallel linear sensor arrays in the second half in terms of an angular position in the first of the x-ray beams and the second of the x-ray beams, respectively.

A study of x-ray microbeam stress measurement for local area

International Nuclear Information System (INIS)

Natsume, Yoshitaka; Miyakawa, Susumu

1987-01-01

A new type X-ray microbeam equipment which is capable of three-dimensional oscillation at an X-ray radiation position was used to measure the residual stress of pure iron powder and bending plate specimens as well as that in the vicinity of fatigue crack tip of 1/2 CT specimen. The results obtained are summerized as follows. (1) Diffraction profiles of pure iron powder with diameter 0.02 ∼ 0.03 μm particle size obtained by the present microbeam technique in the beam area of 80 μm in diamether and measuring time more than 800 sec showed Kα 1 and Kα 2 peaks clearly, so that these profiles are good enough for stress measurement. (2) The measured stress of pure iron powder with diameter 10 ∼ 25 μm particle size in the beam area of 80 μm in diameter was not equal to 0 MPa. The measured stress varied greatly and was independent of measuring time. (3) The measured stress of pure iron powder with diameter 0.02 ∼ 0.03 μm particle size in the beam area of 80 μm in diameter was almost 1 MPa, which shows the good accuracy of this X-ray micro-beam equipment. (4) The relation between the X-ray measured stress and the mechanically applied stress showed good agreement. (5) The distribution of residual stress at the vicinity of fatigue crack tip showed that the residual stress at the fatigue crack tip was compression and the residual stress in front of crack tip was tension. This tensile residual stress in front of crack tip existed in the area from 0.02 mm to 2 mm. (6) The above results show that the present equipment is advantageous in the investigation of local stress, shortening the measuring time without sacrificing the accuracy. (author)

Imaging plate, a new type of x-ray area detector

International Nuclear Information System (INIS)

Kamiya, Nobuo; Amemiya, Yoshiyuki; Miyahara, Junji.

1986-01-01

In respective fields of X-ray crystallography, for the purpose of the efficient collection of reciprocal space information, two-dimensional X-ray detectors such as multiwire proportional chambers and X-ray television sets have been used together with conventional X-ray films. X-ray films are characterized by uniform sensitivity and high positional resolution over a wide area, but the sensitivity is low, and the range of action and the linearity of the sensitivity is problematic. They require the development process, accordingly lack promptitude. The MWPCs and X-ray television sets are superior in the sensitivity, its linearity, the range of action and promptitude, but interior in the uniformity and resolution to the films. Imaging plate is a new X-ray area detector developed by Fuji Photo Film Co., Ltd., for digital X-ray medical image diagnosis. This detector is superior in all the above mentioned performances, and it seems very useful also for X-ray crystallography. In this paper, the system composed of an imaging plate and its reader is described, and the basic performance as an X-ray area detector and the results of having recorded the diffraction images of protein crystals as the example of applying it to X-ray crystallography are reported. The imaging plate is that the crystalline fluorescent powder of BaFBr doped with Eu 2+ ions is applied on plastic films. (Kako, I.)

X-ray film cassette and method of making

International Nuclear Information System (INIS)

1980-01-01

An x-ray film cassette which is capable of providing forces on the film that vary across the surface of the cassette is described. Methods of manufacture are discussed. The system is of particular use when large area films are used in conjunction with intensifying screens. (U.K.)

X-ray interferometric Fourier holography

International Nuclear Information System (INIS)

Balyan, M.K.

2016-01-01

The X-ray interferometric Fourier holography is proposed and theoretically investigated. Fourier The X-ray interferometric Young fringes and object image reconstruction are investigated. It is shown that the interference pattern of two slits formed on the exit surface of the crystal-analyzer (the third plate of the interferometer) is the X-ray interferometric Young fringes. An expression for X-ray interferometric Young fringes period is obtained. The subsequent reconstruction of the slit image as an object is performed by means of Fourier transform of the intensity distribution on the hologram. Three methods of reconstruction of the amplitude transmission complex function of the object are presented: analytical - approximate method, method of iteration and step by step method. As an example the X-ray Fourier interferometric hologram recording and the complex amplitude transmission function reconstruction for a beryllium circular wire are considered

Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

Directory of Open Access Journals (Sweden)

K. Jeyadheepan

2014-01-01

Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

Application of the X-ray fluorescence analysis and X-ray diffraction in geochemical studies of the Pleistocene tills from Holy Cross Mountains

International Nuclear Information System (INIS)

Kubala-Kukuś, A.; Ludwikowska-Kedzia, M.; Banaś, D.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.

2013-01-01

X-ray fluorescence analysis methods (wavelength dispersive X-ray fluorescence analysis (WDXRF) and total reflection X-ray fluorescence (TXRF)) and X-ray powder diffraction (XRPD) have been applied in complementary geochemical studies of the Pleistocene till samples. The XRPD technique gave information about the mineral composition of the analyzed samples while the WDXRF and TXRF studies allowed the fast elemental analysis. The till samples were collected from different regions of Holy Cross Mountains (located in central Poland) which are still not unambiguously described in the context of the geochemical studies of the Quaternary sediments. The analysis was concentrated on the geochemical composition of the till samples both for materials occurring on the surface (characterized by continuous weathering processes) and for samples taken from core borehole. The overriding purpose of these studies is determination of the local lithotype of the tills and its lithologic and petrographic diagnostic properties, including the chemical composition of clay and minerals found in the clay. In the presented work the experimental sets up, sample preparation procedure and measurements programme will be discussed in details. Finally, the elemental and mineral compositions will be presented for studied different groups of the samples. - Highlights: • XRF analysis and X-ray diffraction used in studies of the till samples. • The till samples were collected from different regions of Holy Cross Mountains. • The analysis concentrates both on the samples from surface and from core borehole. • The purpose is determination of the local lithotype of the tills. • The experimental setup, sample preparation, measurements and results are discussed

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

International Nuclear Information System (INIS)

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

2000-01-01

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

Duodenal X-ray diagnostics

International Nuclear Information System (INIS)

Scheppach, W.

1982-01-01

The publication provides an overview of duodenal X-ray diagnostics with the aid of barium meals in 1362 patients. The introducing paragraphs deal with the topographic anatomy of the region and the methodics of X-ray investigation. The chapter entitled ''processes at the duodenum itself'' describes mainly ulcers, diverticula, congenital anomalies, tumors and inflammations. The neighbourhood processes comprise in the first place diseases having their origin at the pancreas and bile ducts. As a conclusion, endoscopic rectograde cholangio-pancreaticography and percutaneous transhepatic cholangiography are pointed out as advanced X-ray investigation methods. In the annex of X-ray images some of the described phenomena are shown in exemplary manner. (orig./MG) [de

Comparison of physical chemical properties of powders and respirable aerosols of industrial mixed uranium and plutonium oxide fuels

International Nuclear Information System (INIS)

Eidson, A.F.

1982-01-01

Studies were performed to characterize physical and chemical properties which may be important in determining the metabolism of accidentally released, inhaled aerosols of industrial mixed uranium and plutonium oxide fuels and to compare the properties of bulk powders and the respirable fraction they include. X-ray diffraction measurements showed that analysis of mixed-oxide powders from four process steps served to characterize their respirable fractions. IR spectroscopy was useful as a method to detect organic binders that were not observed by X-ray diffraction methods. Both X-ray diffraction and IR spectroscopy methods can be used in combination to identify the sources of a complex aerosol that might be released from more than one fabrication step. Isotopic distributions in powders and aerosols showed that information important for radiation dose to tissue calculations or Pu lung burden estimates can be obtained by analysis of powders. (U.K.)

Benchtop phase-contrast X-ray imaging

Energy Technology Data Exchange (ETDEWEB)

Gundogdu, O. [Department of Physics, University of Surrey, Guildford, Surrey GU2 7XH (United Kingdom)], E-mail: o.gundogdu@surrey.ac.uk; Nirgianaki, E.; Che Ismail, E.; Jenneson, P.M.; Bradley, D.A. [Department of Physics, University of Surrey, Guildford, Surrey GU2 7XH (United Kingdom)

2007-12-15

Clinical radiography has traditionally been based on contrast obtained from absorption when X-rays pass through the body. The contrast obtained from traditional radiography can be rather poor, particularly when it comes to soft tissue. A wide range of media of interest in materials science, biology and medicine exhibit very weak absorption contrast, but they nevertheless produce significant phase shifts with X-rays. The use of phase information for imaging purposes is therefore an attractive prospect. Some of the X-ray phase-contrast imaging methods require highly monochromatic plane wave radiation and sophisticated X-ray optics. However, the propagation-based phase-contrast imaging method adapted in this paper is a relatively simple method to implement, essentially requiring only a microfocal X-ray tube and electronic detection. In this paper, we present imaging results obtained from two different benchtop X-ray sources employing the free space propagation method. X-ray phase-contrast imaging provides higher contrast in many samples, including biological tissues that have negligible absorption contrast.

On the methods of determination of x-ray sources protection quality in x-ray diagnostic equipment

International Nuclear Information System (INIS)

Vladimirov, L.V.

1973-01-01

Existing procedures for assessing the quality of shielding of X-ray radiators are compared; these procedures are shown to have a number of shortcomings and to be very time-consuming. A procedure is offered in which shielding quality is tested in two stages: (1) X-ray tests aimed at determining the quality of protection of the X-ray tube unit; and (2) dosimeter tests proper. The results of measurements are compared with maximum permissible dosage rate

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

International Nuclear Information System (INIS)

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

2003-01-01

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

Cone Beam X-Ray Luminescence Tomography Imaging Based on KA-FEM Method for Small Animals.

Science.gov (United States)

Chen, Dongmei; Meng, Fanzhen; Zhao, Fengjun; Xu, Cao

2016-01-01

Cone beam X-ray luminescence tomography can realize fast X-ray luminescence tomography imaging with relatively low scanning time compared with narrow beam X-ray luminescence tomography. However, cone beam X-ray luminescence tomography suffers from an ill-posed reconstruction problem. First, the feasibility of experiments with different penetration and multispectra in small animal has been tested using nanophosphor material. Then, the hybrid reconstruction algorithm with KA-FEM method has been applied in cone beam X-ray luminescence tomography for small animals to overcome the ill-posed reconstruction problem, whose advantage and property have been demonstrated in fluorescence tomography imaging. The in vivo mouse experiment proved the feasibility of the proposed method.

Synchrotron x-ray methods in studies of thin organic film structure

International Nuclear Information System (INIS)

Gentle, I.

2002-01-01

Full text: In recent years, the study of the structures of organic films as thin as a single monolayer has been revolutionized by methods that take advantage of the characteristics of synchrotron radiation. In particular, the methods of grazing incidence X-ray diffraction (GIXD) and X-ray reflectivity have led to a number of valuable insights into structural aspects of thin films at molecular resolution. Our group has been studying films formed at the air/water interface as insoluble monolayers and subsequently transferred to solid substrates using either the vertical (Langmuir-Blodgett) or horizontal (Langmuir-Schaeffer) methods. The main aim of these experiments is to exert control over film structure in the direction parallel to the substrate surface. This is highly desirable in order to design devices that exploit the optical and electrooptical properties of functional materials, but is difficult to do. By varying the chemical structure of the film materials and controlling deposition conditions a degree of control is possible, but only using synchrotron methods can it be easily verified. We have also developed a novel method of rapidly collecting data from GIXD measurements by the application of area detection (imaging plates), which has made possible measurements of dynamic processes such as in-situ annealing. Such measurements are not possible using traditional scanning methods. One area of current interest is films composed of porphyrins as functional materials, either alone or as mixed films with fatty acids. We have been investigating ways of assembling porphyrins in such a way as to overcome the tendency to aggregate, and to produce patterning and ordered structures in the plane of the interface. Examples will be given of how film composition and deposition method affects the final structure, and of how X-ray methods can be used to elucidate both the structures and the mechanisms. Copyright (2002) Australian X-ray Analytical Association Inc

Tokamak physics studies using x-ray diagnostic methods

International Nuclear Information System (INIS)

Hill, K.W.; Bitter, M.; von Goeler, S.

1987-03-01

X-ray diagnostic measurements have been used in a number of experiments to improve our understanding of important tokamak physics issues. The impurity content in TFTR plasmas, its sources and control have been clarified through soft x-ray pulse-height analysis (PHA) measurements. The dependence of intrinsic impurity concentrations and Z/sub eff/ on electron density, plasma current, limiter material and conditioning, and neutral-beam power have shown that the limiter is an important source of metal impurities. Neoclassical-like impurity peaking following hydrogen pellet injection into Alcator C and a strong effect of impurities on sawtooth behavior were demonstrated by x-ray imaging (XIS) measurements. Rapid inward motion of impurities and continuation of m = 1 activity following an internal disruption were demonstrated with XIS measurements on PLT using injected aluminum to enhance the signals. Ion temperatures up to 12 keV and a toroidal plasma rotation velocity up to 6 x 10 5 m/s have been measured by an x-ray crystal spectrometer (XCS) with up to 13 MW of 85-keV neutral-beam injection in TFTR. Precise wavelengths and relative intensities of x-ray lines in several helium-like ions and neon-like ions of silver have been measured in TFTR and PLT by the XCS. The data help to identify the important excitation processes predicted in atomic physics. Wavelengths of n = 3 to 2 silver lines of interest for x-ray lasers were measured, and precise instrument calibration techniques were developed. Electron thermal conductivity and sawtooth dynamics have been studied through XIS measurements on TFTR of heat-pulse propagation and compound sawteeth. A non-Maxwellian electron distribution function has been measured, and evidence of the Parail-Pogutse instability identified by hard x-ray PHA measurements on PLT during lower-hybrid current-drive experiments

Solid-state x-ray receptor and method of making same

International Nuclear Information System (INIS)

Dorman, A.; Glave, W.K.; Birnbach, C.

1985-01-01

An X-ray receptor for producing electrical signals representative of an X-ray image is discussed. An array of semiconductor elements is mounted on at least one support, each element being formed of semiconductor material which is an element of Group 4A of the Periodic Table of Elements or a compound of such an element, or which is at least one element of Group 3A of the Periodic Table of Elements together with at least one element of Group 5A of the Periodic Table of Elements, and having at least one PN junction therein. The array is positioned to receive impinging X-rays and to produce electrical signals in response thereto. Electrical conducting leads are supported on the support, and the electrical signals which are produced by respective ones of the semiconductor elements are coupled to these electrical conducting leads. Output terminals also are supported on the support to provide output image signals; and circuitry including multiplexing circuits additionally is supported on the support for processing and multiplexing the electrical signals from the electrical conducting leads to the output terminals. Also disclosed is a method by which the X-ray receptor is made

Bone X-Ray (Radiography)

Medline Plus

Full Text Available ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures that ...

Photocatalytic Activity in CH3CN Related to the Surface Properties of TiO2 Powders Prepared by Sol-Gel Method

OpenAIRE

Bettoni, Marta; Candori, Pietro; Marmottini, Fabio; Perenze, Nicoletta; Rol, Cesare; Sebastiani, Giovanni V.; Vecchiocattivi, Franco

2009-01-01

Some TiO2 powders, prepared from titanium(IV)tetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka) of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl al...

Thermoluminescent dosemeter in a X-ray diffractometer

International Nuclear Information System (INIS)

Mendoza A, D.; Gonzalez M, P.; Falcon B, T.; Castano, V.M.

1999-01-01

In this work it was presented the results obtained of the dosimetry which was realized in a X-ray diffractometer for powders, trademark Siemens D5000, using the thermoluminescent signal generated by the X-rays in the commercial dosemeter TLD-100 of Harshaw, US. In according to the results obtained, the radiation quantity received by an analysed material in the diffractometer, will be proportional to exposure time and it can vary from unities until tenths of grays. These results are very outstanding when are analysed crystalline materials in a diffractometer, for knowing the present crystalline phases, mainly if these are highly sensitive to the ionizing radiation, as it is the case of the thermoluminescent materials. (Author)

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Determination of copper in geological materials by X-ray fluorescence

International Nuclear Information System (INIS)

Roca, M.; Bayon, A.

1981-01-01

X-ray fluorescence has been applied to the determination of copper content of geological materials in the concentration range of 0.01 to % CuO. A molybdenum target tube Is used, samples being presented in finely-ground powder form. Various methods for the correction for background and Instrumental copper interferences have been considered. To correct for matrix effects different tube scattered primary radiations have been tested as references or internal standards. MoK(41 - (C) provides the most suitable results. The use of influence empirical coefficients for the effect of iron on copper and of mass absorption coefficients has also been considered. For samples with a high content of lead, several procedures to correct for I t s influence have been investigated. Comparison between data obtained by X-ray fluorescence and wet-chemical techniques indicated good agreement. (Author) 6 refs

X ray Production. Chapter 5

Energy Technology Data Exchange (ETDEWEB)

Nowotny, R. [Medical University of Vienna, Vienna (Austria)

2014-09-15

The differential absorption of X rays in tissues and organs, owing to their atomic composition, is the basis for the various imaging methods used in diagnostic radiology. The principles in the production of X rays have remained the same since their discovery. However, much refinement has gone into the design of X ray tubes to achieve the performance required for today’s radiological examinations. In this chapter, an outline of the principles of X ray production and a characterization of the radiation output of X ray tubes will be given. The basic processes producing X rays are dealt with in Section 1.4.

X-ray Absorption Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Yano, Junko; Yachandra, Vittal K.

2009-07-09

This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

Feasibility of using continuous X-ray to simulate cable response under X-ray environment

International Nuclear Information System (INIS)

Ma Liang; Zhou Hui; Cheng Yinhui; Wu Wei; Li Jinxi; Zhao Mo; Guo Jinghai

2014-01-01

The mechanism and simulating method of cable response induced by X-ray were researched, and the relationship of cable response irradiated by continuous and pulsed X-ray was analyzed. A one-dimension model of strip line irradiation response of X-ray was given, which includes the gap between cable shield and dielectric, and induced conductivity in cable dielectric. The calculation result using the model indicates that the cable responses of continuous and rectangular-pulsed X-ray have the similar current waveform and the same gap voltages. Therefore, continuous X-ray can be used to research some cable responses of pulsed X-ray irradiation under the mechanism described in the one-dimension model. (authors)

Characterization of a pulsed x-ray source for fluorescent lifetime measurements

International Nuclear Information System (INIS)

Blankespoor, S.C.; Derenzo, S.E.; Moses, W.W.; Rossington, C.S.; Ito, M.; Oba, K.

1994-01-01

To search for new, fast, inorganic scintillators, the authors have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 μA maximum average cathode current. The laser produces 3 x 10 7 photons at 650 nm per ∼100 ps pulse, with up to 10 7 pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray energy at tube biases of 20, 25, and 30 kV is 9.4, 10.3, and 11.1 keV, respectively. The authors measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian, at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 x 10 6 and 3 x 10 6 photons/sec/steradian at biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented

Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

Energy Technology Data Exchange (ETDEWEB)

Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M.; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie, E-mail: valerie.panneels@psi.ch [Paul Scherrer Institute, OFLC/103, 5232 Villigen-PSI (Switzerland)

2015-06-27

A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

Bone age assessment by dual-energy X-ray absorptiometry in children: an alternative for X-ray?

Science.gov (United States)

Heppe, D H M; Taal, H R; Ernst, G D S; Van Den Akker, E L T; Lequin, M M H; Hokken-Koelega, A C S; Geelhoed, J J M; Jaddoe, V W V

2012-02-01

The aim of the study was to validate dual-energy X-ray absorptiometry (DXA) as a method to assess bone age in children. Paired dual-energy X-ray absorptiometry (DXA) scans and X-rays of the left hand were performed in 95 children who attended the paediatric endocrinology outpatient clinic of University Hospital Rotterdam, the Netherlands. We compared bone age assessments by DXA scan with those performed by X-ray. Bone age assessment was performed by two blinded observers according to the reference method of Greulich and Pyle. Intra-observer and interobserver reproducibility were investigated using the intraclass correlation coefficient (ICC), and agreement was tested using Bland and Altman plots. The intra-observer ICCs for both observers were 0.997 and 0.991 for X-ray and 0.993 and 0.987 for DXA assessments. The interobserver ICC was 0.993 and 0.991 for X-ray and DXA assessments, respectively. The mean difference between bone age assessed by X-ray and DXA was 0.11 years. The limits of agreement ranged from -0.82 to 1.05 years, which means that 95% of all differences between the methods were covered by this range. Results of bone age assessment by DXA scan are similar to those obtained by X-ray. The DXA method seems to be an alternative for assessing bone age in a paediatric hospital-based population.

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

Science.gov (United States)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

Science.gov (United States)

Vogt, Frederick G; Williams, Glenn R

2012-07-01

Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

Fabrication of Ti-Ni-Cu shape memory alloy powders by ball milling method

International Nuclear Information System (INIS)

Kang, S.; Nam, T.

2001-01-01

Ti-Ni and Ti-Ni-Cu shape memory alloy powders have been fabricated by ball milling method, and then alloying behavior and transformation behavior were investigated by means of optical microscopy, electron microscopy, X-ray diffraction and differential scanning calorimetry. As milled Ti-Ni powders fabricated with milling time less than 20 hrs was a mixture of pure elemental Ti and Ni, and therefore it was unable to obtain alloy powders because the combustion reaction between Ti and Ni occurred during heat treatment. Since those fabricated with milling time more than 20 hrs was a mixture of Ti-rich and Ni-rich Ti-Ni solid solution, however, it was possible to obtain alloy powders without the combustion reaction during heat treatment. Clear exothermic and endothermic peaks appeared in the cooling and heating curves, respectively in DSC curves of 20 hrs and 30 hrs milled Ti-Ni powders. On the other hand, in DSC curves of 1 hr, 10 hrs, 50 hrs and 100 hrs, the thermal peaks were almost discernible. The most optimum ball milling time for fabricating Ti-Ni alloy powders was 30 hrs. Ti-40Ni-10Cu(at%) alloy powders were fabricated successfully by ball milling conditions with rotating speed of 100 rpm and milling time of 30 hrs. (author)

X-ray photon-in/photon-out methods for chemical imaging

Energy Technology Data Exchange (ETDEWEB)

Marcus, Matthew A.

2010-03-24

Most interesting materials in nature are heterogeneous, so it is useful to have analytical techniques with spatial resolution sufficient to resolve these heterogeneities.This article presents the basics of X-ray photon-in/photon-out chemical imaging. This family of methods allows one to derive images reflectingthe chemical state of a given element in a complex sample, at micron or deep sub-micron scale. X-ray chemical imaging is relatively non-destructiveand element-selective, and requires minimal sample preparation. The article presents the basic concepts and some considerations of data takingand data analysis, along with some examples.

Comparative study of radiation dose between digital panoramic X-ray unit and general panoramic X-ray unit

International Nuclear Information System (INIS)

Li Qingshan; Duan Tao; Wang Xiaoyun; Zhao Li; Dong Jian; Wei Lei

2010-01-01

Objective: To compare the actual dose of patients who receive the same medical practice by either digital panoramic X-ray unit and general panoramic X-ray unit and give evidence for better selection of oral X-ray examination method. Methods: Round sheet lithium fluoride (LiF) thermoluminescent dosimeters (TLD) were used. The experiment was divided into natural background contrast group, general panoramic X-ray children group, general panoramic X-ray adults group, digital panoramic X-ray children group and digital panoramic X-ray adults group. The dosimeter of natural background radiation was placed at the office of the doctor, the dosimeters of general panoramic X-ray children group and general panoramic X-ray adults group were irradiated by different conditions according to the clinical application of panoramic X-ray to children and adults, the dosimeters of digital panoramic X-ray children group and digital panoramic X-ray adults group were irradiated by different conditions according to the clinical application of digital panoramic X-ray to children and adults. The thermoluminescent dosimeter was used to count and calculate the exposure doses in various groups. Results: The dose of children exposed in general panoramic X-ray unit was 1.28 times of that in digital panoramic X-ray unit, there was significant difference (t=6.904, P<0.01). The dose of adults exposed in general panoramic X-ray unit was 1.55 times of that in the digital panoramic X-ray unit, there also was significant difference (t=-11.514. P< 0.01). Conclusion: The digital panoramic X-ray unit can reduce the dose of patients, so the digital panoramic X-ray unit should be used as far as possible. (authors)

Methods for reduction of scattered x-ray in measuring MTF with the square chart

International Nuclear Information System (INIS)

Hatagawa, Masakatsu; Yoshida, Rie

1982-01-01

A square wave chart has been used to measure the MTF of a screen-film system. The problem is that the scattered X-ray from the chart may give rise to measurement errors. In this paper, the authors proposed two methods to reduce the scattered X-ray: the first method is the use of a Pb mask and second is to provide for an air gap between the chart and the screen-film system. In these methods, the scattered X-ray from the chart was reduced. MTFs were measured by both of the new methods and the conventional method, and MTF values of the new methods were in good agreement while that of the conventional method was not. It was concluded that these new methods are able to reduce errors in the measurement of MTF. (author)

Bone X-Ray (Radiography)

Medline Plus

Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures ...

Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt

Directory of Open Access Journals (Sweden)

Palash Sanphui

2014-03-01

Full Text Available Acemetacin (ACM is a non-steroidal anti-inflammatory drug (NSAID, which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM, isonicotinamide (INA, and picolinamide (PAM], caprolactam (CPR, p-aminobenzoic acid (PABA, and piperazine (PPZ. The structures of an ACM–INA cocrystal and a binary adduct ACM–PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM–PAM and ACM–CPR, and the piperazine salt ACM–PPZ were solved from high-resolution powder X-ray diffraction data. The ACM–INA cocrystal is sustained by the acid...pyridine heterosynthon and N—H...O catemer hydrogen bonds involving the amide group. The acid...amide heterosynthon is present in the ACM–PAM cocrystal, while ACM–CPR contains carboxamide dimers of caprolactam along with acid–carbonyl (ACM hydrogen bonds. The cocrystals ACM–INA, ACM–PAM and ACM–CPR are three-dimensional isostructural. The carboxyl...carboxyl synthon in ACM–PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM–PPZ salt and ACM–nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM–PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable

Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt.

Science.gov (United States)

Sanphui, Palash; Bolla, Geetha; Nangia, Ashwini; Chernyshev, Vladimir

2014-03-01

Acemetacin (ACM) is a non-steroidal anti-inflammatory drug (NSAID), which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM), isonicotinamide (INA), and picolinamide (PAM)], caprolactam (CPR), p-aminobenzoic acid (PABA), and piperazine (PPZ). The structures of an ACM-INA cocrystal and a binary adduct ACM-PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM-PAM and ACM-CPR, and the piperazine salt ACM-PPZ were solved from high-resolution powder X-ray diffraction data. The ACM-INA cocrystal is sustained by the acid⋯pyridine heterosynthon and N-H⋯O catemer hydrogen bonds involving the amide group. The acid⋯amide heterosynthon is present in the ACM-PAM cocrystal, while ACM-CPR contains carboxamide dimers of caprolactam along with acid-carbonyl (ACM) hydrogen bonds. The cocrystals ACM-INA, ACM-PAM and ACM-CPR are three-dimensional isostructural. The carboxyl⋯carboxyl synthon in ACM-PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM-PPZ salt and ACM-nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM-PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable piperazine salt of acemetacin exhibits superior

The reduction methods of operator's radiation dose for portable dental X-ray machines.

Science.gov (United States)

Cho, Jeong-Yeon; Han, Won-Jeong

2012-08-01

This study was aimed to investigate the methods to reduce operator's radiation dose when taking intraoral radiographs with portable dental X-ray machines. Two kinds of portable dental X-ray machines (DX3000, Dexcowin and Rextar, Posdion) were used. Operator's radiation dose was measured with an 1,800 cc ionization chamber (RadCal Corp.) at the hand level of X-ray tubehead and at the operator's chest and waist levels with and without the backscatter shield. The operator's radiation dose at the hand level was measured with and without lead gloves and with long and short cones. The backscatter shield reduced operator's radiation dose at the hand level of X-ray tubehead to 23 - 32%, the lead gloves to 26 - 31%, and long cone to 48 - 52%. And the backscatter shield reduced operator's radiation dose at the operator's chest and waist levels to 0.1 - 37%. When portable dental X-ray systems are used, it is recommended to select X-ray machine attached with a backscatter shield and a long cone and to wear the lead gloves.

Role of X-ray examination methods in the diagnosis of endophytic stomach carcinomas

International Nuclear Information System (INIS)

Gorshkov, A.N.; Akberov, R.F.

1998-01-01

Results of studying potentialities of radiographic methods in the diagnosis of stomach endophytic neoplasms (130 cases) are presented. All of patients were exposed to complex radiographic-endoscopic studies of stomach. X-ray computerized tomography is used as an additional method. It is shown that the complex approach to the diagnosis of endophytic neoplasms of stomach is necessary. Radiographic method is proposed to be used as an initial examination method. Endoscopic method with multiple biopsy is also used. X-ray computerized tomography is used for certain anatomic stomach section at the final stage [ru

X-ray fluorescence imaging with polycapillary X-ray optics

International Nuclear Information System (INIS)

Yonehara, Tasuku; Yamaguchi, Makoto; Tsuji, Kouichi

2010-01-01

X-ray fluorescence spectrometry imaging is a powerful tool to provide information about the chemical composition and elemental distribution of a specimen. X-ray fluorescence spectrometry images were conventionally obtained by using a μ-X-ray fluorescence spectrometry spectrometer, which requires scanning a sample. Faster X-ray fluorescence spectrometry imaging would be achieved by eliminating the process of sample scanning. Thus, we developed an X-ray fluorescence spectrometry imaging instrument without sample scanning by using polycapillary X-ray optics, which had energy filter characteristics caused by the energy dependence of the total reflection phenomenon. In the present paper, we show that two independent straight polycapillary X-ray optics could be used as an energy filter of X-rays for X-ray fluorescence. Only low energy X-rays were detected when the angle between the two optical axes was increased slightly. Energy-selective X-ray fluorescence spectrometry images with projection mode were taken by using an X-ray CCD camera equipped with two polycapillary optics. It was shown that Fe Kα (6.40 keV) and Cu Kα (8.04 keV) could be discriminated for Fe and Cu foils.

La{sub 2-x}Sr{sub x}NiO{sub 4+{delta}} ceramic powders prepared by combustion synthesis

Energy Technology Data Exchange (ETDEWEB)

Colomer, M.T.; Chinarro, E.; Jurado, J.R. [Consejo Nacional de Investigaciones Cientificas, Madrid (Spain). Ist. de Ceramica y Vidrio

2002-07-01

Combustion synthesis provides an attractive method of producing ceramic powders because of its low cost, process simplicity and fastness. Materials based on La{sub 2}NiO{sub 4+{delta}} can be successfully prepared by combustion synthesis. La{sub 2-x}Sr{sub x}NiO{sub 4+{delta}} (x = 0, 0.1) accommodates oxygen excess by oxygen interstitials rather than by the more usual cation vacancies. A high concentration of oxygen interstitials offers the possibility of rapid oxygen transport through the ceramic material and thus provide a new type of mixed ionic-electronic conductor. The fast oxide ion diffusion combined with its thermal stability indicate that these materials would be good candidates for use in ceramic oxygen generators (COGs) and intermediate temperature solid oxide fuel cells (IT-SOFCs). The present work discusses a combustion synthesis technique to prepare La{sub 2-x}Sr{sub x}NiO{sub 4+{delta}} (x = 0, 0.1) powders using the corresponding metal nitrates-urea mixtures, at low temperature and short reaction times. The as-prepared combustion powders were characterized by XRD, DTA-TG, SEM/TEM-EDX and BET. La{sub 2-x}Sr{sub x}NiO{sub 4} (x = 0, 0.1) powders with a good compositional control and homogeneity are attained. The as-prepared powders obtained at 300 C (ignition temperature) showed much higher specific surface area than powders obtained via alternative routes and contained La{sub 2-x}Sr{sub x}NiO{sub 4+{delta}}, as the major phase present, together with La{sub 2}O{sub 3} and a small amount of NiO. La{sub 2-x}Sr{sub x}NiO{sub 4+{delta}} single phase is achieved, respectively at 950 C for x =0.1 and at 975 C for x = 0. (orig.)

Deconvolution of X-ray diffraction profiles using series expansion: a line-broadening study of polycrystalline 9-YSZ

Energy Technology Data Exchange (ETDEWEB)

Sanchez-Bajo, F. [Universidad de Extremadura, Badajoz (Spain). Dept. de Electronica e Ingenieria Electromecanica; Ortiz, A.L.; Cumbrera, F.L. [Universidad de Extremadura, Badajoz (Spain). Dept. de Fisica

2001-07-01

Deconvolution of X-ray diffraction profiles is a fundamental step in obtaining reliable results in the microstructural characterization (crystallite size, lattice microstrain, etc) of polycrystalline materials. In this work we have analyzed a powder sample of 9-YSZ using a technique based on the Fourier series expansion of the pure profile. This procedure, which can be combined with regularization methods, is specially powerful to minimize the effects of the ill-posed nature of the linear integral equation involved in the kinematical theory of X-ray diffraction. Finally, the deconvoluted profiles have been used to obtain microstructural parameters by means of the integral-breadth method. (orig.)

13.1 micrometers hard X-ray focusing by a new type monocapillary X-ray optic designed for common laboratory X-ray source

Science.gov (United States)

Sun, Xuepeng; zhang, Xiaoyun; Zhu, Yu; Wang, Yabing; Shang, Hongzhong; Zhang, Fengshou; Liu, Zhiguo; Sun, Tianxi

2018-04-01

A new type of monocapillary X-ray optic, called 'two bounces monocapillary X-ray optics' (TBMXO), is proposed for generating a small focal spot with high power-density gain for micro X-ray analysis, using a common laboratory X-ray source. TBMXO is consists of two parts: an ellipsoidal part and a tapered part. Before experimental testing, the TBMXO was simulated by the ray tracing method in MATLAB. The simulated results predicted that the proposed TBMXO would produce a smaller focal spot with higher power-density gain than the ellipsoidal monocapillary X-ray optic (EMXO). In the experiment, the TBMXO performance was tested by both an optical device and a Cu target X-ray tube with focal spot of 100 μm. The results indicated that the TBMXO had a slope error of 57.6 μrad and a 13.1 μm focal spot and a 1360 gain in power density were obtained.

Note: Loading method of molecular fluorine using x-ray induced chemistry

International Nuclear Information System (INIS)

Pravica, Michael; Sneed, Daniel; White, Melanie; Wang, Yonggang

2014-01-01

We have successfully loaded molecular fluorine into a diamond anvil cell at high pressure using the synchrotron x-ray induced decomposition of perfluorohexane (C 6 F 14 ). “White” x-ray radiation from the Advanced Photon Source was used to initiate the chemical decomposition of C 6 F 14 , which resulted in the in situ production of F 2 as verified via Raman spectroscopy. Due to the toxic nature of fluorine, this method will offer significant advantages in the ability to easily load a relatively nontoxic and inert substance into a chamber (such as a diamond anvil cell) that, when sealed with other reactants and irradiate with hard x-rays (>7 keV), releases highly reactive and toxic fluorine into the sample/reaction chamber to enable novel chemical synthesis under isolated and/or extreme conditions

X-ray beam size measurements on the Advanced Test Accelerator

International Nuclear Information System (INIS)

Struve, K.W.; Chambers, F.W.; Lauer, E.J.; Slaughter, D.R.

1986-01-01

The electron beam size has been determined on the Advanced Test Accelerator (ATA) by intercepting the beam with a target and measuring the resulting x-ray intensity as a function of time as the target is moved through the beam. Several types of targets have been used. One is a tantalum rod which extends completely across the drift chamber. Another is a tungsten powder filled carbon crucible. Both of these probes are moved from shot to shot so that the x-ray signal intensity varies with probe position. A third is a larger tantalum disk which is inserted on beam axis to allow determining beam size on a one shot basis. The x-ray signals are detected with an MCP photomultiplier tube located at 90 0 to the beamline. It is sufficiently shielded to reject background x-rays and neutrons. The signals were digitized, recorded and later unfolded to produce plots of x-ray intensity versus probe position for several times during the pulse. The presumption that the x-ray intensity is proportional to beam current density is checked computationally. Details of the probe construction and PMT shielding, as well as sample measurements are given

Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data; Funktionale Koordinationspolymere und MOFs aus Reaktionen der Lanthanide und des Bariums mit Azol-Liganden. Synthese und Charakterisierung mit dem Fokus der Strukturbestimmung anhand von Roentgenpulverbeugungsdaten

Energy Technology Data Exchange (ETDEWEB)

Rybak, Jens-Christoph

2012-07-01

��}[BaEu(Im){sub 2}]. Structural characterization of materials from X-ray powder diffraction data is an important aspect of this thesis. A method is presented, which allows, by indexing a diffractogram, intensity extraction and structure solution by charge flipping, to solve the structure of a material, ab initio, from X-ray powder diffraction data exclusively. Moreover it is shown how to refine structures with a high amount of weakly scattering atoms, using rigid body constraints. The structure solutions of {sup 3}{sub ∞}[Ga(Tz){sub 2}], {sup 3}{sub ∞}[Sr(Im){sub 2}]:Ce and {sup 3}{sub ∞}[Yb(Im){sub 3}]ImH from X-ray powder diffraction data are further examples for the successful application of the method presented within this thesis.

Rietveld analysis, powder diffraction and cement

International Nuclear Information System (INIS)

Peterson, V.

2002-01-01

Full text: Phase quantification of cement is essential in its industrial use, however many methods are inaccurate and/or time consuming. Powder diffraction is one of the more accurate techniques used for quantitative phase analysis of cement. There has been an increase in the use of Rietveld refinement and powder diffraction for the analysis and phase quantification of cement and its components in recent years. The complex nature of cement components, existence of solid solutions, polymorphic variation of phases and overlapping phase peaks in diffraction patterns makes phase quantification of cements by powder diffraction difficult. The main phase in cement is alite, a solid solution of tricalcium silicate. Tricalcium silicate has been found to exist in seven modifications in three crystal systems, including triclinic, monoclinic, and rhombohedral structures. Hence, phase quantification of cements using Rietveld methods usually involves the simultaneous modelling of several tricalcium silicate structures to fit the complex alite phase. An industry ordinary Portland cement, industry and standard clinker, and a synthetic tricalcium silicate were characterised using neutron, laboratory x-ray and synchrotron powder diffraction. Diffraction patterns were analysed using full-profile Rietveld refinement. This enabled comparison of x-ray, neutron and synchrotron data for phase quantification of the cement and examination of the tricalcium silicate. Excellent Rietveld fits were achieved, however the results showed that the quantitative phase analysis results differed for some phases in the same clinker sample between various data sources. This presentation will give a short introduction about cement components including polymorphism, followed by the presentation of some problems in phase quantification of cements and the role of Rietveld refinement in solving these problems. Copyright (2002) Australian X-ray Analytical Association Inc

Translate rotate scanning method for X-ray imaging

International Nuclear Information System (INIS)

Eberhard, J.W.; Kwog Cheong Tam.

1990-01-01

Rapid x-ray inspection of objects larger than an x-ray detector array is based on a translate rotate scanning motion of the object related to the fan beam source and detector. The scan for computerized tomography imaging is accomplished by rotating the object through 360 degrees at two or more positions relative to the source and detector array, in moving to another position the object is rotated and the object or source and detector are translated. A partial set of x-ray data is acquired at every position which are combined to obtain a full data set for complete image reconstruction. X-ray data for digital radiography imaging is acquired by scanning the object vertically at a first position at one view angle, rotating and translating the object relative to the source and detector to a second position, scanning vertically, and so on to cover the object field of view, and combining the partial data sets. (author)

Morphological characterization of tungsten trioxide nano powders synthesized by Sol-Gel modified Pechini's method

International Nuclear Information System (INIS)

Ghasemi, Leila; Jafari, Hassan

2017-01-01

Sol-gel modified Pechini's method was used to prepare WO 3 nano powders using dicarboxylic acid and polyethylene glycol as the chelating agent and polymeric source, respectively. WO 3 powders were first prepared by calcination of resin precursor at 550 deg C under various initial concentrations of metal ion (12.5-50 mmol), acid (125-500 mmol), a complexing agent (32-262 mmol), and polyethylene glycol (1-16.5 mmol) in the air atmosphere. The products were characterized using X-ray powder diffraction, field emission scanning electron microscopy, and energy dispersive spectroscopy. The results revealed that the WO 3 nano powders prepared with different amounts of chelating agent and polyethylene glycol, crystallized in monoclinic phase. The nano powders were impurity-free due to the presence of the complexing agent and polyethylene glycol as carbon sources. Morphological evolution indicated that the nano powders evolved from rod-like to regular and spherical shapes, depending on complexing agent and polyethylene glycol amounts. Nano powders with an average particle size of approximately 58 nm and a narrow size distribution were obtained. (author)

Morphological characterization of tungsten trioxide nano powders synthesized by Sol-Gel modified Pechini's method

Energy Technology Data Exchange (ETDEWEB)

Ghasemi, Leila; Jafari, Hassan, E-mail: jafari_h@yahoo.com [Department of Materials Engineering, Faculty of Mechanical Engineering, Shahid Rajaee Teacher Training University, Tehran (Iran, Islamic Republic of)

2017-11-15

Sol-gel modified Pechini's method was used to prepare WO{sub 3} nano powders using dicarboxylic acid and polyethylene glycol as the chelating agent and polymeric source, respectively. WO{sub 3} powders were first prepared by calcination of resin precursor at 550 deg C under various initial concentrations of metal ion (12.5-50 mmol), acid (125-500 mmol), a complexing agent (32-262 mmol), and polyethylene glycol (1-16.5 mmol) in the air atmosphere. The products were characterized using X-ray powder diffraction, field emission scanning electron microscopy, and energy dispersive spectroscopy. The results revealed that the WO{sub 3} nano powders prepared with different amounts of chelating agent and polyethylene glycol, crystallized in monoclinic phase. The nano powders were impurity-free due to the presence of the complexing agent and polyethylene glycol as carbon sources. Morphological evolution indicated that the nano powders evolved from rod-like to regular and spherical shapes, depending on complexing agent and polyethylene glycol amounts. Nano powders with an average particle size of approximately 58 nm and a narrow size distribution were obtained. (author)

Characterization of dense lead lanthanum titanate ceramics prepared from powders synthesized by the oxidant peroxo method

Energy Technology Data Exchange (ETDEWEB)

Pinto, Alexandre H. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, UFSCar-Universidade Federal de Sao Carlos, Rod.Washington Luis km 235, CP 676 Sao Carlos, SP 13565-905 (Brazil); Souza, Flavio L., E-mail: flavio.souza@ufabc.edu.br [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia 166, Bangu, Santo Andre, SP 09210-170 (Brazil); Chiquito, Adenilson J., E-mail: chiquito@df.ufscar.br [Departamento de Fisica, UFSCar-Federal University of Sao Carlos, Rod.Washington Luis km 235, CP 676 Sao Carlos, SP 13565-905 (Brazil); Longo, Elson, E-mail: elson@iq.unesp.br [Instituto de Quimica de Araraquara, UNESP-Universidade Estadual Paulista, Rua Francisco Degni, CP 355 Araraquara, SP 14801-907 (Brazil); Leite, Edson R., E-mail: derl@power.ufscar.br [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, UFSCar-Universidade Federal de Sao Carlos, Rod.Washington Luis km 235, CP 676 Sao Carlos, SP 13565-905 (Brazil); Camargo, Emerson R., E-mail: camargo@ufscar.br [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, UFSCar-Universidade Federal de Sao Carlos, Rod.Washington Luis km 235, CP 676 Sao Carlos, SP 13565-905 (Brazil)

2010-12-01

Nanosized powders of lead lanthanum titanate (Pb{sub 1-x}La{sub x}TiO{sub 3}) were synthesized by means of the oxidant-peroxo method (OPM). Lanthanum was added from 5 to 30% in mol through the dissolution of lanthanum oxide in nitric acid, followed by the addition of lead nitrate to prepare a solution of lead and lanthanum nitrates, which was dripped into an aqueous solution of titanium peroxo complexes, forming a reactive amorphous precipitate that could be crystallized by heat treatment. Crystallized powders were characterized by FT-Raman spectroscopy and X-ray powder diffraction, showing that tetragonal perovskite structure is obtained for samples up to 25% of lanthanum and cubic perovskite for samples with 30% of lanthanum. Powders containing 25 and 30% in mol of lanthanum were calcined at 700 deg. C for 2 h, and in order to determine the relative dielectric permittivity and the phase transition behaviour from ferroelectric-to-paraelectric, ceramic pellets were prepared and sintered at 1100 or 1150 deg. C for 2 h and subjected to electrical characterization. It was possible to observe that sample containing 25% in mol of La presented a normal behaviour for the phase transition, whereas the sample containing 30% in mol of La presented a diffuse phase transition and relaxor behaviour.

Characterization of dense lead lanthanum titanate ceramics prepared from powders synthesized by the oxidant peroxo method

International Nuclear Information System (INIS)

Pinto, Alexandre H.; Souza, Flavio L.; Chiquito, Adenilson J.; Longo, Elson; Leite, Edson R.; Camargo, Emerson R.

2010-01-01

Nanosized powders of lead lanthanum titanate (Pb 1-x La x TiO 3 ) were synthesized by means of the oxidant-peroxo method (OPM). Lanthanum was added from 5 to 30% in mol through the dissolution of lanthanum oxide in nitric acid, followed by the addition of lead nitrate to prepare a solution of lead and lanthanum nitrates, which was dripped into an aqueous solution of titanium peroxo complexes, forming a reactive amorphous precipitate that could be crystallized by heat treatment. Crystallized powders were characterized by FT-Raman spectroscopy and X-ray powder diffraction, showing that tetragonal perovskite structure is obtained for samples up to 25% of lanthanum and cubic perovskite for samples with 30% of lanthanum. Powders containing 25 and 30% in mol of lanthanum were calcined at 700 deg. C for 2 h, and in order to determine the relative dielectric permittivity and the phase transition behaviour from ferroelectric-to-paraelectric, ceramic pellets were prepared and sintered at 1100 or 1150 deg. C for 2 h and subjected to electrical characterization. It was possible to observe that sample containing 25% in mol of La presented a normal behaviour for the phase transition, whereas the sample containing 30% in mol of La presented a diffuse phase transition and relaxor behaviour.

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)

Atom-resolving x-ray holography

International Nuclear Information System (INIS)

Adams, B.; Hiort, T.; Materlik, G.; Nishino, Y.; Novikov, D. V.

2000-01-01

The current state of atomic resolution x-ray holography is discussed on the basis of theory and experimental results. X-ray holography is theoretically described in quantum theory. Presently-used experimental implementations are shown together with the data analysis used. Reconstructions of experimental and simulated holograms are compared for a Cu 3 Au crystal structure. Rigorous experimental realizations of pure direct and reciprocal x-ray holography methods are demonstrated, and future developments and applications of the method are suggested

Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

Science.gov (United States)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

X-ray metrology for ULSI structures

International Nuclear Information System (INIS)

Bowen, D. K.; Matney, K. M.; Wormington, M.

1998-01-01

Non-destructive X-ray metrological methods are discussed for application to both process development and process control of ULSI structures. X-ray methods can (a) detect the unacceptable levels of internal defects generated by RTA processes in large wafers, (b) accurately measure the thickness and roughness of layers between 1 and 1000 nm thick and (c) can monitor parameters such as crystallographic texture and the roughness of buried interfaces. In this paper we review transmission X-ray topography, thin film texture measurement, grazing-incidence X-ray reflectivity and high-resolution X-ray diffraction. We discuss in particular their suitability as on-line sensors for process control

Correction method and software for image distortion and nonuniform response in charge-coupled device-based x-ray detectors utilizing x-ray image intensifier

International Nuclear Information System (INIS)

Ito, Kazuki; Kamikubo, Hironari; Yagi, Naoto; Amemiya, Yoshiyuki

2005-01-01

An on-site method of correcting the image distortion and nonuniform response of a charge-coupled device (CCD)-based X-ray detector was developed using the response of the imaging plate as a reference. The CCD-based X-ray detector consists of a beryllium-windowed X-ray image intensifier (Be-XRII) and a CCD as the image sensor. An image distortion of 29% was improved to less than 1% after the correction. In the correction of nonuniform response due to image distortion, subpixel approximation was performed for the redistribution of pixel values. The optimal number of subpixels was also discussed. In an experiment with polystyrene (PS) latex, it was verified that the correction of both image distortion and nonuniform response worked properly. The correction for the 'contrast reduction' problem was also demonstrated for an isotropic X-ray scattering pattern from the PS latex. (author)

Determination of preferential molecular orientation in porphyrin-fullerene dyad ZnDHD6ee monolayers by the X-ray standing-wave method and X-ray reflectometry

NARCIS (Netherlands)

Seregin, A. Y.; D' Yakova, Y. A.; Yakunin, S. N.; Makhotkin, I. A.; Alekseev, A. S.; Klechkovskaya, V. V.; Tereschenko, E. Y.; Tkachenko, N. V.; Lemmetyinen, H.; Feigin, L. A.; Kovalchuk, M. V.

2013-01-01

Monolayers of porphyrin-fullerene dyad molecules with zinc atoms incorporated into the porphyrin ring (ZnDHD6ee) on the surface of aqueous subphase and on Si substrates have been investigated by the X-ray standing-wave method and X-ray reflectometry. The experiments have been performed under

Room temperature ferromagnetism in Eu-doped ZnO nanoparticulate powders prepared by combustion reaction method

International Nuclear Information System (INIS)

Franco, A.; Pessoni, H.V.S.; Soares, M.P.

2014-01-01

Nanoparticulate powders of Eu-doped ZnO with 1.0, 1.5, 2.0 and 3.0 at% Eu were synthesized by combustion reaction method using zinc nitrate, europium nitrate and urea as fuel without subsequent heat treatments. X-ray diffraction patterns (XRD) of all samples showed broad peaks consistent with the ZnO wurtzite structure. The absence of extra reflections in the diffraction patterns ensures the phase purity, except for x=0.03 that exhibits small reflection corresponding to Eu 2 O 3 phase. The average crystallite size determined from the most prominent (1 0 1) peak of the diffraction using Scherrer's equation was in good agreement with those determined by transmission electron microscopy (TEM); being ∼26 nm. The magnetic properties measurements were performed using a vibrating sample magnetometer (VSM) in magnetic fields up to 2.0 kOe at room temperature. The hysteresis loops, typical of magnetic behaviors, indicating that the presence of an ordered magnetic structure can exist in the Eu-doped ZnO wurtzite structure at room temperature. The room temperature ferromagnetism behavior increases with the Eu 3+ doping concentration. All samples exhibited the same Curie temperature (T C ) around ∼726 K, except for x=0.01; T C ∼643 K. High resolution transmission electron microscopy (HRTEM) images revealed defects/strain in the lattice and grain boundaries of Eu-doped ZnO nanoparticulate powders. The origin of room temperature ferromagnetism in Eu-doped ZnO nanoparticulate powders was discussed in terms of these defects, which increase with the Eu 3+ doping concentration. - Highlights: • Room-temperature ferromagnetism. • Structural and magnetic properties of nanoparticulate powders of Zn 1−x Eu x O. • Combustion reaction method

Compound refractive X-ray lens

International Nuclear Information System (INIS)

Nygren, D.R.; Cahn, R.; Cederstrom, B.; Danielsson, M.; Vestlund, J.

2000-01-01

An apparatus and method are disclosed for focusing X-rays. In one embodiment, his invention is a commercial-grade compound refractive X-ray lens. The commercial-grade compound refractive X-ray lens includes a volume of low-Z material. The volume of low-Z material has a first surface which is adapted to receive X-rays of commercially-applicable power emitted from a commercial-grade X-ray source. The volume of low-Z material also has a second surface from which emerge the X-rays of commercially-applicable power which were received at the first surface. Additionally, the commercial-grade compound refractive X-ray lens includes a plurality of openings which are disposed between the first surface and the second surface. The plurality of openings are oriented such that the X-rays of commercially-applicable power which are received at the first surface, pass through the volume of low-Z material and through the plurality openings. In so doing, the X-rays which emerge from the second surface are refracted to a focal point

Compound refractive X-ray lens

Science.gov (United States)

Nygren, David R.; Cahn, Robert; Cederstrom, Bjorn; Danielsson, Mats; Vestlund, Jonas

2000-01-01

An apparatus and method for focusing X-rays. In one embodiment, his invention is a commercial-grade compound refractive X-ray lens. The commercial-grade compound refractive X-ray lens includes a volume of low-Z material. The volume of low-Z material has a first surface which is adapted to receive X-rays of commercially-applicable power emitted from a commercial-grade X-ray source. The volume of low-Z material also has a second surface from which emerge the X-rays of commercially-applicable power which were received at the first surface. Additionally, the commercial-grade compound refractive X-ray lens includes a plurality of openings which are disposed between the first surface and the second surface. The plurality of openings are oriented such that the X-rays of commercially-applicable power which are received at the first surface, pass through the volume of low-Z material and through the plurality openings. In so doing, the X-rays which emerge from the second surface are refracted to a focal point.

Bone X-Ray (Radiography)

Medline Plus

Full Text Available ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures that those parts of a patient's body not being imaged receive minimal radiation exposure. ...

X-Ray Absorption with Transmission X-Ray Microscopes

NARCIS (Netherlands)

de Groot, F.M.F.

2016-01-01

In this section we focus on the use of transmission X-ray microscopy (TXM) to measure the XAS spectra. In the last decade a range of soft X-ray and hard X-ray TXM microscopes have been developed, allowing the measurement of XAS spectra with 10–100 nm resolution. In the hard X-ray range the TXM

Three-dimensional reciprocal space x-ray coherent scattering tomography of two-dimensional object.

Science.gov (United States)

Zhu, Zheyuan; Pang, Shuo

2018-04-01

X-ray coherent scattering tomography is a powerful tool in discriminating biological tissues and bio-compatible materials. Conventional x-ray scattering tomography framework can only resolve isotropic scattering profile under the assumption that the material is amorphous or in powder form, which is not true especially for biological samples with orientation-dependent structure. Previous tomography schemes based on x-ray coherent scattering failed to preserve the scattering pattern from samples with preferred orientations, or required elaborated data acquisition scheme, which could limit its application in practical settings. Here, we demonstrate a simple imaging modality to preserve the anisotropic scattering signal in three-dimensional reciprocal (momentum transfer) space of a two-dimensional sample layer. By incorporating detector movement along the direction of x-ray beam, combined with a tomographic data acquisition scheme, we match the five dimensions of the measurements with the five dimensions (three in momentum transfer domain, and two in spatial domain) of the object. We employed a collimated pencil beam of a table-top copper-anode x-ray tube, along with a panel detector to investigate the feasibility of our method. We have demonstrated x-ray coherent scattering tomographic imaging at a spatial resolution ~2 mm and momentum transfer resolution 0.01 Å -1 for the rotation-invariant scattering direction. For any arbitrary, non-rotation-invariant direction, the same spatial and momentum transfer resolution can be achieved based on the spatial information from the rotation-invariant direction. The reconstructed scattering profile of each pixel from the experiment is consistent with the x-ray diffraction profile of each material. The three-dimensional scattering pattern recovered from the measurement reveals the partially ordered molecular structure of Teflon wrap in our sample. We extend the applicability of conventional x-ray coherent scattering tomography to

Structural, microstructural and Mössbauer studies of nanocrystalline Fe100-x Alx powders elaborated by mechanical alloying

Directory of Open Access Journals (Sweden)

Akkouche K.

2012-06-01

Full Text Available Nanocrystalline Fe100-xAlx powders (x= 25, 30, 34 and 40 at % were prepared by the mechanical alloying process using a vario-planetary high-energy ball mill for a milling time of 35 h. The formation and physical properties of the alloys were investigated as a function of Al content by means of X-ray diffraction, scanning electron microscopy (SEM, energy dispersive X-ray and Mössbauer spectroscopy. For all Fe100-xAlx samples, the complete formation of bcc phase was observed after 35 h of milling. As Al content increases, the lattice parameter increases, whereas the grain size decreases from 106 to 12 nm. The powder particle morphology for different compositions was observed by SEM. The Mössbauer spectra were adjusted with a singlet line and a sextet containing two components. The singlet was attributed to the formation of paramagnetic A2 disordered structure rich with Al. About the sextet, the first component indicated the formation of Fe clusters/ Fe-rich phases; however, the second component is characteristic of disordered ferromagnetic phase.

X-ray powder diffraction camera for high-field experiments

International Nuclear Information System (INIS)

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

2009-01-01

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

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.)

Radionuclide X-ray fluorescence analysis

International Nuclear Information System (INIS)

Cechak, T.

1994-01-01

The author's achievements in the title field are summarized and discussed. The following topics are dealt with: (i) principles of radionuclide X-ray fluorescence analysis; (ii) mathematical methods in X-ray fluorescence analysis; (iii) Ross differential filters; (iv) application of radionuclide X-ray fluorescence analysis in the coal industry (with emphasis on the determination of the ash content, sulfur content, and arsenic content of coal); and (v) evaluation of the X-ray fluorescence analyzer from the radiological safety point of view. (P.A.)

Interpretation and Utility of the Moments of Small-Angle X-Ray Scattering Distributions.

Science.gov (United States)

Modregger, Peter; Kagias, Matias; Irvine, Sarah C; Brönnimann, Rolf; Jefimovs, Konstantins; Endrizzi, Marco; Olivo, Alessandro

2017-06-30

Small angle x-ray scattering has been proven to be a valuable method for accessing structural information below the spatial resolution limit implied by direct imaging. Here, we theoretically derive the relation that links the subpixel differential phase signal provided by the sample to the moments of scattering distributions accessible by refraction sensitive x-ray imaging techniques. As an important special case we explain the scatter or dark-field contrast in terms of the sample's phase signal. Further, we establish that, for binary phase objects, the nth moment scales with the difference of the refractive index decrement to the power of n. Finally, we experimentally demonstrate the utility of the moments by quantitatively determining the particle sizes of a range of powders with a laboratory-based setup.

A study on the microstructural parameters of Zn {sub (1-x)}La{sub x}Zr{sub x}O nanopowders by X-ray line broadening analysis

Energy Technology Data Exchange (ETDEWEB)

Chenari, Hossein Mahmoudi; Moafi, Hadi Fallah; Rezaee, Omid, E-mail: mahmoudi_hossein@guilan.ac.ir, E-mail: hmahmodiph@yahoo.com [Faculty of Science, University of Guilan, Rasht (Iran, Islamic Republic of)

2016-05-15

In the present study, the pure and La-Zr co-doped ZnO nanoparticles were prepared by sol-gel technique using zinc acetate dehydrate (Zn(Ac){sub 2} ·{sub 2}H{sub 2} O), lanthanum nitrate hexahydrate (La(NO{sub 3}){sub 3} ·6H{sub 2}O) and zirconium chloride (ZrCl{sub 4} ) as precursor. The structure and morphology of the prepared nanoparticle samples were studied using X-ray diffraction and transmission electron microscopy measurements. X-ray diffraction results indicated that all the samples have crystalline wurtzite phase. TEM showed that powder was polycrystalline in nature with random distribution of the pure and La-Zr doped ZnO nanoparticles. We demonstrate strain-size evaluations for pure and doped ZnO nanoparticles from the x-ray line profile analysis. The microstructural effects of crystalline materials in terms of crystallite sizes and lattice strain on the peak broadening were investigated using Williamson-Hall (W-H) analysis and size- strain plot (SSP) method. The average crystallite size of Zn {sub (1-x)}La{sub x} Zr{sub x} O nanoparticles estimated from the W-H analysis and SSP method varied as the doping concentration increased. The incorporation of Zr{sup 4+} ion in the place of Zn{sup {sub 2}{sub +}} caused an increase in the size of nanocrystals as compared to undoped ZnO. The average particle sizes of co-doped ZnO nanoparticles estimated from the USDM model is in good agreement with the TEM results. (author)

Synthesis and X-ray diffraction studies of dysprosium-calcium ferrites Dy1-xCaxFeO3-y (0≤x≤2/3)

International Nuclear Information System (INIS)

Li, J.; Song, D.; Su, Z.; Wang, T.M.

1997-01-01

Samples of dysprosium-calcium ferrites Dy 1-x Ca x FeO 3-y with x ranging from 0 to 2/3 were novelly prepared in air by solid state reaction and characterized by X-ray powder diffraction. These samples are single-phased orthorhombic perovskite-type compounds belonging to the space group D 2h 16 -Pbnm. The lattice constants of the Dy 1-x Ca x FeO 3-y samples have been refined by Cohen's least-squares method. The initial substitution of Ca for Dy leads to a decrease of the lattice constants. Further substitution of Ca for Dy has hardly any influence on the lattice dimensions. (orig.)

Evaluation of undoped ZnS single crystal materials for x-ray imaging applications

Science.gov (United States)

Saleh, Muad; Lynn, Kelvin G.; McCloy, John S.

2017-05-01

ZnS-based materials have a long history of use as x-ray luminescent materials. ZnS was one of the first discovered scintillators and is reported to have one of the highest scintillator efficiencies. The use of ZnS for high energy luminescence has been thus far limited to thin powder screens, such as ZnS:Ag which is used for detecting alpha radiation, due to opacity to its scintillation light, primarily due to scattering. ZnS in bulk form (chemical vapor deposited, powder processed, and single crystal) has high transmission and low scattering compared to powder screens. In this paper, the performance of single crystalline ZnS is evaluated for low energy x-ray (PLE) of several undoped ZnS single crystals is compared to their Radioluminescence (RL) spectra. It was found that the ZnS emission wavelength varies on the excitation source energy.

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

Science.gov (United States)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization

Novel paint design based on nanopowder to protection against X and gamma rays

International Nuclear Information System (INIS)

Movahedi, Mohammad Mehdi; Abdi, Adibe; Mehdizadeh, Alireza; Dehghan, Naser; Heidari, Emad; Masumi, Yusef; Abbaszadeh, Mojtaba

2014-01-01

Lead-based shields are the standard method of intraoperative radiation protection in the radiology and nuclear medicine department. Human lead toxicity is well documented. The lead used is heavy, lacks durability, is difficult to launder, and its disposal is associated with environmental hazards. The aim of this study was to design a lead free paint for protection against X and gamma rays. In this pilot st we evaluated several types of nano metal powder that seemed to have good absorption. The Monte Carlo code, MCNP4C, was used to model the attenuation of X-ray photons in paints with different designs. Experimental measurements were carried out to assess the attenuation properties of each paint design. Among the different nano metal powder, nano tungsten trioxide and nano tin dioxide were the two most appropriate candidates for making paint in diagnostic photon energy range. Nano tungsten trioxide (15%) and nano tin dioxide (85%) provided the best protection in both simulation and experiments. After this step, attempts were made to produce appropriate nano tungsten trioxide-nano tin dioxide paints. The density of this nano tungsten trioxide-nano tin dioxide paint was 4.2 g/cm 3 . The MCNP simulation and experimental measurements for HVL (Half-Value Layer) values of this shield at 100 kVp were 0.25 and 0.23 mm, respectively. The results showed the cost-effective lead-free paint can be a great power in absorbing the X-rays and gamma rays and it can be used instead of lead

Thermal and structural study of guava (Psidium guajava L powders obtained by two dehydration methods

Directory of Open Access Journals (Sweden)

Coralia Osorio

2011-01-01

Full Text Available Two food products (powders were obtained by hot-air drying or lyophilisation methods on the whole guava fruits. The powders were characterised by sensory and thermal analyses (TGA-DSC, infrared spectroscopy (IR, X-ray diffraction (XRD and scanning electron microscopy (SEM. Thermal, morphological and structural characterisations showed a similar behaviour for the two solids. TGA-DSC and IR showed the presence of pectin as the main constituent of solids. A semi-crystalline profile was evidenced by XRD, and lamellar/spherical morphologies were observed by SEM. Sensory analyses revealed an aroma highly related to guava. These value-added food products are an alternative to process guava and avoid loss during postharvest handling.

A novel x-ray circularly polarized ranging method

Science.gov (United States)

Song, Shi-Bin; Xu, Lu-Ping; Zhang, Hua; Gao, Na; Shen, Yang-He

2015-05-01

Range measurement has found multiple applications in deep space missions. With more and further deep space exploration activities happening now and in the future, the requirement for range measurement has risen. In view of the future ranging requirement, a novel x-ray polarized ranging method based on the circular polarization modulation is proposed, termed as x-ray circularly polarized ranging (XCPolR). XCPolR utilizes the circular polarization modulation to process x-ray signals and the ranging information is conveyed by the circular polarization states. As the circular polarization states present good stability in space propagation and x-ray detectors have light weight and low power consumption, XCPolR shows great potential in the long-distance range measurement and provides an option for future deep space ranging. In this paper, we present a detailed illustration of XCPolR. Firstly, the structure of the polarized ranging system is described and the signal models in the ranging process are established mathematically. Then, the main factors that affect the ranging accuracy, including the Doppler effect, the differential demodulation, and the correlation error, are analyzed theoretically. Finally, numerical simulation is carried out to evaluate the performance of XCPolR. Projects supported by the National Natural Science Foundation of China (Grant Nos. 61172138 and 61401340), the Natural Science Basic Research Plan in Shaanxi Province of China (Grant No. 2013JQ8040), the Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20130203120004), the Open Research Fund of the Academy of Satellite Application, China (Grant No. 2014 CXJJ-DH 12), the Xi’an Science and Technology Plan, China (Grant No. CXY1350(4)), the Fundamental Research Funds for the Central Universities, China (Grant Nos. 201413B, 201412B, and JB141303), and the Open Fund of Key Laboratory of Precision Navigation and Timing Technology, National Time Service Center, Chinese

Bone X-Ray (Radiography)

Medline Plus

Full Text Available ... have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures that those parts of a patient's body not being imaged receive minimal radiation exposure. top of page What are the limitations of Bone X-ray (Radiography)? ...

Stellar X-ray sources

International Nuclear Information System (INIS)

Katz, J.I.; Washington Univ., St. Louis, MO

1988-01-01

I Review some of the salient accomplishments of X-rap studies of compact objects. Progress in this field has closely followed the improvement of observational methods, particularly in angular resolution and duration of exposure. Luminous compact X-ray sources are accreting neutron stars or black holes. Accreting neutron stars may have characteristic temporal signatures, but the only way to establish that an X-ray source is a black hole is to measure its mass. A rough phenomenological theory is succesful, but the transport of angular momentum in accretion flows is not onderstood. A number of interesting complications have been observed, including precessing accretion discs, X-ray bursts, and the acceleration of jets in SS433. Many puzzles remain unsolved, including the excitation of disc precession, the nature of the enigmatic A- and gamma-ray source Cyg X-3, the mechanism by which slowly spinning accreting neutron stars lose angular momentum, and the superabundance of X-ray sources in globular clusters. 41 refs.; 5 figs

Easily exchangeable x-ray mirrors and hybrid monochromator modules a study of their performance

Energy Technology Data Exchange (ETDEWEB)

Lin, Fan. [Philips Analytical, Asia Pacific, Toa Payoh, (Singapore); Kogan, V. [Philips Analytical, EA Almelo, (Netherlands); Saito, K. [Philips Analytical, Tokyo, (Japan)

1999-12-01

Full text: PreFix prealigned optical mounts allowing rapid and easily changeover will be presented. The benefits of laterally graded multilayer X-Ray mirrors coupled with these Prefix mounts - conversion of divergent beam to parallel beam, increase of intensity by a factor of 3-7, monochromation to {alpha}1 and {alpha}2 and a dynamic range of 10 {sup 4-5} CpS will be demonstrated in areas such as Thin Film and Powder analysis. Data will be shown on a diffraction profile of thin film (Cr/SiO{sub 2}) with and without a mirror and Si powder with and without a mirror. Further enhancement will be demonstrated by combining a channel cut monochromator-collimator with an X-Ray mirror to produce a high intensity, parallel, pure Cu K{alpha}1 beam with a high intensity of up to 4.5 x 10{sup 8} cps and a divergence down to 0.01 deg. The applicability to various ranging from High Resolution to thin film/reflectivity to Rietveld structural refinement and to phase analysis will be shown. The Rocking curve of HEMT 10nm InGaAs on InP will be presented using various `standard` optics and hybrid optics, also Si powder and a Rietveld refinement of CuS0{sub 4}.5H{sub 2}0 and Aspirin. A comparison of the benefits and application of X-Ray Mirrors and Hybrid Mirror/Monochromators will be given. The data presented will show that by using X-Ray Mirrors and Hybrid modules the performance of standard `Laboratory` Diffractometers can be greatly enhanced to a level previously unachievable with great practical benefits. Copyright (1999) Australian X-ray Analytical Association Inc.

Structure, morphology and optical properties of undoped and MN-doped ZnO{sub (1−x)}S{sub x} nano-powders prepared by precipitation method

Energy Technology Data Exchange (ETDEWEB)

Dejene, F.B., E-mail: dejenebf@qwa.ufs.ac.za [Department of Physics, University of the Free State, (Qwa-Qwa campus), Private Bag X-13, Phuthaditjhaba 9866 (South Africa); Onani, M.O. [Chemistry Department, University of the Western Cape, Private Bag x17, Bellville 7535 (South Africa); Koao, L.F.; Wako, A.H.; Motloung, S.V.; Yihunie, M.T. [Department of Physics, University of the Free State, (Qwa-Qwa campus), Private Bag X-13, Phuthaditjhaba 9866 (South Africa)

2016-01-01

The undoped and Mn-doped ZnO{sub (1−x)}S{sub x} nano-powders were successfully synthesized by precipitation method without using any capping agent. Its structure, morphology, elemental analysis, optical and luminescence properties were determined by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), UV–vis spectroscopy (UV) and photoluminescence spectroscopy (PL). A typical SEM image of the un-doped ZnO{sub (1−x)}S{sub x} nanoparticles exhibit flake like structures that changes to nearly spherical particles with Mn-doping. The XRD of undoped and Mn doped ZnO{sub (1−x)}S{sub x} pattern reveals the formation of a product indexed to the hexagonal wurtzite phase of ZnS. The nanopowders have crystallite sizes estimated from XRD measurements were in the range of 10–20 nm. All the samples showed absorption maximum of ZnO{sub (1−x)}S{sub x} at 271 nm and high transmittance in UV and visible region, respectively. The undoped ZnO{sub (1−x)}S{sub x} nanoparticles show strong room-temperature photoluminescence with four emission bands centering at 338 nm, 384 nm, 448 nm and 705 nm that may originate to the impurity of ZnO{sub (1−x)}S{sub x}, existence of oxide related defects. The calculated bandgap of the nanocrystalline ZnO{sub (1−x)}S{sub x} showed a blue-shift with respect to the Mn-doping. The PL spectra of the Mn-doped samples exhibit a strong orange emission at around 594 nm attributed to the {sup 4}T{sub 1}–{sup 6}A{sub 1} transition of the Mn{sup 2+} ions.

Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

Science.gov (United States)

Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

2012-04-01

A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

International Nuclear Information System (INIS)

Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D.M.; Conway, Barbara R.; Timmins, Peter

2007-01-01

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2 NC(CH 3 ) 3- n (CH 2 OH) n , with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family (n=0, 1, 2), but significantly contrasting structural properties for the member with n=3. - Graphical abstract: Structural properties of a family of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine are discussed and rationalized

Application of physical and chemical characterization techniques to metallic powders

International Nuclear Information System (INIS)

Slotwinski, J. A.; Watson, S. S.; Stutzman, P. E.; Ferraris, C. F.; Peltz, M. A.; Garboczi, E. J.

2014-01-01

Systematic studies have been carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to chemistry, including X-ray diffraction and energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, were also employed. Results of these analyses will be used to shed light on the question: how does virgin powder change after being exposed to and recycled from one or more additive manufacturing build cycles? In addition, these findings can give insight into the actual additive manufacturing process

Method of evaluation of structural (screen) and quantum graininess of X-ray pictures

Energy Technology Data Exchange (ETDEWEB)

Gurvich, A M; Shamanov, A A; Erofeeva, N D [Nauchno-Issledovatel' skij Inst. Rentgenologii i Radiologii, Moscow (USSR)

1979-03-01

Proposed is a method for quantitative determination of graininess of X-ray pictures (gamma-ray images), the graininess being conditioned by the structure of amplifying screens and quantum fluctuations. The method is based on the determination of threshold brightness at which the picture graininess becomes obvious. It is shown that at low effective quantum energy (Esub(eff.) <= 50 keV) the graininess observed is for the most part structural (screen). Its growth is connected with quantum fluctuations when increasing Esub(eff.) up to 150 keV and using screens with high output values of X-ray luminescence and the coefficient of spectral accordance to the film.

Inspection method of optical fiber preforms by x-ray absorption measurements

International Nuclear Information System (INIS)

Takahashi, H.; Nakamura, K.; Shibuya, S.; Kuroha, T.

1980-01-01

A method for measuring the refractive index distribution of optical fiber preforms has been developed by application of the theory of X-ray radiography. The composition of quartz optical fiber materials is, in most cases, limited to the group of five elements - Ge, P, Si, O and B. Of them, Ge is an essential element to determine the structure of refractive index of an optical fiber and the distribution of its density can be regarded approximately as the distribution of refractive index. On the other hand, the coefficient of low-energy X-ray absorption by the elements depends markedly on their atomic numbers, and Ge has a far larger absorption coefficient than the other four elements. Therefore, analysis of the intensity of X-ray absorbed by optical fiber preforms makes it possible to determine the distribution of Ge density and consequently the distribution of refractive index. (author)

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-04-15

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

X-ray fluorescence in geology

International Nuclear Information System (INIS)

Dutra, C.V.; Gomes, C.B.

1990-01-01

This work is about the X-ray fluorescence aplication in geology. It's showing the X-ray origin and excitation. About the instrumentation this work shows the following: X-ray tubes, colimators, analysers crystals, detectors, amplifiers, pulse height selector, and others electronic components. By X-ray fluorescente are done quantitative and qualitative geological analysis and this work shows this analysis and its detection limits. The problems determination is the example. In this work was done yet the comparative analysis of the various instrumental methods in geochemistry. (C.G.) [pt

Nanoparticle-Assisted Scanning Focusing X-Ray Therapy with Needle Beam X Rays.

Science.gov (United States)

Davidson, R Andrew; Guo, Ting

2016-01-01

In this work, we show a new therapeutic approach using 40-120 keV X rays to deliver a radiation dose at the isocenter located many centimeters below the skin surface several hundred times greater than at the skin and how this dose enhancement can be augmented with nanomaterials to create several thousand-fold total dose enhancement effect. This novel approach employs a needle X-ray beam directed at the isocenter centimeters deep in the body while continuously scanning the beam to cover a large solid angle without overlapping at the skin. A Monte Carlo method was developed to simulate an X-ray dose delivered to the isocenter filled with X-ray absorbing and catalytic nanoparticles in a water phantom. An experimental apparatus consisting of a moving plastic phantom irradiated with a stationary 1 mm needle X-ray beam was built to test the theoretical predictions. X-ray films were used to characterize the dose profiles of the scanning X-ray apparatus. Through this work, it was determined that the X-ray dose delivered to the isocenter in a treatment voxel (t-voxel) underneath a 5 cm deep high-density polyethylene (HDPE) phantom was 295 ± 48 times greater than the surface dose. This measured value was in good agreement with the theoretical predicted value of 339-fold. Adding X-ray-absorbing nanoparticles, catalytic nanoparticles or both into the t-voxel can further augment the dose enhancement. For example, we predicted that adding 1 weight percentage (wp) of gold into water could increase the effective dose delivered to the target by onefold. Dose enhancement using 1 mm X-ray beam could reach about 1,600-fold in the t-voxel when 7.5 wp of 88 nm diameter silica-covered gold nanoparticles were added, which we showed in a previously published study can create a dose enhancement of 5.5 ± 0.46-fold without scanning focusing enhancement. Based on the experimental data from that study, mixing 0.02 wp 2.5 nm diameter small tetrakis hydroxymethyl phosphonium chloride (THPC

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

Energy Technology Data Exchange (ETDEWEB)

Freyer, Benjamin

2013-05-02

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

Application of delayed X-ray spectrometry to the analysis of some rare earth elements

International Nuclear Information System (INIS)

Pillay, A.E.; Mboweni, R.C.M.

1991-01-01

The capabilities of delayed x-ray spectrometry preceded by isotope-source thermal neutron activation for the specific determination of some rare earth elements (Sm, Eu, Dy, Ho) in small powdered samples was evaluated. The feasibility study relied heavily on the low-energy sensitivity of the detector used. Detection of the delayed x-rays was achieved with a 100-mm 2 Ge detector with the ability to produce optimum photopeak-to-noise ratios. The rare earth elements were chosen on the basis of their inherent favourable nuclear properties for producing a practicable x-ray yield and on the demand for their analysis. Analytical results are presented over a range of concentrations for the elements of interest and the potential of the technique for application to their general routine analysis is discussed. Interferences from the sample matrix can be suppressed to an extent that makes the method almost independent of the matrix. This and other features make the technique a strong rival to conventional activation analysis. (author)

Synthesis of nanostructured LiTi2(PO4)3 powder by a Pechini-type polymerizable complex method

International Nuclear Information System (INIS)

Mariappan, C.R.; Galven, C.; Crosnier-Lopez, M.-P.; Le Berre, F.; Bohnke, O.

2006-01-01

The nanostructured NASICON-type LiTi 2 (PO 4 ) 3 (LTP) material has been synthesized by Pechini-type polymerizable complex method. The use of water-soluble ammonium citratoperoxotitanate (IV) metal complex instead of alkoxides as precursor allows to prepare monophase material. Thermal analyses have been carried out on the powder precursor to check the weight loss and synthesis temperature. X-ray powder diffraction analysis (XRD) has been performed on the LTP powder obtained after heating the powder precursor over a temperature range from 550 to 1050 deg. C for 2 h. By varying the molar ratio of citric acid to metal ion (CA/Ti) and citric acid to ethylene glycol (CA/EG), the grain size of the LTP powder could be modified. The formation of small and well-crystalline grains, in the order of 50-125 nm in size, has been determined from the XRD patterns and confirmed by transmission electron microscopy

X-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Attekum, P.M.T.M. van.

1979-01-01

The methods and results of X-ray photoelectron spectroscopy in the study of plasmons, alloys and gold compounds are discussed. After a comprehensive introduction, seven papers by the author, previously published elsewhere, are reprinted and these cover a wide range of the uses of X-ray photoelectron spectroscopy. (W.D.L.)

Traditional x-ray imaging

International Nuclear Information System (INIS)

Hay, G.A.

1982-01-01

Methods of imaging x-rays, with particular reference to medicine, are reviewed. The history and nature of x-rays, their production and spectra, contrast, shapes and fine structure, image transducers, including fluorescent screens, radiography, fluoroscopy, and image intensifiers, image detection, perception and enhancement and clinical applications are considered. (U.K.)

Powder diffraction from a continuous microjet of submicrometer protein crystals.

Science.gov (United States)

Shapiro, D A; Chapman, H N; Deponte, D; Doak, R B; Fromme, P; Hembree, G; Hunter, M; Marchesini, S; Schmidt, K; Spence, J; Starodub, D; Weierstall, U

2008-11-01

Atomic-resolution structures from small proteins have recently been determined from high-quality powder diffraction patterns using a combination of stereochemical restraints and Rietveld refinement [Von Dreele (2007), J. Appl. Cryst. 40, 133-143; Margiolaki et al. (2007), J. Am. Chem. Soc. 129, 11865-11871]. While powder diffraction data have been obtained from batch samples of small crystal-suspensions, which are exposed to X-rays for long periods of time and undergo significant radiation damage, the proof-of-concept that protein powder diffraction data from nanocrystals of a membrane protein can be obtained using a continuous microjet is shown. This flow-focusing aerojet has been developed to deliver a solution of hydrated protein nanocrystals to an X-ray beam for diffraction analysis. This method requires neither the crushing of larger polycrystalline samples nor any techniques to avoid radiation damage such as cryocooling. Apparatus to record protein powder diffraction in this manner has been commissioned, and in this paper the first powder diffraction patterns from a membrane protein, photosystem I, with crystallite sizes of less than 500 nm are presented. These preliminary patterns show the lowest-order reflections, which agree quantitatively with theoretical calculations of the powder profile. The results also serve to test our aerojet injector system, with future application to femtosecond diffraction in free-electron X-ray laser schemes, and for serial crystallography using a single-file beam of aligned hydrated molecules.

X-ray astronomy

International Nuclear Information System (INIS)

Giacconi, R.; Gursky, H.

1974-01-01

This text contains ten chapters and three appendices. Following an introduction, chapters two through five deal with observational techniques, mechanisms for the production of x rays in a cosmic setting, the x-ray sky and solar x-ray emission. Chapters six through ten include compact x-ray sources, supernova remnants, the interstellar medium, extragalactic x-ray sources and the cosmic x-ray background. Interactions of x rays with matter, units and conversion factors and a catalog of x-ray sources comprise the three appendices. (U.S.)

Study of a new X-ray protective apron with composite protective sheet

International Nuclear Information System (INIS)

Kanzaki, Ryuji; Ohtsuka, Akiyoshi; Okayama, Akio

1997-01-01

Lead powder and oxygenated lead are widely used as materials in conventional protective aprons. However, the use of lead alone limits weight reduction in an apron. Because the amount of lead can not be decreased without reducing X-ray absorption rate. In this study, we report the efficiency of a new X-ray protective apron with a composite protective sheet. The X-ray absorption rate of the composite sheet was 4.5 percent less than that of the lead sheet. However, the effective protective efficiency of the composite sheet was the same as that of the lead sheet. The uniformity of the new X-ray protective apron was good, and the differences among products were small. The new X-ray protective apron was about 30 percent lighter than a lead apron with a 0.25 mm lead equivalent. The new lighter aprons are more comfortable for the radiology staff. Therefore, the use of a composite protective apron provides the advantages of weight reduction and increased comfort without reducing X-ray absorption rate. (author)

VPD residue search by monitoring scattered x-rays

International Nuclear Information System (INIS)

Mori, Y.; Yamagami, M.; Yamada, T.

2000-01-01

Recently, VPD-TXRF has come into wide use for semiconductor analysis. In VPD-TXRF technique, adjusting the mechanical measuring point to the center of dried residue is of importance for accurate determination. Until now, the following searching methods have been used: monitoring light scattering under bright illumination, using laser scattering particle mapper, applying internal standard as a marker. However, each method has individual disadvantage. For example, interference of Kβ line (ex. Sc-Kβ to Ti-Kα) occurs in the internal standard method. We propose a new searching method 'scattered x-ray search' which utilizes x-ray scattering form the dried residue as a marker. Since the line profile of x-ray scattering agrees with that of fluorescent x-rays, scattered x-ray can be used as an alternative marker instead of internal standard. According to our experimental results, this search method shows the same accuracy as internal standard method. The merits are as follows: 1) no need to add internal standard, 2) rapid search because of high intensity of scattered x-rays, 3) searching software for internal standard can be applied without any modification. In this method, diffraction of incident x-rays by substrate causes irregular change over the detected scattering x-rays. Therefore, this method works better under x-y controlled stage than r-Θ one. (author)

High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

NARCIS (Netherlands)

Groot, F.M.F. de

2000-01-01

In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption

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)

A novel synthesis of polymeric CO via useful hard X-ray photochemistry

Directory of Open Access Journals (Sweden)

Michael Pravica

2016-12-01

Full Text Available We report on the synchrotron hard X-ray-induced decomposition of strontium oxalate (SrC2O4 pressurized to 7 GPa inside a diamond anvil cell (DAC. After some 4 h of irradiation in a white X-ray synchrotron beam, a dark reddish/brown region formed in the area of irradiation which was surrounded by a yellowish brown remainder in the rest of the sample. Upon depressurization of the sample to ambient conditions, the reacted/decomposed sample was recoverable as a dark brown/red and yellow waxy solid. Synchrotron infrared spectroscopy confirmed the strong presence of CO2 even under ambient conditions with the sample exposed to air and other strongly absorbing regions, suggesting that the sample may likely be polymerized CO (in part with dispersed CO2 and SrO trapped within the polymer. These results will have significant implications in the ability to readily produce and trap CO2 in situ via irradiation of a simple powder for useful hard X-ray photochemistry and in the ability to easily manufacture polymeric CO (via loading of powders in a DAC or high volume press without the need for the dangerous and complex loading of toxic CO. A novel means of X-ray-induced polymerization under extreme conditions has also been demonstrated.

Development of X-ray and ion diagnostic methods for plasma focus research

International Nuclear Information System (INIS)

Sadowski, M.

1986-12-01

A review of experimental methods used for investigation of X-rays and ion-beams emmited from plasma focus facilities is presented. The research program has been realized at the Institute for Nuclear Studies in Swierk and at the Institut fuer Plasmaforschung in Stuttgart, within the frames of an international co-operation. The studies on ion emission from different PF facilities are reviewed. The application of CN-films with Al-filters and of different ion-pinhole cameras is described. The use of a Thomson mass-spectrometer adopted for plasma studies is presented. The time-resolved measurements combined with a simultaneous mass- and energy-analysis of the ion beams are also described. The most important results of these studies are summarized. Particular attention is also paid to the studies of the X-ray emission. The use of stereoscopic sets of vacuum pinhole cameras with thin Be-filters is described. The application of X-ray pinhole cameras equipped with miniature scintillators for time-resolved measurements is also presented. The most important results of the X-ray emission studies are summarized. 35 refs., 12 figs. (author)

A NEW METHOD TO QUANTIFY X-RAY SUBSTRUCTURES IN CLUSTERS OF GALAXIES

Energy Technology Data Exchange (ETDEWEB)

Andrade-Santos, Felipe; Lima Neto, Gastao B.; Lagana, Tatiana F. [Departamento de Astronomia, Instituto de Astronomia, Geofisica e Ciencias Atmosfericas, Universidade de Sao Paulo, Geofisica e Ciencias Atmosfericas, Rua do Matao 1226, Cidade Universitaria, 05508-090 Sao Paulo, SP (Brazil)

2012-02-20

We present a new method to quantify substructures in clusters of galaxies, based on the analysis of the intensity of structures. This analysis is done in a residual image that is the result of the subtraction of a surface brightness model, obtained by fitting a two-dimensional analytical model ({beta}-model or Sersic profile) with elliptical symmetry, from the X-ray image. Our method is applied to 34 clusters observed by the Chandra Space Telescope that are in the redshift range z in [0.02, 0.2] and have a signal-to-noise ratio (S/N) greater than 100. We present the calibration of the method and the relations between the substructure level with physical quantities, such as the mass, X-ray luminosity, temperature, and cluster redshift. We use our method to separate the clusters in two sub-samples of high- and low-substructure levels. We conclude, using Monte Carlo simulations, that the method recuperates very well the true amount of substructure for small angular core radii clusters (with respect to the whole image size) and good S/N observations. We find no evidence of correlation between the substructure level and physical properties of the clusters such as gas temperature, X-ray luminosity, and redshift; however, analysis suggest a trend between the substructure level and cluster mass. The scaling relations for the two sub-samples (high- and low-substructure level clusters) are different (they present an offset, i.e., given a fixed mass or temperature, low-substructure clusters tend to be more X-ray luminous), which is an important result for cosmological tests using the mass-luminosity relation to obtain the cluster mass function, since they rely on the assumption that clusters do not present different scaling relations according to their dynamical state.

Synthesis of ceramic powder of TiO_2 doped with Zr by the Pechini Method applied in ceramic membranes for water treatment

International Nuclear Information System (INIS)

Farias, R.F.V.; Fernandes, M.S.M.; Silva, R.S.; Franca, K.B.; Lira, H.L.; Bonifacio, M.A.R.

2016-01-01

This paper describes the synthesis of ceramic powder of TiO2 doped with Zr by the polymeric precursor method, also known as Pechini method applied in ceramic membranes for water treatment. Three compositions were synthesized according to the molar ratio Ti_x-1Zr_xO_2 (x = 0.25, 0.50 and 0.75 moles), calcined at 700° C/1h. The samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and microbiological analysis. The presence of the doping element was not decisive in the average size of crystallite, which ranged from 5.5 to 11.3 nm. The SEM images showed clusters with uniform surface and granular aspect, it is still possible to see a clearly porous structure formed by clusters of uniform size for all samples. The microbiological analyses of powders have revealed that they have bactericidal properties. (author)

Standard test methods for chemical analysis of ceramic whiteware materials using wavelength dispersive X-Ray fluorescence spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition. Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1). 1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the...

Hard-x-ray phase-difference microscopy with a low-brilliance laboratory x-ray source

International Nuclear Information System (INIS)

Kuwabara, Hiroaki; Yashiro, Wataru; Harasse, Sebastien; Momose, Atsushi; Mizutani, Haruo

2011-01-01

We have developed a hard-X-ray phase-imaging microscopy method using a low-brilliance X-ray source. The microscope consists of a sample, a Fresnel zone plate, a transmission grating, and a source grating creating an array of mutually incoherent X-ray sources. The microscope generates an image exhibiting twin features of the sample with opposite signs separated by a distance, which is processed to generate a phase image. The method is quantitative even for non-weak-phase objects that are difficult to be quantitatively examined by the widely used Zernike phase-contrast microscopy, and it has potentially broad applications in the material and biological science fields. (author)

Flash X-ray

International Nuclear Information System (INIS)

Sato, Eiichi

2003-01-01

Generation of quasi-monochromatic X-ray by production of weakly ionized line plasma (flash X-ray), high-speed imaging by the X-ray and high-contrast imaging by the characteristic X-ray absorption are described. The equipment for the X-ray is consisted from the high-voltage power supply and condenser, turbo molecular pump, and plasma X-ray tube. The tube has a long linear anticathode to produce the line plasma and flash X-ray at 20 kA current at maximum. X-ray spectrum is measured by the imaging plate equipped in the computed radiography system after diffracted by a LiF single crystal bender. Cu anticathode generates sharp peaks of K X-ray series. The tissue images are presented for vertebra, rabbit ear and heart, and dog heart by X-ray fluoroscopy with Ce anticathode. Generation of K-orbit characteristic X-ray with extremely low bremsstrahung is to be attempted for medical use. (N.I.)

Ultrashort X-ray pulse science

Energy Technology Data Exchange (ETDEWEB)

Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

1998-05-01

A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90° Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ~ 300 fs, 30 keV (0.4 Å) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been demonstrated as a

Ultrashort X-ray pulse science

International Nuclear Information System (INIS)

Chin, A.H.; Lawrence Berkeley National Lab., CA

1998-01-01

A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90 o Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ∼ 300 fs, 30 keV (0.4 (angstrom)) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been

Evaluation of gamma prime volume fractions and lattice misfits in a nickel base superalloy using the external standard X-ray diffraction method

Energy Technology Data Exchange (ETDEWEB)

Tiley, J., E-mail: jaimie.tiley@wpafb.af.mil [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Viswanathan, G.B. [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Hwang, J.Y. [Materials Engineering Department, University of North Texas, Denton, TX (United States); Shiveley, A. [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Banerjee, R. [Materials Engineering Department, University of North Texas, Denton, TX (United States)

2010-11-25

The unconstrained lattice parameters and volume fractions of {gamma}' for a low misfit nickel based superalloy were evaluated using X-ray diffraction techniques. Extraction techniques were used to provide unconstrained {gamma}' powders for both water quenched and slow cooled samples that were aged at 760 deg. C for 0, 25, 50, 100, and 200 h. The external standard method was used to determine the volume fraction for the unaged water quenched sample and the slow cooled sample aged for 200 h. These two extremes in processing conditions provided an increase in the total volume fraction of {gamma}'.

X-ray imaging with monochromatic synchrotron radiation. Fluorescent and phase-contrast method

Energy Technology Data Exchange (ETDEWEB)

Takeda, Tohoru; Itai, Yuji [Tsukuba Univ., Ibaraki (Japan). Inst. of Clinical Medicine

2002-05-01

To obtain the high sensitive x-ray images of biomedical object, new x-ray imaging techniques using fluorescent x-ray and phase-contrast x-ray are being developed in Japan. Fluorescent x-ray CT can detect very small amounts of specific elements in the order of ppm at one pixel, whereas phase-contrast x-ray imaging with interferometer can detect minute differences of biological object. Here, our recent experimental results are presented. (author)

Charged particle induced delayed X-rays (DEX) for the analysis of intermediate and heavy elements

Science.gov (United States)

Pillay, A. E.; Erasmus, C. S.; Andeweg, A. H.; Sellschop, J. P. F.; Annegarn, H. J.; Dunn, J.

1988-12-01

The emission of K X-rays from proton-rich and metastable radionuclides, following proton activation of the stable isotopes of the elements of interest, has not been widely used as a means of analysis. The thrust of this paper proposes a nuclear technique using delayed X-rays for the analysis of low concentrations of intermediate and heavy elements. The method is similar to the delayed gamma-ray technique. Proton bombardment induces mainly (p, n) reactions whereas the delayed X-rays originate largely from e --capture and isomeric transition. Samples of rare earth and platinum group elements (PGE), in the form of compacted powders, were irradiated with an 11 MeV proton beam and delayed X-rays detected with a 100 mm 2 Ge detector. Single element spectra for a range of rare earths and PGEs are presented. Analytical conditions are demonstrated for Pd in the range 0.1-5%. Spectra from actual geological samples of a PGE ore, preconcentrated by fire-assay, and monazite are presented. All six platinum group elements are visible and interference-free in a single spectrum, a marked advance on other nuclear techniques for these elements, including PIXE and neutron activation analysis (NAA).

A convenient method for X-ray analysis in TEM that measures mass thickness and composition

Science.gov (United States)

Statham, P.; Sagar, J.; Holland, J.; Pinard, P.; Lozano-Perez, S.

2018-01-01

We consider a new approach for quantitative analysis in transmission electron microscopy (TEM) that offers the same convenience as single-standard quantitative analysis in scanning electron microscopy (SEM). Instead of a bulk standard, a thin film with known mass thickness is used as a reference. The procedure involves recording an X-ray spectrum from the reference film for each session of acquisitions on real specimens. There is no need to measure the beam current; the current only needs to be stable for the duration of the session. A new reference standard with a large (1 mm x 1 mm) area of uniform thickness of 100 nm silicon nitride is used to reveal regions of X-ray detector occlusion that would give misleading results for any X-ray method that measures thickness. Unlike previous methods, the new X-ray method does not require an accurate beam current monitor but delivers equivalent accuracy in mass thickness measurement. Quantitative compositional results are also automatically corrected for specimen self-absorption. The new method is tested using a wedge specimen of Inconel 600 that is used to calibrate the high angle angular dark field (HAADF) signal to provide a thickness reference and results are compared with electron energy-loss spectrometry (EELS) measurements. For the new X-ray method, element composition results are consistent with the expected composition for the alloy and the mass thickness measurement is shown to provide an accurate alternative to EELS for thickness determination in TEM without the uncertainty associated with mean free path estimates.

Optics for coherent X-ray applications

Energy Technology Data Exchange (ETDEWEB)

Yabashi, Makina, E-mail: yabashi@spring8.or.jp [RIKEN SPring-8 Center, Kouto 1-1-1, Sayo, Hyogo 679-5148 (Japan); Tono, Kensuke [Japan Synchrotron Radiation Research Institute (JASRI), Kouto 1-1-1, Sayo, Hyogo 679-5198 (Japan); Mimura, Hidekazu [The University of Tokyo, Hongo 7-3-1, Bunkyo-ku, Tokyo 113-8656 (Japan); Matsuyama, Satoshi; Yamauchi, Kazuto [Osaka University, 2-1 Yamada-oka, Suita, Osaka 565-0871 (Japan); Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji [RIKEN SPring-8 Center, Kouto 1-1-1, Sayo, Hyogo 679-5148 (Japan); Ohashi, Haruhiko; Goto, Shunji [Japan Synchrotron Radiation Research Institute (JASRI), Kouto 1-1-1, Sayo, Hyogo 679-5198 (Japan); Ishikawa, Tetsuya [RIKEN SPring-8 Center, Kouto 1-1-1, Sayo, Hyogo 679-5148 (Japan)

2014-08-27

Developments of optics for coherent X-ray applications and their role in diffraction-limited storage rings are described. Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

Integration of the ATHENA mirror modules: development of indirect and x-ray direct AIT methods

Science.gov (United States)

Vernani, Dervis; Blum, Steffen; Seure, Thibault; Bavdaz, Marcos; Wille, Eric; Schaeffer, Uwe; Lièvre, Nicolas; Nazeeruddin, Adeeb; Barrière, Nicolas M.; Collon, Maximilien J.; Cibik, Levent; Krumrey, Michael; Müller, Peter; Burwitz, Vadim

2017-08-01

Within the ATHENA optics technology plan, activities are on-going for demonstrating the feasibility of the mirror module Assembly Integration and Testing (AIT). Each mirror module has to be accurately attached to the mirror structure by means of three isostatic mounts ensuring minimal distortion under environmental loads. This work reports on the status of one of the two parallel activities initiated by ESA to address this demanding task. In this study awarded to the industrial consortium, the integration relies on opto-mechanical metrology and direct X-ray alignment. For the first or "indirect" method the X-ray alignment results are accurately referenced, by means of a laser tracking system, to optical fiducial targets mounted on the mirror modules and finally linked to the mirror structure coordinate system. With the second or "direct" method the alignment is monitored in the X-ray domain, providing figures of merit directly comparable to the final performance. The integration being designed and here presented, foresees combining the indirect method to the X-ray direct method. The characterization of the single mirror modules is planned at PTB's X-ray Parallel Beam Facility (XPBF 2.0) at BESSY II, and the integration and testing campaign at Panter. It is foreseen to integrate and test a demonstrator with two real mirror modules manufactured by cosine.

Development and exploitation of the slit method for the characterization of x-ray screen-film combinations

International Nuclear Information System (INIS)

Hoeschen, D.

1987-01-01

For the determination of the modulation transfer function (MTF) of screen-film combinations which are used in medical x-ray diagnostics a measuring method has been developed: the screen-film combination is exposed to x-rays behind a thin slit and the modulation transfer function is calculated from the resulting rather broad slit images on the film. After solving many technical and photographic problems, the slit method provides high precision in the MTF determination. The only objection against this method is the necessary high dose variation which has to be provided by the x-ray machine

Correction factors for the NMi free-air ionization chamber for medium-energy x-rays calculated with the Monte Carlo method

International Nuclear Information System (INIS)

Grimbergen, T.W.M.; Dijk, E. van; Vries, W. de

1998-01-01

A new method is described for the determination of x-ray quality dependent correction factors for free-air ionization chambers. The method is based on weighting correction factors for mono-energetic photons, which are calculated using the Monte Carlo method, with measured air kerma spectra. With this method, correction factors for electron loss, scatter inside the chamber and transmission through the diaphragm and front wall have been calculated for the NMi free-air chamber for medium-energy x-rays for a wide range of x-ray qualities in use at NMi. The newly obtained correction factors were compared with the values in use at present, which are based on interpolation of experimental data for a specific set of x-ray qualities. For x-ray qualities which are similar to this specific set, the agreement between the correction factors determined with the new method and those based on the experimental data is better than 0.1%, except for heavily filtered x-rays generated at 250 kV. For x-ray qualities dissimilar to the specific set, differences up to 0.4% exist, which can be explained by uncertainties in the interpolation procedure of the experimental data. Since the new method does not depend on experimental data for a specific set of x-ray qualities, the new method allows for a more flexible use of the free-air chamber as a primary standard for air kerma for any x-ray quality in the medium-energy x-ray range. (author)

X-ray photoelectron spectroscopy study on Ba1-xEuxTiO3

International Nuclear Information System (INIS)

Lu, D.-Y.; Sugano, Mikio; Sun Xiuyun; Su Wenhui

2005-01-01

X-ray photoelectron spectroscopy is employed to study inner-shell core-level binding energies Eu 4d, Ti 2p and O 1s, Ba 3d for new single-phase Ba 1-x Eu x TiO 3 (0.1 ≤ x ≤ 0.4) samples prepared by solid state reaction at 4.0 GPa and 1090 deg. C. The peak positions of binding energies determined by linear background subtraction and Gaussian fit are presented. XPS analysis indicates that the mixed-valent Eu 3+ /Eu 2+ ions at A-site and Ti 4+ /Ti 3+ ions at B-site coexisted in the Ba 1-x Eu x TiO 3 powder surface, and the amount of Eu 2+ ions is equal to Eu 3+ ions

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

International Nuclear Information System (INIS)

Czuba, J.; Dziedzic, A.

1978-01-01

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

X-Ray

Science.gov (United States)

... enema. What you can expect During the X-ray X-rays are performed at doctors' offices, dentists' offices, ... as those using a contrast medium. Your child's X-ray Restraints or other techniques may be used to ...

Nuclear Enhanced X-ray Maximum Entropy Method Used to Analyze Local Distortions in Simple Structures

DEFF Research Database (Denmark)

Christensen, Sebastian; Bindzus, Niels; Christensen, Mogens

We introduce a novel method for reconstructing pseudo nuclear density distributions (NDDs): Nuclear Enhanced X-ray Maximum Entropy Method (NEXMEM). NEXMEM offers an alternative route to experimental NDDs, exploiting the superior quality of synchrotron X-ray data compared to neutron data. The method...... proposed to result from anharmonic phonon scattering or from local fluctuating dipoles on the Pb site.[1,2] No macroscopic symmetry change are associated with these effects, rendering them invisible to conventional crystallographic techniques. For this reason PbX was until recently believed to adopt...

Introducing a standard method for experimental determination of the solvent response in laser pump, x-ray probe time-resolved wide-angle x-ray scattering experiments on systems in solution

DEFF Research Database (Denmark)

Kjær, Kasper Skov; Brandt van Driel, Tim; Kehres, Jan

2013-01-01

In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order...... response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We...... is demonstrated to exhibit first order behaviour with respect to the amount of energy deposited in the solution. We introduce a standardized method for recording solvent responses in laser pump, X-ray probe time-resolved X-ray wide-angle scattering experiments by using dye mediated solvent heating. Furthermore...

Computerized method for X-ray angular distribution simulation in radiological systems

International Nuclear Information System (INIS)

Marques, Marcio A.; Oliveira, Henrique J.Q. de; Frere, Annie F.; Schiabel, Homero; Marques, Paulo M.A.

1996-01-01

A method to simulate the changes in X-ray angular distribution (the Heel effect) for radiologic imaging systems is presented. This simulation method is described as to predict images for any exposure technique considering that the distribution is the cause of the intensity variation along the radiation field

Advances in data reduction of high-pressure x-ray powder diffraction data from two-dimensional detectors: a case study of schafarzikite (FeSb{sub 2}O{sub 4})

Energy Technology Data Exchange (ETDEWEB)

Hinrichsen, B [Max-Planck-Institute for Solid State Research, Heisenbergstrasse 1, D-70569 Stuttgart (Germany); Dinnebier, R E [Max-Planck-Institute for Solid State Research, Heisenbergstrasse 1, D-70569 Stuttgart (Germany); Rajiv, P [Max-Planck-Institute for Solid State Research, Heisenbergstrasse 1, D-70569 Stuttgart (Germany); Hanfland, M [European Synchrotron Radiation Facility, 6 rue Jules Horowitz, BP220, 38043 Grenoble Cedex (France); Grzechnik, A [Departamento de Fisica de la Materia Condensada, Facultad de Ciencia y Technologia, Universidad del Pais Vasco, Apartado 644, E-48080 Bilbao (Spain); Jansen, M [Max-Planck-Institute for Solid State Research, Heisenbergstrasse 1, D-70569 Stuttgart (Germany)

2006-06-28

Methods have been developed to facilitate the data analysis of multiple two-dimensional powder diffraction images. These include, among others, automatic detection and calibration of Debye-Scherrer ellipses using pattern recognition techniques, and signal filtering employing established statistical procedures like fractile statistics. All algorithms are implemented in the freely available program package Powder3D developed for the evaluation and graphical presentation of large powder diffraction data sets. As a case study, we report the pressure dependence of the crystal structure of iron antimony oxide FeSb{sub 2}O{sub 4} (p{<=}21 GPa, T = 298 K) using high-resolution angle dispersive x-ray powder diffraction. FeSb{sub 2}O{sub 4} shows two phase transitions in the measured pressure range. The crystal structures of all modifications consist of frameworks of Fe{sup 2+}O{sub 6} octahedra and irregular Sb{sup 3+}O{sub 4} polyhedra. At ambient conditions, FeSb{sub 2}O{sub 4} crystallizes in space group P4{sub 2}/mbc (phase I). Between p = 3.2 GPa and 4.1 GPa it exhibits a displacive second order phase transition to a structure of space group P 2{sub 1}/c (phase II, a = 5.7792(4) A, b = 8.3134(9) A, c = 8.4545(11) A, {beta} = 91.879(10){sup 0}, at p = 4.2 GPa). A second phase transition occurs between p = 6.4 GPa and 7.4 GPa to a structure of space group P4{sub 2}/m (phase III, a = 7.8498(4) A, c = 5.7452(5) A, at p = 10.5 GPa). A nonlinear compression behaviour over the entire pressure range is observed, which can be described by three Vinet equations in the ranges from p = 0.52 GPa to p 3.12 GPa, p = 4.2 GPa to p = 6.3 GPa and from p = 7.5 GPa to p = 19.8 GPa. The extrapolated bulk moduli of the high-pressure phases were determined to K{sub 0} = 49(2) GPa for phase I, K{sub 0} = 27(3) GPa for phase II and K{sub 0} = 45(2) GPa for phase III. The crystal structures of all phases are refined against x-ray powder data measured at several pressures between p = 0.52 GPa

A practical material decomposition method for x-ray dual spectral computed tomography.

Science.gov (United States)

Hu, Jingjing; Zhao, Xing

2016-03-17

X-ray dual spectral CT (DSCT) scans the measured object with two different x-ray spectra, and the acquired rawdata can be used to perform the material decomposition of the object. Direct calibration methods allow a faster material decomposition for DSCT and can be separated in two groups: image-based and rawdata-based. The image-based method is an approximative method, and beam hardening artifacts remain in the resulting material-selective images. The rawdata-based method generally obtains better image quality than the image-based method, but this method requires geometrically consistent rawdata. However, today's clinical dual energy CT scanners usually measure different rays for different energy spectra and acquire geometrically inconsistent rawdata sets, and thus cannot meet the requirement. This paper proposes a practical material decomposition method to perform rawdata-based material decomposition in the case of inconsistent measurement. This method first yields the desired consistent rawdata sets from the measured inconsistent rawdata sets, and then employs rawdata-based technique to perform material decomposition and reconstruct material-selective images. The proposed method was evaluated by use of simulated FORBILD thorax phantom rawdata and dental CT rawdata, and simulation results indicate that this method can produce highly quantitative DSCT images in the case of inconsistent DSCT measurements.