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Sample records for powder diffraction analysis

  1. 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.)

  2. 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

  3. 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.

  4. 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

  5. Development of materials science by Ab initio powder diffraction analysis

    International Nuclear Information System (INIS)

    Fujii, Kotaro

    2015-01-01

    Crystal structure is most important information to understand properties and behavior of target materials. Technique to analyze unknown crystal structures from powder diffraction data (ab initio powder diffraction analysis) enables us to reveal crystal structures of target materials even we cannot obtain a single crystal. In the present article, three examples are introduced to show the power of this technique in the field of materials sciences. The first example is dehydration/hydration of the pharmaceutically relevant material erythrocycin A. In this example, crystal structures of two anhydrous phases were determined from synchrotron X-ray powder diffraction data and their different dehydration/hydration properties were understood from the crystal structures. In the second example, a crystal structure of a three dimensional metal-organic-framework prepared by a mechanochemical reaction was determined from laboratory X-ray powder diffraction data and the reaction scheme has been revealed. In the third example, a crystal structure of a novel oxide-ion conductor of a new structure family was determined from synchrotron X-ray and neutron powder diffraction data which gave an important information to understand the mechanism of the oxide-ion conduction. (author)

  6. Frequency analysis for modulation-enhanced powder diffraction.

    Science.gov (United States)

    Chernyshov, Dmitry; Dyadkin, Vadim; van Beek, Wouter; Urakawa, Atsushi

    2016-07-01

    Periodic modulation of external conditions on a crystalline sample with a consequent analysis of periodic diffraction response has been recently proposed as a tool to enhance experimental sensitivity for minor structural changes. Here the intensity distributions for both a linear and nonlinear structural response induced by a symmetric and periodic stimulus are analysed. The analysis is further extended for powder diffraction when an external perturbation changes not only the intensity of Bragg lines but also their positions. The derived results should serve as a basis for a quantitative modelling of modulation-enhanced diffraction data measured in real conditions.

  7. Profile analysis of neutron powder diffraction data at ISIS

    International Nuclear Information System (INIS)

    David, W.I.F.; Ibberson, R.M.; Matthewman, J.C.

    1992-05-01

    The aim of this manual is to document the current suite of time-of-flight neutron powder diffraction profile refinement programs available to ISIS users. Aspects of data collation and normalisation specific to the individual diffraction instruments are dealt with elsewhere. It will be assumed the user has produced a suitable data file (.DAT file) containing the profile data consisting of point by point values of the corrected diffraction profile across the pattern. The analysis of neutron powder diffraction data at ISIS by profile refinement utilises a suite of ''in-house'' written and supported programs based on the Cambridge Crystallography Subroutine Library (CCSL). A quick scan through the CCSL manual will give the user a general feel for the procedure to adopt in the use of the library and hence of the profile codes. The instructions documented in this handbook are complementary to those in the more specialist CCSL manual, and consequently go into no great detail regarding technical details of any of the CCSL routines. The programs may be run from each individual user account, for example [USER01], once the appropriate login procedure has been set-up by the instrument scientists. The programs are mostly activated by one line commands and only a basic knowledge of a VAX editor should be required; details can be found in the ''VAX primer'' available from Computer Support. (Author)

  8. Diffraction. Powder, amorphous, liquid

    International Nuclear Information System (INIS)

    Sosnowska, I.M.

    1999-01-01

    Neutron powder diffraction is a unique tool to observe all possible diffraction effects appearing in crystal. High-resolution neutron diffractometers have to be used in this study. Analysis of the magnetic structure of polycrystalline materials requires the use of high-resolution neutron diffraction in the range of large interplanar distances. As distinguished from the double axis diffractometers (DAS), which show high resolution only at small interplanar distances, TOF (time-of-flight) diffractometry offers the best resolution at large interplanar distances. (K.A.)

  9. Qualitative analysis of powder x-ray diffraction data

    International Nuclear Information System (INIS)

    Raftery, T.

    1999-01-01

    Full text: The main task of qualitative analysis is the determination of the presence of major, minor and if practical trace phases in a sample. The attainment of this goal is dependent on the quality of alignment (line position and intensity) as well as quality of sample preparation. Identification is generally on the basis of structure and dependent on the use of reference patterns. There are inherent limitations to the use of reference patterns including lack of reference patterns for the phase of interest (rare), solid solutions or substitutions (likely) and poor quality of reference patterns (unusual). With multiphase samples, there are the added problems of line overlap or interference, determining minor or trace phases in the presence of major phases, the decrease of intensity with concentration and influence of mass absorption on intensities. Within multiphase samples there may be many phases, some of which are in low abundance. It is sometimes possible (and usually desirable) to fractionate the sample by some physical or chemical method (while attempting not to create new phases as a result). It is usually important and often critical to have available supplementary information about the sample - either chemical or physical, or a history of preparation or formation. A central issue is what constitutes a match. A match is an adequate accounting of the distribution of intensity in the diffraction pattern. The match can be thought of in terms of a sum of δ2θ (or δd/d) and/or δI/I ref , and the consistency with known information. The calculated measures give rise to the figures of merit (FOM) of search match programs. It must always be remembered that two compounds of the same space group and similar cell parameters (eg. FCC metals) are going to have very similar diffraction patterns - any search/match technique usually arrives at a stage where there is a list of possibilities that must be decided between. The range search-match techniques span manual

  10. ZDS - a computer program for analysis of X-ray powder diffraction patterns

    International Nuclear Information System (INIS)

    Ondrus, P.

    1993-01-01

    The ZDS system creates an integrated environment of procedures for complete and precise analysis of raw powder diffraction patterns. The basis of the ZDS system is a graphic control centre for easy and user-friendly application of all included procedures. It offers a number of application procedures without an interaction with any data base. The program operates either in an automatic or manual mode. The manual mode makes possible specialized applications. The input and output of the data are compatible with Philips and Siemens powder diffraction software. The ZDS system runs with Intel 80286 or 80386-based PC computers with or without math-coprocesor. (orig.)

  11. Incident spectrum determination for time-of-flight neutron powder diffraction data analysis

    International Nuclear Information System (INIS)

    Hodges, J. P.

    1998-01-01

    Accurate characterization of the incident neutron spectrum is an important requirement for precise Rietveld analysis of time-of-flight powder neutron diffraction data. Without an accurate incident spectrum the calculated model for the measured relative intensities of individual Bragg reflections will possess systematic errors. We describe a method for obtaining an accurate numerical incident spectrum using data from a transmitted beam monitor

  12. 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

  13. Neutron Powder Diffraction in Sweden

    International Nuclear Information System (INIS)

    Tellgren, R.

    1986-01-01

    Neutron powder diffraction in Sweden has developed around the research reactor R2 in Studsvik. The article describes this facility and presents a historical review of research results obtained. It also gives some ideas of plans for future development

  14. Hybrid Powder - Single Crystal X-Ray Diffraction Instrument for Planetary Mineralogical Analysis of Unprepared Samples, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop a planetary exploration XRD/XRF instrument based on a hybrid diffraction approach that complements powder XRD analysis, similar to that of the...

  15. A standardless method of quantitative ceramic analysis using X-ray powder diffraction

    International Nuclear Information System (INIS)

    Mazumdar, S.

    1999-01-01

    A new procedure using X-ray powder diffraction data for quantitative estimation of the crystalline as well as the amorphous phase in ceramics is described. Classification of the crystalline and amorphous X-ray scattering was achieved by comparison of the slopes at two successive points of the powder pattern at scattering angles at which the crystalline and amorphous phases superimpose. If the second slope exceeds the first by a stipulated value, the intensity is taken as crystalline; otherwise the scattering is considered as amorphous. Crystalline phase analysis is obtained by linear programming techniques using the concept that each observed X-ray diffraction peak has contributions from n component phases, the proportionate analysis of which is required. The method does not require the measurement of calibration data for use as an internal standard, but knowledge of the approximate crystal structure of each phase of interest in the mixture is necessary. The technique is also helpful in qualitative analysis because each suspected phase is characterized by the probability that it will be present when a reflection zone is considered in which the suspected crystalline phase could contribute. The amorphous phases are determined prior to the crystalline ones. The method is applied to ceramic materials and some results are presented. (orig.)

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

    International Nuclear Information System (INIS)

    Suminar Pratapa; Budi Hartono

    2009-01-01

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

  17. Structure analysis of K3H(SO4)2 by neutron powder diffraction

    International Nuclear Information System (INIS)

    Murakami, Satoshi; Kuroiwa, Yoshihiro; Noda, Yukio; Nakai, Yusuke; Kamiyama, Takashi; Asano, Hajime.

    1993-01-01

    Neutron powder diffraction experiments of K 3 H(SO 4 ) 2 were carried out at KENS-HRP station in order to obtain the positional parameters of hydrogen nuclei. The data was taken at six different temperatures from room temperature to 20K. Even though K 3 H(SO 4 ) 2 contained a hydrogen atom, the structural analysis was successfully performed by using a program RIETAN. Concerning the hydrogen position, four different models give almost the same R-factor so that the state of the hydrogen nucleus is not uniquely determined. The result based on the assumption that a hydrogen nucleus occupies two sites shows that the distance of split hydrogen nuclei is shorter than the distance of hydrogen electron clouds. This result suggests that a large polarizability exists in a hydrogen atom. (author)

  18. 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…

  19. 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.)

  20. Powder Neutron Diffraction and Magnetic structures

    International Nuclear Information System (INIS)

    Vigneron, F.

    1986-01-01

    The determination of the magnetic structures of materials (ferromagnetic, antiferromagnetic, helimagnetic, .) can be achieved only by neutron diffraction. A general survey of the powder technique is given: 2-axis spectrometer and analysis of the magnetic data. For the REBe/sb13/ intermetallic compounds (RE = Rare Earth), commensurate and/or incommensurate magnetic structures are observed and discussed as a function of RE (Gd, Tb, Dy, Ho, Er)

  1. The IPNS rietveld analysis software package for TOF [time-of-flight] powder diffraction data: Recent developments

    International Nuclear Information System (INIS)

    Rotella, F.J.; Richardson, J.W. Jr.

    1987-01-01

    A system of FORTRAN programs for the analysis of time-of-flight (TOF) neutron powder diffraction data via the Rietveld method at IPNS has been modified recently, making it possible to analyze data that exhibit diffraction maxima broadened due to anisotropic strain and that can be modeled by individual atomic anharmonic thermal vibrations. The observation of noncrystalline scattering in data from some powder samples has led to the development of software to fit such scattering by a function related to a radial distribution function through Fourier-filtering techniques. The ''user friendliness'' of the IPNS Rietveld package has been enhanced by the development of ''RIETVELD,'' a menu-based VAX/VMS command language routine for interactive file manipulation and program execution

  2. 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.

  3. 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.

  4. 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.)

  5. 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.)

  6. High Resolution Powder Diffraction and Structure Determination

    International Nuclear Information System (INIS)

    Cox, D. E.

    1999-01-01

    It is clear that high-resolution synchrotrons X-ray powder diffraction is a very powerful and convenient tool for material characterization and structure determination. Most investigations to date have been carried out under ambient conditions and have focused on structure solution and refinement. The application of high-resolution techniques to increasingly complex structures will certainly represent an important part of future studies, and it has been seen how ab initio solution of structures with perhaps 100 atoms in the asymmetric unit is within the realms of possibility. However, the ease with which temperature-dependence measurements can be made combined with improvements in the technology of position-sensitive detectors will undoubtedly stimulate precise in situ structural studies of phase transitions and related phenomena. One challenge in this area will be to develop high-resolution techniques for ultra-high pressure investigations in diamond anvil cells. This will require highly focused beams and very precise collimation in front of the cell down to dimensions of 50 (micro)m or less. Anomalous scattering offers many interesting possibilities as well. As a means of enhancing scattering contrast it has applications not only to the determination of cation distribution in mixed systems such as the superconducting oxides discussed in Section 9.5.3, but also to the location of specific cations in partially occupied sites, such as the extra-framework positions in zeolites, for example. Another possible application is to provide phasing information for ab initio structure solution. Finally, the precise determination of f as a function of energy through an absorption edge can provide useful information about cation oxidation states, particularly in conjunction with XANES data. In contrast to many experiments at a synchrotron facility, powder diffraction is a relatively simple and user-friendly technique, and most of the procedures and software for data analysis

  7. Shock diffraction in alumina powder

    International Nuclear Information System (INIS)

    Venz, G.; Killen, P.D.; Page, N.W.

    1996-01-01

    In order to produce complex shaped components by dynamic compaction of ceramic powders detailed knowledge of their response under shock loading conditions is required. This work attempts to provide data on release effects and shock attenuation in 1 μm and 5 μm α-alumina powders which were compacted to between 85 % and 95 % of the solid phase density by the impact of high velocity steel projectiles. As in previous work, the powder was loaded into large cylindrical dies with horizontal marker layers of a contrasting coloured powder to provide a record of powder displacement in the recovered specimens. After recovery and infiltration with a thermosetting resin the specimens were sectioned and polished to reveal the structure formed by the passage of the projectile and shock wave. Results indicate that the shock pressures generated were of the order of 0.5 to 1.4 GPa and higher, with shock velocities and sound speeds in the ranges 650 to 800 m/s and 350 to 400 m/s respectively

  8. High resolution Neutron and Synchrotron Powder Diffraction

    International Nuclear Information System (INIS)

    Hewat, A.W.

    1986-01-01

    The use of high-resolution powder diffraction has grown rapidly in the past years, with the development of Rietveld (1967) methods of data analysis and new high-resolution diffractometers and multidetectors. The number of publications in this area has increased from a handful per year until 1973 to 150 per year in 1984, with a ten-year total of over 1000. These papers cover a wide area of solid state-chemistry, physics and materials science, and have been grouped under 20 subject headings, ranging from catalysts to zeolites, and from battery electrode materials to pre-stressed superconducting wires. In 1985 two new high-resolution diffractometers are being commissioned, one at the SNS laboratory near Oxford, and one at the ILL in Grenoble. In different ways these machines represent perhaps the ultimate that can be achieved with neutrons and will permit refinement of complex structures with about 250 parameters and unit cell volumes of about 2500 Angstrom/sp3/. The new European Synchotron Facility will complement the Grenoble neutron diffractometers, and extend the role of high-resolution powder diffraction to the direct solution of crystal structures, pioneered in Sweden

  9. A structural investigation into the compaction behavior of pharmaceutical composites using powder X-ray diffraction and total scattering analysis.

    Science.gov (United States)

    Moore, Michael D; Steinbach, Alison M; Buckner, Ira S; Wildfong, Peter L D

    2009-11-01

    To use advanced powder X-ray diffraction (PXRD) to characterize the structure of anhydrous theophylline following compaction, alone, and as part of a binary mixture with either alpha-lactose monohydrate or microcrystalline cellulose. Compacts formed from (1) pure theophylline and (2) each type of binary mixture were analyzed intact using PXRD. A novel mathematical technique was used to accurately separate multi-component diffraction patterns. The pair distribution function (PDF) of isolated theophylline diffraction data was employed to assess structural differences induced by consolidation and evaluated by principal components analysis (PCA). Changes induced in PXRD patterns by increasing compaction pressure were amplified by the PDF. Simulated data suggest PDF dampening is attributable to molecular deviations from average crystalline position. Samples compacted at different pressures were identified and differentiated using PCA. Samples compacted at common pressures exhibited similar inter-atomic correlations, where excipient concentration factored in the analyses involving lactose. Practical real-space structural analysis of PXRD data by PDF was accomplished for intact, compacted crystalline drug with and without excipient. PCA was used to compare multiple PDFs and successfully differentiated pattern changes consistent with compaction-induced disordering of theophylline as a single component and in the presence of another material.

  10. Uniting Electron Crystallography and Powder Diffraction

    CERN Document Server

    Shankland, Kenneth; Meshi, Louisa; Avilov, Anatoly; David, William

    2012-01-01

    The polycrystalline and nanocrystalline states play an increasingly important role in exploiting the properties of materials, encompassing applications as diverse as pharmaceuticals, catalysts, solar cells and energy storage. A knowledge of the three-dimensional atomic and molecular structure of materials is essential for understanding and controlling their properties, yet traditional single-crystal X-ray diffraction methods lose their power when only polycrystalline and nanocrystalline samples are available. It is here that powder diffraction and single-crystal electron diffraction techniques take over, substantially extending the range of applicability of the crystallographic principles of structure determination.  This volume, a collection of teaching contributions presented at the Crystallographic Course in Erice in 2011, clearly describes the fundamentals and the state-of-the-art of powder diffraction and electron diffraction methods in materials characterisation, encompassing a diverse range of discipl...

  11. The peak in neutron powder diffraction

    International Nuclear Information System (INIS)

    Laar, B. van; Yelon, W.B.

    1984-01-01

    For the application of Rietveld profile analysis to neutron powder diffraction data a precise knowledge of the peak profile, in both shape and position, is required. The method now in use employs a Gaussian shaped profile with a semi-empirical asymmetry correction for low-angle peaks. The integrated intensity is taken to be proportional to the classical Lorentz factor calculated for the X-ray case. In this paper an exact expression is given for the peak profile based upon the geometrical dimensions of the diffractometer. It is shown that the asymmetry of observed peaks is well reproduced by this expression. The angular displacement of the experimental profile with respect to the nominal Bragg angle value is larger than expected. Values for the correction to the classical Lorentz factor for the integrated intensity are given. The exact peak profile expression has been incorporated into a Rietveld profile analysis refinement program. (Auth.)

  12. 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.

  13. Advances in powder diffraction crystallography

    International Nuclear Information System (INIS)

    Magneli, A.

    1986-01-01

    This is the first conference to be arranged within the framework of an agreement on scientific exchange and co-operation between l Academie des Sciences de l Institut de France and the Royal Swedish Academy of Sciences. The responsibility for the scientific program of the conference has been shared between members of the two Academies. The contributions include glimpses of the historical background and broad reviews of the present status of development and of recent work in powder crystallography. Reports are given on a number of studies, basic as well as applied in character, currently conducted in the two countries in a large variety of fields. Prospects of further developments in the area are also presented

  14. 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)

  15. Accurate Charge Densities from Powder Diffraction

    DEFF Research Database (Denmark)

    Bindzus, Niels; Wahlberg, Nanna; Becker, Jacob

    Synchrotron powder X-ray diffraction has in recent years advanced to a level, where it has become realistic to probe extremely subtle electronic features. Compared to single-crystal diffraction, it may be superior for simple, high-symmetry crystals owing to negligible extinction effects and minimal...... peak overlap. Additionally, it offers the opportunity for collecting data on a single scale. For charge densities studies, the critical task is to recover accurate and bias-free structure factors from the diffraction pattern. This is the focal point of the present study, scrutinizing the performance...

  16. Neutron Powder Diffraction and Constrained Refinement

    DEFF Research Database (Denmark)

    Pawley, G. S.; Mackenzie, Gordon A.; Dietrich, O. W.

    1977-01-01

    The first use of a new program, EDINP, is reported. This program allows the constrained refinement of molecules in a crystal structure with neutron diffraction powder data. The structures of p-C6F4Br2 and p-C6F4I2 are determined by packing considerations and then refined with EDINP. Refinement is...

  17. 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].

  18. Pulsed Neutron Powder Diffraction for Materials Science

    Science.gov (United States)

    Kamiyama, T.

    2008-03-01

    structure materials with the highest resolution of Δd/d = 0.2% (corresponding to 10˜5 to 10˜6 strain precision). The typical gauge volume will be 1 mm3. JED has transmission radiography detectors to support stress mapping. Software group is planning so that basic software to cover data acquisition and data treatment should be common. Since 1 Gbyte data are typically obtained for single experiment in an instrument, the basic software is quite important. International TV conference between ISIS, IPNS, SNS has been held every month to exchange information on each development. KEK developed manyo-lib to help basic analysis. Analysis software development including powder diffraction is strongly related with the activity of the software group. However, users of IPD will be from various field of science and their background is different. It should cover wide topics and help both beginners and well-trained users. We have started with neutron intensity database, peak-search software, peak-match software, pattern simulation, whole pattern fitting, PDF and RDF analysis, and now start coding Rietveld software.

  19. Time-resolved Neutron Powder Diffraction

    International Nuclear Information System (INIS)

    Pannetier, J.

    1986-01-01

    The use of a high-flux neutron source together with a large position sensitive detector (PSD) allows a powder diffraction pattern to be recorded at a time-scale of a few minutes so that crystalline systems under non-equilibrium conditions may now conveniently be investigated. This introduces a new dimension into powder diffraction (the time and transient phenomena like heterogeneous chemical reactions can now be easily studied. The instrumental parameters relevant for the design of such time-dependent experiments are briefly surveyed and the current limits of the method are discussed. The applications are illustrated by two kinds of experiment in the field of inorganic solid state chemistry: true kinetic studies of heterogeneous chemical reactions and thermodiffractometry experiments

  20. Rietveld profile analysis of calcined AlPO/sub 4/-11 using pulsed neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Richardson, J.W. Jr.; Pluth, J.J.; Smith, J.V.

    1988-08-01

    Aluminium phosphate, AlPO/sub 4/, M/sub r/=121.95, orthorhombic, Icmm (disordered Al, P), Icm2 (ordered Al, P), a=13.5333(8), b=18.4845(10), c=8.3703(4) A, V=2094 A/sup 3/, Z=20, D/sub x/=1.93 g cm/sup -3/, T approx. = 295 K, R/sub wp/=0.031, R/sub F//sup 2/=0.109 (Icmm) and R/sub wp/=0.027, R/sub F//sup 2/=0.058 (Icm2) for 1017 independent reflections. Sample calcined at 873 K and dehydrated at 573 K. Time-of-flight neutron powder diffraction data were taken on the GPPD diffractometer at the Argonne National Laboratory Intense Pulsed Neutron Source. The structure was refined by Rietveld profile analysis in the range d=0.86-3.91 A in two space groups: Icmm assuming no ordering of Al and P, and Icm2 assuming strict alternation of Al and P on tetrahedral nodes. (orig./BHo).

  1. 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

  2. Operation manual for EDXRDDA - a software package for Bragg peak analysis of energy dispersive powder X-ray diffraction data

    International Nuclear Information System (INIS)

    Jayaswal, Balhans; Vijaykumar, V.; Momin, S.N.; Sikka, S.K.

    1992-01-01

    EDXRDDA is a software package for analysis of raw data for energy dispersive x-ray diffraction from powder samples. It resolves the spectra into individual peaks by a constrained non-linear least squares method (Hughes and Sexton, 1988). The profile function adopted is the Gaussian/Lorentzian product with the mixing ratio refinable in the program. The program is implemented on an IBM PC and is highly interactive with extensive plotting facilities. This report is a user's guide for running the program. In the first step after inputting the spectra, the full spectra is plotted on the screen. The user then chooses a portion of this for peak resolution. The initial guess for the peak intensity, peak position are input with the help of a cursor or a mouse. Upto twenty peaks can be fitted at a time in an interval of 500 channels. For overlapping peaks, various constraints can be applied. Bragg peaks and fluorescence peaks with different half widths can be handled simultaneously. The program on execution produces a look up table which contains the refined values of the peak position, half width, peak intensity, integrated intensity, and their error estimates of each peak. The program is very general and can also be used for curve fitting of data from many other experiments. (author). 2 refs., 7 figs., 2 appendices

  3. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, Norihiro [Meikai Univ., Sakado, Saitama (Japan). School of Dentistry

    2000-07-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), ({beta}-calcium pyrophosphate) and ({beta}-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 {theta}) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, {beta}-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of {beta}-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no {beta}-TCP could be detected in the 12-week-old samples, indicating that the amount of {beta}-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, {beta}-CPP, and {beta}-TCP. Further, DCPD and {beta}-CPP samples shared

  4. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    International Nuclear Information System (INIS)

    Tamura, Norihiro

    2000-01-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), (β-calcium pyrophosphate) and (β-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 θ) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, β-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of β-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no β-TCP could be detected in the 12-week-old samples, indicating that the amount of β-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, β-CPP, and β-TCP. Further, DCPD and β-CPP samples shared the same diffraction pattern, and OCP

  5. Synchrotron powder diffraction on Aztec blue pigments

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez del Rio, M. [European Synchrotron Radiation Facility, B.P. 220, Grenoble Cedex (France); Gutierrez-Leon, A.; Castro, G.R.; Rubio-Zuazo, J. [Spanish CRG Beamline at the European Synchrotron Radiation Facility, SpLine, B.P. 220, Grenoble Cedex (France); Solis, C. [Universidad Nacional Autonoma de Mexico, Instituto de Fisica, Mexico, D.F. (Mexico); Sanchez-Hernandez, R. [INAH Subdireccion de Laboratorios y Apoyo Academico, Mexico, D.F. (Mexico); Robles-Camacho, J. [INAH Centro Regional Michoacan, Morelia, Michoacan (Mexico); Rojas-Gaytan, J. [INAH Direccion de Salvamento Arqueologico, Naucalpan de Juarez (Mexico)

    2008-01-15

    Some samples of raw blue pigments coming from an archaeological rescue mission in downtown Mexico City have been characterized using different techniques. The samples, some recovered as a part of a ritual offering, could be assigned to the late Aztec period (XVth century). The striking characteristic of these samples is that they seem to be raw pigments prior to any use in artworks, and it was possible to collect a few {mu}g of pigment after manual grain selection under a microscopy monitoring. All pigments are made of indigo, an organic colorant locally known as anil or xiuhquilitl. The colorant is always found in combination with an inorganic matrix, studied by powder diffraction. In one case the mineral base is palygorskite, a rare clay mineral featuring micro-channels in its structure, well known as the main ingredient of the Maya blue pigment. However, other samples present the minerals sepiolite (a clay mineral of the palygorskite family) and calcite. Another sample contains barite, a mineral never reported in prehispanic paints. We present the results of characterization using high resolution powder diffraction recorded at the European Synchrotron Radiation Facility (BM25A, SpLine beamline) complemented with other techniques. All of them gave consistent results on the composition. A chemical test on resistance to acids was done, showing a high resistance for the palygorskite and eventually sepiolite compounds, in good agreement with the excellent resistance of the Maya blue. (orig.)

  6. Synchrotron powder diffraction on Aztec blue pigments

    Science.gov (United States)

    Sánchez Del Río, M.; Gutiérrez-León, A.; Castro, G. R.; Rubio-Zuazo, J.; Solís, C.; Sánchez-Hernández, R.; Robles-Camacho, J.; Rojas-Gaytán, J.

    2008-01-01

    Some samples of raw blue pigments coming from an archaeological rescue mission in downtown Mexico City have been characterized using different techniques. The samples, some recovered as a part of a ritual offering, could be assigned to the late Aztec period (XVth century). The striking characteristic of these samples is that they seem to be raw pigments prior to any use in artworks, and it was possible to collect a few μg of pigment after manual grain selection under a microscopy monitoring. All pigments are made of indigo, an organic colorant locally known as añil or xiuhquilitl. The colorant is always found in combination with an inorganic matrix, studied by powder diffraction. In one case the mineral base is palygorskite, a rare clay mineral featuring micro-channels in its structure, well known as the main ingredient of the Maya blue pigment. However, other samples present the minerals sepiolite (a clay mineral of the palygorskite family) and calcite. Another sample contains barite, a mineral never reported in prehispanic paints. We present the results of characterization using high resolution powder diffraction recorded at the European Synchrotron Radiation Facility (BM25A, SpLine beamline) complemented with other techniques. All of them gave consistent results on the composition. A chemical test on resistance to acids was done, showing a high resistance for the palygorskite and eventually sepiolite compounds, in good agreement with the excellent resistance of the Maya blue.

  7. 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.

  8. 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)

  9. 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)

  10. 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

  11. 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.

  12. Phase and Chemical Composition Analysis on Neolithic Painted Ceramics Sherds Using Synchrotron Radiation X-Ray Powder Diffraction (SRXPD)

    International Nuclear Information System (INIS)

    Constantinescu, B.

    2003-01-01

    Full text: Synchrotron Radiation X-ray Powder Diffraction studies were performed at the wiggler beamline 1711 of MAX II Synchrotron accelerator from Lund, Sweden, in the frame of EU FPV Access to Large Scale Facilities programme. Diffraction data were collected using radiation of wavelength 1.36 A, which was detected by a Brucker system with a Smart 1000 CCD detector. The main goal of our studies was to distinguish different clays and mineral pigments of various Neolithic pottery-producing centres on Romanian territory in relation with possible inter-regional trade route connections. As main results we can mention: - identification of black pigment composition from Cucuteni (Northern Moldavia), Ariusd (South-Eastern Transylvania) and Cris-Starcevo (Oltenia) type pottery (VI - IV Millennia B. Chr.) as a combination of jacobsite, bixbyite (Manganese oxides), magnetite and goethite (Iron oxides) originary from North Moldova mineral deposits of Iacobeni (150 km up on the river Bistritza from analyzed Cucuteni archaeological sites), and as a combination of pyrolusite, magnetite and hematite for Cris-Starcevo samples, probably from local clay (enriched in Mn-Fe oxides) - identification of white pigment composition as calcite (CaCO3) for Cris- Starcevo culture sites from Central Transylvania (from the local abundant chalk deposits) and as calcium silicates mixed with illite (K, H2))Al2[(H2O, OH)2]AlSi3O10 for Cucuteni culture sites - identification of read-brown pigment composition as various mixtures of hematite - goethite - magnetite, all of local provenance - identification of all examined sherds as having local provenance for the clay The main conclusion is that during Neolithic period, the pottery workshops, largely extended on Romanian territory, used local clays but traded black mineral pigments across the Carpathian mountains (Cucuteni and Ariusd areas are separated by these mountains by easily crossed by passes along small rivers)

  13. Analysis of an industrial production suspension of Bacillus lentus subtilisin crystals by powder diffraction: a powerful quality-control tool.

    Science.gov (United States)

    Frankaer, Christian G; Moroz, Olga V; Turkenburg, Johan P; Aspmo, Stein I; Thymark, Majbritt; Friis, Esben P; Stahl, Kenny; Nielsen, Jens E; Wilson, Keith S; Harris, Pernille

    2014-04-01

    A microcrystalline suspension of Bacillus lentus subtilisin (Savinase) produced during industrial large-scale production was analysed by X-ray powder diffraction (XRPD) and X-ray single-crystal diffraction (MX). XRPD established that the bulk microcrystal sample representative of the entire production suspension corresponded to space group P212121, with unit-cell parameters a = 47.65, b = 62.43, c = 75.74 Å, equivalent to those for a known orthorhombic crystal form (PDB entry 1ndq). MX using synchrotron beamlines at the Diamond Light Source with beam dimensions of 20 × 20 µm was subsequently used to study the largest crystals present in the suspension, with diffraction data being collected from two single crystals (∼20 × 20 × 60 µm) to resolutions of 1.40 and 1.57 Å, respectively. Both structures also belonged to space group P2(1)2(1)2(1), but were quite distinct from the dominant form identified by XRPD, with unit-cell parameters a = 53.04, b = 57.55, c = 71.37 Å and a = 52.72, b = 57.13, c = 65.86 Å, respectively, and refined to R = 10.8% and Rfree = 15.5% and to R = 14.1% and Rfree = 18.0%, respectively. They are also different from any of the forms previously reported in the PDB. A controlled crystallization experiment with a highly purified Savinase sample allowed the growth of single crystals of the form identified by XRPD; their structure was solved and refined to a resolution of 1.17 Å with an R of 9.2% and an Rfree of 11.8%. Thus, there are at least three polymorphs present in the production suspension, albeit with the 1ndq-like microcrystals predominating. It is shown how the two techniques can provide invaluable and complementary information for such a production suspension and it is proposed that XRPD provides an excellent quality-control tool for such suspensions.

  14. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  15. Ninety Years of Powder Diffraction: from Birth to Maturity

    International Nuclear Information System (INIS)

    Paszkowicz, W.

    2006-01-01

    The expression ''powder diffraction '' denotes the phenomenon of diffraction of any electromagnetic waves or particles on polycrystalline (powdered, bulk or thin film) materials which is used in a wide variety experimental settings. The X-ray powder-diffraction method was devised and developed during the First World War (1916) by a Dutch/Swiss team, Peter Debye and Paul Scherrer, in Goettingen, Germany, and independently, marginally later, by an American, Albert W. Hull in Schenectady, USA. The birth of powder diffraction came four years after the discovery of the phenomenon of single-crystal diffraction made in 1912 by Walther Friedrich, Paul Knipping and Max Laue in Munich and developed from 1912/1913 by William Henry Bragg (father) and William Lawrence Bragg (son), and later by many others. Powder diffraction became a milestone towards an understanding of the nature of materials, especially of those which cannot be prepared in the form of suitable single crystals, and permitted rapid progress in solid state physics and chemistry. The events leading to the discovery of powder-diffraction phenomenon are briefly reviewed. The importance of synchrotron powder diffraction studies, which have developed since 1980s, is emphasised. (author)

  16. Structure determination of modulated structures by powder X-ray diffraction and electron diffraction

    Czech Academy of Sciences Publication Activity Database

    Zhou, Z.Y.; Palatinus, Lukáš; Sun, J.L.

    2016-01-01

    Roč. 3, č. 11 (2016), s. 1351-1362 ISSN 2052-1553 Institutional support: RVO:68378271 Keywords : electron diffraction * incommensurate structure * powder diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 4.036, year: 2016

  17. 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 ...

  18. Powder diffraction studies using anomalous dispersion

    International Nuclear Information System (INIS)

    Cox, D.E.; Wilkinson, A.P.

    1993-01-01

    With the increasing availability and accessibility of high resolution powder diffractometers at many synchrotron radiation sources throughout the world, there is rapidly-growing interest in the exploitation of anomalous dispersion techniques for structural studies of polycrystalline materials. In conjunction with the Rietveld profile method for structure refinement, such studies are especially useful for the determination of the site distributions of two or more atoms which are near neighbors in the periodic table, or atoms which are distributed among partially occupied sites. Additionally, it is possible to (1) determine the mean-square displacements associated with different kinds of atoms distributed over a single set of sites, (2) distinguish between different oxidation states and coordination geometries of a particular atom in a compound and (3) to determine f' for a wide range of atomic species as a function of energy in the vicinity of an absorption edge. Experimental methods for making anomalous dispersion measurements are described in some detail, including data collection strategies, data analysis and correlation problems, possible systematic errors, and the accuracy of the results. Recent work in the field is reviewed, including cation site-distribution studies (e.g. doped high T c superconductors, ternary alloys, FeCo 2 (PO 4 ) 3 , FeNi 2 BO 5 ), oxidation-state contrast (e.g. YBa 2 Cu 3 O 6+x , Eu 3 O 4 , GaCl 2 , Fe 2 PO 5 ), and the effect of coordination geometry (e.g. Y 3 Ga 5 O l2 )

  19. High pressure neutron powder diffraction at LANSCE

    International Nuclear Information System (INIS)

    Von Dreele, R.B.

    1994-01-01

    By making use of the recently developed ''Paris-Edinburgh'' high pressure cell, the author has successfully performed neutron powder experiments to 10GPa at ambient temperature. Results for the structural compression of the high Tc 1223-Hg superconductor to 9.2 GPa, the compression and possible hydrogen bond formation in brucite, Mg(OD) 2 , to 9.3 GPa, and the molecular reorientation in nitromethane to 5.5 GPa will be presented

  20. Application of Powder Diffraction Methods to the Analysis of the Atomic Structure of Nanocrystals: The Concept of the Apparent Lattice Parameter (ALP)

    Science.gov (United States)

    Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    The applicability of standard methods of elaboration of powder diffraction data for determination of the structure of nano-size crystallites is analysed. Based on our theoretical calculations of powder diffraction data we show, that the assumption of the infinite crystal lattice for nanocrystals smaller than 20 nm in size is not justified. Application of conventional tools developed for elaboration of powder diffraction data, like the Rietveld method, may lead to erroneous interpretation of the experimental results. An alternate evaluation of diffraction data of nanoparticles, based on the so-called 'apparent lattice parameter' (alp) is introduced. We assume a model of nanocrystal having a grain core with well-defined crystal structure, surrounded by a surface shell with the atomic structure similar to that of the core but being under a strain (compressive or tensile). The two structural components, the core and the shell, form essentially a composite crystal with interfering, inseparable diffraction properties. Because the structure of such a nanocrystal is not uniform, it defies the basic definitions of an unambiguous crystallographic phase. Consequently, a set of lattice parameters used for characterization of simple crystal phases is insufficient for a proper description of the complex structure of nanocrystals. We developed a method of evaluation of powder diffraction data of nanocrystals, which refers to a core-shell model and is based on the 'apparent lattice parameter' methodology. For a given diffraction pattem, the alp values are calculated for every individual Bragg reflection. For nanocrystals the alp values depend on the diffraction vector Q. By modeling different a0tomic structures of nanocrystals and calculating theoretically corresponding diffraction patterns using the Debye functions we showed, that alp-Q plots show characteristic shapes which can be used for evaluation of the atomic structure of the core-shell system. We show, that using a simple

  1. A sample holder for in-house X-ray powder diffraction studies of protein powders

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

    2011-01-01

    A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin....

  2. The refractive-index correction in powder diffraction

    International Nuclear Information System (INIS)

    Hart, M.; Parrish, W.; Bellotto, M.; Lim, G.S.

    1988-01-01

    Throughout the history of powder diffraction practice there has been uncertainty about whether or not a refractive-index correction should be made to Bragg's law. High-precision Bragg-angle measurements have been performed with synchrotron radiation on SRM-640 silicon powders at glancing angles; it is found that little or no correction is necessary for the usual 2θ angle range. (orig.)

  3. Applications of neutron powder diffraction in materials research

    International Nuclear Information System (INIS)

    Kennedy, S.J.

    1996-01-01

    The aim of this article is to provide an overview of the applications of neutron powder diffraction in materials science. The technique is introduced with particular attention to comparison with the X-ray powder diffraction technique to which it is complementary. The diffractometers and special environment ancillaries operating around the HIFAR research reactor at the Australian Nuclear Science and Technology Organisation (ANSTO) are described. Applications of the technique which the advantage of the unique properties of thermal neutrons have been selected from recent materials studies undertaken at ANSTO

  4. X-ray powder diffraction data on miscellaneous lanthanide compounds

    International Nuclear Information System (INIS)

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

    1978-08-01

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

  5. 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.

  6. Polarized neutron powder diffraction studies of antiferromagnetic order in bulk and nanoparticle NiO

    DEFF Research Database (Denmark)

    Brok, Erik; Lefmann, Kim; Deen, Pascale P.

    2015-01-01

    surface contribution to the magnetic anisotropy. Here we explore the potential use of polarized neutron diffraction to reveal the magnetic structure in NiO bulk and nanoparticle powders by applying the XYZ-polarization analysis method. Our investigations address in particular the spin orientation in bulk....... The results show that polarization analyzed neutron powder diffraction is a viable method to investigate magnetic order in powders of antiferromagnetic nanoparticles.......In many materials it remains a challenge to reveal the nature of magnetic correlations, including antiferromagnetism and spin disorder. Revealing the spin structure in magnetic nanoparticles is further complicated by the large incoherent neutron scattering cross section from water adsorbed...

  7. 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.

  8. 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

  9. 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.

  10. 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

  11. American Crystallographic Association Project: numerical ratings of powder diffraction patterns

    International Nuclear Information System (INIS)

    Smith, G.S.; Snyder, R.L.

    1977-01-01

    At present, nearly 30,000 powder diffraction patterns are available as references. It is proposed that the patterns in this file as well as new patterns submitted for publication be given quantitative quality factors. A simple-to-use figure of merit, F/sub N/, covering both accuracy of d-values and completeness of a pattern was derived. This figure of merit provides the user with a means of rapid evaluation of powder patterns in much the same way that the R-factor does for single-crystal structure determinations. The present F/sub N/ ranking scheme is shown to be superior to de Wolff's M 20 ranking scheme. It is recommended that the latter be discontinued. Guidelines are given on the use and implementation of F/sub N/ rating of powder diffraction patterns

  12. 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.

  13. 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

  14. Neutron powder diffraction under high pressure at J-PARC

    International Nuclear Information System (INIS)

    Utsumi, Wataru; Kagi, Hiroyuki; Komatsu, Kazuki; Arima, Hiroshi; Nagai, Takaya; Okuchi, Takuo; Kamiyama, Takashi; Uwatoko, Yoshiya; Matsubayashi, Kazuyuki; Yagi, Takehiko

    2009-01-01

    It is expected that high-pressure material science and the investigation of the Earth's interior will progress greatly using the high-flux pulse neutrons of J-PARC. In this article, we introduce our plans for in situ neutron powder diffraction experiments under high pressure at J-PARC. The use of three different types of high-pressure devices is planned; a Paris-Edinburgh cell, a new opposed-anvil cell with a nano-polycrystalline diamond, and a cubic anvil high-pressure apparatus. These devices will be brought to the neutron powder diffraction beamlines to conduct a 'day-one' high-pressure experiment. For the next stage of research, we propose construction of a dedicated beamline for high-pressure material science. Its conceptual designs are also introduced here.

  15. MacDUST - a powder diffraction package developed for the ''ADONE'' high resolution diffraction station

    International Nuclear Information System (INIS)

    Burattini, E.; Cappuccio, G.; Maistrelli, P.; Simeoni, S.

    1993-01-01

    A High Resolution Powder Diffraction Station (PO.DI.STA.) was installed at the beginning of 1991 on the ADONE-Wiggler magnet beam line. The station and the first powder diffraction spectra, collected with synchrotron radiation, were presented at the EPDIC-1 Conference. More details can also be found in. For this station, a very sophisticated software package ''MacDUST'' has been developed on an Apple Macintosh computer, using the Microsoft QuickBASIC compiler. It allows very easy and comfortable operations by means of a graphical user interface environment, typical of the Macintosh system. The package consists of five major programs. The main program, MacDIFF, performs all the graphic operations on the experimental data, including zooming, overlapping, cursor scanning and editing of patterns, control of output operations to printers and HPGL plotters. It also includes several analysis routines for data smoothing, a first derivative peak search algorithm, two background subtraction routines and two profile fitting programs: one based on the simplex method and the other on the Marquardt modification of a least-square algorithm. MacPDF and MacRIC are both dedicated to phase identification. The first program is an archive manager for searching, displaying and printing phase records; MacRIC is a graphic aided search-match program based on the Hanawalt algorithm. Mac3-DIM is a plot program, useful, e.g., for representing kinetics three dimensionally. MacRIET is a Macintosh version of the well known Rietveld refinement program. This version, besides conventional structure refinements, also allows the determination of micro structural parameters, i.e. micro strain and crystallite size. The program can also be used to simulate a pattern, once the structure of the compound is known. Taking advantage of the very intuitive Macintosh graphic user interface, through dialog and alert boxes, the program allows straightforward introduction and modification of the structure

  16. 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.

  17. 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

  18. Application of Powder Diffraction Methods to the Analysis of Short- and Long-Range Atomic Order in Nanocrystalline Diamond and SiC: The Concept of the Apparent Lattice Parameter (alp)

    Science.gov (United States)

    Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.

    2003-01-01

    Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.

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

    Science.gov (United States)

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

    2015-10-01

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

  20. Unit-cell refinement from powder diffraction scans

    International Nuclear Information System (INIS)

    Pawley, G.S.

    1981-01-01

    A procedure for the refinement of the crystal unit cell from a powder diffraction scan is presented. In this procedure knowledge of the crystal structure is not required, and at the end of the refinement a list of indexed intensities is produced. This list may well be usable as the starting point for the application of direct methods. The problems of least-squares ill-conditioning due to overlapping reflections are overcome by constraints. An example using decafluorocyclohexene, C 6 F 10 , shows the quality of fit obtained in a case which may even be a false minimum. The method should become more relevant as powder scans of improved resolution become available, through the use of pulsed neutron sources. (Auth.)

  1. 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...

  2. Acquiring the fundamentals: an accredited powder diffraction course on the internet

    International Nuclear Information System (INIS)

    Crockcroft, J.K.; Barnes, P.; Attfield, M.P.; Cranswick, L.M.D.

    2002-01-01

    Full text: In August 1999, building on accredited academic-based crystallographic web courses pioneered by Birkbeck College, University of London, for Protein Crystallography and Principles of Protein Structure, a new 'Advanced Certificate in Powder Diffraction' was officially announced at the International Union of Crystallography congress in Glasgow. Offering tuition via the Internet on the fundamentals in powder diffraction, it is now running successfully into its third year. The background of student intake ranges from new PhD students to scientists, technicians and X-ray analysts in commercial companies. The work for this 1 year long course, takes around 6 to 8 hours a week to complete; and should not be considered equivalent to recreational web browsing, but as serious study. If this course is done as part of staff training and development, it is important that the employer recognize this; and that adequate training time is set aside as part of the working week. The 'Advanced Certificate in Powder Diffraction' is assessed by a mixture of 'coursework', computer based data analysis project and a formal written exam taken at a local university. To obtain the full qualification, the exam must be taken, but it is optional if only training and no formal qualification is required. The course content covers a broad range of knowledge required for an 'understanding' of powder diffraction. These include the Internet Skills required to do the course, Diffraction Instrumentation, Laboratory Methods, Synchrotron Sources and Methods, Neutron Sources, Diffraction Theory, Electron Scattering to Structure Factors, Structure Factors to Diffraction Intensities, the concept of Symmetry to 3-D Symmetry Elements, Point Groups, Space Groups, Space-Group Determination, Interpreting the IUCr International Tables, Qualitative Analysis, Quantitative Analysis, Indexing, Unit-Cell Refinement, Peak Shapes, Structure Refinement and the Rietveld Method, Modern Techniques and Applications

  3. New synchrotron powder diffraction facility for long-duration experiments.

    Science.gov (United States)

    Murray, Claire A; Potter, Jonathan; Day, Sarah J; Baker, Annabelle R; Thompson, Stephen P; Kelly, Jon; Morris, Christopher G; Yang, Sihai; Tang, Chiu C

    2017-02-01

    A new synchrotron X-ray powder diffraction instrument has been built and commissioned for long-duration experiments on beamline I11 at Diamond Light Source. The concept is unique, with design features to house multiple experiments running in parallel, in particular with specific stages for sample environments to study slow kinetic systems or processes. The instrument benefits from a high-brightness X-ray beam and a large area detector. Diffraction data from the commissioning work have shown that the objectives and criteria are met. Supported by two case studies, the results from months of measurements have demonstrated the viability of this large-scale instrument, which is the world's first dedicated facility for long-term studies (weeks to years) using synchrotron radiation.

  4. The CCP14 for single crystal and powder diffraction

    International Nuclear Information System (INIS)

    Cranswick, L.M.D.

    1999-01-01

    Full text: The Collaborative Computation Project Number 14 for Single Crystal and Powder Diffraction (CCP14) is continuing in its objective to provide freely available software and resources for the powder diffraction and crystallographic community. Using the Internet and World Wide Web, we are presently compiling software and web resources, creating tutorials and help files. It also endeavours to encourage and provide resources to assist program authors with developing their software. The CCP14 presently has its web-site at and a mirror at (at CSIRO, Melbourne, Australia). Auto web-mirroring is being implemented to allow users to obtain software and access to resources in a more time effective manner. For people in countries isolated from the Internet, the CCP14 on CD-ROM can be snail mailed on request. This is in the form of a Virtual World Wide Web/Virtual Internet; in the same vein as the existing Crystallographic Nexus CD-ROM. Copyright (1999) Australian X-ray Analytical Association Inc

  5. 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.

  6. 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...

  7. High-resolution neutron powder-diffraction in CMR manganates

    Energy Technology Data Exchange (ETDEWEB)

    Suard, E; Radaelli, P G [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France)

    1997-04-01

    Manganese-oxide materials have recently been the subject of renewed attention, due to the `colossal` magnetoresistance (CMR) displayed near the spin-ordering temperature T{sub c} by some of these compounds. CMR has been evidenced in at least three families of manganese oxides. In most cases, the CMR compounds behave as paramagnetic semiconductors at high temperatures, and as ferromagnetic metals below T{sub c}. The study of this metallization process has lead some theorists to challenge its traditional interpretation in terms of the so-called double-exchange mechanism, and to propose alternative scenarios in which the coupling of the charge carriers with the lattice plays a paramount role. Powder diffraction method, being at the forefront of CMR research is presented. (author). 4 refs.

  8. 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

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

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

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

  10. High throughput screening of ligand binding to macromolecules using high resolution powder diffraction

    Science.gov (United States)

    Von Dreele, Robert B.; D'Amico, Kevin

    2006-10-31

    A process is provided for the high throughput screening of binding of ligands to macromolecules using high resolution powder diffraction data including producing a first sample slurry of a selected polycrystalline macromolecule material and a solvent, producing a second sample slurry of a selected polycrystalline macromolecule material, one or more ligands and the solvent, obtaining a high resolution powder diffraction pattern on each of said first sample slurry and the second sample slurry, and, comparing the high resolution powder diffraction pattern of the first sample slurry and the high resolution powder diffraction pattern of the second sample slurry whereby a difference in the high resolution powder diffraction patterns of the first sample slurry and the second sample slurry provides a positive indication for the formation of a complex between the selected polycrystalline macromolecule material and at least one of the one or more ligands.

  11. Multipole electron-density modelling of synchrotron powder diffraction data: the case of diamond

    DEFF Research Database (Denmark)

    Svendsen, H.; Overgaard, J.; Busselez, R.

    2010-01-01

    between experiment and theory, and the study therefore demonstrates that synchrotron powder diffraction can indeed provide accurate structure-factor values based on data measured in minutes with limited sample preparation. Thus, potential systematic errors such as extinction and twinning commonly......Accurate structure factors are extracted from synchrotron powder diffraction data measured on crystalline diamond based on a novel multipole model division of overlapping reflection intensities. The approach limits the spherical-atom bias in structure factors extracted from overlapping powder data...

  12. Characterization of Synthesized and Commercial Forms of Magnesium Stearate Using Differential Scanning Calorimetry, Thermogravimetric Analysis, Powder X-Ray Diffraction, and Solid-State NMR Spectroscopy.

    Science.gov (United States)

    Delaney, Sean P; Nethercott, Matthew J; Mays, Christopher J; Winquist, Nickolas T; Arthur, Donia; Calahan, Julie L; Sethi, Manish; Pardue, Daniel S; Kim, Junghyun; Amidon, Gregory; Munson, Eric J

    2017-01-01

    Magnesium stearate is the salt of a complex mixture of fatty acids, with the majority being stearate and palmitate. It has multiple crystalline forms and, potentially, an amorphous form. Magnesium stearate is used in the pharmaceutical manufacturing industry as a powder lubricant, and typically is added at low levels (∼1%) during the manufacturing process and blended for a relatively short time (∼5 min). Proper levels and mixing times are needed, as too short a mixing time or too small a quantity will result in improper lubrication, and too much can negatively impact dissolution rates. The complex mixture of multiple fatty acids and crystalline forms in magnesium stearate leads to variability between commercial sources, and switching between sources can impact both the amount of lubricant and mixing time needed for proper lubrication. In order to better understand the complex nature of magnesium stearate, a variety of analytical techniques were used to characterize both synthesized and commercial magnesium stearate samples. The results show that correlation among differential scanning calorimetry, thermogravimetric analysis, solid-state NMR spectroscopy, and other techniques provides a unique insight into the forms of magnesium stearate. Finally, the ability to monitor form changes of magnesium stearate in an intact tablet using solid-state NMR spectroscopy is shown. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  13. 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.

  14. 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)

  15. 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)

  16. Structural study on the gas adsorption phenomena in porous coordination polymers by synchrotron powder diffraction method

    International Nuclear Information System (INIS)

    Kubota, Yoshiki

    2017-01-01

    In situ synchrotron powder diffraction measurement of gas adsorption and crystal structure analysis for porous coordination polymers (PCPs) were performed. From the obtained accurate crystal structure in both atomic and charge density levels, not only the position and orientation of adsorbed gas molecules but also the interaction between the adsorbed gas molecule and host framework were found. The information enables us to understand the mechanism of gas adsorption phenomena and functions of PCPs. It will give us the guiding principles for the novel functional materials design. (author)

  17. Nanocrystallite characterization of milled simulated dry process fuel powders by neutron diffraction

    International Nuclear Information System (INIS)

    Ryu, Ho Jin; Kang, Kwon Ho; Moon, Je Sun; Song, Kee Chan; Choi, Yong Nam

    2003-01-01

    The nano-scale crystallite sizes of simulated spent fuel powders were measured by the neutron diffraction line broadening method in order to analyze the sintering behavior of the dry process fuel. The mixed U0 2 and fission product oxide powders were dry-milled in an attritor for 30, 60, and 120 min. The diffraction patterns of the powders were obtained by using the high resolution powder diffractometer in the HANARO research reactor. Diffraction line broadening due to crystallite size was measured using various techniques such as the Stokes' deconvolution, profile fitting methods using Cauchy function, Gaussian function, and Voigt function, and the Warren-Averbach method. The r.m.s. strain, stacking fault, twin and dislocation density were measured using the information from the diffraction pattern. The realistic crystallite size can be obtained after separation of the contribution from the non-uniform strain, stacking fault and twin

  18. Rietveld refinement with time-of-flight powder diffraction data from pulsed neutron sources

    International Nuclear Information System (INIS)

    David, W.I.F.; Jorgensen, J.D.

    1990-10-01

    The recent development of accelerator-based pulsed neutron sources has led to the widespread use of the time-of-flight technique for neutron powder diffraction. The properties of the pulsed source make possible unusually high resolution over a wide range of d spacings, high count rates, and the ability to collect complete data at fixed scattering angles. The peak shape and other instrument characteristics can be accurately modelled, which make Rietveld refinement possible for complex structures. In this paper we briefly review the development of the Rietveld method for time-of-flight diffraction data from pulsed neutron sources and discuss the latest developments in high resolution instrumentation and advanced Rietveld analysis methods. 50 refs., 12 figs., 14 tabs

  19. Monitoring protein precipitates by in-house X-ray powder diffraction

    DEFF Research Database (Denmark)

    Ståhl, Kenny; Frankær, Christian Grundahl; Petersen, Jakob

    2013-01-01

    of such calculated powder patterns from insulin and lysozyme have been included in the powder diffraction database and successfully used for search-match identification. However, the fit could be much improved if peak asymmetry and multiple bulk-solvent corrections were included. When including a large number...

  20. X-Ray powder diffraction analysis: Synthesis and spectroscopic studies on the stoichiometric elpasolite Cs2NaTmCl6

    International Nuclear Information System (INIS)

    Acevedo, R.; Poblete, V.; Elgueta, R.; Pozo, J.

    2000-01-01

    The elpasolite Cs 2 NaTmCl 6 belonging to the spatial group Fm3m, has been synthesized and characterized by powder DRX and spectroscopic studies. The synthesis was carried out by means of a solid state reaction at 802.9 o C, for two hours, with a temperature gradient of 4 o C/min. and 2 o C/min, at the beginning and end of the reaction, respectively. The optimum crystallization temperature occurs between 764.5 o C and 838.5 o C. The following crystallographic parameters were obtained: a 0 = 10,6866 o A, V =1220,45( o A) 3 , Z = 4, M = 802.90, D x =3,65 y D exp =3,67. The 32 experimental lines that were analyzed show great accuracy considering that R exp less than R wp . The Raman spectrums allowed for precise identification and assignation so that we can make progress in calculating the crystal dynamics and mechanistic aspects, still unexplored in the literature (C.W)

  1. Identification of phases in zinc alloy powders using electron backscatter diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Perez, Martin G. [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States); Kenik, Edward A. [Oak Ridge National Laboratory, 100 Bethel Valley Rd., Bldg. 4515, MS-6064, P.O. Box 2008, Oak Ridge, TN 37831 (United States); O' Keefe, Matthew J. [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States)]. E-mail: mjokeefe@umr.edu; Miller, F. Scott [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States); Johnson, Benedict [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States)

    2006-05-25

    Scanning electron microscopy and electron backscatter diffraction (EBSD) were used for the structural characterization of phases in Zn alloy powders. Commercial Zn alloy powders contained additions of <1000 ppm of Bi, In, Al or Mg. Bismuth and In have extremely low solubility in Zn and form intermetallic Bi-In compounds which segregate to the Zn grain boundaries. The Bi-In phases were <0.3 {mu}m in size, had low melting points, and were not abundant enough for EBSD analysis. Increasing the alloying additions 20-40-fold resulted in Bi-In phases >1 {mu}m that could be used for EBSD analysis for phase characterization. Deformation-free microstructures were obtained by mechanical polishing and ion milling. The Zn matrix was characterized as Zn via EBSD. A BiIn{sub 2} phase was identified in the powder microstructures via EBSD. An In phase with 8-9 wt.% Bi was identified using low voltage energy dispersive spectroscopy and closely matched the composition predicted by the Bi-In phase diagram.

  2. X-ray powder diffraction in forensic practice

    Czech Academy of Sciences Publication Activity Database

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

    Roč. 13, č. 3 (2006), s. 153-155 ISSN 1210-8529 R&D Projects: GA MV RN20052005001 Institutional research plan: CEZ:AV0Z40320502 Keywords : X-ray powder microdiffraction * pigments * forensic practice Subject RIV: CA - Inorganic Chemistry

  3. 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.

  4. 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.

  5. Application of powder X-ray diffraction and the Rietveld method to the analysis of oxidation processes and products in sulphidic mine tailings

    DEFF Research Database (Denmark)

    Balic Zunic, Tonci; Katerinopoulou, Anna; Edsberg, Anders

    2011-01-01

    silica were applied as proper models. The procedures developed on test mixtures result in estimated errors of determination typically lower than 2 wt%. The approach was applied to the analysis of the complex problem of estimating mass balance in oxidized mine tailings from the Nanisivik Mine, Nunavut......, Canada revealing an oxidized proportion of 9 % of total pyrite content in the well drained tailings during a period of 8 years and a negligible oxidation in the water-covered tailings....

  6. 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...

  7. Development of powder diffraction anomalous fine structure method and applications to electrode materials for rechargeable batteries

    International Nuclear Information System (INIS)

    Kawaguchi, Tomoya; Fukuda, Katsutoshi; Oishi, Masatsugu; Ichitsubo, Tetsu; Matsubara, Eiichiro; Mizuki, Jun'ichiro

    2015-01-01

    A powder diffraction anomalous fine structure (P-DAFS) method is developed both in analytical and experimental techniques and applied to cathode materials for lithium ion batteries. The DAFS method, which is an absorption spectroscopic technique through a scattering measurement, enables us to analyze the chemical states and the local structures of a certain element at different sites, thanks to the nature of x-ray diffraction, where the contributions from each site are different at each diffraction. Electrode materials for rechargeable batteries frequently exhibit the interchange between Li and a transition metal, which is known as the cation mixing phenomena. This cation mixing significantly affects the whole electrode properties; therefore, the site-distinguished understanding of the roles of the transition metal is essential for further material design by controlling and positively utilizing this cation mixing phenomenon. However, the developments of the P-DAFS method are required for the applications to the practical materials such as the electrode materials. In the present study, a direct analysis technique to extract the absorption spectrum from the scattering without using the conventional iterative calculations, fast and accurate measurement techniques of the P-DAFS method, and applications to a typical electrode material of Li 1-x Ni 1+x O 2 , which exhibits the significant cation mixing, are described. (author)

  8. Beamline I11 at Diamond: a new instrument for high resolution powder diffraction.

    Science.gov (United States)

    Thompson, S P; Parker, J E; Potter, J; Hill, T P; Birt, A; Cobb, T M; Yuan, F; Tang, C C

    2009-07-01

    The performance characteristics of a new synchrotron x-ray powder diffraction beamline (I11) at the Diamond Light Source are presented. Using an in-vacuum undulator for photon production and deploying simple x-ray optics centered around a double-crystal monochromator and a pair of harmonic rejection mirrors, a high brightness and low bandpass x-ray beam is delivered at the sample. To provide fast data collection, 45 Si(111) analyzing crystals and detectors are installed onto a large and high precision diffractometer. High resolution powder diffraction data from standard reference materials of Si, alpha-quartz, and LaB6 are used to characterize instrumental performance.

  9. Crystal structure determination from powder diffraction data of the coumarin vanillin chalcone

    Czech Academy of Sciences Publication Activity Database

    Ghouili, A.; Rohlíček, Jan; Ayed, T.B.; Hassen, R.B.

    2014-01-01

    Roč. 29, č. 4 (2014), s. 361-365 ISSN 0885-7156 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : chalcone * absorption spectra * powder diffraction * crystal structure determination * coumarin derivatives Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.636, year: 2014

  10. Dihydroxycoumarin Schiff base synthesis and structure determination from powder diffraction data

    Czech Academy of Sciences Publication Activity Database

    Rohlíček, Jan; Ketata, I.; Ben Ayed, T.; Ben Hassen, R.

    2013-01-01

    Roč. 1051, NOV (2013), s. 280-284 ISSN 0022-2860 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : powder diffraction * structure solution * Schiff base * dihydroxycoumarine Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.599, year: 2013

  11. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lawson, A.C.; Smith, K. (comps.)

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs.

  12. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    International Nuclear Information System (INIS)

    Lawson, A.C.; Smith, K.

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs

  13. Application of the ellipsoid modeling of the average shape of nanosized crystallites in powder diffraction

    DEFF Research Database (Denmark)

    Katerinopoulou, Anna; Balic Zunic, Tonci; Lundegaard, Lars Fahl

    2012-01-01

    Anisotropic broadening correction in X-ray powder diffraction by an ellipsoidal formula is applied on samples with nanosized crystals. Two cases of minerals with largely anisotropic crystallite shapes are presented. The properly applied formalism not only improves the fitting of the theoretical...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-03-07

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

  15. 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

  16. 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

  17. Application of new synchrotron powder diffraction techniques to anomalous scattering from glasses

    International Nuclear Information System (INIS)

    Beno, M.A.; Knapp, G.S.; Armand, P.; Price, D.L.; Saboungi, M.

    1995-01-01

    We have applied two synchrotron powder diffraction techniques to the measurement of high quality anomalous scattering diffraction data for amorphous materials. One of these methods, which uses a curved perfect crystal analyzer to simultaneously diffract multiple powder lines into a position sensitive detector has been shown to possess high resolution, low background, and very high counting rates. This data measurement technique provides excellent energy resolution while minimizing systematic errors resulting from detector nonlinearity. Anomalous scattering data for a Cesium Germanate glass collected using this technique will be presented. The second powder diffraction technique uses a flat analyzer crystal to deflect multiple diffraction lines out of the equatorial plane. Calculations show that this method possesses sufficient energy resolution for anomalous scattering experiments when a perfect crystal analyzer is used and is experimentally much simpler. Future studies will make use of a rapid sample changer allowing the scattering from the sample and a standard material (a material not containing the anomalous scatterer) to be measured alternately at each angle, reducing systematic errors due to beam instability or sample misalignment

  18. A QCD analysis of ZEUS diffractive data

    Energy Technology Data Exchange (ETDEWEB)

    Chekanov, S.; Derrick, M.; Magill, S. [Argonne National Laboratory, Argonne, IL (US)] (and others)

    2009-11-15

    ZEUS inclusive diffractive cross-section measurements have been used in a DGLAP next-to-leading-order QCD analysis to extract the diffractive parton distribution functions. Data on diffractive dijet production in deep inelastic scattering have also been included to constrain the gluon density. Predictions based on the extracted parton densities are compared to diffractive charm and dijet photoproduction data. (orig.)

  19. A QCD analysis of ZEUS diffractive data

    International Nuclear Information System (INIS)

    Chekanov, S.; Derrick, M.; Magill, S.

    2009-11-01

    ZEUS inclusive diffractive cross-section measurements have been used in a DGLAP next-to-leading-order QCD analysis to extract the diffractive parton distribution functions. Data on diffractive dijet production in deep inelastic scattering have also been included to constrain the gluon density. Predictions based on the extracted parton densities are compared to diffractive charm and dijet photoproduction data. (orig.)

  20. ATALANTA: a multicomponent pulsed neutron diffraction analysis code

    International Nuclear Information System (INIS)

    Benham, M.J.; Ross, D.K.

    1986-01-01

    The analysis of powder diffraction patterns from metal hydrogen systems present certain problems which have been addressed in a restructured profile analysis program. The heart of this program, ATALANTA, is a routine which locates and processes small sections of the data field to which a minimal number of Bragg peaks contribute intensity. The analysis of a three component test data set is presented in order to demonstrate the method. (author)

  1. Neutron powder diffraction analysis of (Tm{sub 0.50}Ca{sub 0.50})MnO{sub 3} and (Lu{sub 0.50}Ca{sub 0.50})MnO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Martinelli, A., E-mail: alberto.martinelli@spin.cnr.it [SPIN-CNR, C.so Perrone 24, 16152 Genova (Italy); Ferretti, M. [SPIN-CNR, C.so Perrone 24, 16152 Genova (Italy); Universita degli Studi di Genova, Dipartimento di Chimica e Chimica Industriale, Via Dodecaneso 31, 16146 Genova (Italy); Cimberle, M.R. [IMEM-CNR, Via Dodecaneso 33, 16146, Genova (Italy); Ritter, C. [Institute Laue-Langevin, 6 rue Jules Horowitz, 38042 Grenoble Cedex 9 (France)

    2012-12-15

    The crystal and magnetic structures of (Tm{sub 0.50}Ca{sub 0.50})MnO{sub 3} and (Lu{sub 0.50}Ca{sub 0.50})MnO{sub 3} have been investigated between 5 K and 300 K by means of high resolution neutron powder diffraction followed by Rietveld refinement and dc magnetic measurements. During cooling orbital ordering at the Mn sub-lattice takes place at T{sub OO}{approx}280 K in both compounds, inducing an orthorhombic to monoclinic phase transition. As the temperature is further decreased an antiferromagnetic CE-type structure occurs in both compounds at T{sub N}{approx}105 K. The comparison with other (Ln{sub 0.50}Ca{sub 0.50})MnO{sub 3} compounds reveals that at room temperature the average Jahn-Teller distortion increases sharply with the decrease of the ionic radius for lanthanides heavier than Sm. The ordered magnetic moment progressively decreases as the lanthanide ionic radius decreases on account of the decreased values of the Mn-O-Mn bond angles. - Graphical abstract: Rietveld refinement plot for (Tm{sub 0.50}Ca{sub 0.50})MnO{sub 3} obtained from neutron powder diffraction data collected at 5 K; the inset shows the CE-type spin ordering taking place at the Mn sub-lattice. Highlights: Black-Right-Pointing-Pointer The crystal and magnetic structures of (Tm{sub 0.50}Ca{sub 0.50})MnO{sub 3} and (Lu{sub 0.50}Ca{sub 0.50})MnO{sub 3} were analyzed by neutron powder diffraction. Black-Right-Pointing-Pointer Orbital ordering takes place below T{sub OO}{approx}280 K in both compounds. Black-Right-Pointing-Pointer An antiferromagnetic CE-type structure occurs in both compounds below T{sub N}{approx}105 K. Black-Right-Pointing-Pointer A Comparison with other (Ln{sub 0.50}Ca{sub 0.50})MnO{sub 3} compounds is reported.

  2. 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

  3. 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

  4. Neutron powder diffraction studies of Hydrogen and Denterium in Palladium Phosphides

    International Nuclear Information System (INIS)

    Andersson, Y.

    1986-01-01

    The use of the Rietveld-type profile refinements on neutron powder diffraction intensity data for determining crystallographic positions of hydrogen and deuterium in metal hydrides is illustrated by results obtained on some hydrogenated and deuterated palladium phosphides. The structural features of the solid solutions of hydrogen and deuterium in Pd/sb15/P/sb2/ Pd/sb6/P and Pd/sb3/P/sb1-u/ (0< u<0.28) are briefly presented and discussed

  5. A high-resolution neutron powder diffraction study of neodymium doping in barium cerate

    DEFF Research Database (Denmark)

    Knight, K.S.; Bonanos, N.

    1995-01-01

    High-resolution neutron powder diffraction data have been collected on 6 perovskites of composition BaCe1-xNdxO3-x/(2), with 0 less than or equal to x less than or equal to 0.2, in which structural phase transitions Pmcn-->P4/mbm at x=0.05, and P4/mbm-->Pm3m at x=0.1, were inferred from a recent ...

  6. 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.

  7. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    Energy Technology Data Exchange (ETDEWEB)

    Cui, J., E-mail: jun.cui@pnnl.gov; Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J. [Energy and Environment Directorate, Pacific Northwest National Laboratory, Richland, Washington 99354 (United States); Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D. [Materials Sciences and Engineering Division, Ames Laboratory, Ames, Iowa 50011 (United States); Marinescu, M. [Electron Energy Corporation, Landisville, Pennsylvania 17538 (United States); Huang, Q. Z.; Wu, H. [NIST Center for Neutron Research, National Institute of Standards and Technology, Gaithersburg, Maryland 20899-6102 (United States); Vuong, N. V.; Liu, J. P. [Department of Physics, University of Texas at Arlington, Arlington, Texas 76019 (United States)

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 μ{sub B} at 50 K and 300 K, respectively.

  8. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    Energy Technology Data Exchange (ETDEWEB)

    Cui, J; Choi, JP; Li, G; Polikarpov, E; Darsell, J; Kramer, MJ; Zarkevich, NA; Wang, LL; Johnson, DD; Marinescu, M; Huang, QZ; Wu, H; Vuong, NV; Liu, JP

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 mu(B) at 50 K and 300 K, respectively. (C) 2014 AIP Publishing LLC.

  9. 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.

  10. Rietveld refinement of magnetic structures from pulsed-neutron-source powder-diffraction data

    International Nuclear Information System (INIS)

    Robinson, R.A.; Lawson, A.C.; Larson, A.C.; Von Dreele, R.B.; Goldstone, J.A.

    1994-01-01

    The General Structure Analysis System, GSAS, has recently been modified to include magnetic neutron- scattering cross-sections. Low-temperature diffraction data have been taken on the hexagonal noncollinear antiferromagnet UPdSn on both the HIPD and the NPD powder diffractometers ail LANSCE. The low-resolution data reveal that the magnetic structure has orthorhombic symmetry (magnetic space group P c m'c2 1 ) between 25K and 40K, and monoclinic symmetry (magnetic space group PC 1121 ) below 25K. The high-resolution data reveal that there are structural distortions with corresponding symmetry changes in each of these phases, to give chemical space groups Cmc2 1 and P2 1 , respectively, while the paramagnetic phase above 40K has space group P6 3 mc. Using GSAS, we have refined data sets from both diffractometers simultaneously, including both magnetic and structural cross-sections. Magnetoelastic coefficients for the distortions have been extracted and we have determined the sign of the coupling between the structural monoclinicity and the magnetic monoclinicity. The magnetic results from Rietveld refinement are in good agreement with model fitting to the integrated intensities of seven independent magnetic reflections and these, in turn, agree with measurements made on the same sample using the constant-wavelength reactor technique. Our results therefore validate, to some level, both the technique of using spallation sources for complicated magnetic structures and the specifics of the GSAS Rietveld code

  11. Neutron Powder Diffraction Studies of Ca2-xSrxCoWO6 Double Perovskites

    International Nuclear Information System (INIS)

    Zhou, Qingdi; Kennedy, Brendan; Elcombe, Margaret

    2005-01-01

    Full text: A series of double perovskite compounds of A 2-x Sr x CoWO 6 (A = Ca, Ba) were synthesized and the room- and variable-temperature structural phase transitions have been studied by synchrotron and neutron powder diffraction techniques. These studies demonstrated that the symmetry increases as the average size of the A-site cation increases. These transitions are associated with the gradual reduction and ultimately removal of the octahedral tiles of the BO 6 octahedra. Temperature dependent structural studies have been undertaken for selected samples. The transition to cubic is continuous in the three Ca doped samples studied as a function of temperature, Ca 2-x Sr x CoWO 6 x = 1.8, 1.7, 1.6, however in each case analysis of the spontaneous strain shows the transition to be tricritical rather than second order in nature. Where observed the temperature induced P2 1 /n to I4/m transition is first order as required by symmetry. (authors)>>>>

  12. 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.

  13. 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

  14. Powder neutron diffraction study on Pb2Sr2YCu3O8+δ(δ = 0.0 and 1.67)

    International Nuclear Information System (INIS)

    Fujishita, Hideshi; Sato, Masatoshi; Morii, Yukio; Funahashi, Satoru.

    1993-01-01

    Powder neutron diffraction patterns of Pb 2 Sr 2 YCu 3 O 8+δ (δ = 0.0 and 1.67) were analyzed by Rietveld method. For δ = 0, it had been indicated, by powder X-ray diffraction, that the structure was a monoclinic one. The R factors of the present analysis for the monoclinic structure were about 3/4 of those for the previous orthorhombic ones. The structure was almost the same as the previous X-ray result except z (02). For the annealed phase, the tetragonal and the orthorhombic structures had been presented by X-ray diffraction and by neutron diffraction, respectively. The R factors of the present analysis for the orthorhombic structure were about 5/6 of those for the tetragonal structure. The distance between the Pb plane and the oxygen deficient Cu plane was found to become larger in proportion to δ, though there occurs a phase separation in low δ region. (author)

  15. Tolerance analysis on diffraction efficiency and polychromatic integral diffraction efficiency for harmonic diffractive optics

    Science.gov (United States)

    Shan, Mao

    2016-10-01

    In this dissertation, the mathematical model of effect of manufacturing errors including microstructure relative height error and relative width error on diffraction efficiency for the harmonic diffractive optical elements (HDEs) is set up. According to the expression of the phase delay and diffraction efficiency of the HDEs, the expression of diffraction efficiency of refraction and diffractive optical element with the microstructure height and periodic width errors in fabrication process is presented in this paper. Furthermore, the effect of manufacturing errors on diffraction efficiency for the harmonic diffractive optical elements is studied, and diffraction efficiency change is analyzed as the relative microstructure height-error in the same and in the opposite sign as well as relative width-error in the same and in the opposite sign. Example including infrared wavelength with materials GE has been discussed in this paper. Two kinds of manufacturing errors applied in 3.7 4.3um middle infrared and 8.7-11.5um far infrared optical system which results in diffraction efficiency and PIDE of HDEs are studied. The analysis results can be used for manufacturing error control in micro-structure height and periodic width. Results can be used for HDEs processing.

  16. 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.

  17. 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...

  18. A new parallel and GPU version of a TREOR-based algorithm for indexing powder diffraction data

    Czech Academy of Sciences Publication Activity Database

    Šimeček, I.; Rohlíček, Jan; Zahradnický, T.; Langr, D.

    2015-01-01

    Roč. 48, Feb (2015), 166-170 ISSN 0021-8898 Institutional support: RVO:68378271 Keywords : indexing powder diffraction * TREOR algorithm * GPGPU Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.720, year: 2014

  19. 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.

  20. In situ observation and neutron diffraction of NiTi powder sintering

    International Nuclear Information System (INIS)

    Chen, Gang; Liss, Klaus-Dieter; Cao, Peng

    2014-01-01

    This study investigated NiTi powder sintering behaviour from elemental powder mixtures of Ni/Ti and Ni/TiH 2 using in situ neutron diffraction and in situ scanning electron microscopy. The sintered porous alloys have open porosities ranging from 2.7% to 36.0%. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH 2 compact leads to less densification yet higher chemical homogenization only after high-temperature sintering. For the first time, direct evidence of the eutectoid phase transformation of NiTi at 620 °C is reported by in situ neutron diffraction. A comparative study of cyclic stress–strain behaviours of the porous NiTi alloys made from Ni/Ti and Ni/TiH 2 compacts indicate that the samples sintered from the Ni/TiH 2 compact exhibited a much higher porosity, larger pore size, lower fracture strength, lower close-to-overall porosity ratio and lower Young’s modulus. Instead of enhanced densification by the use of TiH 2 as reported in the literature, this study shows an adverse effect of TiH 2 on powder densification in NiTi

  1. 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.)

  2. 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

  3. Structural characterisation of 1- and 2-dimensional transition metal polymers using powder neutron diffraction

    International Nuclear Information System (INIS)

    James, M.

    1999-01-01

    Powder neutron diffraction provides an alternate technique for the structural study of transition metal polymers and finds utility over standard X-ray methods in two significant ways. Firstly, due to a different instrument geometry, preferred orientation effects are removed from the system. The second advantage gained by utilising neutrons is that H atoms in the sample contribute much more to the nuclear scattering of the diffraction profile - allowing their atomic position to be accurately determined. In X-ray diffraction studies, where H atoms typically account for only ∼3-5% of the scattering from the sample, it is essentially impossible to refine their position in the molecular structure. The structures of several transition metal polymers have been determined using neutrons from the HIFAR reactor at ANSTO and the Powder Diffractometers HRPD and MRPD, along with Rietveld refinement methods. The 1-dimensional polymer dibromobis(thiazole)nickel(II) illustrated in the paper is characteristic of these types of systems which are comprised of transition metal centres bridged by halogen atoms with pendant amine side groups

  4. Extending the reach of powder diffraction modelling by user defined macros

    CERN Document Server

    Scardi, Paolo

    2010-01-01

    The main focus of this special topic volume is the development and possibilities of the MACRO language within TOPAS, with a specific session dedicated to WPPM. The collection is presented here in the form of a ""macro tutorial"" for the benefit of the entire powder diffraction community. More than a collection of standard scientific papers, the contributions to this special issue provide methods, tutorials and practical suggestions and solutions for the proper use of TOPAS and WPPM in a number of applications; ranging from the most common to the most refined and specific cases.Readers will fin

  5. 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

  6. Parallel beam powder diffraction study on the A1C60 system (A=K, Rb)

    International Nuclear Information System (INIS)

    Faigel, G.; Tegze, M.; Bortel, G.; Forro, L.; Oszlanyi, G.; Stephens, P.W.

    1994-01-01

    We report x-ray powder diffraction studies on Rb x C 60 and K x C 60 . It is shown that at room temperature there exist stoichiometric compounds in the Rb x C 60 and K x C 60 systems at the x = 1 composition. Their equilibrium structures are pseudo body centered orthorhombic. The C 60 -C 60 intermolecular separation (9.1 A) is the shortest among the known alkali-fullerides. A first order phase transition is observed at about 380 K from the high temperature fcc phase to the room temperature orthorhombic phase. (orig.)

  7. 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 ...

  8. 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...

  9. A new energy-dispersive powder diffraction facility at the SRS

    International Nuclear Information System (INIS)

    Clark, S.M.

    1996-01-01

    A new energy-dispersive powder diffraction facility has been constructed on the 6 T wiggler beam line of the Daresbury Laboratory Synchrotron Radiation Source. This paper describes the facility, in particular the beam definition apparatus (front end), the detector positioning system (back end), a 10 000 kN loading frame and high pressure cell and the counting and control electronics. Some recent results are presented including a study of the compressibility of talc and the phase I→II transition of ammonium chloride. (orig.)

  10. 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

  11. Location of adsorbed species in NO-reduction catalysts by high resolution neutron powder diffraction

    International Nuclear Information System (INIS)

    Fowkes, A.J.; Rosseinsky, M.J.

    1999-01-01

    Complete text of publication follows. Catalysts containing copper ion exchanged into zeolites are attracting considerable attention due to their efficiency for both NO decomposition and the selective catalytic reduction of NO x in so-called lean-burn conditions in automotive exhausts. This presentation will describe the application of in-situ high resolution neutron powder diffraction to study active sites in a Cu-zeolite Y catalyst active for NO decomposition. The study under NO pressure reveals the location of two distinct copper sites for sorption. The influence of copper oxidation state on the structure of both the pristine and NO-loaded zeolites will be discussed. (author)

  12. Neutron powder diffraction and theory-aided structure refinement of rubidium and cesium ureate

    Energy Technology Data Exchange (ETDEWEB)

    Sterri, Kjersti B.; Deringer, Volker L.; Houben, Andreas; Jacobs, Philipp [RWTH Aachen Univ. (Germany). Inst. of Inorganic Chemistry; Kumar, Chogondahalli M.N. [Forschungszentrum Juelich GmbH, Juelich Centre for Neutron Science (JCNS), Outstation at SNS, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Oak Ridge National Laboratory, TN (United States). Chemical and Engineering Materials Div.; Dronskowski, Richard [RWTH Aachen Univ. (Germany). Inst. of Inorganic Chemistry; RWTH Aachen Univ. (Germany). Juelich-Aachen Research Alliance (JARA-HPC)

    2016-08-01

    Urea (CN{sub 2}H{sub 4}O) is a fundamental biomolecule whose derivatives are abundant throughout chemistry. Among the latter, rubidium ureate (RbCN{sub 2}H{sub 3}O) and its cesium analog (CsCN{sub 2}H{sub 3}O) have been described only very recently and form the first structurally characterized salts of deprotonated urea. Here, we report on a neutron diffraction study on the aforementioned alkaline-metal ureates, which affords the positions for all hydrogen atoms (including full anisotropic displacement tensors) and thus allows us to gain fundamental insights into the hydrogen-bonding networks in the title compounds. The structure refinements of the experimental neutron data proceeded successfully using starting parameters from ab initio simulations of atomic positions and anisotropic displacement parameters. Such joint experimental-theoretical refinement procedures promise significant practical potential in cases where complex solids (organic, organometallic, framework materials) are studied by powder diffraction.

  13. 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.

  14. Crystal structure solution of hydrides containing natEu from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Kohlmann, H.

    1999-01-01

    Complete text of publication follows. The location of hydrogen in crystal structures of metal hydrides usually requires neutron diffraction data. Some elements, however, show excessively high absorption cross sections, σ a , for neutrons, thus making this technique seemingly impractical. Therefore no complete, refined crystal structure data of europium hydrides (σ a ( nat Eu) = .4530 barns at λ = 179.8 pm [1]) have been reported so far. It is shown that the absorption can be reduced to a value reasonable for neutron diffraction experiments by taking advantage of the wavelength dependence of σ a combined with the use of annular samples at advanced diffractometers. Neutron powder diffraction data on several nat Eu containing deuterides suitable for the ab initio crystal structure solution and refinement have been taken at D20 and D4 (ILL, Grenoble). The crystal chemistry of these europium hydrides, among them the two new compounds EuMg 2 H 6 and EuMgH 4 [2], is discussed. (author) [1] V.F. Sears, Neutron News 1992, 3, 26-37.; [2] H. Kohlmann, F. Gingl, T. Hansen, K. Yvon, Angew. Chem. Int. Ed. Eng. 1999, 38, accepted

  15. 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)

  16. 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.

  17. PIXE analysis of powdered milk

    International Nuclear Information System (INIS)

    Hallak, A.B.

    1983-01-01

    An accelerator-based study, using proton-induced x-ray emission (PIXE) was performed on four full-cream and four half-cream brands of powdered milk commonly consumed in Jordan. The elements detected in the samples are S, Cl, K, Ca, Fe, Cu, Zn, Br and Rb. The significance of some of these elements is discussed from the viewpoint of nutrition and also their effect on milk processing and dairy technology. The standard reference milk sample, A-11, which is distributed by IAEA was also examined, and the results for trace elements detected are compared with the values certified by IAEA. (author)

  18. Diffraction analysis of the microstructure of materials

    CERN Document Server

    Scardi, Paolo

    2004-01-01

    Diffraction Analysis of the Microstructure of Materials provides an overview of diffraction methods applied to the analysis of the microstructure of materials. Since crystallite size and the presence of lattice defects have a decisive influence on the properties of many engineering materials, information about this microstructure is of vital importance in developing and assessing materials for practical applications. The most powerful and usually non-destructive evaluation techniques available are X-ray and neutron diffraction. The book details, among other things, diffraction-line broadening methods for determining crystallite size and atomic-scale strain due, e.g. to dislocations, and methods for the analysis of residual (macroscale) stress. The book assumes only a basic knowledge of solid-state physics and supplies readers sufficient information to apply the methods themselves.

  19. Neutron diffraction studies on GdB{sub 6} and TbB{sub 6} powders

    Energy Technology Data Exchange (ETDEWEB)

    Luca, S.E.; Amara, M.; Galera, R.M.; Givord, F.; Granovsky, S.; Isnard, O.; Beneu, B

    2004-07-15

    We report here the first powder neutron diffraction study of GdB{sub 6} and TbB{sub 6}. GdB{sub 6} and TbB{sub 6} order antiferromagnetically at 15 and 21 K, respectively. In both compounds the transition at T{sub N} is of the first order. Moreover GdB{sub 6} presents a second spontaneous magnetic transition at T{sup *}=8 K. The present study shows that, in both compounds, the magnetic propagation vectors belong to the <((1)/(4)) ((1)/(4)) ((1)/(2))> star and that the direction of the magnetic moment is perpendicular to the ((1)/(2)) component of the wave-vector in GdB{sub 6}, while in TbB{sub 6} the moment is parallel to it. The deduced low-temperature values of the magnetic moments agree with those of the respective rare-earth trivalent ions.

  20. Neutron diffraction studies on GdB6 and TbB6 powders

    International Nuclear Information System (INIS)

    Luca, S.E.; Amara, M.; Galera, R.M.; Givord, F.; Granovsky, S.; Isnard, O.; Beneu, B.

    2004-01-01

    We report here the first powder neutron diffraction study of GdB 6 and TbB 6 . GdB 6 and TbB 6 order antiferromagnetically at 15 and 21 K, respectively. In both compounds the transition at T N is of the first order. Moreover GdB 6 presents a second spontaneous magnetic transition at T * =8 K. The present study shows that, in both compounds, the magnetic propagation vectors belong to the star and that the direction of the magnetic moment is perpendicular to the ((1)/(2)) component of the wave-vector in GdB 6 , while in TbB 6 the moment is parallel to it. The deduced low-temperature values of the magnetic moments agree with those of the respective rare-earth trivalent ions

  1. Phase transitions in Rb2UBr6 observed by neutron powder diffraction

    International Nuclear Information System (INIS)

    Maletka, K.; Ressouche, E.; Tellgren, R.; Delaplane, R.; Szczepaniak, W.; Rycerz, L.; Zablocka-Malecka, M.

    1997-01-01

    The behaviour of the Rb 2 UBr 6 ionic conductor is studied as a function of the temperature by neutron powder diffraction. The low- room and high temperature structures have been determined. At low temperature range 4.2-80 K the compound crystallizes in a monoclinic unit cell with P2 1 /c space group. Among 80 and 853 K the compound crystallizes in a tetragonal unit cell with space group P4/mnc. At 300 K the lattice constants are; a = b 7,745(1), c = 11.064(1) A. At the temperature range 853-960 K is observed the trigonal phase with P-3m1 space group. Above the phase transitions occurring at 960 K the compound crystallizes in the cubic unit cell with Fm3m space group. (author)

  2. 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...

  3. A powder neutron diffraction study of stoichiometric silver beta alumina at 4.2 K

    International Nuclear Information System (INIS)

    Newsam, J.M.; Tofield, B.C.

    1980-10-01

    The low-temperature structure of stoichiometric silver beta alumina, AgAl 11 O 17 , is described for the first time. A powder neutron diffraction study at 4.2 K reveals that there is a single three-fold silver location of unit occupancy in each mirror plane. The silver site lies between the mid-oxygen and Beevers-Ross positions where the Ag-O contact distances can be minimised. The Ag-O interactions, in particular the cooperative movement of the spacer oxygens, are responsible for the superlattice which has been described previously. The Beevers-Ross, anti-Beevers-Ross and interstitial aluminium sites are vacant and the c-axis constant is expanded relative to the non-stoichiometric parent. (author)

  4. 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.

  5. 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

  6. Diffraction analysis of customized illumination technique

    Science.gov (United States)

    Lim, Chang-Moon; Kim, Seo-Min; Eom, Tae-Seung; Moon, Seung Chan; Shin, Ki S.

    2004-05-01

    Various enhancement techniques such as alternating PSM, chrome-less phase lithography, double exposure, etc. have been considered as driving forces to lead the production k1 factor towards below 0.35. Among them, a layer specific optimization of illumination mode, so-called customized illumination technique receives deep attentions from lithographers recently. A new approach for illumination customization based on diffraction spectrum analysis is suggested in this paper. Illumination pupil is divided into various diffraction domains by comparing the similarity of the confined diffraction spectrum. Singular imaging property of individual diffraction domain makes it easier to build and understand the customized illumination shape. By comparing the goodness of image in each domain, it was possible to achieve the customized shape of illumination. With the help from this technique, it was found that the layout change would not gives the change in the shape of customized illumination mode.

  7. Bragg's Law diffraction simulations for electron backscatter diffraction analysis

    International Nuclear Information System (INIS)

    Kacher, Josh; Landon, Colin; Adams, Brent L.; Fullwood, David

    2009-01-01

    In 2006, Angus Wilkinson introduced a cross-correlation-based electron backscatter diffraction (EBSD) texture analysis system capable of measuring lattice rotations and elastic strains to high resolution. A variation of the cross-correlation method is introduced using Bragg's Law-based simulated EBSD patterns as strain free reference patterns that facilitates the use of the cross-correlation method with polycrystalline materials. The lattice state is found by comparing simulated patterns to collected patterns at a number of regions on the pattern using the cross-correlation function and calculating the deformation from the measured shifts of each region. A new pattern can be simulated at the deformed state, and the process can be iterated a number of times to converge on the absolute lattice state. By analyzing an iteratively rotated single crystal silicon sample and recovering the rotation, this method is shown to have an angular resolution of ∼0.04 o and an elastic strain resolution of ∼7e-4. As an example of applications, elastic strain and curvature measurements are used to estimate the dislocation density in a single grain of a compressed polycrystalline Mg-based AZ91 alloy.

  8. Crystal structures of new cuprates containing CO3 analyzed by the Rietveld method of neutron powder diffraction

    International Nuclear Information System (INIS)

    Miyazaki, Y.; Yamane, H.; Kajitani, T.; Hiraga, K.; Hirai, T.; Morii, Y.; Funahashi, S.

    1993-01-01

    New compounds containing CO 3 groups, Sr 2 CuO 2 (CO 3 ), (C 0.4 Cu 0.6 )Sr 2 (Y 0.86 Sr 0.14 )Cu 2 O 7 and (C 0.35 Cu 0.65 )Sr 2 (Y 0.73 Ce 0.27 ) 2 Cu 2 O 9 , were prepared as stable phases at 1273-1303 K in a flowing gas of O 2 -CO 2 . The crystal structures of these compounds were refined by means of the Rietveld analysis for neutron powder diffraction data collected using a high resolution powder diffractometer (HRPD) in the JRR-3M reactor hall of the Japan Atomic Energy Research Institute (JAERI). Positions of CO 3 groups were satisfactorily determined. The distances of C-O bonds in the CO 3 groups were around 1.3A and the O-C-O angles were almost equal to the ideal bond angle of 120deg. (author)

  9. Quantitative phase analysis by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Chang Hee; Song, Su Ho; Lee, Jin Ho; Shim, Hae Seop [Korea Atomic Energy Research Institute, Taejon (Korea)

    1999-06-01

    This study is to apply quantitative phase analysis (QPA) by neutron diffraction to the round robin samples provided by the International Union of Crystallography(IUCr). We measured neutron diffraction patterns for mixed samples which have several different weight percentages and their unique characteristic features. Neutron diffraction method has been known to be superior to its complementary methods such as X-ray or Synchrotron, but it is still accepted as highly reliable under limited conditions or samples. Neutron diffraction has strong capability especially on oxides due to its scattering cross-section of the oxygen and it can become a more strong tool for analysis on the industrial materials with this quantitative phase analysis techniques. By doing this study, we hope not only to do one of instrument performance tests on our HRPD but also to improve our ability on the analysis of neutron diffraction data by comparing our QPA results with others from any advanced reactor facilities. 14 refs., 4 figs., 6 tabs. (Author)

  10. 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

  11. Reactor applications of quantitative diffraction analysis

    International Nuclear Information System (INIS)

    Feguson, I.F.

    1976-09-01

    Current work in quantitative diffraction analysis was presented under the main headings of: thermal systems, fast reactor systems, SGHWR applications and irradiation damage. Preliminary results are included on a comparison of various new instrumental methods of boron analysis as well as preliminary new results on Zircaloy corrosion, and materials transfer in liquid sodium. (author)

  12. Simvastatin: structure solution of two new low-temperature phases from synchrotron powder diffraction and ss-NMR

    Czech Academy of Sciences Publication Activity Database

    Hušák, M.; Kratochvíl, B.; Jegorov, A.; Brus, Jiří; Maixner, J.; Rohlíček, J.

    2010-01-01

    Roč. 21, č. 3 (2010), s. 511-518 ISSN 1040-0400 R&D Projects: GA AV ČR IAA400500602; GA MŠk 2B08021 Institutional research plan: CEZ:AV0Z40500505 Keywords : crystal structure * simvastatin * powder diffraction Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.727, year: 2010

  13. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D)

    DEFF Research Database (Denmark)

    van de Streek, Jacco; Neumann, Marcus A

    2014-01-01

    In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published...

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

    International Nuclear Information System (INIS)

    Tanaka, M; Katsuya, Y; Matsushita, Y

    2013-01-01

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

  15. An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

    Directory of Open Access Journals (Sweden)

    Gang Chen

    2015-04-01

    Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

  16. 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.

  17. 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)

  18. 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.

  19. Neutron powder diffraction at a pulsed neutron source: a study of resolution effects

    International Nuclear Information System (INIS)

    Faber, J. Jr.; Hitterman, R.L.

    1985-11-01

    The General Purpose Powder Diffractometer (GPPD), a high resolution (Δd/d = 0.002) time-of-flight instrument, exhibits a resolution function that is almost independent of d-spacing. Some of the special properties of time-of-flight scattering data obtained at a pulsed neutron source will be discussed. A method is described that transforms wavelength dependent data, obtained at a pulsed neutron source, so that standard structural least-squares analyses can be applied. Several criteria are given to show when these techniques are useful in time-of-flight data analysis. 14 refs., 6 figs., 1 tab

  20. Structure solution from powder neutron and x-ray diffraction data: getting the best of both worlds

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    Full text: Powder diffraction methods have traditionally been used in three main areas: phase identification and quantification, lattice parameter determination and structure refinement. Until recently structure solution has been the almost exclusive domain of single crystal diffraction methods, predominantly using x-rays. The increasing use of synchrotron and neutron sources, and the unrelenting advances in computing hardware and software means that powder methods are challenging single crystal methods as a practical method for structure solution, especially when single crystal method can not be applied. It is known that structural refinements from a known starting structure using combined X-ray and neutron data sets are capable of providing highly accurate structures. Likewise, using combined x-ray and neutron powder diffraction data in the structure solution process should also be a powerful technique, although to date no one is pursuing this methodology. This paper present examples of solutions to the problem. Namely we are using high resolution powder X-ray and neutron methods to solve the structures of molecular materials and minerals, then refining the structures using both sets of data. In this way we exploit the advantages of both methods while minimising the disadvantages. We present our solution for a small amino acid structure, a metalorganic and a mineral structure

  1. Spectral analysis of allogeneic hydroxyapatite powders

    Science.gov (United States)

    Timchenko, P. E.; Timchenko, E. V.; Pisareva, E. V.; Vlasov, M. Yu; Red'kin, N. A.; Frolov, O. O.

    2017-01-01

    In this paper we discuss the application of Raman spectroscopy to the in vitro analysis of the hydroxyapatite powder samples produced from different types of animal bone tissue during demineralization process at various acid concentrations and exposure durations. The derivation of the Raman spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. Were experimentally found spectral features of hydroxyapatite, based on analysis of the line amplitude at wave numbers 950-965 cm-1 ((PO4)3- (ν1) vibration) and 1065-1075 cm-1 ((CO3)2-(ν1) B-type replacement). Control of physicochemical properties of hydroxyapatite was carried out by Raman spectroscopy. Research results are compared with an infrared Fourier spectroscopy.

  2. Spectral analysis of allogeneic hydroxyapatite powders

    International Nuclear Information System (INIS)

    Timchenko, P E; Timchenko, E V; Pisareva, E V; Vlasov, M Yu; Red’kin, N A; Frolov, O O

    2017-01-01

    In this paper we discuss the application of Raman spectroscopy to the in vitro analysis of the hydroxyapatite powder samples produced from different types of animal bone tissue during demineralization process at various acid concentrations and exposure durations. The derivation of the Raman spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. Were experimentally found spectral features of hydroxyapatite, based on analysis of the line amplitude at wave numbers 950-965 cm -1 ((PO 4 ) 3- (ν 1 ) vibration) and 1065-1075 cm -1 ((CO 3 ) 2- (ν 1 ) B-type replacement). Control of physicochemical properties of hydroxyapatite was carried out by Raman spectroscopy. Research results are compared with an infrared Fourier spectroscopy. (paper)

  3. The high-resolution powder diffraction station PO DI STA is ''running'' at Adone

    International Nuclear Information System (INIS)

    Burattini, E.; Simeoni, S.; Cappuccio, G.; Maistrelli, P.

    1992-01-01

    At the end of February 1991, a ''triple-axis'' high-resolution diffractometer for on powder sample measurements with synchrotron radiation was put in operation on the Adone wiggler line BX1 at Frascati. The diffractometer is based on a Seifert goniometer, designed according to our specifications. During the project, particular attention was paid in assuring the highest reliability together with great flexibility in the use. In fact, the diffractometer can also be used in a ''medium resolution'' configuration. For preliminary alignment and data collection, it is possible to operate with a traditional x-ray tube, too. The alignment procedure of the diffractometer to the x-ray beam is very easy. Powder samples can be measured both on the flat holder and on the capillary. An IBM PC computer is used for the instrument actuation and preliminary on-line data collection, while a large software package has been developed for the data analysis performed by a Macintosh IIcx. The instrument performance has been tested with a standard Si sample and quartz and Ni oxide samples. For the two possible resolution configurations, a test on a NiO sample gave FWHM values of 0.16 degree and 0.04 degree, respectively, for the [012] peak

  4. A neutron powder diffraction study of deuterated α-resorcinol: a test of profile refinement using TLS constraints

    International Nuclear Information System (INIS)

    Bacon, G.E.; Lisher, E.J.

    1979-01-01

    Constrained TL, TLX and TLS refinements have been used, with the powder-profile method, in the analysis of accurate neutron powder data for deuterated α-resorcinol at room temperature. There is good agreement between the translational and librational parameters derived from the TL refinement and those obtained from an equivalent analysis of accurate single-crystal neutron measurements. The fine details of the benzene ring are lost in the powder analysis, but the molecular orientation and the OH bond angles are in good agreement with the single-crystal values. No significant improvement could be found in the powder fit by applying the full TLS theory and, therefore, the approximate TLX model appears to be adequate for powder data. (Auth.)

  5. The crystal structures and powder diffraction patterns of the uranium tellurides

    Energy Technology Data Exchange (ETDEWEB)

    Snyder, R.L. (State Univ. of New York, Alfred, NY (USA). Inst. of Ceramic Superconductivity); Nichols, M.C.; Boehme, D.R. (Sandia National Labs., Livermore, CA (USA))

    1990-10-03

    A critical review of all of the reported structures and powder diffraction patterns in the uranium telluride system has been undertaken. Structures that are correct: Cubic -- UTe: no experimental pattern exists. Retain calculated 15--865. Cubic --U{sub 3}Te{sub 4}: retain the poor quality 12--610 but adopt the pattern calculated here. Cubic U{sub 2}Te{sub 3}: no experimental pattern exists. Adopt pattern calculated here. Orthorhombic UTe{sub 2}: Adopt the new pattern of Boehme et al. Monoclinic {alpha}UTe{sub 3} Adopt the new pattern of Boehme et al. Monoclinic {alpha}UTe{sub 3} Adopt the new pattern of Boehme et al. Orthorhombic {beta}UTe{sub 3}: Adopt pattern calculated here. Orthorhombic UTe{sub 5}: Adopt the new pattern of Boehme et al. Structures in need of refinement: Orthorhombic U{sub 2}Te{sub 3}:Adopt pattern calculated here over 34--807. Hexagonal U{sub 7}Te{sub 12}: Adopt pattern calculated here but retain 24--1368. Orthorhombic UTe{sub 1.78}: Adopt pattern calculated here and retain our modified 21--1404 reported for U{sub 4}Te{sub 7}. Orthorhombic UTe{sub 2.5}: Adopt pattern calculated here. Orthorhombic UTe{sub 3.4}: Accept recent pattern of Boehme et al. Phases for which no structures or reliable patterns exist: Orthorhombic U{sub 3}Te{sub 4}: no published pattern. Tetragonal U{sub 3}Te{sub 5}: three patterns 21--1407, 34--766 and 34--896 exit but all are of very poor quality. Phases which probably do not exist: Tetragonal UTe{sub 1.78}, Tetragonal UTe{sub 2}, Cubic UTe{sub 2} U{sub 3}Te{sub 7}(21--1402), U{sub 3}Te{sub 8}(21--1406).

  6. 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 ...

  7. The role of iron in tetrahedrite and tennantite determined by Rietveld refinement of neutron powder diffraction data

    DEFF Research Database (Denmark)

    Andreasen, Jens Wenzel; Makovicky, Emil; Lebech, Bente

    2008-01-01

    Rietveld refinement of neutron powder diffraction data on four samples of synthetic, iron-bearing tetrahedrite (Cu12-xFexSb4S13) with x = 0.28, 0.69, 0.91, 2.19 and four samples of synthetic tennantite (Cu12-xFexAs4S13) with x = 0.33, 0.38, 0.86, 1.5 indicate unambiguously that iron is incorporated...

  8. 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

  9. Crystal structure refinement of α-Si3N4 using synchrotron radiation powder diffraction data: unbiased refinement strategy

    International Nuclear Information System (INIS)

    Toraya, H.

    2000-01-01

    The crystal structure of α-silicon nitride (Si 3 N 4 ) was refined by the Rietveld method using synchrotron radiation powder diffraction data (wavelength = 1.2 A) collected at station BL-4B2 in the photon factory. A refinement procedure that adopted a new weight function, w = 1/Y o e (Y o is the observed profile intensity and e ≅ 2), for the least-squares fitting [Toraya (1998). J. Appl. Cryst. 31, 333-343] was studied. The most reasonable structural parameters were obtained with e = 1.7. Crystal data of α-Si 3 N 4 : trigonal, P31c, a = 7.75193 (3), c = 5.61949 (4) A, V = 292.447 (3) A 3 , Z = 4; R p = 5.08, R wp = 6.50, R B = 3.36, R F = 2.26%. The following five factors are considered equally important for deriving accurate structural parameters from powder diffraction data: (i) sufficiently large sin θ/λ range of >0.8 A -1 ; (ii) adequate counting statistics; (iii) correct profile model; (iv) proper weighting on observations to give a uniform distribution of the mean weighted squared residuals; (v) high-angular-resolution powder diffraction data. (orig.)

  10. Laser diffraction analysis of colloidal crystals

    Energy Technology Data Exchange (ETDEWEB)

    Sogami, Ikuo S.; Shinohara, Tadatomi; Yoshiyama, Tsuyoshi [Kyoto Sangyo Univ., Department of Physics, Kyoto (Japan)

    2001-10-01

    Laser diffraction analysis is made on crystallization in salt-free aqueous suspensions of highly-charged colloidal particles for semi-dilute specimens of concentration 0.1-10.0 vol%. Kossel diffraction patterns which represent faithfully accurate information on lattice symmetries in the suspensions enable us to investigate the time evolution of colloidal crystals. The results show that the crystallization proceeds by way of the following intermediate phase transitions: two-dimensional hcp structure {yields} random layer structure {yields} layer structure with one sliding degree of freedom {yields} stacking disorder structure {yields} stacking structure with multivariant periodicity {yields} fcc twin structure with twin plane (111) {yields} normal fcc structure {yields} bcc twin structure with twin plane (11-bar2) or (1-bar12) {yields} normal bcc structure. For concentrated suspensions (>2 vol %), the phase transition ceases to proceed at the normal fcc structure. (author)

  11. Laser diffraction analysis of colloidal crystals

    International Nuclear Information System (INIS)

    Sogami, Ikuo S.; Shinohara, Tadatomi; Yoshiyama, Tsuyoshi

    2001-01-01

    Laser diffraction analysis is made on crystallization in salt-free aqueous suspensions of highly-charged colloidal particles for semi-dilute specimens of concentration 0.1-10.0 vol%. Kossel diffraction patterns which represent faithfully accurate information on lattice symmetries in the suspensions enable us to investigate the time evolution of colloidal crystals. The results show that the crystallization proceeds by way of the following intermediate phase transitions: two-dimensional hcp structure → random layer structure → layer structure with one sliding degree of freedom → stacking disorder structure → stacking structure with multivariant periodicity → fcc twin structure with twin plane (111) → normal fcc structure → bcc twin structure with twin plane (11-bar2) or (1-bar12) → normal bcc structure. For concentrated suspensions (>2 vol %), the phase transition ceases to proceed at the normal fcc structure. (author)

  12. Geometrically frustrated magnetic structures of the heavy-fermion compound CePdAl studied by powder neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Doenni, A.; Fischer, P.; Zolliker, M. [Laboratory for Neutron Scattering, ETH Zuerich and Paul Scherrer Institute, CH-5232 Villigen PSI (Switzerland); Ehlers, G.; Maletta, H. [Hahn Meitner Institute Berlin, Glienicker Strasse 100, D-14092 Berlin (Germany); Kitazawa, H. [National Research Institute for Metals, Tsukuba, Ibaraki 305 (Japan)

    1996-12-09

    The heavy-fermion compound CePdAl with ZrNiAl-type crystal structure (hexagonal space group P6-bar2m) was investigated by powder neutron diffraction. The triangular coordination symmetry of magnetic Ce atoms on site 3f gives rise to geometrical frustration. CePdAl orders below T{sub N} = 2.7 K with an incommensurate antiferromagnetic propagation vector k=[1/2, 0, {tau}], {tau} approx. 0.35, and a longitudinal sine-wave (LSW) modulated spin arrangement. Magnetically ordered moments at Ce(1) and Ce(3) coexist with frustrated disordered moments at Ce(2). The experimentally determined magnetic structure is in agreement with group theoretical symmetry analysis considerations, calculated by the program MODY, which confirm that for Ce(2) an ordered magnetic moment parallel to the magnetically easy c-axis is forbidden by symmetry. Further low-temperature experiments give evidence for a second magnetic phase transition in CePdAl between 0.6 and 1.3 K. Magnetic structures of CePdAl are compared with those of the isostructural compound TbNiAl, where a non-zero ordered magnetic moment for the geometrically frustrated Tb(2) atoms is allowed by symmetry. (author)

  13. 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)

  14. High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

    Science.gov (United States)

    Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

    2013-12-01

    We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

  15. Structural study of CaMn_1_−_xMo_xO_3 (0.08 ≤ x ≤ 0.12) system by neutron powder diffraction

    International Nuclear Information System (INIS)

    Supelano, G.I.; Parra Vargas, C.A.; Barón-González, A.J.; Sarmiento Santos, A.; Frontera, C.

    2016-01-01

    Neutron powder diffraction experiments and magnetic measurements in polycrystalline CaMn_1_−_xMo_xO_3 (x = 0.08, 0.10, 0.12) point towards a possible charge and orbital order in this system. The analysis of structural and magnetic data show that the samples present structural phase transformation from Pnma to P2_1/m space group and the system has a C-type antiferromagnetic configuration at low temperature. A detailed analysis of the bond distances signals a small Jahn-Teller distortion of only one (x = 0.08) or of the two Mn ions (x = 0.10, 0.12). We identify the partially occupied e_g orbitals and this explains the C-type magnetic structure. - Highlights: • CaMn_1_−_xMo_xO_3 (x = 0.08, 0.10, 0.12) is investigated by neutron powder diffraction. • Analysis of individual Mn-O distances demonstrates the apparition of orbital order. • By symmetry analysis, we find that the low temperature magnetic structure is C-type. • Magnetic interactions foreseen by the orbital order explain the magnetic structure.

  16. 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

  17. 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.

  18. 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

  19. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D)

    International Nuclear Information System (INIS)

    Streek, Jacco van de; Neumann, Marcus A.

    2014-01-01

    The accuracy of 215 experimental organic crystal structures from powder diffraction data is validated against a dispersion-corrected density functional theory method. In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom

  20. 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

  1. Structural study of Sr{sub 2}CuO{sub 3+delta} by neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Shimakawa, Y. [NEC Corp., Tsukuba (Japan). Fundamental Research Labs.; Jorgensen, J.D.; Mitchell, J.F.; Hunter, B.A. [Argonne National Lab., IL (United States); Shaked, S. [Israel Atomic Energy Commission, Beersheba (Israel). Nuclear Research Center-Negev][Ben-Gurion Univ. of the Negev, Beersheba (Israel). Dept. of Physics; Hinks, D.G.; Hitterman, R.L. [Argonne National Lab., IL (United States); Hiroi, Z.; Takano, M. [Kyoto Univ., Uji (Japan). Inst. for Chemical Research

    1996-11-01

    Average crystal structures of superconducting Sr{sub 2}CuO{sub 3+{delta}} synthesized at ambient pressure from a hydroxometallate precursor were refined from neutron powder diffraction data. A simplified model was used to fit the modulated superstructures. Both compounds have an oxygen deficient La{sub 2}CuO{sub 4}-type tetragonal T structure with O vacancies located in the CuO{sub 2} planes, not in the Sr{sub 2}O{sub 2} layers. This raises important questions about the superconductivity in Sr{sub 2}CuO{sub 3+{delta}} reported to be a 70 K superconductor.

  2. 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.)

  3. 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...

  4. 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)

  5. Physcio chemical analysis of browning inhibitors treated solanum turberosum powder

    International Nuclear Information System (INIS)

    Alizai, M.N.K.; Abid, H.

    2008-01-01

    White potatoes (Solanum turberosum) were procured from agriculture Research Institute Tarnab Farm Peshawar to use for the preparation of potato powder. The process involves sorting. Washing, peeling slicing, blanching, treating with poly phenol oxidase inhibitors, dehydration, grinding and packing. All these parameters used in process were standardized. Chemical analysis of fresh potato and potato powder were carried out. Microbiological examination, functional properties and storage life studies of the potato powder were also performed. The product prepared by drying in cabinet dryer at 55 C for 7 hours was off white colour potatoes chips which was grinded to make off white potato powder. The potato powder possessed taste and texture. (author)

  6. 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.

  7. Structure of orthorhombic SrZrO/sub 3/ by neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ahtee, A; Ahtee, M [Helsinki Univ. (Finland). Dept. of Physics; Glazer, A M [Cambridge Univ. (UK). Cavendish Lab.; Hewat, A W [Institut Max von Laue - Paul Langevin, 38 - Grenoble (France)

    1976-12-15

    The room-temperature structure of SrZrO/sub 3/ has been established by neutron powder-profile refinement. The space group is Pbnm and SrZrO/sub 3/ is isostructural with other perovskites, such as CaTiO/sub 3/.

  8. High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal–organic framework material HKUST-1

    Energy Technology Data Exchange (ETDEWEB)

    Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I.F. [ISIS Facility, Rutherford Appleton Laboratory, Harwell Science and Innovation Campus, Didcot, OX11 0QX (United Kingdom); Millange, Franck [Institut Lavoisier Versailles (CNRS UMR 8180), Université de Versailles, 78035 Versailles (France); Walton, Richard I., E-mail: r.i.walton@warwick.ac.uk [Department of Chemistry, University of Warwick, CV4 7AL, Coventry (United Kingdom)

    2013-12-12

    Highlights: • Binding sites for dihydrogen in a metal–organic framework have been identified. • The combination of diffraction and spectroscopy shows competitive filling of various adsorption sites. • Inelastic neutron scattering over wide-momentum transfer reveals new models for hydrogen-framework interactions. - Abstract: We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal–organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal–organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

  9. High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal–organic framework material HKUST-1

    International Nuclear Information System (INIS)

    Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I.F.; Millange, Franck; Walton, Richard I.

    2013-01-01

    Highlights: • Binding sites for dihydrogen in a metal–organic framework have been identified. • The combination of diffraction and spectroscopy shows competitive filling of various adsorption sites. • Inelastic neutron scattering over wide-momentum transfer reveals new models for hydrogen-framework interactions. - Abstract: We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal–organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal–organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host

  10. A novel isomorphic phase transition in β-pyrochlore oxide KOs2O6: a study using high resolution neutron powder diffraction

    Science.gov (United States)

    Sasai, Kenzo; Kofu, Maiko; Ibberson, Richard M.; Hirota, Kazuma; Yamaura, Jun-ichi; Hiroi, Zenji; Yamamuro, Osamu

    2010-01-01

    We have carried out adiabatic calorimetric and neutron powder diffraction experiments on the β-pyrochlore oxide KOs2O6, which has a superconducting transition at Tc = 9.6 K and another novel transition at Tp = 7.6 K. A characteristic feature of this compound is that the K ions exhibit rattling vibrations in the cages formed by O atoms even at very low temperatures. The temperature and entropy of the Tp transition is in good agreement with previous data measured using a heat relaxation method, indicating that the present sample is of high purity and the transition entropy, 0.296 J K-1 mol-1, does not depend on the calorimetric method used. The neutron powder diffraction data show no peak splitting nor extra peaks over the temperature range between 2 and 295 K, suggesting that the Tp transition is a rather unusual isomorphic transition. Rietveld analysis revealed an anomalous expansion of the lattice and a deformation of the O atom cage below 7.6 K. In the low-temperature phase, the distribution of scattering density corresponding to the K ions becomes broader whilst maintaining its maximum at the cage center. Based on these findings, we suggest that the Tp transition is due to the expansion of the cage volume and cooperative condensation of the K ions into the ground state of the rattling motion.

  11. Evidence for existence of functional monoclinic phase in sodium niobate based solid solution by powder neutron diffraction

    Science.gov (United States)

    Mishra, S. K.; Jauhari, Mrinal; Mittal, R.; Krishna, P. S. R.; Reddy, V. R.; Chaplot, S. L.

    2018-04-01

    We have carried out systematic temperature-dependent neutron diffraction measurements in conjunction with dielectric spectroscopy from 6 to 300 K for sodium niobate based compounds (1-x) NaNbO3-xBaTiO3 (NNBTx). The dielectric constant is measured as a function of both temperature and frequency. It shows an anomaly at different temperatures in cooling and heating cycles and exhibits a large thermal hysteresis of ˜150 K for the composition x = 0.03. The dielectric constant is found to be dispersive in nature and suggests a relaxor ferroelectric behavior. In order to explore structural changes as a function of temperature, we analyzed the powder neutron diffraction data for the compositions x = 0.03 and 0.05. Drastic changes are observed in the powder profiles near 2θ ˜ 30.6°, 32.1°, and 34.6° in the diffraction pattern below 200 K during cooling and above 190 K in heating cycles, respectively. The disappearance of superlattice reflection and splitting in main perovskite peaks provide a signature for structural phase transition. We observed stabilization of a monoclinic phase (Cc) at low temperature. This monoclinic phase is believed to provide a flexible polarization rotation and considered to be directly linked to the high performance piezoelectricity in materials. The thermal hysteresis for composition x = 0.03 is larger than that for x = 0.05. This suggests that the addition of BaTiO3 to NaNbO3 suppresses the thermal hysteresis. It is also observed that the structural phase transition temperature decreases upon increasing the dopant concentration.

  12. Neutron diffraction measurements of residual stress in a powder metallurgy component

    International Nuclear Information System (INIS)

    Schneider, L.C.R.; Hainsworth, S.V.; Cocks, A.C.F.; Fitzpatrick, M.E.

    2005-01-01

    Residual stresses in a typical industrial green component were determined using neutron diffraction. The measured residual stresses were found to correlate with cross-sectional variations. Residual stress at the edge of the compact in contact with the die wall during compaction reached up to +80 MPa (tension) and -100 MPa (compression)

  13. The magnetic structure of GdNi2B2C investigated by neutron powder diffraction

    International Nuclear Information System (INIS)

    Barcza, A.; Rotter, M.; Doerr, M.; Beuneu, B.

    2005-01-01

    Full text: The group of ReT 2 B 2 C (Re=rare earth, T=transition metal) shows a very interesting interplay between magnetism and superconductivity due to the rare earth metals. In this work the magnetism of GdNi 2 B 2 C was studied with neutron diffraction. Previous investigations with x-ray diffraction methods have determined the crystal structure as a body centered tetragonal structure (I 4/mmm). Hot neutrons were used for the diffraction experiment, because the absorption cross section of Gd is significantly smaller for short wavelengths. The investigated compound orders magnetically at TN=19.5 K, and so the experiment was carried out at two temperatures, namely 30 K and 2.2 K. The results show a incommensurate spin structure with a propagation vector of (0.55 0 0). To confirm this results additional simulations of the spin structure were done based on the Standard Model of rare earth magnetism. A neutron diffraction pattern was calculated using the McPhase program package and is compared to the experimental data. (author)

  14. Quantitative determination of amorphous content in ceramic materials using x-ray powder diffraction

    International Nuclear Information System (INIS)

    Kuchinski, M.A.; Hubbard, C.R.

    1988-01-01

    A quantitative technique which employs a modified method of additions approach to analyze for low amorphous content in crystalline matrices was developed and tested. Known amounts of amorphous material are added to the starting powder. The method uses the ratio of a measure of the intensity of the amorphous phase corrected for background to the background corrected intensity of a reference line from a crystalline phase. The amorphous spiking phase must be close in composition to the amorphous phase existing in the analyte. A critical step of the method is to correctly establish the background intensity. A completely crystalline material of similar scattering power was used to establish background intensity

  15. 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/

  16. 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.

  17. 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

  18. 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.)

  19. 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.

  20. Structures of Bi14WO24 and Bi14MoO24 from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Ling, C.D.; Withers, R.L.; Thompson, J.G.; Schmid, S.

    1999-01-01

    The (isomorphous) structures of Bi 14 WO 24 , tetradecabismuth tungsten tetracosaoxide, and Bi 14 MoO 24 , tetradecabismuth molybdenum tetracosaoxide, have been solved and refined using neutron powder diffraction data in the space group I4/m. The metal-atom array is fully ordered in terms of composition, and in terms of atomic positions deviates only slightly from a fluorite-type δ-Bi 2 O 3 -related parent structure. Three independent O-atom sites (accounting for 70 out of 78 O atoms in the unit cell) are also very close to fluorite-type parent positions. The remaining two O-atom sites, which coordinate W, exhibit partial occupancies and displacive disorder, neither of which could be better modelled by lowering of symmetry. The W site is coordinated by four O atoms in highly distorted tetrahedral coordination, the tetrahedron necessarily being orientationally disordered on that site. Nonetheless, the structure appears to be chemically reasonable. (orig.)

  1. Neutron powder diffraction study of nuclear and magnetic structures of oxidized and reduced YBa2Fe3O8+w

    International Nuclear Information System (INIS)

    Karen, P.; Kjekshus, A.; Huang, Q.; Karen, V.L.; Lynn, J.W.; Rosov, N.; Natali Sora, I.; Santoro, A.

    2003-01-01

    YBa 2 Fe 3 O 8+w has been investigated by neutron powder diffraction as function of temperature and oxygen nonstoichiometry close to the limits of the homogeneity range, -0.24 0) in the structural layers of Y, or by creating oxygen vacancies (w 2 Cu 3 O 6+w' upon oxidation. The effects of nonstoichiometry on these related crystal structures are discussed in terms of bond-valence sums. The cooperative magnetic structure for all compositions is based on a larger cell related to the nuclear cell by the transformation matrix (11-bar0/110/002), having orthorhombic symmetry when the nuclear structure is tetragonal and monoclinic symmetry when the nuclear structure is orthorhombic. The iron moments are coupled antiferromagnetically in all three directions, the Neel temperature is almost constant as a function of w (T N ∼660 K), and so is also the low-temperature saturation moment μ AF ∼4.0μ B

  2. 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.

  3. About some practical aspects of X-ray diffraction : From single crystal to powders

    Energy Technology Data Exchange (ETDEWEB)

    Giacovazzo, C [Bari Univ. (Italy). Dip. Geomineralogico

    1996-09-01

    An ideal polycrystalline material or power is an ensemble of a very large number of randomly oriented crystallites. It is shown the effect that this random orientation has on the diffraction of a specimen assumed to contain only one reciprocal lattice node. The most remarkable difference with the single-crystal case is that now must think of scattering vectors not as lying on discrete nodes of reciprocal lattice vectors, the distances from the single-crystal reciprocal lattice nodes to the origin of reciprocal space.

  4. About some practical aspects of X-ray diffraction : From single crystal to powders

    International Nuclear Information System (INIS)

    Giacovazzo, C.

    1996-01-01

    An ideal polycrystalline material or power is an ensemble of a very large number of randomly oriented crystallites. It is shown the effect that this random orientation has on the diffraction of a specimen assumed to contain only one reciprocal lattice node. The most remarkable difference with the single-crystal case is that now must think of scattering vectors not as lying on discrete nodes of reciprocal lattice vectors, the distances from the single-crystal reciprocal lattice nodes to the origin of reciprocal space

  5. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D).

    Science.gov (United States)

    van de Streek, Jacco; Neumann, Marcus A

    2014-12-01

    In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom.

  6. Cation-dependent anomalous compression of gallosilicate zeolites with CGS topology: A high-pressure synchrotron powder diffraction study

    International Nuclear Information System (INIS)

    Lee, Yongjae; Lee, Hyun-Hwi; Lee, Dong Ryeol; Kim, Sun Jin; Kao, Chi-chang

    2008-01-01

    The high-pressure compression behaviour of 3 different cation forms of gallosilicate zeolite with CGS topology has been investigated using in situ synchrotron X-ray powder diffraction and a diamond-anvil cell technique. Under hydrostatic conditions mediated by a nominally penetrating pressure-transmitting medium, unit-cell lengths and volume compression is modulated by different degrees of pressure-induced hydration and accompanying channel distortion. In a Na-exchanged CGS (Na 10 Ga 10 Si 22 O 64 .16H 2 O), the unit-cell volume expands by ca. 0.6% upon applying hydrostatic pressure to 0.2 GPa, whereas, in an as-synthesized K-form (K 10 Ga 10 Si 22 O 64 .5H 2 O), this initial volume expansion is suppressed to ca. 0.1% at 0.16 GPa. In the early stage of hydrostatic compression below ∼1 GPa, relative decrease in the ellipticity of the non-planar 10-rings is observed, which is then reverted to a gradual increase in the ellipticity at higher pressures above ∼1 GPa, implying a change in the compression mechanism. In a Sr-exchanged sample (Sr 5 Ga 10 Si 22 O 64 .19H 2 O), on the other hand, no initial volume expansion is observed. Instead, a change in the slope of volume contraction is observed near 1.5 GPa, which leads to a 2-fold increase in the compressibility. This is interpreted as pressure-induced rearrangement of water molecules to facilitate further volume contraction at higher pressures. - Graphical abstract: Three different cation forms of gallosilicate CGS zeolites have been investigated using synchrotron X-ray powder diffraction and a diamond-anvil cell. Under hydrostatic conditions, unit-cell lengths and volume show anomalous compression behaviours depending on the non-framework cation type and initial hydration level, which implies different modes of pressure-induced hydration and channel distortion

  7. 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

  8. Quantitative measurement of phase variation amplitude of ultrasonic diffraction grating based on diffraction spectral analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Meiyan, E-mail: yphantomohive@gmail.com; Zeng, Yingzhi; Huang, Zuohua, E-mail: zuohuah@163.com [Laboratory of Quantum Engineering and Quantum Materials, School of Physics and Telecommunication Engineering, South China Normal University, Guangzhou, Guangdong 510006 (China)

    2014-09-15

    A new method based on diffraction spectral analysis is proposed for the quantitative measurement of the phase variation amplitude of an ultrasonic diffraction grating. For a traveling wave, the phase variation amplitude of the grating depends on the intensity of the zeroth- and first-order diffraction waves. By contrast, for a standing wave, this amplitude depends on the intensity of the zeroth-, first-, and second-order diffraction waves. The proposed method is verified experimentally. The measured phase variation amplitude ranges from 0 to 2π, with a relative error of approximately 5%. A nearly linear relation exists between the phase variation amplitude and driving voltage. Our proposed method can also be applied to ordinary sinusoidal phase grating.

  9. Temperature-Induced Desorption of Methyl tert-Butyl Ether Confined on ZSM-5: An In Situ Synchrotron XRD Powder Diffraction Study

    Directory of Open Access Journals (Sweden)

    Elisa Rodeghero

    2017-02-01

    Full Text Available The temperature-induced desorption of methyl tert-butyl ether (MTBE from aqueous solutions onto hydrophobic ZSM-5 was studied by in situ synchrotron powder diffraction and chromatographic techniques. This kind of information is crucial for designing and optimizing the regeneration treatment of such zeolite. The evolution of the structural features monitored by full profile Rietveld refinements revealed that a monoclinic (P21/n to orthorhombic (Pnma phase transition occurred at about 100 °C. The MTBE desorption process caused a remarkable change in the unit-cell parameters. Complete MTBE desorption was achieved upon heating at about 250 °C. Rietveld analysis demonstrated that the desorption process occurred without any significant zeolite crystallinity loss, but with slight deformations in the channel apertures.

  10. 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.

  11. Microstructural characterisation of battery materials using powder diffraction data: DIFFaX, FAULTS and SH-FullProf approaches

    Energy Technology Data Exchange (ETDEWEB)

    Casas-Cabanas, M.; Canales-Vazquez, J.; Palacin, M.R. [Institut de Ciencia de Materials de Barcelona (CSIC), Barcelona 08913 (Spain); Rodriguez-Carvajal, J. [Laboratoire Leon Brillouin (CEA-CNRS), Saclay, 91191 Gif-sur-Ivette Cedex (France); Laligant, Y.; Lacorre, P. [Laboratoire des Oxydes et Fluorures, UMR CNRS 6010, Universite du Maine, 72085 Le Mans Cedex (France)

    2007-12-06

    The microstructure of Li{sub 2}PtO{sub 3}, isostructural with Li{sub 2}MnO{sub 3}, and {beta}-Ni(OH){sub 2} is analyzed from powder diffraction data using two approaches. Firstly, the recently developed FAULTS program (a modification of the DIFFaX program to allow refinement of the diffraction pattern) is used to include different amounts and types of stacking faults in the microstructural description of the material. This approach treats size effects mostly isotropically and assigns most of the anisotropic peak broadening to stacking faults. On the other hand, the FullProf program is also used to perform Rietveld refinement with microstructural models that treat the effects of anisotropic size and hence considers that this is the main contribution to broadening. The simultaneous use of these two approaches allows choosing the most adequate model in each particular case in order to obtain an accurate description of the microstructure of the material. (author)

  12. Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

    Science.gov (United States)

    Lunt, A. J. G.; Xie, M. Y.; Baimpas, N.; Zhang, S. Y.; Kabra, S.; Kelleher, J.; Neo, T. K.; Korsunsky, A. M.

    2014-08-01

    Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

  13. Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

    Energy Technology Data Exchange (ETDEWEB)

    Lunt, A. J. G., E-mail: alexander.lunt@eng.ox.ac.uk; Xie, M. Y.; Baimpas, N.; Korsunsky, A. M. [Department of Engineering Science, University of Oxford, Parks Road, Oxford OX1 3PJ (United Kingdom); Zhang, S. Y.; Kabra, S.; Kelleher, J. [ISIS Neutron and Muon Source, Rutherford Appleton Laboratory, Harwell, Oxford OX11 0QX (United Kingdom); Neo, T. K. [Specialist Dental Group, Mount Elizabeth Orchard, 3 Mount Elizabeth, #08-03/08-08/08-10, Singapore 228510 (Singapore)

    2014-08-07

    Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

  14. Report on neutron powder diffraction for the Australian Replacement Research Reactor

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    There is a clear need for two neutron powder diffractometers at the Australian Replacement Research Reactor when it starts operation in 2005. The high-intensity instrument should be capable of measuring a 10mg sample of moderate complexity, or perform single-shot time-resolved experiments with 1-second time slices, or perform stroboscopic measurements with time slices of order 50 microseconds. The high-resolution instrument should have a target resolution of Δd/d∼6x10 -4 , and be capable of collecting data at this resolution within 1-48 hours depending on sample size and crystal complexity. Key questions that need to be answered in the next 9 months include: (1) a detailed study of monochromator options, (2) analysing the detector options for the high-intensity machine and exploring ways in which the solid angle can be maximised for both instruments, (3) whether the instruments are better situated at the reactor face or on super mirror guides, (4) how to integrate the two instruments (physically, if they are only the same guide), and scientifically as regards detailed performance specifications. The user community clearly wants a wide range of sample-environment options, and these are listed in the report. Combinations of these options will be important

  15. Holographic analysis of diffraction structure factors

    International Nuclear Information System (INIS)

    Marchesini, S.; Bucher, J.J.; Shuh, D.K.; Fabris, L.; Press, M.J.; West, M.W.; Hussain, Z.; Mannella, N.; Fadley, C.S.; Van Hove, M.A.; Stolte, W.C.

    2002-01-01

    We combine the theory of inside-source/inside-detector x-ray fluorescence holography and Kossel lines/ x ray standing waves in kinematic approximation to directly obtain the phases of the diffraction structure factors. The influence of Kossel lines and standing waves on holography is also discussed. We obtain partial phase determination from experimental data obtaining the sign of the real part of the structure factor for several reciprocal lattice vectors of a vanadium crystal

  16. Comparative study of macrotexture analysis using X-ray diffraction and electron backscattered diffraction techniques

    International Nuclear Information System (INIS)

    Serna, Marilene Morelli

    2002-01-01

    The macrotexture is one of the main characteristics in metallic materials, which the physical properties depend on the crystallographic direction. The analysis of the macrotexture to middles of the decade of 80 was just accomplished by the techniques of Xray diffraction and neutrons diffraction. The possibility of the analysis of the macrotexture using, the technique of electron backscattering diffraction in the scanning electronic microscope, that allowed to correlate the measure of the orientation with its location in the micro structure, was a very welcome tool in the area of engineering of materials. In this work it was studied the theoretical aspects of the two techniques and it was used of both techniques for the analysis of the macrotexture of aluminum sheets 1050 and 3003 with intensity, measured through the texture index 'J', from 2.00 to 5.00. The results obtained by the two techniques were shown reasonably similar, being considered that the statistics of the data obtained by the technique of electron backscatter diffraction is much inferior to the obtained by the X-ray diffraction. (author)

  17. Phasor analysis of binary diffraction gratings with different fill factors

    International Nuclear Information System (INIS)

    MartInez, Antonio; Sanchez-Lopez, Ma del Mar; Moreno, Ignacio

    2007-01-01

    In this work, we present a simple analysis of binary diffraction gratings with different slit widths relative to the grating period. The analysis is based on a simple phasor technique directly derived from the Huygens principle. By introducing a slit phasor and a grating phasor, the intensity of the diffracted orders and the grating's resolving power can be easily obtained without applying the usual Fourier transform operations required for these calculations. The proposed phasor technique is mathematically equivalent to the Fourier transform calculation of the diffraction order amplitude, and it can be useful to explain binary diffraction gratings in a simple manner in introductory physics courses. This theoretical analysis is illustrated with experimental results using a liquid crystal device to display diffraction gratings with different fill factors

  18. Phasor analysis of binary diffraction gratings with different fill factors

    Energy Technology Data Exchange (ETDEWEB)

    MartInez, Antonio [Departamento de Ciencia de Materiales, Optica y TecnologIa Electronica, Universidad Miguel Hernandez, 03202 Elche (Spain); Sanchez-Lopez, Ma del Mar [Instituto de BioingenierIa y Departamento de Fisica y Arquitectura de Computadores, Universidad Miguel Hernandez, 03202 Elche (Spain); Moreno, Ignacio [Departamento de Ciencia de Materiales, Optica y TecnologIa Electronica, Universidad Miguel Hernandez, 03202 Elche (Spain)

    2007-09-11

    In this work, we present a simple analysis of binary diffraction gratings with different slit widths relative to the grating period. The analysis is based on a simple phasor technique directly derived from the Huygens principle. By introducing a slit phasor and a grating phasor, the intensity of the diffracted orders and the grating's resolving power can be easily obtained without applying the usual Fourier transform operations required for these calculations. The proposed phasor technique is mathematically equivalent to the Fourier transform calculation of the diffraction order amplitude, and it can be useful to explain binary diffraction gratings in a simple manner in introductory physics courses. This theoretical analysis is illustrated with experimental results using a liquid crystal device to display diffraction gratings with different fill factors.

  19. Crystal Engineering on Industrial Diaryl Pigments Using Lattice Energy Minimizations and X-ray Powder Diffraction

    International Nuclear Information System (INIS)

    Schmidt, M.; Dinnebier, R.; Kalkhof, H.

    2007-01-01

    Diaryl azo pigments play an important role as yellow pigments for printing inks, with an annual pigment production of more than 50,000 t. The crystal structures of Pigment Yellow 12 (PY12), Pigment Yellow 13 (PY13), Pigment Yellow 14 (PY14), and Pigment Yellow 83 (PY83) were determined from X-ray powder data using lattice energy minimizations and subsequent Rietveld refinements. Details of the lattice energy minimization procedure and of the development of a torsion potential for the biphenyl fragment are given. The Rietveld refinements were carried out using rigid bodies, or constraints. It was also possible to refine all atomic positions individually without any constraint or restraint, even for PY12 having 44 independent non-hydrogen atoms per asymmetric unit. For PY14 (23 independent non-hydrogen atoms), additionally all atomic isotropic temperature factors could be refined individually. PY12 crystallized in a herringbone arrangement with twisted biaryl fragments. PY13 and PY14 formed a layer structure of planar molecules. PY83 showed a herringbone structure with planar molecules. According to quantum mechanical calculations, the twisting of the biaryl fragment results in a lower color strength of the pigments, whereas changes in the substitution pattern have almost no influence on the color strength of a single molecule. Hence, the experimentally observed lower color strength of PY12 in comparison with that of PY13 and PY83 can be explained as a pure packing effect. Further lattice energy calculations explained that the four investigated pigments crystallize in three different structures because these structures are the energetically most favorable ones for each compound. For example, for PY13, PY14, or PY83, a PY12-analogous crystal structure would lead to considerably poorer lattice energies and lower densities. In contrast, lattice energy calculations revealed that PY12 could adopt a PY13-type structure with only slightly poorer energy. This structure was

  20. The structural phase diagram and oxygen equilibrium partial pressure of YBa2CU3O6+x studied by neutron powder diffraction and gas volumetry

    DEFF Research Database (Denmark)

    Andersen, N.H.; Lebech, B.; Poulsen, H.F.

    1990-01-01

    An experimental technique based on neutron powder diffraction and gas volumetry is presented and used to study the structural phase diagram of YBa2Cu3O6+x under equilibrium conditions in an extended part of (x, T)-phase (0.15

  1. Magnetic interactions in HoCr{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.2) investigated by neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xinzhi, E-mail: liuxinzhi1984.cn@163.com [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Hao, Lijie; Ma, Xiaobai [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Wang, Chin-Wei [Neutron Group, National Synchrotron Radiation Research Center, Hsinchu 30077, Taiwan (China); Klose, Frank [Australian Nuclear Science and Technology Organization, Lucas Heights, New South Wales 2234 (Australia); Department of Physics and Materials Science, The City University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Liu, Yuntao, E-mail: ytliu@ciae.ac.cn [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Sun, Kai; Li, Yuqing [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Chen, Dongfeng, E-mail: dongfeng@ciae.ac.cn [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China)

    2017-07-01

    Highlights: • The temperature dependent magnetism of HoCr{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.2) were investigated by neutron diffraction. • Cr{sup 3+} moment follows a mean field theory while Ho{sup 3+} follows a spin 1/2 model. • An magneto-elastic strain was observed accompanying with the ordering of Cr{sup 3+}. - Abstract: The temperature dependent magnetism of Fe-doped rare earth orthochromite HoCr{sub 1-x}Fe{sub x}O{sub 3}(x = 0, 0.2) was investigated by neutron powder diffraction. It is found that the magnetism of Cr(Fe){sup 3+} can be well understood within mean field theory, while the ordering of Ho{sup 3+} was induced by the Cr(Fe){sup 3+} sublattice and can be satisfyingly described by an effective S = 1/2 model. The absences of both the most common G{sub x}F{sub z} configuration of Cr{sup 3+} and the ordering of Ho{sup 3+} caused by Ho-Ho interaction evidence a strong Ho{sup 3+}-Cr{sup 3+} interaction which dominates this system. On the other hand, a remarkable magnetoelastic strain was observed accompanying the Cr(Fe){sup 3+} ordering. An analysis based on the equation of state with a Grüneisen approximation was performed and revealed magnetic origin of this strain.

  2. Real-time method of powder diffraction for non-periodic and nearly periodic materials

    International Nuclear Information System (INIS)

    Egami, T.; Toby, B.H.; Dmowski, T.W.; Jorgensen, J.D.

    1989-12-01

    The use of high-energy neutrons from pulsed or hot sources allows the method of atomic pair distribution analysis to be applied to the structural determination of crystalline as well as amorphous solids. This method complements the standard crystallographic methods in studying non-periodic aspects of solids with or without long range order. 14 refs., 3 figs

  3. Real space method of powder diffraction for non-periodic and nearly periodic materials

    International Nuclear Information System (INIS)

    Egami, T.; Toby, B.H.; Dmowski, W.; Janot, C.; Jorgensen, J.D.

    1990-01-01

    The use of high-energy neutrons from pulsed or hot sources allows the method of atomic pair distribution analysis to be applied to the structural determination of crystalline as well as amorphous solids. This method complements the standard crystallographic methods in studying non-periodic aspects of solids with or without long range order

  4. Analysis of natural milk and milk powder samples by NAA

    International Nuclear Information System (INIS)

    Al-Jobori, S. M.; Itawi, R. K.; Saad, A; Shihab, K. M.; Jalil, M.; Farhan, S. S.

    1993-01-01

    As a part of the Iraqi food analysis program (IFAP) the concentration of Na, Mg, P, Cl, K, Ca, Zn, Se, Br, Rb, and I in natural milk collected from different regions of Iraq, and in milk powder samples have been determined by using the NAA techniques. It was found that except for the elements I, Rb, and Br the concentrations of the elements was approximately identical in both the natural milk and milk powder. (author)

  5. Analysis of natural milk and milk powder samples by NAA

    International Nuclear Information System (INIS)

    Al-Jobori, S.M.; Itawi, R.K.; Saad, A.; Shihab, K.M.; Jalil, M.; Farhan, S.S.

    1990-01-01

    As a part of the Iraqi Food Analysis Programme the concentration of Na, Mg, P, Cl, K, Ca, Zn, Se, Br, Rb and I in natural milk collected from different regions of Iraq, and in milk powder samples was determined by NAA technique. It was found that except for the elements I, Rb and Br the concentration of the elements was approximately identical in both natural milk and milk powders. (author) 4 refs.; 3 figs.; 5 tabs

  6. Quantitative Analysis of Graphene Sheet Content in Wood Char Powders during Catalytic Pyrolysis

    Institute of Scientific and Technical Information of China (English)

    Yan-Jia Liou; Wu-Jang Huang

    2013-01-01

    The quantitative characterization of the graphene sheet content in carbon-containing materials is arguable and has not yet been developed.The authors report on a feasible method to characterize graphene sheet content quantitatively in pyrolized carbon materials using an X-ray diffraction (XRD) spectrometer.A direct carbonation at 300 ℃ followed by catalytic pyrolysis (heat-treatment temperature was set at 700-1400 ℃)under a vacuum condition was used for turning wood waste into pyrolized wood char powders.The graphene content in the samples was calculated through an analysis of full width at half maximum (FWHM) of the carbon (100) crystal plane at around 42°-43° in XRD.Results showed that the FWHM and the calculated graphene sheet content of pyrolized wood char powders depended on the heat-treatment temperature,and the FWHM of wood char powder with well-developed graphene sheets (100%) was determined to be 5.0.In addition,the trend to 100% graphene sheet-contained pyrolized carbon powder was obtained at a heattreatment temperature of 2700 ℃.The resistivity of the wood char powder with 100% graphene sheets was predicted to be 0.01 Ω cm,close to our experimental data of 0.012 and 0.006 Ω cm for commercial graphite and graphene products,respectively.

  7. A study of nitrogenation of a NdFe12-xMox compound by in situ neutron powder diffraction

    International Nuclear Information System (INIS)

    Loong, C.; Short, S.M.; Lin, J.; Ding, Y.

    1998-01-01

    The effects on the crystal lattice of a NdFe 12-x Mo x (x congruent 1.7) during controlled nitrogenation over the 25 endash 600 degree C temperature range were studied by neutron powder diffraction. Prior to nitrogenation the sample contained a major phase of NdFe 10.3 Mo 1.7 and a minor phase (∼12vol%) of bcc-Fe. The sample inside the furnace was connected to a closed volume of ultrapure nitrogen gas while neutron data were collected over regular time intervals during sequential heating. Substantial nitrogen absorption occurred between 500 and 600 degree C. During the nitrogenation process the NdFe 12-x Mo x N y lattice expanded while the bcc-Fe lattice contracted. An increasing decomposition of the compound into bcc-Fe at 600 degree C was observed. The average size of the NdFe 12-x Mo x N y crystalline grains decreased starting at ∼300 degree C, reaching a minimum at ∼500 degree C and then increased markedly at higher temperatures. The development of lattice strains, on the other hand, showed an opposite trend, i.e., a maximum at 500 degree C. copyright 1998 American Institute of Physics

  8. Ab initio determination of the novel perovskite-related structure of La7Mo7O30 from powder diffraction

    International Nuclear Information System (INIS)

    Goutenoire, F.; Retoux, R.; Lacorre, P.

    1999-01-01

    A new mixed valence molybdate, La 7 Mo 7 O 30 , first prepared by high energy ball milling, has been successfully synthesized by controlled hydrogen reduction of La 2 Mo 2 O 9 . Its original crystal structure was determined from X-ray and neutron powder diffraction (space group R 3 ; a = b = 17.0051(2) angstrom, c = 6.8607(1) angstrom; Z = 3; reliability factors: R p = 0.081, R wp = 0.091, χ 2 = 3.1, R Bragg = 0.049, R F = 0.033). It consists in the hexagonal stacking of individual cylinders of perovskite-type arrangement. These cylinders are built up from perovskite cages sharing corners in trans-position along their diagonal axis. Two different mixed-valence molybdenum sites coexist, with more (Mo +5.75 ) or less (Mo +4.5 ) distorted octahedral environments. Lanthanum atoms are located within the perovskite cages and around them, very close to their regular positions in the perovskite structure. Lanthanum and molybdenum atoms thus form two rows of almost perfect cubes, shifted from each other by c/2. An electron microscopy study revealed the defect-free cationic and octahedral arrangements in the (a,b) plane

  9. Numerical analysis of air effect on the powder flow dynamics in the FT4 Powder Rheometer

    Directory of Open Access Journals (Sweden)

    Nan Wenguang

    2017-01-01

    Full Text Available The FT4 powder rheometer of Freeman Technology is widely used nowadays in industry for characterisation of particle flow under dynamic conditions of shear strain rate. It measures the work (termed flow energy required to penetrate a rotating impeller into a powder bed. However, little is known about its underlying powder mechanics, i.e. the relationship between the flow energy and the prevailing local shear stress. This has recently been studied, but only for very simple and ideal systems amenable to analysis by DEM. We analyse the effect of gas flow through the powder bed on the flow behaviour of cohesionless particles in FT4 by DEM-CFD simulation. The results show that the relative particle velocities induced by the mean shear speed, is of the same order as that produced by the root of granular temperature. The shear stress in both cases with and without gas flow could be quantified by the inertial number. The flow energy correlates well with the shear stress in front of the blade, and both increase with the inertial number and could be significantly reduced by the upward gas flow.

  10. Small area analysis using micro-diffraction techniques

    International Nuclear Information System (INIS)

    Goehner, Raymond P.; Tissot, Ralph G. Jr.; Michael, Joseph R.

    2000-01-01

    An overall trend toward smaller electronic packages and devices makes it increasingly important and difficult to obtain meaningful diffraction information from small areas. X-ray micro-diffraction, electron back-scattered diffraction (EBSD) and Kossel are micro-diffraction techniques used for crystallographic analysis including texture, phase identification and strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements of areas between 10 microm to 100 microm. For areas this small glass capillary optics are used for producing a usable collimated x-ray beam. These optics are designed to reflect x-rays below the critical angle therefore allowing for larger solid acceptance angle at the x-ray source resulting in brighter smaller x-ray beams. The determination of residual strain using micro-diffraction techniques is very important to the semiconductor industry. Residual stresses have caused voiding of the interconnect metal which then destroys electrical continuity. Being able to determine the residual stress helps industry to predict failures from the aging effects of interconnects due to this stress voiding. Stress measurements would be impossible using a conventional x-ray diffractometer; however, utilizing a 30 microm glass capillary these small areas are readily assessable for analysis. Kossel produces a wide angle diffraction pattern from fluorescent x-rays generated in the sample by an e-beam in a SEM. This technique can yield very precise lattice parameters for determining strain. Fig. 2 shows a Kossel pattern from a Ni specimen. Phase analysis on small areas is also possible using an energy dispersive spectrometer (EBSD) and x-ray micro-diffraction techniques. EBSD has the advantage of allowing the user to observe the area of interest using the excellent imaging capabilities of the SEM. An EDS detector has been

  11. 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)

  12. 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)

  13. Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

    Energy Technology Data Exchange (ETDEWEB)

    Chagas, L.H.; De Carvalho, G.S.G. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); San Gil, R.A.S. [Universidade Federal do Rio de Janeiro, Instituto de Química, 21949-900 Rio de Janeiro, RJ (Brazil); Chiaro, S.S.X. [PETROBRAS-CENPES, 21941-915 Rio de Janeiro, RJ (Brazil); Leitão, A.A. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); Diniz, R., E-mail: renata.diniz@ufjf.edu.br [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil)

    2014-01-01

    Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

  14. ENERGY AND EXERGY ANALYSIS OF A POWDER DETERGENT UNIT

    International Nuclear Information System (INIS)

    G. Bektas; F. Balkan

    2008-01-01

    In the recent years, there is a growing interest on minimization of energy utilization in various plants and thereby improving the performance. As an efficient tool for examining the processes, the exergy analysis gains importance. In the present work, the application of exergy analysis to powder detergent unit of a powder detergent production plant located at Izmir, Turkey were performed y using actual plant operational data. Also the energy analyses were considered for comparison. Although there are a number of energy and exergy analyses in various areas of industry, this study will be likely the first one for powder detergent production. The energy and exergy efficiencies of the equipments were calculated and it was concluded that according to the overall balance around the unit, the energy efficiency was 0.76 and the exergy efficiency was 0.40

  15. ENERGY AND EXERGY ANALYSIS OF A POWDER DETERGENT UNIT

    Energy Technology Data Exchange (ETDEWEB)

    G. Bektas; F. Balkan [Ege University, Chemical Engineering Department, Izmir (Turkey)

    2008-09-30

    In the recent years, there is a growing interest on minimization of energy utilization in various plants and thereby improving the performance. As an efficient tool for examining the processes, the exergy analysis gains importance. In the present work, the application of exergy analysis to powder detergent unit of a powder detergent production plant located at Izmir, Turkey were performed y using actual plant operational data. Also the energy analyses were considered for comparison. Although there are a number of energy and exergy analyses in various areas of industry, this study will be likely the first one for powder detergent production. The energy and exergy efficiencies of the equipments were calculated and it was concluded that according to the overall balance around the unit, the energy efficiency was 0.76 and the exergy efficiency was 0.40.

  16. Quantitative analysis of phases by x-ray diffraction and thermogravimetry in Cuban phosphorite ores

    International Nuclear Information System (INIS)

    Casanova Gomez, Abdel; Martinez Montalvo, Asor; Cilano Campos, Guillermo; Arostegui Aguirre, Miladys; Ferreiro Fernandez, Adalyz; Alonso Perez, Jose A.

    2016-01-01

    Phases analysis is performed by instrumental techniques X - ray diffraction and Thermal Analysis in two groups of samples of Cuban minerals carriers'phosphorus, candidates to reference materials. To this end, the variant of structural refinement of the diffraction pattern in the form of adjustment profile is applied, using the Full prof program of Juan Rodriguez-Carvajal. This analysis is the first step to develop the standard specification of these resources and classify them as phosphate rock and / or phospharite from their mass content. The statistical evaluation of the uncertainty of the quantitative analysis (standard deviation) was carried out in ten replicate samples of phosphate rock and eight of phosphate from the field Trinidad de Guedes. The qualitative phase analysis reflected the following phase composition: carbonate fluoroapatite (CFA), Calcite, Quartz and Halloysite (present only in the clayey granular phosphorite ore; FGA). By the method of setting pattern powder diffraction profile, the quantitative phase composition is reported in the sample FGA: 87 (2) % of CFA, 4 (1) % of Calcite, 1% Quartz, and 8 (3) % Halloysite. For granular limestone ore (FGC), the following contents were obtained: 87 (3) % Calcite, 8 (3) % of CFA and 5 (1) % Quartz: The obtained values are corroborated by Thermogravimetric Analysis (TG) through the calculation of the mass content of the thermally active phases (Calcite and CFA) in the range (27-10000 0 C), confirming the validity of the results of XRD. (Author)

  17. 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

  18. 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...

  19. Truncation in diffraction pattern analysis. Pt. 1

    International Nuclear Information System (INIS)

    Delhez, R.; Keijser, T.H. de; Mittemeijer, E.J.; Langford, J.I.

    1986-01-01

    An evaluation of the concept of a line profile is provoked by truncation of the range of intensity measurement in practice. The measured truncated line profile can be considered either as part of the total intensity distribution which peaks at or near the reciprocal-lattice points (approach 1), or as part of a component line profile which is confined to a single reciprocal-lattice point (approach 2). Some false conceptions in line-profile analysis can then be avoided and recipes can be developed for the extrapolation of the tails of the truncated line profile. Fourier analysis of line profiles, according to the first approach, implies a Fourier series development of the total intensity distribution defined within [l - 1/2, l + 1/2] (l indicates the node considered in reciprocal space); the second approach implies a Fourier transformation of the component line profile defined within [ - ∞, + ∞]. Exact descriptions of size broadening are provided by both approaches, whereas combined size and strain broadening can only be evaluated adequately within the first approach. Straightforward methods are given for obtaining truncation-corrected values for the average crystallite size. (orig.)

  20. Quantitative multiphase analysis of archaeological bronzes by neutron diffraction

    CERN Document Server

    Siano, S; Celli, M; Pini, R; Salimbeni, R; Zoppi, M; Kockelmann, W A; Iozzo, M; Miccio, M; Moze, O

    2002-01-01

    In this paper, we report the first investigation on the potentials of neutron diffraction to characterize archaeological bronze artifacts. The preliminary feasibility of phase and structural analysis was demonstrated on standardised specimens with a typical bronze alloy composition. These were realised through different hardening and annealing cycles, simulating possible ancient working techniques. The Bragg peak widths that resulted were strictly dependent on the working treatment, thus providing an important analytical element to investigate ancient making techniques. The diagnostic criteria developed on the standardised specimens were then applied to study two Etruscan museum pieces. Quantitative multiphase analysis by Rietveld refinement of the diffraction patterns was successfully demonstrated. Furthermore, the analysis of patterns associated with different artifact elements also yielded evidence for some peculiar perspective of the neutron diffraction diagnostics in archeometric applications. (orig.)

  1. 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

    This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs 3 ∞ [Ln(Tz * ) 3 ]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln 3+ -ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds 2 ∞ [Ln(Tz * ) 3 ], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer 1 ∞ [Eu(Btz) 2 (BtzH) 2 ], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF 3 ∞ [Eu(Btz) 2 ] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds 3 ∞ [Ba 1-x Eu x (Im) 2 ], which were obtained from reaction of the salt-like hydrides BaH 2 and EuH 2 with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound 3 ∞ [BaEu(Im) 2 ]. Structural characterization of materials from X-ray powder diffraction data is an important aspect

  2. Quantifying low amorphous or crystalline amounts of alpha-lactose-monohydrate using X-ray powder diffraction, near-infrared spectroscopy, and differential scanning calorimetry.

    Science.gov (United States)

    Fix, I; Steffens, K J

    2004-05-01

    Efficient and accurate quantification of low amorphous and crystalline contents within pharmaceutical materials still remains a challenging task in the pharmaceutical industry. Since X-ray powder diffraction (XRPD) equipment has improved in recent years, our aim was 1) to investigate the possibility of substantially lowering the detection limits of amorphous or crystalline material to about 1% or 0.5% w/w respectively by applying conventional Bragg Brentano optics, combined with a fast and simple evaluation technique; 2) to perform these measurements within a short time to make it suitable for routine analysis; and 3) to subject the same data sets to a partial least squares regression (PLSR) in order to investigate whether it is possible to improve accuracy and precision compared to the standard integration method. Near-infrared spectroscopy (NIRS) and differential scanning calorimetry (DSC) were chosen as reference method. As model substance, alpha lactose monohydrate was chosen to create calibration curves based on predetermined mixtures of highly crystalline and amorphous substance. In contrast to DSC, XRPD and NIRS revealed an excellent linearity, precision, and accuracy with the percent of crystalline amount and a detectability down to about 0.5% w/w. Chemometric evaluation (partial least squares regression) applied to the XRPD data further improved the quality of our calibration.

  3. Twin-domain size and bulk oxygen in-diffusion kinetics of YBa 2Cu 3O 6+x studied by neutron powder diffraction and gas volumetry

    Science.gov (United States)

    Poulsen, H. F.; Andersen, N. H.; Lebech, B.

    1991-02-01

    We report experimental results of twin-domain size and bulk oxygen in-diffusion kinetics of YBa 2Cu 3O 6+ x, which supplement a previous and simultaneous study of the structural phase diagram and oxygen equilibrium partial pressure. Analysis of neutron powder diffraction peak broadening show features which are identified to result from temperature independent twin-domain formation in to different orthorhombic phases with domain sizes and 250 and 350Å, respectively. The oxygen in-diffusion flow shows simple relaxation type behaviour J=J 0 exp( {-t}/{τ}) despite a rather broad particle size distribution. At higher temperatures, τ is activated with activation energies 0.55 and 0.25 eV in the tetragonal and orthorhombic phases, respectively. Comparison between twin-domain sizes and bulk oxygen in-diffusion time constants indicates that the twin-domain boundaries may contribute to the effective bulk oxygen in-diffusion. All our results may be interpreted in terms of the 2D ASYNNNI model description of the oxygen basal plane ordering, and they suggest that recent first principles interaction parameters should be modified.

  4. Precise structural analysis of methane hydrate by neutron diffraction

    International Nuclear Information System (INIS)

    Igawa, Naoki; Hoshikawa, Akinori; Ishii, Yoshinobu

    2006-01-01

    Methane hydrate has attracted great interest as an energy resource to replace natural gas since this material is deposited in the seafloor and the deposits are estimated to exceed those of natural gas. Understanding the physical proprieties, such as the temperature dependence of the crystal structure, helps to specify the optimum environmental temperature and pressure during drilling, transport, and storage of methane hydrate. Clathrate hydrates consisted of encaging atomic and/or molecular species as a guest and host water formed by a hydrogen bonding. Although many studies on the clathrate hydrate including methane hydrate were reported, no detailed crystallographic property has yet been cleared. We focused on the motion of methane in the clathrate hydrate by the neutron diffraction. The crystal structure of the methane hydrate was analyzed by the applying the combination of the Rietveld refinement and the maximum entropy method (MEM) to neutron powder diffraction. Temperature dependence of the scattering-length density distribution maps revealed that the motion of methane molecules differs between the shapes of dodecahedron and tetrakaidecahedron. (author)

  5. Diffraction imaging and velocity analysis using oriented velocity continuation

    KAUST Repository

    Decker, Luke

    2014-08-05

    We perform seismic diffraction imaging and velocity analysis by separating diffractions from specular reflections and decomposing them into slope components. We image slope components using extrapolation in migration velocity in time-space-slope coordinates. The extrapolation is described by a convection-type partial differential equation and implemented efficiently in the Fourier domain. Synthetic and field data experiments show that the proposed algorithm is able to detect accurate time-migration velocities by automatically measuring the flatness of events in dip-angle gathers.

  6. Analysis of XFEL serial diffraction data from individual crystalline fibrils

    Directory of Open Access Journals (Sweden)

    David H. Wojtas

    2017-11-01

    Full Text Available Serial diffraction data collected at the Linac Coherent Light Source from crystalline amyloid fibrils delivered in a liquid jet show that the fibrils are well oriented in the jet. At low fibril concentrations, diffraction patterns are recorded from single fibrils; these patterns are weak and contain only a few reflections. Methods are developed for determining the orientation of patterns in reciprocal space and merging them in three dimensions. This allows the individual structure amplitudes to be calculated, thus overcoming the limitations of orientation and cylindrical averaging in conventional fibre diffraction analysis. The advantages of this technique should allow structural studies of fibrous systems in biology that are inaccessible using existing techniques.

  7. Structural study of CaMn{sub 1−x}Mo{sub x}O{sub 3} (0.08 ≤ x ≤ 0.12) system by neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Supelano, G.I., E-mail: ivan.supelano@uptc.edu.co [Grupo Física de Materiales, Escuela de Física, Universidad Pedagógica y Tecnológica de Colombia, Tunja (Colombia); Parra Vargas, C.A.; Barón-González, A.J. [Grupo Física de Materiales, Escuela de Física, Universidad Pedagógica y Tecnológica de Colombia, Tunja (Colombia); Sarmiento Santos, A. [Grupo Superficies Electroquímica y Corrosión, Escuela de Física, Universidad Pedagógica y Tecnológica de Colombia, Tunja (Colombia); Frontera, C. [Institut de Ciència de Materials de Barcelona, CSIC, Campus Universitari de Bellaterra, E-08193, Bellaterra, Barcelona (Spain)

    2016-08-15

    Neutron powder diffraction experiments and magnetic measurements in polycrystalline CaMn{sub 1−x}Mo{sub x}O{sub 3} (x = 0.08, 0.10, 0.12) point towards a possible charge and orbital order in this system. The analysis of structural and magnetic data show that the samples present structural phase transformation from Pnma to P2{sub 1}/m space group and the system has a C-type antiferromagnetic configuration at low temperature. A detailed analysis of the bond distances signals a small Jahn-Teller distortion of only one (x = 0.08) or of the two Mn ions (x = 0.10, 0.12). We identify the partially occupied e{sub g} orbitals and this explains the C-type magnetic structure. - Highlights: • CaMn{sub 1−x}Mo{sub x}O{sub 3} (x = 0.08, 0.10, 0.12) is investigated by neutron powder diffraction. • Analysis of individual Mn-O distances demonstrates the apparition of orbital order. • By symmetry analysis, we find that the low temperature magnetic structure is C-type. • Magnetic interactions foreseen by the orbital order explain the magnetic structure.

  8. An analysis of un-dissolved powders of instant powdered soup by using ultrasonographic image

    Science.gov (United States)

    Kawaai, Yukinori; Kato, Kunihito; Yamamoto, Kazuhiko; Kasamatsu, Chinatsu

    2008-11-01

    Nowadays, there are many instant powdered soups around us. When we make instant powdered soup, sometimes we cannot dissolve powders perfectly. Food manufacturers want to improve this problem in order to make better products. Therefore, they have to measure the state and volume of un-dissolved powders. Earlier methods for analyzing removed the un-dissolved powders from the container, the state of the un-dissolved power was changed. Our research using ultrasonographic image can measure the state of un-dissolved powders with no change by taking cross sections of the soup. We then make 3D soup model from these cross sections of soup. Therefore we can observe the inside of soup that we do not have ever seen. We construct accurate 3D model. We can visualize the state and volume of un-dissolved powders with analyzing the 3D soup models.

  9. A program for Warren-Averbach analysis of diffraction data

    International Nuclear Information System (INIS)

    Fan, Zhijian; Chen, Bo; Chen, Xiping

    2009-04-01

    X-ray or neutron diffraction experiment can provide microstructural information of crystalline materials. At the moment without the model of micro-structure, Warren-Averbach analysis is regarded as an important tool. For this purpose, a program of Warren-Averbach analysis has been developed. The pro- gram has nearly all basic functions, it can be conveniently used through a graphic user interface as well. In the end, the efficiency of the program is illustrated by an example of ceria. (authors)

  10. Analysis of tablet compaction. I. Characterization of mechanical behavior of powder and powder/tooling friction.

    Science.gov (United States)

    Cunningham, J C; Sinka, I C; Zavaliangos, A

    2004-08-01

    In this first of two articles on the modeling of tablet compaction, the experimental inputs related to the constitutive model of the powder and the powder/tooling friction are determined. The continuum-based analysis of tableting makes use of an elasto-plastic model, which incorporates the elements of yield, plastic flow potential, and hardening, to describe the mechanical behavior of microcrystalline cellulose over the range of densities experienced during tableting. Specifically, a modified Drucker-Prager/cap plasticity model, which includes material parameters such as cohesion, internal friction, and hydrostatic yield pressure that evolve with the internal state variable relative density, was applied. Linear elasticity is assumed with the elastic parameters, Young's modulus, and Poisson's ratio dependent on the relative density. The calibration techniques were developed based on a series of simple mechanical tests including diametrical compression, simple compression, and die compaction using an instrumented die. The friction behavior is measured using an instrumented die and the experimental data are analyzed using the method of differential slices. The constitutive model and frictional properties are essential experimental inputs to the finite element-based model described in the companion article. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:2022-2039, 2004

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

    Science.gov (United States)

    Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

    2010-10-15

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

  12. 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.

  13. 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

  14. Effect of Sr substitution on superconductivity in Hg2(Ba1-ySry)2YCu2O8-d (part 1): a neutron powder diffraction study

    OpenAIRE

    Toulemonde, P.; Odier, P.; Bordet, P.; Floch, S. Le; Suard, E.

    2002-01-01

    The effect of Sr chemical pressure on superconductivity was investigated in Hg2(Ba1-ySry)2YCu2O8-d. The samples were synthesized at high pressure-high temperature from y = 0.0 to full substitution, y = 1.0. These Sr-substituted compounds are superconducting, without Ca doping on the Y site, and show an increasing Tc with Sr, reaching 42 K for y = 1.0. A detailed neutron powder diffraction study compares the structural changes induced by this chemical Sr/Ba substitution and the mechanical pres...

  15. 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....

  16. 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

  17. A general method for baseline-removal in ultrafast electron powder diffraction data using the dual-tree complex wavelet transform

    Directory of Open Access Journals (Sweden)

    Laurent P. René de Cotret

    2017-07-01

    Full Text Available The general problem of background subtraction in ultrafast electron powder diffraction (UEPD is presented with a focus on the diffraction patterns obtained from materials of moderately complex structure which contain many overlapping peaks and effectively no scattering vector regions that can be considered exclusively background. We compare the performance of background subtraction algorithms based on discrete and dual-tree complex (DTCWT wavelet transforms when applied to simulated UEPD data on the M1–R phase transition in VO2 with a time-varying background. We find that the DTCWT approach is capable of extracting intensities that are accurate to better than 2% across the whole range of scattering vector simulated, effectively independent of delay time. A Python package is available.

  18. Analysis of Pelletizing of Granulometric Separation Powder from Cork Industries

    Directory of Open Access Journals (Sweden)

    Irene Montero

    2014-09-01

    Full Text Available Cork industries generate a considerable amount of solid waste during their processing. Its management implies a problem for companies that should reconsider its reuse for other purposes. In this work, an analysis of pelletizing of granulometric separation powder, which is one of the major wastes in cork industries and which presents suitable properties (as an raw material for its thermal use, is studied. However, its characteristic heterogeneity, along with its low bulk density (which makes its storage and transportation difficult are restrictive factors for its energy use. Therefore, its densified form is a real alternative in order to make the product uniform and guarantee its proper use in boiler systems. Thus, the cork pellets (from granulometric separation powder in the study met, except for ash content specification, the specifications in standard European Norm EN-Plus (B for its application as fuel for domestic use.

  19. Analysis of Pelletizing of Granulometric Separation Powder from Cork Industries.

    Science.gov (United States)

    Montero, Irene; Miranda, Teresa; Sepúlveda, Francisco José; Arranz, José Ignacio; Nogales, Sergio

    2014-09-18

    Cork industries generate a considerable amount of solid waste during their processing. Its management implies a problem for companies that should reconsider its reuse for other purposes. In this work, an analysis of pelletizing of granulometric separation powder, which is one of the major wastes in cork industries and which presents suitable properties (as an raw material) for its thermal use, is studied. However, its characteristic heterogeneity, along with its low bulk density (which makes its storage and transportation difficult) are restrictive factors for its energy use. Therefore, its densified form is a real alternative in order to make the product uniform and guarantee its proper use in boiler systems. Thus, the cork pellets (from granulometric separation powder) in the study met, except for ash content specification, the specifications in standard European Norm EN-Plus (B) for its application as fuel for domestic use.

  20. 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.

  1. 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.

  2. X-Ray Diffraction for In-Situ Mineralogical Analysis of Planetesimals.

    Science.gov (United States)

    Sarrazin, P.; Blake, D. F.; Dera, P.; Downs, R. T.; Taylor, J.

    2017-12-01

    X-ray diffraction (XRD) is a general purpose technique for definitive, quantitative mineralogical analysis. When combined with XRF data for sample chemistry, XRD analyses yield as complete a characterization as is possible by any spacecraft-capable techniques. The MSL CheMin instrument, the first XRD instrument flown in space, has been used to establish the quantitative mineralogy of the Mars global soil, to discover the first habitable environment on another planet, and to provide the first in-situ evidence of silicic volcanism on Mars. CheMin is now used to characterize the depositional and diagenetic environments associated with the mudstone sediments of lower strata of Mt. Sharp. Conventional powder XRD requires samples comprised of small grains presented in random orientations. In CheMin, sample cells are vibrated to cause loose powder to flow within the cell, driven by granular convection, which relaxes the requirement for fine grained samples. Nevertheless, CheMin still requires mechanisms to collect, crush, sieve and deliver samples before analysis. XTRA (Extraterrestrial Regolith Analyzer) is an evolution of CheMin intended to analyze fines in as-delivered surface regolith, without sample preparation. Fine-grained regolith coats the surfaces of most airless bodies in the solar system, and because this fraction is typically comminuted from the rocky regolith, it can often be used as a proxy for the surface as a whole. HXRD (Hybrid-XRD) is concept under development to analyze rocks or soils without sample preparation. Like in CheMin, the diffracted signal is collected with direct illumination CCD's. If the material is sufficiently fine-grained, a powder XRD pattern of the characteristic X-ray tube emission is obtained, similar to CheMin or XTRA. With coarse grained crystals, the white bremsstrahlung radiation of the tube is diffracted into Laue patterns. Unlike typical Laue applications, HXRD uses the CCD's capability to distinguish energy and analyze the

  3. Fourier-Based Diffraction Analysis of Live Caenorhabditis elegans.

    Science.gov (United States)

    Magnes, Jenny; Hastings, Harold M; Raley-Susman, Kathleen M; Alivisatos, Clara; Warner, Adam; Hulsey-Vincent, Miranda

    2017-09-13

    This manuscript describes how to classify nematodes using temporal far-field diffraction signatures. A single C. elegans is suspended in a water column inside an optical cuvette. A 632 nm continuous wave HeNe laser is directed through the cuvette using front surface mirrors. A significant distance of at least 20-30 cm traveled after the light passes through the cuvette ensures a useful far-field (Fraunhofer) diffraction pattern. The diffraction pattern changes in real time as the nematode swims within the laser beam. The photodiode is placed off-center in the diffraction pattern. The voltage signal from the photodiode is observed in real time and recorded using a digital oscilloscope. This process is repeated for 139 wild type and 108 "roller" C. elegans. Wild type worms exhibit a rapid oscillation pattern in solution. The "roller" worms have a mutation in a key component of the cuticle that interferes with smooth locomotion. Time intervals that are not free of saturation and inactivity are discarded. It is practical to divide each average by its maximum to compare relative intensities. The signal for each worm is Fourier transformed so that the frequency pattern for each worm emerges. The signal for each type of worm is averaged. The averaged Fourier spectra for the wild type and the "roller" C. elegans are distinctly different and reveal that the dynamic worm shapes of the two different worm strains can be distinguished using Fourier analysis. The Fourier spectra of each worm strain match an approximate model using two different binary worm shapes that correspond to locomotory moments. The envelope of the averaged frequency distribution for actual and modeled worms confirms the model matches the data. This method can serve as a baseline for Fourier analysis for many microscopic species, as every microorganism will have its unique Fourier spectrum.

  4. Crystal structures of eight mono-methyl alkanes (C26–C32 via single-crystal and powder diffraction and DFT-D optimization

    Directory of Open Access Journals (Sweden)

    Lee Brooks

    2015-09-01

    Full Text Available The crystal structures of eight mono-methyl alkanes have been determined from single-crystal or high-resolution powder X-ray diffraction using synchrotron radiation. Mono-methyl alkanes can be found on the cuticles of insects and are believed to act as recognition pheromones in some social species, e.g. ants, wasps etc. The molecules were synthesized as pure S enantiomers and are (S-9-methylpentacosane, C26H54; (S-9-methylheptacosane and (S-11-methylheptacosane, C28H58; (S-7-methylnonacosane, (S-9-methylnonacosane, (S-11-methylnonacosane and (S-13-methylnonacosane, C30H62; and (S-9-methylhentriacontane, C32H66. All crystallize in space group P21. Depending on the position of the methyl group on the carbon chain, two packing schemes are observed, in which the molecules pack together hexagonally as linear rods with terminal and side methyl groups clustering to form distinct motifs. Carbon-chain torsion angles deviate by less than 10° from the fully extended conformation, but with one packing form showing greater curvature than the other near the position of the methyl side group. The crystal structures are optimized by dispersion-corrected DFT calculations, because of the difficulties in refining accurate structural parameters from powder diffraction data from relatively poorly crystalline materials.

  5. 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.

  6. A re-analysis of neutron diffraction data from UO2

    International Nuclear Information System (INIS)

    Cooper, M.J.; Sakata, M.

    1979-04-01

    The results of a re-analysis of recent single crystal and powder neutron diffraction data from UO2 are presented and discussed. It is shown that apparent inconsistencies in the results of previous analyses of these data arose from differences between the values assumed for some of the parameters and that the various sets of data are in fact extremely consistent. These data also provide a more accurate value for the ratio of the scattering amplitudes, i.e. bU/bO = 1.451(2), which gives a value for bU = 0.842(2) x 10(-12) cm on the assumption of a value for b0 = 0.5805(11) x 10(-12) cm. The temperature factors for the atoms at room temperature are determined to be BU = 0.23(1)Angstrom and BO = 0.44(1)Angstrom(2). (author)

  7. Bragg's Law diffraction simulations for electron backscatter diffraction analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kacher, Josh, E-mail: jkacherbyu@gmail.com [Department of Mechanical Engineering, Brigham Young University, 455B Crabtree Technology Building, Provo, UT 84602 (United States); Landon, Colin; Adams, Brent L.; Fullwood, David [Department of Mechanical Engineering, Brigham Young University, 455B Crabtree Technology Building, Provo, UT 84602 (United States)

    2009-08-15

    In 2006, Angus Wilkinson introduced a cross-correlation-based electron backscatter diffraction (EBSD) texture analysis system capable of measuring lattice rotations and elastic strains to high resolution. A variation of the cross-correlation method is introduced using Bragg's Law-based simulated EBSD patterns as strain free reference patterns that facilitates the use of the cross-correlation method with polycrystalline materials. The lattice state is found by comparing simulated patterns to collected patterns at a number of regions on the pattern using the cross-correlation function and calculating the deformation from the measured shifts of each region. A new pattern can be simulated at the deformed state, and the process can be iterated a number of times to converge on the absolute lattice state. By analyzing an iteratively rotated single crystal silicon sample and recovering the rotation, this method is shown to have an angular resolution of {approx}0.04{sup o} and an elastic strain resolution of {approx}7e-4. As an example of applications, elastic strain and curvature measurements are used to estimate the dislocation density in a single grain of a compressed polycrystalline Mg-based AZ91 alloy.

  8. Crystal structure of aspartame anhydrate from powder diffraction data. Structural aspects of the dehydration process of aspartame

    NARCIS (Netherlands)

    Guguta, C.; Meekes, H.L.M.; Gelder, R. de

    2006-01-01

    Aspartame has three pseudo-polymorphic forms, two hydrates and a hemi-hydrate, for which crystal structures were determined from single-crystal diffraction data. This paper presents the crystal structure of the anhydrate, which was obtained by dehydrating the hemi-hydrate. The crystal structure of

  9. In situ synchrotron powder diffraction study of the setting reaction kinetics of magnesium-potassium phosphate cements

    Czech Academy of Sciences Publication Activity Database

    Viani, Alberto; Pérez-Estébanez, Marta; Pollastri, S.; Gualtieri, A. F.

    2016-01-01

    Roč. 79, January (2016), s. 344-352 ISSN 0008-8846 R&D Projects: GA MŠk(CZ) LO1219 Keywords : kinetics * reaction * X-ray diffraction * MgO * chemically bonded ceramics Subject RIV: JN - Civil Engineering Impact factor: 4.762, year: 2016 http://www.sciencedirect.com/science/article/pii/S0008884615002690

  10. X-ray powder microdiffraction in the analysis of art works

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Bayerová, T.; Hradil, David

    2004-01-01

    Roč. 11, 1a (2004), s. 43 ISSN 1211-5894. [European Powder Diffraction Conference /9./. Prague, 02.09.2004-05.09.2004] R&D Projects: GA MŠk LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z4032918 Keywords : X-ray powder microdiffraction * pigments * colour layers of artworks Subject RIV: CA - Inorganic Chemistry

  11. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  12. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  13. X-ray diffraction from thin films : Size/strain analysis and whole pattern fitting

    Energy Technology Data Exchange (ETDEWEB)

    Scardi, P [Trento Univ. (Italy). Dept. of Materials Engineering

    1996-09-01

    Line Profile Analysis (LPA) and whole pattern fitting may be used with success for the characterization of thin films from XRD data collected with the traditional Bragg-Brentano geometry. The size/strain analysis was conducted by an integrated procedure of profile modelling-assisted Fourier analysis, in order to measure the content of lattice imperfections and crystalline domain size along the growth direction in heteroepitaxial thin films. The microstructure of these films is typical of several PVD processes for the production of highly textured and low-defect thin crystalline layers. The same analysis could be conducted on random thin films as well, and in this case it is possible to determine an average crystallite size and shape. As will be shown in the paper, structural and microstructural parameters obtained by these methods may be correlated with thin film properties of technological interest. The whole pattern analysis may be used to obtain the information contained in a wide region of the diffraction pattern. This approach, currently used for the quantitative analysis of phase mixtures in traditional powder samples, was modified to account both for the size/strain effects, according to a simplified LPA, and for the structure of thin films and multi-layer systems. In this way, a detailed analysis based on a structural model for the present phases can be performed considering the real geometry of these samples. In particular, the quantitative phase analysis could be conducted in terms of layer thickness instead of volume or weight fractions.

  14. X-ray diffraction from thin films : Size/strain analysis and whole pattern fitting

    International Nuclear Information System (INIS)

    Scardi, P.

    1996-01-01

    Line Profile Analysis (LPA) and whole pattern fitting may be used with success for the characterization of thin films from XRD data collected with the traditional Bragg-Brentano geometry. The size/strain analysis was conducted by an integrated procedure of profile modelling-assisted Fourier analysis, in order to measure the content of lattice imperfections and crystalline domain size along the growth direction in heteroepitaxial thin films. The microstructure of these films is typical of several PVD processes for the production of highly textured and low-defect thin crystalline layers. The same analysis could be conducted on random thin films as well, and in this case it is possible to determine an average crystallite size and shape. As will be shown in the paper, structural and microstructural parameters obtained by these methods may be correlated with thin film properties of technological interest. The whole pattern analysis may be used to obtain the information contained in a wide region of the diffraction pattern. This approach, currently used for the quantitative analysis of phase mixtures in traditional powder samples, was modified to account both for the size/strain effects, according to a simplified LPA, and for the structure of thin films and multi-layer systems. In this way, a detailed analysis based on a structural model for the present phases can be performed considering the real geometry of these samples. In particular, the quantitative phase analysis could be conducted in terms of layer thickness instead of volume or weight fractions

  15. Study on the microstructure of recycled zircaloy by X-ray diffraction line profile analysis

    International Nuclear Information System (INIS)

    Ichikawa, Rodrigo U.; Pereira, Luiz A.T.; Imakuma, Kengo; Martinez, Luis G.; Turrillas, Xavier

    2013-01-01

    In the fabrication of nuclear fuel elements parts, Zircaloy machining chips are generated and, as this material is high-valued and controlled, its recycling presents high interest not only in economic aspects but also for environmental reasons and due to its strategic role in nuclear technology. Two processes for the recovery of these Zircaloy chips are being studied at IPEN-CNEN/SP. One of the processes is by conventional remelting of the material in a VAR (Vacuum Arc Remelting) furnace for producing solid ingots. Concurrently it is being studied an alternative process, by powder metallurgy methods, by which the chips are hydrided in order to become brittle and be grinded. The resulting ground powder is then compacted and finally vacuum-dehydrided and sintered in one step to form solid pieces. The VAR-remelted samples were also submitted to heat treatments in order to refine their microstructures, resulting in three different samples named 'as cast', 'annealed' and 'tempered'. The microstructures resulting from both processes and also from heat treatments were studied by metallography and X-ray diffraction (XRD). In this work, results of a XRD study are presented applying X-ray diffraction Line Profile Analysis (XLPA) methods in order to determine the mean crystallite sizes and the RMS microstrains on these samples. Additionally, a study for verify the influence of different standard materials used for the correction of the instrumental breadth in the XLPA was developed. The XLPA results show the influence of the processes and also of heat treatments on mean crystallite sizes and microstrains of the samples and were compared to their metallographic study and hardness. (author)

  16. Water Outgassing from PBX-9502 powder by isoconversional thermal analysis

    International Nuclear Information System (INIS)

    Dinh, L.N.; Glascoe, E.L.; Small, W.

    2009-01-01

    Temperature programmed desorption/decomposition (TPD) were performed on PBX-9502 after 3 hours of vacuum pump. TPD data were analyzed by the technique of isoconversional analysis to obtain outgassing kinetics and moisture content of PBX-9502 powder as well as to construct water outgassing models for PBX-9502 powder as a function of time and temperature. Following 3 hours of vacuum pump, dry storage of PBX-9502 at 300K, quickly gives rise to 180-330 ppm moisture in the first few years. Thereafter, the moisture outgassing continues at a much slower rate, totaling only to ∼ 210-380 ppm after 100 years of storage. In an effort to understand the nature of the moisture outgassing in PBX-9502, we have measured moisture content and outgassing kinetics in PBX-9502 by the experimental technique of TPD and the isoconversional thermal analysis. The results of these measurements were then used to construct moisture outgassing models for PBX-9502 in a dry environment (following 3 hours of vacuum pump)

  17. Surface quality analysis of die steels in powder-mixed electrical discharge machining using titan powder in fine machining

    Directory of Open Access Journals (Sweden)

    Banh Tien Long

    2016-06-01

    Full Text Available Improving the quality of surface molds after electrical discharge machining is still being considered by many researchers. Powder-mixed dielectric in electrical discharge machining showed that it is one of the processing methods with high efficiency. This article reports on the results of surface quality of mold steels after powder-mixed electrical discharge machining using titanium powder in fine machining. The process parameters such as electrode material, workpiece material, electrode polarity, pulse on-time, pulse off-time, current, and titanium powder concentration were considered in the research. These materials are most commonly used with die-sinking electrical discharge machining in the manufacture of molds and has been selected as the subject of research: workpiece materials were SKD61, SKT4, and SKD11 mold steels, and electrode materials were copper and graphite. Taguchi’s method is used to design experiments. The influence of the parameters on surface roughness was evaluated through the average value and ratio (S/N. Results showed that the parameters such as electrical current, electrode material, pulse on-time, electrode polarity, and interaction between the electrode materials with concentration powder mostly influence surface roughness and surface roughness at optimal parameters SRopt = 1.73 ± 0.39 µm. Analysis of the surface layer after powder-mixed electrical discharge machining using titanium powder in optimal conditions has shown that the white layer with more uniform thickness and increased hardness (≈861.0 HV, and amount and size of microscopic cracks, is reduced. This significantly leads to the increase in the quality of the surface layer.

  18. Analysis and interpretation of diffraction data from complex, anisotropic materials

    Science.gov (United States)

    Tutuncu, Goknur

    Most materials are elastically anisotropic and exhibit additional anisotropy beyond elastic deformation. For instance, in ferroelectric materials the main inelastic deformation mode is via domains, which are highly anisotropic crystallographic features. To quantify this anisotropy of ferroelectrics, advanced X-ray and neutron diffraction methods were employed. Extensive sets of data were collected from tetragonal BaTiO3, PZT and other ferroelectric ceramics. Data analysis was challenging due to the complex constitutive behavior of these materials. To quantify the elastic strain and texture evolution in ferroelectrics under loading, a number of data analysis techniques such as the single peak and Rietveld methods were used and their advantages and disadvantages compared. It was observed that the single peak analysis fails at low peak intensities especially after domain switching while the Rietveld method does not account for lattice strain anisotropy although it overcomes the low intensity problem via whole pattern analysis. To better account for strain anisotropy the constant stress (Reuss) approximation was employed within the Rietveld method and new formulations to estimate lattice strain were proposed. Along the way, new approaches for handling highly anisotropic lattice strain data were also developed and applied. All of the ceramics studied exhibited significant changes in their crystallographic texture after loading indicating non-180° domain switching. For a full interpretation of domain switching the spherical harmonics method was employed in Rietveld. A procedure for simultaneous refinement of multiple data sets was established for a complete texture analysis. To further interpret diffraction data, a solid mechanics model based on the self-consistent approach was used in calculating lattice strain and texture evolution during the loading of a polycrystalline ferroelectric. The model estimates both the macroscopic average response of a specimen and its hkl

  19. Size and surface AREA analysis of some metallic and intermetallic powders

    International Nuclear Information System (INIS)

    Elmasry, M.A.A.; Elsayed, A.A.; Abadir, M.F.

    1988-01-01

    The powder characterization of three intermetallic compounds ( Cr B, B 4 c and S ib 4 ) and three metallic powders (Fe, Co, and Ni) has been performed. This included the determination of powder density, chemical analysis, impurity analysis, shape factor, particle size analysis and specific surface area. The particle size analysis for the six powders was carried out using three techniques, namely; the 0-23, the microtrac and the fisher sub sieve and size. It was found that the analysis of the two powders and deviates from the log-normal probability distribution and the deviation was corrected. The specific surface area of the powders was measured using the high speed surface area analysis (BET method), and it was also calculated from surface area analysis findings, the BET technique was found to give the highest specific surface area values, and was attributed to the inclusion of internal porosity in the measurement. 8 fig., 10 tab

  20. Structure and thermal expansion of Ca9Gd(VO4)7: A combined powder-diffraction and dilatometric study of a Czochralski-grown crystal

    Science.gov (United States)

    Paszkowicz, Wojciech; Shekhovtsov, Alexei; Kosmyna, Miron; Loiko, Pavel; Vilejshikova, Elena; Minikayev, Roman; Romanowski, Przemysław; Wierzchowski, Wojciech; Wieteska, Krzysztof; Paulmann, Carsten; Bryleva, Ekaterina; Belikov, Konstantin; Fitch, Andrew

    2017-11-01

    Materials of the Ca9RE(VO4)7 (CRVO) formula (RE = rare earth) and whitlockite-related structures are considered for applications in optoelectronics, e.g., in white-light emitting diodes and lasers. In the CRVO structure, the RE atoms are known to share the site occupation with Ca atoms at two or three among four Ca sites, with partial occupancy values depending on the choice of the RE atom. In this work, the structure and quality of a Czochralski-grown crystal of this family, Ca9Gd(VO4)7 (CGVO), are studied using X-ray diffraction methods. The room-temperature structure is refined using the powder diffraction data collected at a high-resolution synchrotron beamline ID22 (ESRF, Grenoble); for comparison purposes, a laboratory diffraction pattern was collected and analyzed, as well. The site occupancies are discussed on the basis of comparison with literature data of isostructural synthetic crystals of the CRVO series. The results confirm the previously reported site-occupation scheme and indicate a tendency of the CGVO compound to adopt a Gd-deficient composition. Moreover, the thermal expansion coefficient is determined for CGVO as a function of temperature in the 302-1023 K range using laboratory diffraction data. Additionally, for CGVO and six other single crystals of the same family, thermal expansion is studied in the 298-473 K range, using the dilatometric data. The magnitude and anisotropy of thermal expansion, being of importance for laser applications, are discussed for these materials.

  1. Quantitative description of microstructure defects in hexagonal boron nitrides using X-ray diffraction analysis

    International Nuclear Information System (INIS)

    Schimpf, C.; Motylenko, M.; Rafaja, D.

    2013-01-01

    A routine for simultaneous quantification of turbostratic disorder, amount of puckering and the dislocation and stacking fault density in hexagonal materials was proposed and tested on boron nitride powder samples that were synthesised using different methods. The routine allows the individual microstructure defects to be recognised according to their effect on the anisotropy of the X-ray diffraction line broadening. For quantification of the microstructure defects, the total line broadening is regarded as a linear combination of the contributions from the particular defects. The total line broadening is obtained from the line profile fitting. As testing material, graphitic boron nitride (h-BN) was employed in the form of hot-isostatically pressed h-BN, pyrolytic h-BN or a h-BN, which was chemically vapour deposited at a low temperature. The kind of the dominant microstructure defects determined from the broadening of the X-ray diffraction lines was verified by high resolution transmission electron microscopy. Their amount was attempted to be verified by alternative methods. - Highlights: • Reliable method for quantification of microstructure defects in BN was suggested. • The method is based on the analysis of anisotropic XRD line broadening. • This XRD line broadening is unique and characteristic of the respective defect. • Thus, the quantification of coexistent microstructure defects is possible. • The method was tested on hexagonal BN, which was produced by different techniques

  2. Validation of missed space-group symmetry in X-ray powder diffraction structures with dispersion-corrected density functional theory.

    Science.gov (United States)

    Hempler, Daniela; Schmidt, Martin U; van de Streek, Jacco

    2017-08-01

    More than 600 molecular crystal structures with correct, incorrect and uncertain space-group symmetry were energy-minimized with dispersion-corrected density functional theory (DFT-D, PBE-D3). For the purpose of determining the correct space-group symmetry the required tolerance on the atomic coordinates of all non-H atoms is established to be 0.2 Å. For 98.5% of 200 molecular crystal structures published with missed symmetry, the correct space group is identified; there are no false positives. Very small, very symmetrical molecules can end up in artificially high space groups upon energy minimization, although this is easily detected through visual inspection. If the space group of a crystal structure determined from powder diffraction data is ambiguous, energy minimization with DFT-D provides a fast and reliable method to select the correct space group.

  3. X-ray mapping in heterocyclic design: IV. Crystal structure determination of 3-(p-nitrobenzoyl)-2-oxooxazolo[3,2-a]pyridine from powder diffraction data

    International Nuclear Information System (INIS)

    Rybakov, V.B.; Zhukov, S.G.; Babaev, E.V.; Sonneveld, E.J.

    2001-01-01

    The structure of 3-(p-nitrobenzoy)-2-oxooxazolo[3,2-a]pyridine is determined by the powder diffraction technique. The crystals are monoclinic, a = 13.642(2) A, b = 22.278(3) A, c = 3.917(1) A, β = 90.63(2) deg., Z 4, and space group P2 1 /n. The structure is solved by a modified Monte Carlo method and refined by the Reitveld method. The six-membered heterocycle is characterized by the alternation of partially single and partially double bonds. The system of two conjugated heterocycles is planar and forms a dihedral angle of 46.1(1) deg. with the plane of the phenyl ring. The nitro group is virtually coplanar with the phenyl fragment. An extensive system of intramolecular and intermolecular contacts involving hydrogen, oxygen, and nitrogen atoms is observed in the crystal

  4. Quadrupole lamp furnace for high temperature (up to 2050 K) synchrotron powder x-ray diffraction studies in air in reflection geometry

    International Nuclear Information System (INIS)

    Sarin, P.; Yoon, W.; Jurkschat, K.; Zschack, P.; Kriven, W. M.

    2006-01-01

    A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures ≤2050 K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A material with well characterized lattice expansion properties was used as an internal crystallographic thermometer to determine the specimen temperature and displacement. The performance of the apparatus was verified by measurement of the thermal expansion properties of CeO 2 , MgO, and Pt which were found to be within ±3% of the acceptable values. The advantages, limitations, and important considerations of the instrument developed are discussed

  5. X-ray diffraction analysis of InAs nanowires

    International Nuclear Information System (INIS)

    Davydok, Anton

    2013-01-01

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

  6. Diffraction stress analysis of thin films; investigating elastic grain interaction

    International Nuclear Information System (INIS)

    Kumar, A.

    2005-12-01

    This work is dedicated to the investigation of specimens exhibiting anisotropic microstructures (and thus macroscopic elastic anisotropy) and/or inhomogeneous microstructures, as met near surfaces and in textured materials. The following aspects are covered: (i) Analysis of specimens with direction-dependent (anisotropic) elastic grain-interaction. Elastic grain-interaction determines the distribution of stresses and strains over the (crystallographically) differently oriented grains of a mechanically stressed polycrystal and the mechanical and diffraction (X-ray) elastic constants (relating (diffraction) lattice strains to mechanical stresses). Grain interaction models that allow for anisotropic, direction-dependent grain interaction have been developed very recently. The notion 'direction-dependent' grain-interaction signifies that different grain-interaction constraints prevail along different directions in a specimen. Practical examples of direction-dependent grain interaction are the occurrence of surface anisotropy in thin films and the surface regions of bulk polycrystals and the occurrence of grain-shape (morphological) texture. In this work, for the first time, stress analyses of thin films have been performed on the basis of these newly developed grain-interaction models. It has also been demonstrated that the identification of the (dominant) source of direction-dependent grain interaction is possible. The results for the grain interaction have been discussed in the light of microstructural investigations of the specimens by microscopic techniques. (ii) Analysis of specimens with depth gradients: Diffraction stress analysis can be hindered if gradients of the stress state, the composition or the microstructure occur in the specimen under investigation, as the so-called information depth varies in the course of a traditional stress measurement: Ambiguous results are thus generally obtained. In this work, a strategy for stress measurements at fixed

  7. 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...

  8. Resolution of the crystal structure of the deficient perovskite LaNiO2.5 from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Alonso, J.A.; Martinez-Lope, M.J.

    1996-01-01

    The oxygen-deficient perovskite LaNiO 2.5 has been prepared by controlled reduction of LaNiO 3 with Zr metal. The XRD pattern could be indexed in a monoclinic unit-cell with dimensions a 0 xa 0 xa 0 (a 0 : lattice parameter of the ideal cubic perovskite). The indexing of the neutron powder diffraction pattern needed a doubled cell to account for the superstructure reflections originated by the oxygen vacancy ordering and the tilting of the Ni coordination polyhedra. The structure was solved and refined from the neutron powder data. The oxygen vacancies are ordered in such a way that square planar NiO 4 and NiO 6 octahedra alternate in the ab plane along the [110] direction. Both kinds of Ni polyhedra are fairly distorted and tilted in order to optimize the La-O distances, giving rise to a highly strained structure of metastable character. In fact, the compound readily takes oxygen, above 175 C in air, to give the much more stable LaNiO 3 perovskite. (orig.)

  9. X-ray Microprobe for Fluorescence and Diffraction Analysis

    International Nuclear Information System (INIS)

    Ice, G.E.

    2005-01-01

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

  10. Soil texture analysis by laser diffraction - standardization needed

    DEFF Research Database (Denmark)

    Callesen, Ingeborg; Palviainen, M.; Kjønaas, O. Janne

    2017-01-01

    Soil texture is a central soil quality property. Laser diffraction (LD) for determination of particle size distribution (PSD) is now widespread due to easy analysis and low cost. However, pretreatment methods and interpretation of the resulting soil PSD’s are not standardized. Comparison of LD data...... with sedimentation and sieving data may cause misinterpretation and confusion. In literature that reports PSD’s based on LD, pretreatment methods, operating procedures and data methods are often underreported or not reported, although literature stressing the importance exists (e.g. Konert and Vandenberghe, 1997...... and many newer; ISO 13320:2009). PSD uncertainty caused by pretreatments and PSD bias caused by plate-shaped clay particles still calls for more method standardization work. If LD is used more generally, new pedotransfer functions for other soil properties (e.g water retention) based on sieving...

  11. Dynamics from diffraction

    International Nuclear Information System (INIS)

    Goodwin, Andrew L.; Tucker, Matthew G.; Cope, Elizabeth R.; Dove, Martin T.; Keen, David A.

    2006-01-01

    We explore the possibility that detailed dynamical information might be extracted from powder diffraction data. Our focus is a recently reported technique that employs statistical analysis of atomistic configurations to calculate dynamical properties from neutron total scattering data. We show that it is possible to access the phonon dispersion of low-frequency modes using such an approach, without constraining the results in terms of some pre-defined dynamical model. The high-frequency regions of the phonon spectrum are found to be less well preserved in the diffraction data

  12. Crystal structure relation between tetragonal and orthorhombic CsAlD{sub 4}: DFT and time-of-flight neutron powder diffraction studies

    Energy Technology Data Exchange (ETDEWEB)

    Bernert, Thomas; Krech, Daniel; Felderhoff, Michael; Weidenthaler, Claudia [Department of Heterogeneous Catalysis, Max-Planck-Institut fuer Kohlenforschung, Muelheim/Ruhr (Germany); Kockelmann, Winfried [Rutherford Appleton Laboratory, Harwell Oxford, Didcot (United Kingdom); Frankcombe, Terry J. [Research School of Chemistry, The Australian National University, Canberra, ACT (Australia); School of Physical, Environmental and Mathematic Sciences, The University of New South Wales, Canberra, ACT (Australia)

    2015-11-15

    The crystal structures of orthorhombic and tetragonal CsAlD{sub 4} were refined from time-of-flight neutron powder diffraction data starting from atomic positions predicted from DFT calculations. The earlier proposed crystal structure of orthorhombic CsAlH{sub 4} is confirmed. For tetragonal CsAlH{sub 4}, DFT calculations predicted a crystal structure in I4{sub 1}/amd as potential minimum structure, while from neutron diffraction studies of CsAlD{sub 4} best refinement is obtained for a disordered structure in the space group I4{sub 1}/a, with a = 5.67231(9) Aa, c = 14.2823(5) Aa. While the caesium atoms are located on the Wyckoff position 4b and aluminium at Wyckoff position 4a, there are two distinct deuterium positions at the Wyckoff position 16f with occupancies of 50 % each. From this structure, the previously reported phase transition between the orthorhombic and tetragonal polymorphs could be explained. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Fine crystalline powders. Analysis of scientific and technical literature

    International Nuclear Information System (INIS)

    Denisenko, Eh.T.; Kulik, O.P.; Eremina, T.V.

    1983-01-01

    The state of development and studies of fine crystalline powders for recent five years is reviewed in the paper. Based on data available in literature, the most significant methods for fine metal and alloy powder production are considered and physicochemical properties of ultrafine particles are discussed from the standpoint of their interrelation with promising techniques for powder production. It is stated that the most important feature of ultrafine powder production technique at the present stage is a transition from the stage of data accumulation to that of controlled production of ultrafine structures of various metals and alloys under controllable conditions

  14. Neutron powder diffraction investigation of magnetic structure and spin reorientation transition of HoFe{sub 1-x}Cr{sub x}O{sub 3} solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xinzhi [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Hao, Lijie, E-mail: haolijie@ciae.ac.cn [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Liu, Yuntao; Ma, Xiaobai; Meng, Siqin; Li, Yuqing; Gao, Jianbo; Guo, Hao; Han, Wenze; Sun, Kai; Wu, Meimei [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China); Chen, Xiping; Xie, Lei [Institute of Nuclear Physics and Chemistry, CAEP, Mianyang 621900 (China); Klose, Frank [Australian Nuclear Science and Technology Organization, Lucas Heights, New South Wales 2234 (Australia); Department of Physics and Materials Science, The City University of Hong Kong, Hong Kong (China); Chen, Dongfeng, E-mail: dongfeng@ciae.ac.cn [Department of Nuclear Physics, China Institute of Atomic Energy, Beijing 102413 (China)

    2016-11-01

    Orthoferrite solid solution HoFe{sub 1−x}Cr{sub x}O{sub 3} (x=0, 0.2,…,1.0) was synthesized via solid state reaction methods. The crystal structure, magnetism and spin reorientation properties of this system were investigated by X-ray diffraction, neutron powder diffraction and magnetic measurements. For compositions of x≤0.6, the system exhibits similar magnetic properties to HoFeO{sub 3}. With increasing Cr-doping, the system adopts a Γ{sub 4}(G{sub x}A{sub y}F{sub z}) magnetic configuration with a decreased Neel temperature from 640 K to 360 K. A Γ{sub 42} spin reorientation of Fe(Cr){sup 3+} was also observed in this system with an increase in transition temperature from 56 K to about 200 K due to competition between the Fe(Cr)–Fe(Cr) and Ho–Fe(Cr) interactions. For the x≥0.8, the system behaves more like HoCrO{sub 3} which adopts a Γ{sub 2}(F{sub x}C{sub y}G{sub z}) configuration with no spin reorientation below the Neel temperature T{sub N}. Throughout the whole substitution range, we found that the saturated moment of Fe(Cr) was less than the ideal value for a free ion, which implies the existence of spin fluctuation in this system. A systematic magnetic structure variation with Cr-substitution is revealed by Rietveld refinement. A phase diagram combining the results of the magnetic measurements and neutron powder diffraction results was obtained. - Highlights: • With Cr-substitution in the HoFe{sub 1−x}Cr{sub x}O{sub 3} system, A Γ{sub 42} spin reorientation of Fe(Cr){sup 3+} was observed with an increase in transition temperature from 56 K to about 200 K for x=0−0.6. • The saturated moment of Fe(Cr) position was found to be systematically less than the ideal value of free ion, and thus implies the presence of spin quantum fluctuation. • A composition–temperature phase diagram throughout x=0–1 for HoFe{sub 1−x}Cr{sub x}O{sub 3} system was established.

  15. Rapid flow cytometry analysis of antimicrobial properties of nettle powder and cranberry powder

    Science.gov (United States)

    Hattuniemi, Maarit; Korhonen, Johanna; Jaakkola, Mari; Räty, Jarkko; Virtanen, Vesa

    2010-11-01

    Both nettle (Urtica dioica) and cranberry (Vaccinium oxycoccus) are widely known to have good influence on health. The aim of this study was to investigate antimicrobial properties of nettle powder and cranberry powder against Escherichia coli (E. coli) and monitor the growth of the bacteria by a rapid flow cytometry (FCM) method. For FCM measurements samples were stained with fluorescent dyes. The inhibitory effects of plant material on growth of E. coli were estimated by comparing the results of control sample (E. coli) to E. coli samples with plant material. FCM offers both a brilliant tool to investigate the kinetics of the growth of bacterium, since subsamples can be taken from the same liquid medium during the growing period and with fluorescent dyes a rapid method to investigate viability of the bacterium.

  16. ATLAS - analysis of time-of-flight diffraction data from liquid and amorphous samples

    International Nuclear Information System (INIS)

    Soper, A.K.; Howells, W.S.; Hannon, A.C.

    1989-05-01

    The purpose of this manual is to describe a package of data analysis routines which have been developed at the Rutherford Appleton Laboratory for the analysis of time-of-flight diffraction data from liquids, gases, and amorphous materials. There is no fundamental barrier to diffraction data being accurately analysed to structure factor or even pair correlation function within a very short time of the completion of the experiment. Section 1 describes the time-of-flight neutron diffraction experiment and looks at diffraction theory. Section 2 indicates the steps in data analysis of time-of-flight diffraction data and Section 3 gives details of how to run the procedures. (author)

  17. Polymorphous transformation in the crystal structure of [Mg(H.sub.2./sub.O).sub.6./sub. Br.sub.2./sub.][(C.sub.7./sub.H.sub.14./sub.N.sub.4./sub.).sub.2./sub.] . 4 (H.sub.2./sub.O) studied by powder and single crystal X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Rivera, A.; Rohlíček, Jan; Sadat-Bernal, J.; Ríos-Motta, J.; Dušek, Michal

    2014-01-01

    Roč. 229, č. 4 (2014), s. 319-327 ISSN 0044-2968 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : polymorphism * powder X-ray * single crystal diffraction * 1,3,6,8-tetraazatricyclo[4.3.1.13,ˑ 8]undecane * phase transformation * crystal structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.310, year: 2014

  18. Effect of Cu{sup 2+} and Ni{sup 2+} substitution at the Mn site in (La{sub 0.63}Ca{sub 0.37})MnO{sub 3}: A neutron powder diffraction investigation

    Energy Technology Data Exchange (ETDEWEB)

    Martinelli, A., E-mail: alberto.martinelli@spin.cnr.it [CNR-SPIN, C.so Perrone 24, 16152 Genova (Italy); Ferretti, M. [CNR-SPIN, C.so Perrone 24, 16152 Genova (Italy); Dipartimento di Chimica e Chimica Industriale, Università di Genova, Via Dodecaneso 31, 16146 Genova (Italy); Castellano, C. [Università degli Studi di Milano, Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Via G. Venezian 21, 20133 Milano (Italy); Cimberle, M.R. [IMEM-CNR, Via Dodecaneso 33, 16146 Genova (Italy); Ritter, C. [Institute Laue—Langevin, 6 rue Jules Horowitz, 38042 Grenoble Cedex 9 (France)

    2013-04-15

    The crystal and magnetic structures of the (La{sub 0.63}Ca{sub 0.37})(Mn{sub 1−x}TM{sub x})O{sub 3} compounds (x=0.00, 0.03, 0.08; TM=Cu{sup 2+}, Ni{sup 2+}) were investigated between 5 K and 300 K by means of dc magnetic measurements and neutron powder diffraction analysis followed by Rietveld refinement. Both substituting cations lead to a reduction of the long range ferromagnetic ordering temperature; ferromagnetism is strongly suppressed in the 8% Cu-substituted sample, where long- and short-range FM magnetic orders coexist together with short-range A-type AFM order. This particular feature can be related to the Jahn–Teller character of Cu{sup 2+}, absent in Ni{sup 2+}, and suggests the occurrence of a quantum critical point in the (La{sub 0.63}Ca{sub 0.37})(Mn{sub 1−x}Cu{sub x})O{sub 3} system. - Graphical abstract: Rietveld refinement plot of (La{sub 0.63}Ca{sub 0.37})(Mn{sub 0.92}Cu{sub 0.08})O{sub 3} showing in the inset the coexistence of broad A-type AFM peaks with FM ones. Highlights: ► (La{sub 0.63}Ca{sub 0.37})MnO{sub 3} was substituted with Ni and Cu. ► Neutron powder diffraction and Rietveld refinement were carried out. ► A quantum critical point possibly occurs in the (La{sub 0.63}Ca{sub 0.37})(Mn{sub 1−x}Cu{sub x})O{sub 3} system.

  19. Sensory analysis of cosmetic powders: personal care ingredients and emulsions.

    Science.gov (United States)

    Moussour, M; Lavarde, M; Pensé-Lhéritier, A-M; Bouton, F

    2017-02-01

    The powders are ingredients increasingly used in the formulation of cosmetic products for the sensory qualities they give. The objective of this study was the development of a lexicon and a referential for sensory characterization of these pure raw materials as well as formulations which contain them. Eleven expert panellists from Ecole de biologie industrielle de Cergy (France) developed a lexicon and a referential based on 12 powders of different chemical natures. The selected attributes were then used for performing a quantitative descriptive profile of two powders and an emulsion containing or not one of these two powders. A lexicon has been established through a consensus approach of the panel. It contains seven attributes that allow the evaluation of the powders in four phases: the appearance, the pickup, the application and the after-feel. This lexicon contains definitions and assessment protocols and provides references products. The quantitative descriptive profile of two powders of the same chemical nature, but different in physical quality showed significant differences in sensory level between products. These same attributes used to evaluate an emulsion containing the powder or not allowed to prove the contribution of these raw materials on the sensory specificities of the emulsion. The lexicon developed in this study can be used for assessment of other powders but also to define the quantities necessary to put in the formulation to meet the sensory characteristics of these raw materials powder. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  20. Application of the whole powder pattern decomposition procedure in the residual stress analysis of layers and coatings

    International Nuclear Information System (INIS)

    Schoderböck, Peter; Brechbühl, Jens

    2015-01-01

    The X-ray investigation of stress states in materials, based on the determination of elastic lattice strains which are converted to stresses by means of theory of elasticity, is a necessity in quality control of thin layers and coatings for optimizing manufacturing steps and process parameters. This work introduces the evaluation of residual stress from complex and overlapping diffraction patterns using a whole-powder pattern decomposition procedure defining a 2θ-offset caused by residual stresses. Furthermore corrections for sample displacement and refraction are directly implemented in the calculation procedure. The correlation matrices of the least square fitting routines have been analyzed for parameter interactions and obvious interdependencies have been decoupled by the introduction of an internal standard within the diffraction experiment. This decomposition based evaluation has been developed on tungsten as a model material system and its efficiency was demonstrated by X-ray diffraction analysis of a solid oxide fuel cell multilayer system. The results are compared with those obtained by the classical sin 2 Ψ-method. - Highlights: • Analysis of complex multiphase diffraction patterns with respect to residual stress • Stress-gradient determination with in situ correction of displacement and refraction • Consideration of the elastic anisotropy within the refinement

  1. Neutron Powder Diffraction Measurements of the Spinel MgGa2O4:Cr3+ - A Comparative Study between the High Flux Diffractometer D2B at the ILL and the High Resolution Powder Diffractometer Aurora at IPEN

    International Nuclear Information System (INIS)

    Da Silva, M A F M; Sosman, L P; Yokaichiya, F; Henry, P F; Bordallo, H N; Mazzocchi, V L; Parente, C B R; Mestnik-Filho, J

    2012-01-01

    Optical materials that emit from the visible to the near-infrared spectral region are of great interest due to their possible application as tunable radiation sources, as signal transmission, display, optoelectronics signal storage, cellulose industry as well as in dosimetry. One important family of such systems are the spinel compounds doped with Cr 3+ , in which the physical the properties are related to the insertion of punctual defects in the crystalline structure. The purpose of our work is two fold. First, we compare the luminescence of the MgGa 2 O 4 -Ga 2 O 3 system with the single phase Ga 2 O 3 and MgGa 2 O 4 and relate structural changes observed in MgGa 2 O 4 -Ga 2 O 3 system to the optical properties, and secondly, to compare the neutron powder diffraction results obtained using two diffractometers: D2B located at the ILL (Grenoble, France) and Aurora located at IPEN (São Paulo, Brazil). In the configuration chosen, Aurora shows an improved resolution, which is related to the design of its silicon focusing monochromator.

  2. Comparison of laser diffraction and image analysis for measurement of Streptomyces coelicolor cell clumps and pellets

    DEFF Research Database (Denmark)

    Rønnest, Nanna Petersen; Stocks, Stuart M; Eliasson Lantz, Anna

    2012-01-01

    and pellets of Streptomyces coelicolor compare to image analysis. Samples, taken five times during fed-batch cultivation, were analyzed by image analysis and laser diffraction. The volume-weighted size distribution was calculated for each sample. Laser diffraction and image analysis yielded similar size...

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  4. 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

  5. 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.

  6. 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)

  7. Pressure dependence of hydrogen bonding in metal deuteroxides: a neutron powder diffraction study of Mn(OD)2 and β-Co(OD)2

    International Nuclear Information System (INIS)

    Parise, J.B.; Theroux, B.; Li, R.; Loveday, J.S.; Marshall, W.G.; Klotz, S.

    1998-01-01

    The structures of deuterated pyrochroite, Mn(OD) 2 and β-Co(OD) 2 have been refined using the Rietveld method and neutron powder diffraction data collected in an opposed-anvil high pressure (Paris-Edinburgh) cell from room pressure to 9 GPa. The equation of state for Mn(OD) 2 was determined (K=41(3) GPa for fixed K'=4.7) and found to be consistent with previous studies of the isostructural brucite, Mg(OD) 2 . The compressibility of β-Co(OD) 2 on the other hand is apparently anomalous. The c-axis initially decreases at 3 times the rate of decrease of the a-axis; the ratio decreases to about 1.5 at an estimated 6 GPa before increasing again beyond this pressure. There is no obvious corresponding anomaly in the details of the atomic structure. In both materials there is an increase in the D-site disorder with pressure. A split-site model for the D-positions best fits the data at pressures above 8 GPa. There is no statistically significant increase in the O-D interatomic distance at increased pressure while the hydrogen bonding interaction D..O appears to increase as this distance decreases and the O-D..O angle increases. The intramolecular O-D bond valences, determined indirectly from the intermolecular D..O distances, decrease steadily for both materials as pressure is increased. (orig.)

  8. Magnetic and electronic properties of RNiO{sub 3} (R = Pr, Nd, Eu, Ho and Y) perovskites studied by resonant soft x-ray magnetic powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Bodenthin, Y; Staub, U; Piamonteze, C; Garcia-Fernandez, M [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Martinez-Lope, M J; Alonso, J A, E-mail: urs.staub@psi.ch [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2011-01-26

    Soft x-ray resonant magnetic powder diffraction of the (1/2 0 1/2) reflection at the Ni L{sub 2,3} edges is used to study the magnetic and electronic properties of a series of RNiO{sub 3} materials (with R = Pr, Nd, Eu, Ho and Y) below the metal-insulator transition. The polarization and energy dependence of the reflection gives further support for a non-collinear magnetic structure and charge disproportionation in the whole RNiO{sub 3} series. Only small changes in the spectra of the magnetic (1/2 0 1/2) reflection and in the absorption spectra could be detected. The results are discussed with comparison to charge transfer multiplet calculations. Our results emphasize that the lighter and heavier RNiO{sub 3} compounds are very similar from the point of view of their local electronic and magnetic state despite the strong change of the metal-to-insulator transition temperature.

  9. The structural phase diagram and oxygen equilibrium partial pressure of YBa 2Cu 3O 6+ x studied by neutron powder diffraction and gas volumetry

    Science.gov (United States)

    Andersen, N. H.; Lebech, B.; Poulsen, H. F.

    1990-12-01

    An experimental technique based on neutron powder diffraction and gas volumetry is presented and used to study the structural phase diagram of YBa 2Cu 3O 6+ x under equilibrium conditions in an extended part of ( x, T)-phase (0.15< x<0.92 and 25° C< T<725°C). Our experimental observations lend strong support to a recent two-dimensional anisotropic next-nearest-neighbour Ising model calculation (the ASYNNNI model) of the basal plane oxygen ordering based of first principle interaction parameters. Simultaneous measurements of the oxygen equilibrium partial pressure show anomalies, one of which proves the thermodynamic stability of the orthorhombic OII double cell structure. Striking similarity with predictions of recent model calculations support that another anomaly may be interpreted to result from local one-dimensional fluctuations in the distribution of oxygen atoms in the basal plane of tetragonal YBCO. Our pressure data also indicate that x=0.92 is a maximum obtainable oxygen concentration for oxygen pressures below 760 Torr.

  10. Stacking Faults and Polytypes for Layered Double Hydroxides: What Can We Learn from Simulated and Experimental X-ray Powder Diffraction Data?

    Science.gov (United States)

    Sławiński, Wojciech A; Sjåstad, Anja Olafsen; Fjellvåg, Helmer

    2016-12-19

    Layered double hydroxides (LDH) are a broad group of widely studied materials. The layered character of those materials and their high flexibility for accommodating different metals and anions make them technologically interesting. The general formula for the LDH compound is [M 1-x II M x III (OH) 2 ][A n- ] x/n ·mH 2 O, where M II is a divalent metal cation which can be substituted by M III trivalent cation, and A n- is a charge compensating anion located between positively charged layers. In this paper we present a comprehensive study on possible structural disorder in LDH. We show how X-ray powder diffraction (XRPD) can be used to reveal important features of the LDH crystal structure such as stacking faults, random interlayer shifts, anion-molecule orientation, crystal water content, distribution of interlayer distances, and also LDH slab thickness. All calculations were performed using the Discus package, which gives a better flexibility in defining stacking fault sequences, simulating and refining XRPD patterns, relative to DIFFaX, DIFFaX+, and FAULTS. Finally, we show how the modeling can be applied to two LDH samples: Ni 0.67 Cr 0.33 (OH) 2 (CO 3 ) 0.16 ·mH 2 O (3D structure) and Mg 0.67 Al 0.33 (OH) 2 (NO 3 ) 0.33 (2D layered structure).

  11. The structure of denisovite, a fibrous nanocrystalline polytypic disordered `very complex' silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

    Directory of Open Access Journals (Sweden)

    Ira V. Rozhdestvenskaya

    2017-05-01

    Full Text Available Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD, electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM, selected-area electron diffraction (SAED, high-angle annular dark-field imaging (HAADF, high-resolution transmission electron microscopy (HRTEM, precession electron diffraction (PED and electron diffraction tomography (EDT. A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1, b = 19.554 (1 and c = 7.1441 (5 Å, β = 95.99 (3°, V = 4310.1 (5 Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100. Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being

  12. Production of muscovite-feldspathic glass composite: scanning electron microscopy and X-ray diffraction analysis

    International Nuclear Information System (INIS)

    Costa, F.P.F.; Ogasawara, T.; Santos, S.F.

    2009-01-01

    The objective of this work was to find the sintering conditions for the feldspathic glass + muscovite mixture to produce a dense composite block for manufacturing dental prosthesis by using CAD-CAM. Each 20g of the glass-frit had : 15.55g of Armil-feldspar; 0.53g of Al 2 O 3 ; 1.56g of Na 2 CO 3 ; 0.5g of borax; 1.74g of K 2 CO 3 ; 0.13g of CeO 2 . Frit's powder finer than 350 Tyler mesh was mixed with 0 wt%, 10 wt%, 20 wt% and 100 wt% of muscovite pressed cylinders (5600 pounds force) 16mm in diameter and sintered under vacuum Vacumat (VITA) furnace at 850 deg C, 900 deg C, 950 deg C, 1000 deg C, 1050 deg C, 1100 deg C and 1150 deg C. X-ray diffraction analysis and scanning electron microscopy were carried out. The necessary temperature for high densification depended on the composition of the mixture: 850 deg C (for pure frit); 1050 deg C (for 10 wt% mica) and 1150 deg C (for 20 wt% mica); pure mica degraded during sintering. (author)

  13. Classification using diffraction patterns for single-particle analysis

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Hongli; Zhang, Kaiming [Department of Biophysics, the Health Science Centre, Peking University, Beijing 100191 (China); Meng, Xing, E-mail: xmeng101@gmail.com [Wadsworth Centre, New York State Department of Health, Albany, New York 12201 (United States)

    2016-05-15

    An alternative method has been assessed; diffraction patterns derived from the single particle data set were used to perform the first round of classification in creating the initial averages for proteins data with symmetrical morphology. The test protein set was a collection of Caenorhabditis elegans small heat shock protein 17 obtained by Cryo EM, which has a tetrahedral (12-fold) symmetry. It is demonstrated that the initial classification on diffraction patterns is workable as well as the real-space classification that is based on the phase contrast. The test results show that the information from diffraction patterns has the enough details to make the initial model faithful. The potential advantage using the alternative method is twofold, the ability to handle the sets with poor signal/noise or/and that break the symmetry properties. - Highlights: • New classification method. • Create the accurate initial model. • Better in handling noisy data.

  14. Classification using diffraction patterns for single-particle analysis

    International Nuclear Information System (INIS)

    Hu, Hongli; Zhang, Kaiming; Meng, Xing

    2016-01-01

    An alternative method has been assessed; diffraction patterns derived from the single particle data set were used to perform the first round of classification in creating the initial averages for proteins data with symmetrical morphology. The test protein set was a collection of Caenorhabditis elegans small heat shock protein 17 obtained by Cryo EM, which has a tetrahedral (12-fold) symmetry. It is demonstrated that the initial classification on diffraction patterns is workable as well as the real-space classification that is based on the phase contrast. The test results show that the information from diffraction patterns has the enough details to make the initial model faithful. The potential advantage using the alternative method is twofold, the ability to handle the sets with poor signal/noise or/and that break the symmetry properties. - Highlights: • New classification method. • Create the accurate initial model. • Better in handling noisy data.

  15. Analysis of Minor Component Segregation in Ternary Powder Mixtures

    Directory of Open Access Journals (Sweden)

    Asachi Maryam

    2017-01-01

    Full Text Available In many powder handling operations, inhomogeneity in powder mixtures caused by segregation could have significant adverse impact on the quality as well as economics of the production. Segregation of a minor component of a highly active substance could have serious deleterious effects, an example is the segregation of enzyme granules in detergent powders. In this study, the effects of particle properties and bulk cohesion on the segregation tendency of minor component are analysed. The minor component is made sticky while not adversely affecting the flowability of samples. The segregation extent is evaluated using image processing of the photographic records taken from the front face of the heap after the pouring process. The optimum average sieve cut size of components for which segregation could be reduced is reported. It is also shown that the extent of segregation is significantly reduced by applying a thin layer of liquid to the surfaces of minor component, promoting an ordered mixture.

  16. Determination of interplanar distances starting from diffraction spectra for PC microcomputer

    International Nuclear Information System (INIS)

    Macias B, L.R.

    1991-07-01

    The objective of this work, consists in that starting of a digitized diffraction spectra result of the structural analysis technique, it is possible by means of the analysis of a computer program, to detect the diffraction peaks and well-known the wavelength to obtain the values of the interplanar distances to be compared with the JCPDS (Joint Committee on Powder Diffraction Standards). (Author)

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  18. Fast and accurate focusing analysis of large photon sieve using pinhole ring diffraction model.

    Science.gov (United States)

    Liu, Tao; Zhang, Xin; Wang, Lingjie; Wu, Yanxiong; Zhang, Jizhen; Qu, Hemeng

    2015-06-10

    In this paper, we developed a pinhole ring diffraction model for the focusing analysis of a large photon sieve. Instead of analyzing individual pinholes, we discuss the focusing of all of the pinholes in a single ring. An explicit equation for the diffracted field of individual pinhole ring has been proposed. We investigated the validity range of this generalized model and analytically describe the sufficient conditions for the validity of this pinhole ring diffraction model. A practical example and investigation reveals the high accuracy of the pinhole ring diffraction model. This simulation method could be used for fast and accurate focusing analysis of a large photon sieve.

  19. Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cummins, Dustin Ray [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Vogel, Sven C. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Hollis, Kendall Jon [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Donald William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dombrowski, David E. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-10-18

    This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to

  20. Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

    International Nuclear Information System (INIS)

    Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon; Brown, Donald William; Dombrowski, David E.

    2016-01-01

    This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to

  1. Quantitative mineralogical analysis of sandstones using x-ray diffraction techniques

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  2. Crystallization and diffraction analysis of thioredoxin reductase from Streptomyces coelicolor

    International Nuclear Information System (INIS)

    Koháryová, Michaela; Brynda, Jiří; Řezáčová, Pavlína; Kollárová, Marta

    2011-01-01

    Thioredoxin reductase from S. coelicolor was crystallized and diffraction data were collected to 2.4 Å resolution. Thioredoxin reductases are homodimeric flavoenzymes that catalyze the transfer of electrons from NADPH to oxidized thioredoxin substrate. Bacterial thioredoxin reductases represent a promising target for the development of new antibiotics. Recombinant thioredoxin reductase TrxB from Streptomyces coelicolor was crystallized using the hanging-drop vapour-diffusion method. X-ray diffraction data were collected from cryocooled crystals to 2.4 Å resolution using a synchrotron-radiation source. The crystals belonged to the primitive monoclinic space group P2 1 , with unit-cell parameters a = 82.9, b = 60.6, c = 135.4 Å, α = γ = 90.0, β = 96.5°

  3. Electron diffraction, elemental and image analysis of nanocrystals

    Czech Academy of Sciences Publication Activity Database

    Šlouf, Miroslav; Pavlova, Ewa; Hromádková, Jiřina; Králová, Daniela; Tyrpekl, Václav

    2009-01-01

    Roč. 16, 2a (2009), s. 33-34 ISSN 1211-5894. [Struktura - Colloquium of Czech and Slovak Crystallographic Association. Hluboká nad Vltavou, 22.06.2009-25.06.2009] R&D Projects: GA AV ČR KAN200520704; GA ČR GA203/07/0717 Institutional research plan: CEZ:AV0Z40500505 Keywords : TEM * electron diffraction * nanocrystals Subject RIV: CD - Macromolecular Chemistry

  4. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

    Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

    2015-07-01

    Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

  5. 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.

  6. Spectroscopic studies, theoretical models and structural characterization. II. Synthesis and X-ray powder diffraction of the elpasolites Cs2NaSmCl6

    International Nuclear Information System (INIS)

    Poblete, V.; Acevedo, R.

    1998-01-01

    In this research work, we report the synthesis and structural characterization of the stoichiometric elpasolite Cs 2 NaSmCl 6 . The synthesis was performed under a solid state reaction in nitrogen atmosphere from the chemicals CsCl, NaCl and SmCl 3 weighted stoichiometrically. The best possible crystallization temperature was obtained using thermal studies of the type DTA/TGA (the thermal treatment was allowed to proceed for 2.5 hours at 755 Centigrade, showing a temperature gradient of 10 Centigrade/minute). The structural characterization by powder X-ray diffraction (XDR) indicates that this elpasolite belongs to the Fm 3m (O h 5 ) space group and the optimized structural parameters are as follows: a 0 = 10.8342 Armstrong, V 1271.72 Armstrong 3 , Z=4, M=651.88, D x =3.406 y D exp=3.41 ± 0.01. The profile refinement, using the Rietveld method, allowed us to fit the experimental and the calculated intensities of a total of 32 lines. The above result indicates that the condition R exp 2+ + 3Cl -1 and the counter ions filling the octahedral holes, in full agreement with anti fluorite type crystal. According to the above description, these elpasolite adopt the form (M 1/3 □ 2/3 ) 4 X 2 , where M labels the central metal, X stand for the chlorine ions and □ represent the vacancies, which may accommodate a significant amount of defects without collapsing. This experimental study provides the necessary input to test theoretical models against experimental data. (Author)

  7. A global analysis of inclusive diffractive cross sections at HERA

    Energy Technology Data Exchange (ETDEWEB)

    Royon, C.; Schoeffel, L. [Service de Physique des Particules, CE-Saclay, F-91191 Gif-sur-Yvette Cedex (France); Sapeta, S. [M. Smoluchowski Institue of Physics Jagellonian University Reymonta 4, 30-059 Krakow (Poland); Peschanski, R. [Service de Physique Theorique, CE-Saclay, F-91191 Gif-sur-Yvette Cedex (France); Sauvan, E. [CPPM, IN2P3-CNRS et Universitie de la Mediterranee, F-13288 Marseille Cedex 09 (France)

    2006-10-15

    We describe the most recent data on the diffractive structure functions from the H1 and ZEUS Collaborations at HERA using four models. First, a Pomeron Structure Function (PSF) model, in which the Pomeron is considered as an object with parton distribution functions. Then, the Bartels Ellis Kowalski Wuesthoff (BEKW) approach is discussed, assuming the simplest perturbative description of the Pomeron using a two-gluon ladder. A third approach, the Bialas Peschanski (BP) model, based on the dipole formalism is then described. Finally, we discuss the Golec-Biernat-Wuesthoff (GBW) saturation model which takes into account saturation effects. The best description of all available measurements can be achieved with either the PSF based model or the BEKW approach. In particular, the BEKW prediction allows to include the highest {beta} measurements, which are dominated by higher twists effects and provide an efficient and compact parametrisation of the diffractive cross section. The two other models also give a good description of cross section measurements at small x with a small number of parameters. The comparison of all predictions allows us to identify interesting differences in the behaviour of the effective pomeron intercept and in the shape of the longitudinal component of the diffractive structure functions. In this last part, we present some features that can be discriminated by new experimental measurements, completing the HERA program. (authors)

  8. A global analysis of inclusive diffractive cross sections at HERA

    International Nuclear Information System (INIS)

    Royon, C.; Schoeffel, L.; Sapeta, S.; Peschanski, R.; Sauvan, E.

    2006-10-01

    We describe the most recent data on the diffractive structure functions from the H1 and ZEUS Collaborations at HERA using four models. First, a Pomeron Structure Function (PSF) model, in which the Pomeron is considered as an object with parton distribution functions. Then, the Bartels Ellis Kowalski Wuesthoff (BEKW) approach is discussed, assuming the simplest perturbative description of the Pomeron using a two-gluon ladder. A third approach, the Bialas Peschanski (BP) model, based on the dipole formalism is then described. Finally, we discuss the Golec-Biernat-Wuesthoff (GBW) saturation model which takes into account saturation effects. The best description of all available measurements can be achieved with either the PSF based model or the BEKW approach. In particular, the BEKW prediction allows to include the highest β measurements, which are dominated by higher twists effects and provide an efficient and compact parametrisation of the diffractive cross section. The two other models also give a good description of cross section measurements at small x with a small number of parameters. The comparison of all predictions allows us to identify interesting differences in the behaviour of the effective pomeron intercept and in the shape of the longitudinal component of the diffractive structure functions. In this last part, we present some features that can be discriminated by new experimental measurements, completing the HERA program. (authors)

  9. Effect of thermal treatment on mechanically milled cobalt powder

    CSIR Research Space (South Africa)

    Bolokang, AS

    2012-03-01

    Full Text Available Stabilization of the metastable FCC phase has been achieved after 10 h milled Co powder sintering at 1400 °C. Phase identification of the Co powders was performed by the X-ray diffraction analysis, while the microstructural analyses were performed...

  10. 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

  11. Quantum diffraction and interference of spatially correlated photon pairs and its Fourier-optical analysis

    International Nuclear Information System (INIS)

    Shimizu, Ryosuke; Edamatsu, Keiichi; Itoh, Tadashi

    2006-01-01

    We present one- and two-photon diffraction and interference experiments involving parametric down-converted photon pairs. By controlling the divergence of the pump beam in parametric down-conversion, the diffraction-interference pattern produced by an object changes from a quantum (perfectly correlated) case to a classical (uncorrelated) one. The observed diffraction and interference patterns are accurately reproduced by Fourier-optical analysis taking into account the quantum spatial correlation. We show that the relation between the spatial correlation and the object size plays a crucial role in the formation of both one- and two-photon diffraction-interference patterns

  12. Light extinction in metallic powder beds: Correlation with powder structure

    International Nuclear Information System (INIS)

    Rombouts, M.; Froyen, L.; Gusarov, A.V.; Bentefour, E.H.; Glorieux, C.

    2005-01-01

    A theoretical correlation between the effective extinction coefficient, the specific surface area, and the chord length distribution of powder beds is verified experimentally. The investigated powder beds consist of metallic particles of several tens of microns. The effective extinction coefficients are measured by a light-transmission technique at a wavelength of 540 nm. The powder structure is characterized by a quantitative image analysis of powder bed cross sections resulting in two-point correlation functions and chord length distributions. The specific surface area of the powders is estimated by laser-diffraction particle-size analysis and by the two-point correlation function. The theoretically predicted tendency of increasing extinction coefficient with specific surface area per unit void volume is confirmed by the experiments. However, a significant quantitative discrepancy is found for several powders. No clear correlation of the extinction coefficient with the powder material and particle size, and morphology is revealed, which is in line with the assumption of geometrical optics

  13. X-ray diffraction analysis device with electronic photon counter

    International Nuclear Information System (INIS)

    Fillit, R.Y.; Bruyas, H.; Patay, F.

    1985-01-01

    The means provided to control the movements around the three axes are composed of step-by-step motors related to exits control logic which is connected to the calculation and monitored by a clock. The clock monitors also the calculator so as that the calculator controls, together with the programmable clock and control logic, the coordination of the whole rotation movements, along the three rotation axes, their velocity, their duration and the acquisition of the measured intensities of the diffracted X-ray beam [fr

  14. Diffraction analysis of materials under strong plastic deformation

    International Nuclear Information System (INIS)

    Pyzalla, A.

    2001-01-01

    The applicability of X-ray diffraction in analyses of the microstructure texture and intrinsic stresses of materials under strong plastic deformation is illustrated by examples and discussed. The experimental methods and findings are supplemented by numeric calculations. It is shown how the microstructure, texture and intrinsic stresses can thus be optimized already in the production process. Analyses of changes in materials during operation of a component provide information on loads and material response to loads which can then be used for optimization of the component, e.g. by constructional modifications or selective heat treatment [de

  15. 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 ...

  16. Quantitative analysis of minerals by X-ray diffraction

    International Nuclear Information System (INIS)

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

    1982-01-01

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

  17. 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

    This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs {sup 3}{sub ∞}[Ln(Tz{sup *}){sub 3}]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln{sup 3+}-ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds {sup 2}{sub ∞}[Ln(Tz{sup *}){sub 3}], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer {sup 1}{sub ∞}[Eu(Btz){sub 2}(BtzH){sub 2}], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF {sup 3}{sub ∞}[Eu(Btz){sub 2}] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds {sup 3}{sub ∞}[Ba{sub 1-x}Eu{sub x}(Im){sub 2}], which were obtained from reaction of the salt-like hydrides BaH{sub 2} and EuH{sub 2} with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound {sup 3}{sub

  18. Analysis of urinary stone constituents using powder X-ray diffraction ...

    Indian Academy of Sciences (India)

    WINTEC

    drug and bacteria induced factors are all external factors causing urinary stones. ... gion of hot climate, low rain fall, and increased salin- ity of ground water, is a ... Gender the patient stones the stones habit and age. Stone removal procedure. KSHP. 1. KSHP1 Vegetarian. Male, 50. Natural excretion in the urine. KSHIM. 1.

  19. Coherent diffraction microscopy at SPring-8: instrumentation, data acquisition and data analysis

    International Nuclear Information System (INIS)

    Xu, Rui; Salha, Sara; Raines, Kevin S.; Jiang, Huaidong; Chen, Chien-Chun; Takahashi, Yukio; Kohmura, Yoshiki; Nishino, Yoshinori; Song, Changyong; Ishikawa, Tetsuya; Miao, Jianwei

    2011-01-01

    An instrumentation and data analysis review of coherent diffraction microscopy at SPring-8 is given. This work will be of interest to those who want to apply coherent diffraction imaging to studies of materials science and biological samples. Since the first demonstration of coherent diffraction microscopy in 1999, this lensless imaging technique has been experimentally refined by continued developments. Here, instrumentation and experimental procedures for measuring oversampled diffraction patterns from non-crystalline specimens using an undulator beamline (BL29XUL) at SPring-8 are presented. In addition, detailed post-experimental data analysis is provided that yields high-quality image reconstructions. As the acquisition of high-quality diffraction patterns is at least as important as the phase-retrieval procedure to guarantee successful image reconstructions, this work will be of interest for those who want to apply this imaging technique to materials science and biological samples

  20. Analysis of the corium phases by X-ray diffraction; Analyses des phases du corium par diffraction des rayons X

    Energy Technology Data Exchange (ETDEWEB)

    Trillon, G

    2004-07-01

    In the framework of the severe accidents R and D studies led by CEA, the better knowledge of the corium behaviour, corium coming from the melting of a nuclear reactor, are fundamental stakes in order to master this kind of accident. Among the available physical properties of the corium, the nature of the final crystalline compounds which have been made during the, cooling gives information about its solidification and its stabilisation. X-Rays Diffraction is the reference method used in order to characterize the corium coming from the different facilities of the European platform PLINIUS of CEA-Cadarache. This work presents the scientific approach that has been followed in order to obtain information both qualitative and quantitative on corium, using X-Rays Diffraction. For instance, a specific method for identifying U{sub 1-x}Zr{sub x}O{sub 2} solid solutions has been developed, and the validity of quantitative analysis of corium crystalline phases using the Rietveld method (with an internal standard), has been tested. This last method has also permitted semi-quantitative measurements of amorphous phases within corium. For these studies, analysis of prototypical corium has been conducted on samples coming from the experiences led on the different facilities of the PLINIUS platform. These analysis allowed for the first time to obtain quantitative data of the corium crystalline phases in order to validate thermodynamic databases and has been used to estimate the thereto-physical properties of the corium. New information on crystalline phases of corium has also been found, especially for the UO{sub 2}-ZrO{sub 2} pseudo binary system. (author)

  1. Assessment of the optimum degree of Sr{sub 3}Fe{sub 2}MoO{sub 9} electron-doping through oxygen removal: An X-ray powder diffraction and {sup 57}Fe Moessbauer spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, Carlos A.; Viola, Maria del C. [Area de Quimica General e Inorganica, Departamento de Quimica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700 San Luis (Argentina); Pedregosa, Jose C., E-mail: jpedreg@unsl.edu.ar [Area de Quimica General e Inorganica, Departamento de Quimica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700 San Luis (Argentina); Mercader, Roberto C., E-mail: mercader@fisica.unlp.edu.ar [Departamento de Fisica, IFLP-CONICET, Facultad de Ciencias Exactas, Universidad Nacional de La Plata, C.C. 67, 1900 La Plata (Argentina)

    2010-10-15

    We describe the preparation and structural characterization by X-ray powder diffraction (XRPD) and Moessbauer spectroscopy of three electron-doped perovskites Sr{sub 3}Fe{sub 2}MoO{sub 9-{delta}} with Fe/Mo = 2 obtained from Sr{sub 3}Fe{sub 2}MoO{sub 9}. The compounds were synthesized by topotactic reduction with H{sub 2}/N{sub 2} (5/95) at 600, 700 and 800 {sup o}C. Above 800 {sup o}C the Fe/Mo ratio changes from Fe/Mo = 2-1 < Fe/Mo < 2. The structural refinements of the XRPD data for the reduced perovskites were carried out by the Rietveld profile analysis method. The crystal structure of these phases is cubic, space group Fm3-bar m, with cationic disorder at the two different B sites that can be populated in variable proportions by the Fe atoms. The Moessbauer spectra allowed determining the evolution of the different species formed after the treatments at different temperatures and confirm that Fe ions in the samples reduced at 600, 700 and 800 {sup o}C are only in the high-spin Fe{sup 3+} electronic state.

  2. Structure resolution of Ba5Al3F19 and Iivestigation of fluorine ion dynamics by synchrotron powder diffraction, variable-temperature solid-state NMR, and quantum computations

    International Nuclear Information System (INIS)

    Martineau, C.; Fayon, F.; Suchomel, M.R.; Allix, M.; Massiot, D.; Taulelle, F.

    2011-01-01

    The room temperature structure of Ba 5 Al 3 F 19 has been solved using electron microscopy and synchrotron powder diffraction data. One-dimensional (1D) 27 Al and ultrafast magic-angle-spinning (MAS) 19 F NMR spectra have been recorded and are in agreement with the proposed structural model for Ba 5 Al 3 F 19 . The 19 F isotropic chemical shift and 27 Al quadrupolar parameters have been calculated using the CASTEP code from the experimental and density functional theory geometry-optimized structures. After optimization, the calculated NMR parameters of both the 19 F and 27 Al nuclei show improved consistency with the experimental values, demonstrating that the geometry optimization step is necessary to obtain more accurate and reliable structural data. This also enables a complete and unambiguous assignment of the 19 F MAS NMR spectrum of Ba 5 Al 3 F 19 . Variable-temperature 1D MAS 19 F NMR experiments have been carried out, showing the occurrence of fluorine ion mobility. Complementary insights were obtained from both two-dimensional (2D) exchange and 2D double-quantum dipolar recoupling NMR experiments, and a detailed analysis of the anionic motion in Ba 5 Al 3 F 19 is proposed, including the distinction between reorientational processes and chemical exchange involving bond breaking and re-formation.

  3. Stepwise effects of the BCR sequential chemical extraction procedure on dissolution and metal release from common ferromagnesian clay minerals: A combined solution chemistry and X-ray powder diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Ryan, P.C. [Geology Department, Middlebury College, Middlebury, Vermont 05753 (United States)], E-mail: pryan@middlebury.edu; Hillier, S. [Macaulay Institute, Aberdeen, AB15 8QH UK (United Kingdom); Wall, A.J. [Department of Geosciences, Penn State University, University Park, Pennsylvania, 16802 (United States)

    2008-12-15

    Sequential extraction procedures (SEPs) are commonly used to determine speciation of trace metals in soils and sediments. However, the non-selectivity of reagents for targeted phases has remained a lingering concern. Furthermore, potentially reactive phases such as phyllosilicate clay minerals often contain trace metals in structural sites, and their reactivity has not been quantified. Accordingly, the objective of this study is to analyze the behavior of trace metal-bearing clay minerals exposed to the revised BCR 3-step plus aqua regia SEP. Mineral quantification based on stoichiometric analysis and quantitative powder X-ray diffraction (XRD) documents progressive dissolution of chlorite (CCa-2 ripidolite) and two varieties of smectite (SapCa-2 saponite and SWa-1 nontronite) during steps 1-3 of the BCR procedure. In total, 8 ({+-} 1) % of ripidolite, 19 ({+-} 1) % of saponite, and 19 ({+-} 3) % of nontronite (% mineral mass) dissolved during extractions assumed by many researchers to release trace metals from exchange sites, carbonates, hydroxides, sulfides and organic matter. For all three reference clays, release of Ni into solution is correlated with clay dissolution. Hydrolysis of relatively weak Mg-O bonds (362 kJ/mol) during all stages, reduction of Fe(III) during hydroxylamine hydrochloride extraction and oxidation of Fe(II) during hydrogen peroxide extraction are the main reasons for clay mineral dissolution. These findings underscore the need for precise mineral quantification when using SEPs to understand the origin/partitioning of trace metals with solid phases.

  4. Contemporary Use of Anomalous Diffraction in Biomolecular Structure Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Liu Q.; Hendrickson, W.

    2017-01-01

    The normal elastic X-ray scattering that depends only on electron density can be modulated by an ?anomalous? component due to resonance between X-rays and electronic orbitals. Anomalous scattering thereby precisely identifies atomic species, since orbitals distinguish atomic elements, which enables the multi- and single-wavelength anomalous diffraction (MAD and SAD) methods. SAD now predominates in de novo structure determination of biological macromolecules, and we focus here on the prevailing SAD method. We describe the anomalous phasing theory and the periodic table of phasing elements that are available for SAD experiments, differentiating between those readily accessible for at-resonance experiments and those that can be effective away from an edge. We describe procedures for present-day SAD phasing experiments and we discuss optimization of anomalous signals for challenging applications. We also describe methods for using anomalous signals as molecular markers for tracing and element identification. Emerging developments and perspectives are discussed in brief.

  5. Measurement and QCD analysis of diffractive jet cross sections in deep inelastic scattering at HERA

    Energy Technology Data Exchange (ETDEWEB)

    Mozer, M.U.

    2006-07-24

    Differential cross sections for the production of two jets in diffractive deep inelastic scattering (DIS) at HERA are presented. The process studied is of the type ep{yields}eXY, where the central hadronic system X contains at least two jets and is separated from the system Y by a gap in rapidity. The forward system Y consists of an elastically scattered proton or a low mass dissociation system. The data were taken with the H1 detector during the years of 1999 and 2000 and correspond to an integrated luminosity of 51.5 pb{sup -1}. The measured cross sections are compared to fixed order NLO QCD predictions, that use diffractive parton densities which have previously been determined by a NLO QCD analysis of inclusive diffractive DIS at H1. The prediction and the data show significant differences. However, the dijet cross section is dominated by the diffractive gluon density, which can be extracted by the above mentioned analysis only with considerable uncertainty. Hence a combined QCD analysis of the previously published inclusive diffractive data and the dijet data is performed. This combined fit analysis allows the determination of diffractive quark and gluon densities with comparable precision. The common description of inclusive diffractive data and the dijet data confirms QCD factorization. (orig.)

  6. Probing the role of ceramide hydroxylation in skin barrier lipid models by 2H solid-state NMR spectroscopy and X-ray powder diffraction.

    Science.gov (United States)

    Kováčik, Andrej; Vogel, Alexander; Adler, Juliane; Pullmannová, Petra; Vávrová, Kateřina; Huster, Daniel

    2018-05-01

    In this work, we studied model stratum corneum lipid mixtures composed of the hydroxylated skin ceramides N-lignoceroyl 6-hydroxysphingosine (Cer[NH]) and α-hydroxylignoceroyl phytosphingosine (Cer[AP]). Two model skin lipid mixtures of the composition Cer[NH] or Cer[AP], N-lignoceroyl sphingosine (Cer[NS]), lignoceric acid (C24:0) and cholesterol in a 0.5:0.5:1:1 molar ratio were compared. Model membranes were investigated by differential scanning calorimetry and 2 H solid-state NMR spectroscopy at temperatures from 25 °C to 80 °C. Each component of the model mixture was specifically deuterated for selective detection by 2 H NMR. Thus, the exact phase composition of the mixture at varying temperatures could be quantified. Moreover, using X-ray powder diffraction we investigated the lamellar phase formation. From the solid-state NMR and DSC studies, we found that both hydroxylated Cer[NH] and Cer[AP] exhibit a similar phase behavior. At physiological skin temperature of 32 °C, the lipids form a crystalline (orthorhombic) phase. With increasing temperature, most of the lipids become fluid and form a liquid-crystalline phase, which converts to the isotropic phase at higher temperatures (65-80 °C). Interestingly, lignoceric acid in the Cer[NH]-containing mixture has a tendency to form two types of fluid phases at 65 °C. This tendency was also observed in Cer[AP]-containing membranes at 80 °C. While Cer[AP]-containing lipid models formed a short periodicity phase featuring a repeat spacing of d = 5.4 nm, in the Cer[NH]-based model skin lipid membranes, the formation of unusual long periodicity phase with a repeat spacing of d = 10.7 nm was observed. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. Coherent 3D nanostructure of γ-Al{sub 2}O{sub 3}: Simulation of whole X-ray powder diffraction pattern

    Energy Technology Data Exchange (ETDEWEB)

    Pakharukova, V.P., E-mail: verapakh@catalysis.ru [Boreskov Institute of Catalysis SB RAS, Pr. Lavrentieva 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk (Russian Federation); Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Yatsenko, D.A. [Boreskov Institute of Catalysis SB RAS, Pr. Lavrentieva 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk (Russian Federation); Gerasimov, E. Yu.; Shalygin, A.S.; Martyanov, O.N.; Tsybulya, S.V. [Boreskov Institute of Catalysis SB RAS, Pr. Lavrentieva 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk (Russian Federation); Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090 (Russian Federation)

    2017-02-15

    The structure and nanostructure features of nanocrystalline γ-Al{sub 2}O{sub 3} obtained by dehydration of boehmite with anisotropic platelet-shaped particles were investigated. The original models of 3D coherent nanostructure of γ-Al{sub 2}O{sub 3} were constructed. The models of nanostructured γ-Al{sub 2}O{sub 3} particles were first confirmed by a direct simulation of powder X–Ray diffraction (XRD) patterns using the Debye Scattering Equation (DSE) with assistance of high-resolution transmission electron microscopy (HRTEM) study. The average crystal structure of γ-Al{sub 2}O{sub 3} was shown to be tetragonally distorted. The experimental results revealed that thin γ-Al{sub 2}O{sub 3} platelets were heterogeneous on a nanometer scale and nanometer-sized building blocks were separated by partially coherent interfaces. The XRD simulation results showed that a specific packing of the primary crystalline blocks in the nanostructured γ-Al{sub 2}O{sub 3} particles with formation of planar defects on (001), (100), and (101) planes nicely accounted for pronounced diffuse scattering, anisotropic peak broadening and peak shifts in the experimental XRD pattern. The identified planar defects in cation sublattice seem to be described as filling cation non-spinel sites in existing crystallographic models of γ-Al{sub 2}O{sub 3} structure. The overall findings provided an insight into the complex nanostructure, which is intrinsic to the metastable γ-Al{sub 2}O{sub 3} oxide. - Highlights: • Thin plate-like crystallites of γ-Al{sub 2}O{sub 3} were obtained. • Models of 3D coherent nanostructure of γ-Al{sub 2}O{sub 3} were constructed. • Models were verified by simulating XRD patterns using the Debye Scattering Equation. • Specific broadening of XRD peaks was explained in terms of planar defects. • Primary crystalline blocks in γ-Al{sub 2}O{sub 3} are separated by partially coherent interfaces.

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

    International Nuclear Information System (INIS)

    Johnsen, Rune E.; 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-CO 3 →CoAl-Cl →CoAl-CO 3 , CoAl-Cl→CoAl-NO 3 and CoAl-CO 3 →CoAl-SO 4 . The XRPD data show that the CoAl-CO 3 →CoAl-Cl process is a two-phase transformation, where the amount of the CoAl-CO 3 phase decreases exponentially while that of the CoAl-Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl-CO 3 LDH sample along with in situ XRPD data suggested that the individual particles in the CoAl-CO 3 sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl-CO 3 →CoAl-Cl transformation, the XRPD data show that the reverse CoAl-Cl→CoAl-CO 3 process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl-Cl→CoAl-NO 3 anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl-Cl and final CoAl-NO 3 phases. The in situ data indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl-CO 3 →CoAl-SO 4 anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure. (orig.)

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

    Data.gov (United States)

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

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

    Data.gov (United States)

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

  11. 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)

  12. 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)

  13. Powdering of Hot-dip Galvannealed steel using Finite Element Analysis

    International Nuclear Information System (INIS)

    Kim, D. W.; Jang, Y. C.; Lee, Y. S.; Kim, S. I.

    2007-01-01

    Demand for hot-dip galvannealed steel has been increased due to it high corrosion resistance, paintability, and formability in automotive industry. Coating of Hot-dip galvannealed steel consists of various Fe-Zn intermetallic compounds. Since the coating is hard and therefore it is very brittle, the surface of steel sheet is easy to be ruptured during second manufacturing processing. This is called as powdering. Hence, various research have been carried out to prohibit powdering for improving the quality of GA steel during second manufacturing processing. This paper performed finite element analysis to evaluate local powdering and compared FEA results with V-bending test. The effects of punch radius and coating strength on the powdering was examined

  14. Nano-scale analysis of titanium dioxide fingerprint-development powders

    International Nuclear Information System (INIS)

    Reynolds, A J; Jones, B J; Sears, V; Bowman, V

    2008-01-01

    Titanium dioxide based powders are regularly used in the development of latent fingerprints on dark surfaces. For analysis of prints on adhesive tapes, the titanium dioxide is suspended in a surfactant and used in the form of a small particle reagent (SPR). Analysis of commercially available products shows varying levels of effectiveness of print development, with some powders adhering to the background as well as the print. Scanning electron microscopy (SEM) images of prints developed with different powders show a range of levels of aggregation of particles. Analytical transmission electron microscopy (TEM) of the fingerprint powder shows TiO 2 particles with a surrounding coating, tens of nanometres thick, consisting of Al and Si rich material. X ray photoelectron spectroscopy (XPS) is used to determine the composition and chemical state of the surface of the powders; with a penetration depth of approximately 10nm, this technique demonstrates differing Ti: Al: Si ratios and oxidation states between the surfaces of different powders. Levels of titanium detected with this technique demonstrate variation in the integrity of the surface coating. The thickness, integrity and composition of the Al/Si-based coating is related to the level of aggregation of TiO 2 particles and efficacy of print development.

  15. Nano-scale analysis of titanium dioxide fingerprint-development powders

    Energy Technology Data Exchange (ETDEWEB)

    Reynolds, A J; Jones, B J [Experimental Techniques Centre, Brunei University, Kingston Lane, Uxbridge, Middlesex, UB8 3PH (United Kingdom); Sears, V; Bowman, V [Fingerprint and Footwear Forensics, Home Office Scientific Development Branch, Sandridge, St Albans, Hertfordshire, AL4 9HQ (United Kingdom)], E-mail: b.j.jones@physics.org

    2008-08-15

    Titanium dioxide based powders are regularly used in the development of latent fingerprints on dark surfaces. For analysis of prints on adhesive tapes, the titanium dioxide is suspended in a surfactant and used in the form of a small particle reagent (SPR). Analysis of commercially available products shows varying levels of effectiveness of print development, with some powders adhering to the background as well as the print. Scanning electron microscopy (SEM) images of prints developed with different powders show a range of levels of aggregation of particles. Analytical transmission electron microscopy (TEM) of the fingerprint powder shows TiO{sub 2} particles with a surrounding coating, tens of nanometres thick, consisting of Al and Si rich material. X ray photoelectron spectroscopy (XPS) is used to determine the composition and chemical state of the surface of the powders; with a penetration depth of approximately 10nm, this technique demonstrates differing Ti: Al: Si ratios and oxidation states between the surfaces of different powders. Levels of titanium detected with this technique demonstrate variation in the integrity of the surface coating. The thickness, integrity and composition of the Al/Si-based coating is related to the level of aggregation of TiO{sub 2} particles and efficacy of print development.

  16. X-ray diffraction analysis of mudstone from nw sudan

    International Nuclear Information System (INIS)

    Salih, Suad Z.Elabdeen

    1997-03-01

    This study deals with the theoretical and experimental aspects of the x-ray diffraction technique (XRD). The XRD technique is used to investigate fine structure of matter, and it is most efficient method for the determination of the mineralogical composition of rocks. The XRD technique is used also to investigate the clay mineralogical of mud-stones of the Nubian sandstones of north western Sudan. The XRD results revealed that the mud-stone samples are composed, in decreasing abundance's of kaolinite, smectite, chlorite and illite. Non-clay minerals reported include quartz, feldspars and geothite. Kaolinite dominates in most of samples with percentages ranging between 78-96%. Smectite comes second in abundance and ranges between 10-24%, followed by chlorite and illite which showed the lowest abundance's. The dominance of kaolinite over smectite indicates that intense chemical weathering and leaching occurred under warm humid climate interrupted by dry periods. Most probably these clay minerals were produced by inheritance and partly by neo formation. The variation of the chemical composition of these mud stones is due basically to differences in clay mineralogy which was controlled by source rock geology, weathering physicochemical behavior of elements, local environment and climatic condition in the past. (Author)

  17. Quantitative evaluation of fluctuation error in X-ray diffraction profiles with fractal analysis

    International Nuclear Information System (INIS)

    Kurose, Masashi; Hirose, Yukio; Sasaki, Toshihiko; Yoshioka, Yasuo.

    1995-01-01

    A method of the fractal analysis was applied to the diffraction profiles for its quantitative evaluation. The fractal dimension was analyzed according to both Box counting method and FFT method. The relationship between the fractal dimension and the measurement criteria in X-ray diffraction analysis was discussed with diffraction data obtained under various conditions of the measurement. It was concluded that the fractal analysis is effective for the quantitative evaluation of diffraction data. Box counting method is suitable for evaluation of a whole profile, and FFT method is for that of a fundamental profile. The range of desirable condition of measurement is 1.0≤D≤1.2, where D is a fractal dimension. The appropriate range of measurement becomes 0.01≤Sw/HVB≤0.03, where Sw is the step width and the HVB is the half-value breadth. Stresses with higher precision were obtained from measurements under this new criteria. (author)

  18. Preparation of nanosize carbon powders by pulsed wire discharge

    Energy Technology Data Exchange (ETDEWEB)

    Minami, C.; Kinemuchi, Y.; Suzuki, T.; Suematsu, H.; Jiang, W.; Yatsui, K. [Nagaoka Univ. of Technology, Extreme Energy-Density Research Inst., Nagaoka, Niigata (Japan); Hirata, T.; Hatakeyama, R. [Tohoku Univ., Graduate School of Engineering, Sendai, Miyagi (Japan)

    2002-06-01

    Nanosize powders of carbons were tried to be synthesized by pulsed discharge of graphite wires in several kinds of ambient gases. When the wire was discharged in N{sub 2} gas, nanosize powders have been successfully produced. The result of X-ray diffraction analysis indicated that nanosize powders produced in N{sub 2} gas at 750 Torr were amorphous carbon containing glassy carbons, while mass-spectrum analysis demonstrated the production of fullerenes at 600 Torr. If the wire is discharged in Ar gas, dielectric breakdown takes place between electrodes, producing no carbon powders. (author)

  19. COMPARING PARTICLE SIZE DISTRIBUTION ANALYSIS BY SEDIMENTATION AND LASER DIFFRACTION METHOD

    Directory of Open Access Journals (Sweden)

    Vito Ferro

    2009-06-01

    Full Text Available In this paper a brief review of the laser diffraction method is firstly carried out. Then, for 30 soil samples having a different texture classification sampled in Sicilian basin, a comparison between the two techniques is developed. The analysis demonstrated that the sand content measured by Sieve-Hydrometer method can be assumed equal to the one determinated by laser diffraction technique while an overestimation of the clay fraction measured by Sieve-Hydrometer method respect to laser diffraction technique was obtained. Finally a set of equations useful to refer LD measurements to SH method was proposed.

  20. The use dynamic avalanching and fractal analysis to characterise uranium oxide powders

    International Nuclear Information System (INIS)

    Hobbs, J.W.; Rhodes, D.

    2000-01-01

    Direct thermal denitration is an attractive method of co-converting mixed-metal nitrate solutions of plutonium and uranium into oxide because of its apparent simplicity. Such benefits are often marred by the relatively poor powder quality and handling characteristics, which can be overcome by modifications to the process chemistry. To ensure that powder synthesis routes under assessment require the minimal further processing it is necessary to be able to characterise the powder fully in term of the key fundamental properties. This paper will demonstrate the use of a dynamic avalanching technique, fractal analysis and morphology to assess processing behaviour. The use of dynamic avalanching to uniquely characterise the chaotic flow properties of urania powders has proved successful and results have shown that this technique is capable of detecting small differences in processing behaviour due changes in morphologies and particle size distribution. This technique has promise for being able to provide nearly instantaneous feedback to the powder generation process being monitored (e.g. calcination, milling, mixing). The use of fractals to describe powders is an interesting characterisation tool when combined with morphological shape factors and the flow index. (authors)

  1. Crystallization and preliminary X-ray diffraction analysis of West Nile virus

    International Nuclear Information System (INIS)

    Kaufmann, Bärbel; Plevka, Pavel; Kuhn, Richard J.; Rossmann, Michael G.

    2010-01-01

    Crystals of infectious West Nile virus were obtained and diffracted at best to about 25 Å resolution. Preliminary analysis of the diffraction pattern suggested tight hexagonal packing of the intact virus. West Nile virus, a human pathogen, is closely related to other medically important flaviviruses of global impact such as dengue virus. The infectious virus was purified from cell culture using polyethylene glycol (PEG) precipitation and density-gradient centrifugation. Thin amorphously shaped crystals of the lipid-enveloped virus were grown in quartz capillaries equilibrated by vapor diffusion. Crystal diffraction extended at best to a resolution of about 25 Å using synchrotron radiation. A preliminary analysis of the diffraction images indicated that the crystals had unit-cell parameters a ≃ b ≃ 480 Å, γ = 120°, suggesting a tight hexagonal packing of one virus particle per unit cell

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

    International Nuclear Information System (INIS)

    Andreeva, N. S.

    2006-01-01

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

  3. Diffraction efficiency and noise analysis of hidden image holograms

    DEFF Research Database (Denmark)

    Tamulevičius, Sigitas; Andrulevičius, Mindaugas; Puodžiukynas, Linas

    2017-01-01

    recorded in a photoresist layer spin-coated on glass substrates applying laser interference lithography technique. Both analogue and digital analysis approaches showed the similar results thus confirming the appropriateness of the used analysis methods. It was found that holograms recorded at higher laser...

  4. COMPARING PARTICLE SIZE DISTRIBUTION ANALYSIS BY SEDIMENTATION AND LASER DIFFRACTION METHOD

    OpenAIRE

    Vito Ferro; Stefano Mirabile

    2009-01-01

    In this paper a brief review of the laser diffraction method is firstly carried out. Then, for 30 soil samples having a different texture classification sampled in Sicilian basin, a comparison between the two techniques is developed. The analysis demonstrated that the sand content measured by Sieve-Hydrometer method can be assumed equal to the one determinated by laser diffraction technique while an overestimation of the clay fraction measured by Sieve-Hydrometer method respect to laser diffr...

  5. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

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

    International Nuclear Information System (INIS)

    Almeida, Ana P.G.; Braz, Delson

    2009-01-01

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

  8. Structural and optical analysis of ZnBeMgO powder and thin films

    International Nuclear Information System (INIS)

    Panwar, Neeraj; Liriano, J.; Katiyar, Ram S.

    2011-01-01

    Research highlights: → Structural and optical studies of Zn 1-x-y Be x Mg y O (0 ≤ x ≤0.10; 0 ≤ y ≤ 0.20) powders and thin films. → Raman studies of the pure ZnO powder showed all the characteristic peaks of the wurtzite hexagonal structure and with (Be, Mg) co-doping new modes appeared which can be attributed to arise as a result of doping effect. → The XRD of the films prepared from the powders using pulsed laser deposition (PLD) technique exhibited the preferential orientation and with doping the (0 0 0 2) peak also shifts to higher 2θ values suggesting the incorporation of Be/Mg at the Zn-site. → From the UV-visible optical band gap measurement it was noticed that the band gap of the pristine ZnO film is 3.3 eV which enhanced up to 4.51 eV for Zn 0.7 Be 0.1 Mg 0.2 O film which lies in the solar blind region and is very useful for the deep UV detection. - Abstract: We here report the structural and optical studies of Zn 1-x-y Be x Mg y O (0 ≤ x ≤ 0.15; 0 ≤ y ≤ 0.20) powders and thin films. From the Rietveld refinement of the powder X-ray diffraction (XRD) patterns it was revealed that the value of 'a' lattice parameter remains almost unchanged whereas 'c' parameter reduces with Be and Mg co-doping in ZnO. The Zn-O bond length also decreases in co-doped samples. Raman studies of the pure ZnO powder showed all the characteristic peaks of the wurtzite hexagonal structure and with (Be, Mg) co-doping new modes appeared which can be attributed to arise as a result of substitution. The XRD of the films prepared from the powders using pulsed laser deposition (PLD) technique exhibited the preferential orientation and with increase in co-doping the (0 0 0 2) peak also shifts to higher 2θ values suggesting the incorporation of Be/Mg at the Zn-site. From the UV-visible optical transmittance measurement it was noticed that the band gap of the pristine ZnO film is 3.3 eV which enhanced up to 4.51 eV for Zn 0.7 Be 0.1 Mg 0.2 O film which lies in the

  9. Analysis of Hazards Associated with a Process Involving Uranium Metal and Uranium Hydride Powders

    Energy Technology Data Exchange (ETDEWEB)

    Bullock, J.S.

    2000-05-01

    An analysis of the reaction chemistry and operational factors associated with processing uranium and uranium hydride powders is presented, focusing on a specific operation in the Development Division which was subjected to the Job Hazard Analysis (JHA) process. Primary emphasis is on the thermodynamic factors leading to pyrophoricity in common atmospheres. The discussion covers feed powders, cold-pressed and hot-pressed materials, and stray material resulting from the operations. The sensitivity of the various forms of material to pyrophoricity in common atmospheres is discussed. Operational recommendations for performing the work described are given.

  10. X-ray diffraction analysis with diffractometer DRON-1

    International Nuclear Information System (INIS)

    Bochenin, V.I.

    1978-01-01

    Rapid methods of phase quantitative analysis of wolframite (FeMn)WO 4 and molybdenite MoS 2 in industrial materials using DRON-1 diffractometer are suggested. Diffractometer with spectrometric attachment was used for determination of (FeMn)WO 4 in industrial raw materials. Results of the above analysis have been compared with the data of chemical analysis, their good agreement has been shown. Time of wolframite determination in one sample is 8-10 min. Method of standard background with respect to absorption properties of medium has been developed for MoS 2 rapid determination in enriched molybdenum ore. Time of molybdenite determination in one sample is 3-4min., error is 4 % rel. in MoS 2 concentration range from 15.4 to 36.7 %

  11. Granulometric analysis of metallic oxide in ceramic powder form synthesized by different methods

    International Nuclear Information System (INIS)

    Neiva, L.S.; Simoes, A.N.; Simoes, V.N.; Bispo, A.; Gama, L.

    2012-01-01

    The aim of this work is to synthesize ceramic powders based on CuO/CeO 2 by means two different synthesis methods, they are: the combustion reaction method and Pechini method. It's part of the aim of this work subject all samples to a synthesized qualitative and quantitative chemical analysis, using the technique EDX and then to a granulometric analysis. The samples of the ceramic powder based on CuO/CeO 2 synthesized in this work by means of the two above synthesis methods, contain various concentrations of CuO ranging between 0 and 0.5 mol. According to the results, only the Pechini method of synthesis exerted a significant and defined influence on the capacity of particle unit agglomeration in these powders (author)

  12. Thermal Analysis of Braille Formed by Using Screen Printing and Inks with Thermo Powder

    Directory of Open Access Journals (Sweden)

    Svіtlana HAVENKO

    2015-03-01

    Full Text Available In order to improve the integration of blind people into society, suitable conditions should be provided for them. The expansion of Braille (BR use could serve the purpose. Depending on the materials used for Braille, it can be formed or printed in different ways: embossing, screen printing, thermoforming, digital printing. The aim of this research is to determine the effect of thermal properties of screen printing inks and inks with thermo-powder on the qualitative parameters of Braille. Screen printing inks and inks with thermo-powder were chosen for the research. Carrying out the qualitative analysis of printouts with Braille, the thermal stability was evaluated by analyzing the thermograms obtained with derivatograph Q-1500. This paper presents the findings of the thermogravimetric (TG, differential thermogravimetric (DTG and differential thermal analysis (DTA of printouts printed on paperboard Plike and using traditional screen printing inks and screen printing inks with thermo-powder. Based on the testing findings it is determined that thermal stability of printouts printed with thermo-powder ink is higher than printed with screen printing inks. It is determined that the appropriate temperature range of screen printing inks with thermo-powder drying is 98 ºC – 198 ºC because in this case better relief of Braille dots is obtained.DOI: http://dx.doi.org/10.5755/j01.ms.21.1.5702

  13. X-ray diffraction analysis of the ammonium nitrate IV-III-II and IV-II phase changes under controlled humidity conditions

    International Nuclear Information System (INIS)

    Boeyens, J.C.A.; Ferg, E.; Levendis, D.C.; Schoening, F.R.L.

    1992-01-01

    The first phase transition above room temperature of ammonium nitrate has been investigated as a function of humidity and sample preparation by means of a Weissenberg camera, modified to record the powder diffraction pattern as a function of temperature. Heterogeneous nucleation at the grain surface, inferred from the observed texture that develops in the powder specimens, is related to the effect of humidity during sample preparation on the stability of prills or powders. 19 refs., 4 figs

  14. Characterization of Cobalt F-75 powder for biomedical application

    International Nuclear Information System (INIS)

    Zuraidawani, C.D.; Shamsul, J.B.; Fazlul, B.; Nur Hidayah, A.Z.

    2007-01-01

    Cobalt F-75 alloys is commonly used for surgical implants because of their strength, corrosion resistance, non-magnetic behaviour and biocompatibility. In this paper, gas atomized of Cobalt F-75 powders were selected for evaluation. These powders supplied by Sandvik Osprey Ltd. The characteristics of these powders were investigated by using particle size analysis, X-ray Diffraction (XRD), X-ray Fluorescence (XRF) and Scanning Electron Microscope (SEM). Two different powder sizes (8.8 μm and 11.5 μm) have showed spherical morphology and the value of densities are 7.9 and 7.6 g/cm 3 respectively. (author)

  15. Analysis of the production of U3O8 powder for low enrichment fuel plates

    International Nuclear Information System (INIS)

    Boero, N.L.; Celora, J.; Parodi, C.A.; Ponieman, G.; Kellner, M.; Marajofsky, A.

    1987-01-01

    Description is made of the processes used in the production of U 3 O 8 powder for low enrichment plates for fuel elements for Research Reactors. The analysis of the efficiency of each batch is foccused on the relationship between milling and sieving times and the morphology of the product in each production step. (Author)

  16. In situ diffraction profile analysis during tensile deformation motivated by molecular dynamics

    International Nuclear Information System (INIS)

    Van Swygenhoven, H.; Budrovic, Z.; Derlet, P.M.; Froseth, A.G.; Van Petegem, S.

    2005-01-01

    Molecular dynamics simulations can provide insight into the slip mechanism at the atomic scale and suggest that in nanocrystalline metals dislocations are nucleated and absorbed by the grain boundaries. However, this technique is limited by very short simulation times. Using suggestions from molecular dynamics, we have developed a new in situ X-ray diffraction technique wherein the profile analysis of several Bragg diffraction peaks during tensile deformation is possible. Combining experiment and careful structural analysis the results confirm the suggestions from atomistic simulations

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1975-01-07

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

  18. Analysis of soft magnetic materials by electron backscatter diffraction as a powerful tool

    Directory of Open Access Journals (Sweden)

    David Schuller

    2018-04-01

    Full Text Available The current work demonstrates that electron backscatter diffraction (EBSD is a powerful and versatile characterization technique for investigating soft magnetic materials. The properties of soft magnets, e.g., magnetic losses strongly depend on the materials chemical composition and microstructure, including grain size and shape, texture, degree of plastic deformation and elastic strain. In electrical sheet stacks for e-motor applications, the quality of the machined edges/surfaces of each individual sheet is of special interest. Using EBSD, the influence of the punching process on the microstructure at the cutting edge is quantitatively assessed by evaluating the crystallographic misorientation distribution of the deformed grains. Using an industrial punching process, the maximum affected deformation depth is determined to be 200 - 300 μm. In the case of laser cutting, the affected deformation depth is determined to be approximately zero. Reliability and detection limits of the developed EBSD approach are evaluated on non-affected sample regions and model samples containing different indentation test bodies. A second application case is the investigation of the recrystallization process during the annealing step of soft magnetic composites (SMC toroids produced by powder metallurgy as a function of compaction pressure, annealing parameters and powder particle size. With increasing pressure and temperature, the recrystallized area fraction (e.g., grains with crystallographic misorientations 3°.

  19. 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

  20. Crystallization and preliminary X-ray diffraction analysis of rat autotaxin

    International Nuclear Information System (INIS)

    Day, Jacqueline E.; Hall, Troii; Pegg, Lyle E.; Benson, Timothy E.; Hausmann, Jens; Kamtekar, Satwik

    2010-01-01

    Autotaxin (ATX), a pyrophosphatase/phosphodiesterase enzyme, is a promising drug target for many indications and is only distantly related to enzymes of previously determined structure. Here, the cloning, expression, purification, crystallization and preliminary diffraction analysis of ATX are reported. Rat autotaxin has been cloned, expressed, purified to homogeneity and crystallized via hanging-drop vapour diffusion using PEG 3350 as precipitant and ammonium iodide and sodium thiocyanate as salts. The crystals diffracted to a maximum resolution of 2.05 Å and belonged to space group P1, with unit-cell parameters a = 53.8, b = 63.3, c = 70.5 Å, α = 98.8, β = 106.2, γ = 99.8°. Preliminary X-ray diffraction analysis indicated the presence of one molecule per asymmetric unit, with a solvent content of 47%

  1. Regge analysis of diffractive and leading baryon structure functions from deep inelastic scattering

    International Nuclear Information System (INIS)

    Batista, M.; Covolan, R.J.M.; Montanha, J.

    2002-01-01

    In this paper we present a combined analysis of the H1 data on leading baryon and diffractive structure functions from DIS, which are handled as two components of the same semi-inclusive process. The available structure function data are analyzed in a series of fits in which three main exchanges are taken into account: the Pomeron, Reggeon, and pion. For each of these contributions, Regge factorization of the correspondent structure function is assumed. By this procedure, we extract information about the interface between the diffractive, Pomeron-dominated, region and the leading proton spectrum, which is mostly ruled by secondary exchanges. One of the main results is that the relative Reggeon contribution to the semi-inclusive structure function is much smaller than the one obtained from an analysis of the diffractive structure function alone

  2. Structure analysis of liquids and disordered materials using pulsed neutron diffraction and total scattering

    International Nuclear Information System (INIS)

    Suzuya, Kentaro

    2011-01-01

    Neutron diffraction·total scattering at pulsed neutron source is a powerful method to analyze the complex structure of disordered materials: liquids, glasses, amorphous materials and disordered crystals. The basic idea of the structure of disordered materials, the fundamental diffraction theory for disordered materials, and structure analysis of disordered materials using pulsed neutron diffraction·total scattering technique (TOF method) are described in detail. In addition, the precise information of the world highest class J-PARC MLF spallation neutron source and typical J-PARC neutron total scattering instrument NOVA are also given. Recent structural modelling methods of disordered materials such like reverse Monte Carlo (RMC) simulation method is briefly described using an example of the analysis of a typical disordered material silica glass. (author)

  3. Determination of interplanar distances starting from diffraction spectra for PC microcomputer; Determinacion de distancias interplanares a partir de espectros de difraccion para microcomputadora PC

    Energy Technology Data Exchange (ETDEWEB)

    Macias B, L.R

    1991-07-15

    The objective of this work, consists in that starting of a digitized diffraction spectra result of the structural analysis technique, it is possible by means of the analysis of a computer program, to detect the diffraction peaks and well-known the wavelength to obtain the values of the interplanar distances to be compared with the JCPDS (Joint Committee on Powder Diffraction Standards). (Author)

  4. Quantitative analysis of mineral powders by DRIFTS: Determination of SrCO3 in superconductor precursor powders

    DEFF Research Database (Denmark)

    Bak, J.; Kindl, B.

    1997-01-01

    An application of diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) has been demonstrated to be able to determine small concentrations, down to the 100-ppm level, of carbonates in powdery superconductor (SPC) precursor samples, The detection of carbonates in SPC precursor powders...

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  6. Production and analysis of ultradispersed uranium oxide powders

    Science.gov (United States)

    Zajogin, A. P.; Komyak, A. I.; Umreiko, D. S.; Umreiko, S. D.

    2010-05-01

    Spectroscopic studies are made of the laser plasma formed near the surface of a porous body containing nanoquantities of uranium compounds which is irradiated by two successive laser pulses. The feasibility of using laser chemical methods for obtaining nanoclusters of uranium oxide particles in the volume of a porous body and the simultaneous possibility of determining the uranium content with good sensitivity are demonstrated. The thermochemical and spectral characteristics of the analogs of their compounds with chlorine are determined and studied. The possibility of producing uranium dioxides under ordinary conditions and their analysis in the reaction products is demonstrated.

  7. Role of diffraction and electron analysis in the fast reactor programme

    Energy Technology Data Exchange (ETDEWEB)

    Ferguson, I. F. [ed.

    1975-09-15

    After first discussing irradiation damage, the whole range of new methods of probe analysis were reviewed with a special reference to the study of surfaces. Further papers discussed scanning auger microscopy and the nuclear microprobe. Current diffraction studies were then described on uranium dioxide and the neutron poisons: boron carbide and europia. Finally, new techniques were covered with special reference to the scanning electron microscope and the application of the Harwell 6000 series electronics to x-ray diffraction. Separate records were prepared for each paper covered.

  8. The Gaussian beam mode analysis of classical phase aberrations in diffraction-limited optical systems

    Science.gov (United States)

    Trappe, Neil; Murphy, J. Anthony; Withington, Stafford

    2003-07-01

    Gaussian beam mode analysis (GBMA) offers a more intuitive physical insight into how light beams evolve as they propagate than the conventional Fresnel diffraction integral approach. In this paper we illustrate that GBMA is a computationally efficient, alternative technique for tracing the evolution of a diffracting coherent beam. In previous papers we demonstrated the straightforward application of GBMA to the computation of the classical diffraction patterns associated with a range of standard apertures. In this paper we show how the GBMA technique can be expanded to investigate the effects of aberrations in the presence of diffraction by introducing the appropriate phase error term into the propagating quasi-optical beam. We compare our technique to the standard diffraction integral calculation for coma, astigmatism and spherical aberration, taking—for comparison—examples from the classic text 'Principles of Optics' by Born and Wolf. We show the advantages of GBMA for allowing the defocusing of an aberrated image to be evaluated quickly, which is particularly important and useful for probing the consequences of astigmatism and spherical aberration.

  9. The Gaussian beam mode analysis of classical phase aberrations in diffraction-limited optical systems

    International Nuclear Information System (INIS)

    Trappe, Neil; Murphy, J Anthony; Withington, Stafford

    2003-01-01

    Gaussian beam mode analysis (GBMA) offers a more intuitive physical insight into how light beams evolve as they propagate than the conventional Fresnel diffraction integral approach. In this paper we illustrate that GBMA is a computationally efficient, alternative technique for tracing the evolution of a diffracting coherent beam. In previous papers we demonstrated the straightforward application of GBMA to the computation of the classical diffraction patterns associated with a range of standard apertures. In this paper we show how the GBMA technique can be expanded to investigate the effects of aberrations in the presence of diffraction by introducing the appropriate phase error term into the propagating quasi-optical beam. We compare our technique to the standard diffraction integral calculation for coma, astigmatism and spherical aberration, taking - for comparison - examples from the classic text 'Principles of Optics' by Born and Wolf. We show the advantages of GBMA for allowing the defocusing of an aberrated image to be evaluated quickly, which is particularly important and useful for probing the consequences of astigmatism and spherical aberration

  10. Crystallization and preliminary X-ray diffraction analysis of mevalonate kinase from Methanosarcina mazei

    International Nuclear Information System (INIS)

    Zhuang, Ningning; Seo, Kyung Hye; Chen, Cong; Zhou, Jia; Kim, Seon Won; Lee, Kon Ho

    2012-01-01

    Recombinant mevalonate kinase from M. mazei has been crystallized. Diffraction data were collected to 2.08 Å resolution. Mevalonate kinase (MVK), which plays an important role in catalysing the biosynthesis of isoprenoid compounds derived from the mevalonate pathway, transforms mevalonate to 5-phosphomevalonate using ATP as a cofactor. Mevalonate kinase from Methanosarcina mazei (MmMVK) was expressed in Escherichia coli, purified and crystallized for structural analysis. Diffraction-quality crystals of MmMVK were obtained by the vapour-diffusion method using 0.32 M MgCl 2 , 0.08 M bis-tris pH 5.5, 16%(w/v) PEG 3350. The crystals belonged to space group P2 1 2 1 2, with unit-cell parameters a = 97.11, b = 135.92, c = 46.03 Å. Diffraction data were collected to 2.08 Å resolution

  11. Crystallization and preliminary X-ray diffraction analysis of the middle domain of Paip1

    International Nuclear Information System (INIS)

    Kanaan, Ahmad Seif; Frank, Filipp; Maedler-Kron, Chelsea; Verma, Karan; Sonenberg, Nahum; Nagar, Bhushan

    2009-01-01

    The crystallization of the putative MIF4G domain of Paip1 is described. The crystals belonged to the monoclinic space group P2 1 and diffracted X-rays to beyond 2.2 Å resolution. The poly(A)-binding protein (PABP) simultaneously interacts with the poly(A) tail of mRNAs and the scaffolding protein eIF4G to mediate mRNA circularization, resulting in stimulation of protein translation. PABP is regulated by the PABP-interacting protein Paip1. Paip1 is thought to act as a translational activator in 5′ cap-dependent translation by interacting with PABP and the initiation factors eIF4A and eIF3. Here, the crystallization and preliminary diffraction analysis of the middle domain of Paip1 (Paip1M), which produces crystals that diffract to a resolution of 2.2 Å, are presented

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-31

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

  13. Evaluation of pressed powders and thin section standards for multi-elemental analysis by conventional and micro-PIXE analysis

    International Nuclear Information System (INIS)

    Homma-Takeda, Shino; Iso, Hiroyuki; Ito, Masaki

    2010-01-01

    For multi-elemental analysis, various standards are used to quantify the elements consists of environmental and biological samples. In this paper two different configuration standards, pressed powders and thin section standards, were assessed for their purpose as standards by conventional and micro-PIXE analysis. Homogeneity of manganese, iron, zinc (Zn), copper and yttrium added to pressed powder standard materials were validated and the relative standard deviation (RSD) of the X-ray intensity of the standards was 2 area and the metal concentration was acceptable. (author)

  14. Neutron diffraction of γ-aluminium oxynitride

    NARCIS (Netherlands)

    Willems, H.X.; With, de G.; Metselaar, R.; Helmholdt, R.B.; Petersen, K.K.

    1993-01-01

    Neutron diffraction expts. were performed on Al oxynitride (Alon) powders with compns. corresponding to 67.5, 73 and 77.5 mol.% Al2O3. The 73 mol.% powder was produced by reacting Al2O3 and AlN powders for 3 h at 1750 Deg. After reaction the resultant powder was ground with a mortar and pestle to

  15. Comparative kinetic analysis of89 Sr,60 Co and65 Zn Uptake by human bone powder

    International Nuclear Information System (INIS)

    Abdel-Fatah, A.T.A.; Essa, M.W.A.; Mohamed, S.A.; Molokhia, M.K.

    1990-01-01

    Human bone powder samples were prepared from recent femurs. The Bone particles range between 30 and 40 MU in diameter. One portion of this powder was prepared fat-free (FFB), the second portion as protein-free (PFB) and the last portion was left as raw bone powder-(RB). The sequence of uptake of 89 Sr by these types of bone powder is : FFB > RB > PFB, while that of 60 Co and 65 Zn is: PFB > FFB > RB. Kinetic analysis of the uptake curves of the 3 isotopes indicated that these processes proceed in 3 distinct steps; very fast initial, moderate intermediate and slow last step. The obtained rates of uptake indicated that : (1) the uptake by PEB is faster in its third step than the other types, (2) the most predominant step in case of 89 Sr and 60 Co is the third step (ion exchange step) while in case of 65 Zn it is the first step (physical adsorption), (3) defatenisation or deproteinisation, in general, inhances the uptake process

  16. Effect of powder compaction on radiation-thermal synthesis of lithium-titanium ferrites

    Science.gov (United States)

    Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

    2017-01-01

    Effect of powder compaction on the efficiency of thermal and radiation-thermal synthesis of lithium-substituted ferrites was investigated by X-Ray diffraction and specific magnetization analysis. It was shown that the radiation-thermal heating of compacted powder reagents mixture leads to an increase in efficiency of lithium-titanium ferrites synthesis.

  17. A new theory for X-ray diffraction.

    Science.gov (United States)

    Fewster, Paul F

    2014-05-01

    This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the `Bragg position' even if the `Bragg condition' is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many `Bragg positions'. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on `Bragg-type' scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the `background'. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models.

  18. Hydrothermal treatment of coprecipitated YSZ powders

    International Nuclear Information System (INIS)

    Arakaki, Alexander Rodrigo; Yoshito, Walter Kenji; Ussui, Valter; Lazar, Dolores Ribeiro Ricci

    2009-01-01

    Zirconia stabilized with 8.5 mol% yttria (YSZ) were synthesized by coprecipitation and resulting gels were hydrothermally treated at 200°C and 220 PSI for 4, 8 and 16 hours. Products were oven dried at 70°C for 24 hours, uniaxially pressed as pellets and sintered at 1500 °C for 1 hour. Powders were characterized for surface area with N 2 gas adsorption, X-ray diffraction, laser diffraction granulometric analysis and scanning and transmission electronic microscopy. Density of ceramics was measured by an immersion method based on the Archimedes principle. Results showed that powders dried at 70°C are amorphous and after treatment has tetragonal/cubic symmetry. Surface area of powders presented a significant reduction after hydrothermal treatment. Ceramics prepared from hydrothermally treated powders have higher green density but sintered pellets are less dense when compared to that made with powders calcined at 800°C for 1 hour due to the agglomerate state of powders. Solvothermal treatment is a promising procedure to enhance density. (author)

  19. 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

  20. Production of nanocrystalline cermet thermal spray powders for wear resistant coatings by high-energy milling

    International Nuclear Information System (INIS)

    Eigen, N.; Klassen, T.; Aust, E.; Bormann, R.; Gaertner, F.

    2003-01-01

    TiC-Ni based nanocrystalline cermet powders for thermal spraying were produced by high-energy milling. Milling experiments were performed in an attrition mill and a vibration mill in kilogram scale, and powder morphologies and microstructures were characterized using scanning electron microscopy, X-ray diffraction, and laser scattering for particle size analysis. Milling time and powder input were optimized with respect to the desired microstructure and particle sizes, and the results using both types of mill were compared. Powders with homogeneously dispersed hard phase particles below 300 nm could be produced in both mills. Additional processes for the refinement of powder morphology and particle size distribution are discussed

  1. Application of Microscopy and X-ray Diffraction in Optimization of the Production of NiTi Alloy by Powder Metallurgy

    Czech Academy of Sciences Publication Activity Database

    Novák, P.; Školáková, A.; Vojtěch, V.; Knaislová, A.; Pokorný, P.; Moravec, H.; Kopeček, Jaromír; Karlík, M.; Kubatík, Tomáš František

    2014-01-01

    Roč. 14, č. 3 (2014), s. 387-392 ISSN 1213-2489. [Mezinárodní konference „Mikroskopie a nedestruktivní zkoušení materiálů/3./. Litoměřice, 22.10.2014-24.10.2014] R&D Projects: GA ČR(CZ) GA14-03044S Institutional support: RVO:61389021 ; RVO:68378271 Keywords : powder metallurgy * NiTi, * mechanical alloying * reactive sintering Subject RIV: JG - Metallurgy; JG - Metallurgy (FZU-D) http://journal.strojirenskatechnologie.cz/templates/obalky_casopis/XIV_2014-3.pdf

  2. Assessment of firing conditions in old fired-clay bricks. The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Czech Academy of Sciences Publication Activity Database

    Viani, Alberto; Sotiriadis, Konstantinos; Len, A.; Šašek, Petr; Ševčík, Radek

    2016-01-01

    Roč. 116, June (2016), s. 33-43 ISSN 1044-5803 R&D Projects: GA MŠk(CZ) LO1219 Keywords : fired- clay brick * Rietveld method * small angle neutron scattering * X-ray diffraction * firing temperature Subject RIV: AL - Art, Architecture, Cultural Heritage Impact factor: 2.714, year: 2016 http://www.sciencedirect.com/science/article/pii/S1044580316300870

  3. High temperature neutron powder diffraction study of the Cu{sub 12}Sb{sub 4}S{sub 13} and Cu{sub 4}Sn{sub 7}S{sub 16} phases

    Energy Technology Data Exchange (ETDEWEB)

    Lemoine, Pierric, E-mail: pierric.lemoine@univ-rennes1.fr [Institut des Sciences Chimiques de Rennes, UMR-CNRS 6226, 263 Avenue du Général Leclerc, CS 74205, 35042 Rennes Cedex (France); Bourgès, Cédric; Barbier, Tristan [Laboratoire CRISMAT, UMR-CNRS 6508, ENSICAEN, 6 Boulevard du Maréchal Juin, 14050 Caen Cedex 04 (France); Nassif, Vivian [CNRS Institut NEEL, F-38000 Grenoble (France); Université de Grenoble Alpes, Institut NEEL, F-38000 Grenoble (France); Cordier, Stéphane [Institut des Sciences Chimiques de Rennes, UMR-CNRS 6226, 263 Avenue du Général Leclerc, CS 74205, 35042 Rennes Cedex (France); Guilmeau, Emmanuel [Laboratoire CRISMAT, UMR-CNRS 6508, ENSICAEN, 6 Boulevard du Maréchal Juin, 14050 Caen Cedex 04 (France)

    2017-03-15

    Ternary copper-containing sulfides Cu{sub 12}Sb{sub 4}S{sub 13} and Cu{sub 4}Sn{sub 7}S{sub 16} have attracted considerable interest since few years due to their high-efficiency conversion as absorbers for solar energy and promising thermoelectric materials. We report therein on the decomposition study of Cu{sub 12}Sb{sub 4}S{sub 13} and Cu{sub 4}Sn{sub 7}S{sub 16} phases using high temperature in situ neutron powder diffraction. Our results obtained at a heating rate of 2.5 K/min indicate that: (i) Cu{sub 12}Sb{sub 4}S{sub 13} decomposes above ≈792 K into Cu{sub 3}SbS{sub 3}, and (ii) Cu{sub 4}Sn{sub 7}S{sub 16} decomposes above ≈891 K into Sn{sub 2}S{sub 3} and a copper-rich sulfide phase of sphalerite ZnS-type structure with an assumed Cu{sub 3}SnS{sub 4} stoichiometry. Both phase decompositions are associated to a sulfur volatilization. While the results on Cu{sub 12}Sb{sub 4}S{sub 13} are in fair agreement with recent published data, the decomposition behavior of Cu{sub 4}Sn{sub 7}S{sub 16} differs from other studies in terms of decomposition temperature, thermal stability and products of reaction. Finally, the crystal structure refinements from neutron powder diffraction data are reported and discussed for the Cu{sub 4}Sn{sub 7}S{sub 16} and tetrahedrite Cu{sub 12}Sb{sub 4}S{sub 13} phases at 300 K, and for the high temperature form of skinnerite Cu{sub 3}SbS{sub 3} at 843 K. - Graphical abstract: In situ neutron powder diffraction data (heating rate of 2.5 K/min) indicates that (i) the ternary Cu{sub 12}Sb{sub 4}S{sub 13} phase is stable up to 792 K and decomposes at higher temperature into Cu{sub 3}SbS{sub 3} and Cu{sub 1.5}Sb{sub 0.5}S{sub 2}, and (ii) the Cu{sub 4}Sn{sub 7}S{sub 16} phase is stable up to 891 K and decomposes at higher temperature into Sn{sub 2}S{sub 3} and a cubic phase of sphalerite ZnS-type structure. Sulfur volatilization likely occurs in order to balance the overall stoichiometry.

  4. X-ray diffraction phase analysis of crystalline copper corrosion products after treatment in different chloride solutions

    International Nuclear Information System (INIS)

    Chmielova, M.; Seidlerova, J.; Weiss, Z.

    2003-01-01

    The corrosion products Cu 2 (OH) 3 Cl, Cu 2 O, and CuCl 2 were identified on the surface of copper plates after their four days treating in three different sodium chloride, sodium/magnesium, and sodium/calcium chloride solutions using X-ray diffraction powder analysis. However, the quantitative proportions of individual corrosion products differ and depend on the type of chloride solution used. Treating of copper plates only in the sodium chloride solution produced the mixture of corrosion products where Cu 2 O is prevailing over the Cu 2 (OH) 3 Cl and CuCl 2 was not identified. The sample developed after treating of the cooper surface in the sodium/magnesium chloride solution contains Cu 2 (OH) 3 Cl and CuCl 2 prevailing over the Cu 2 O, while the sample developed after treatment of copper in sodium/calcium chloride solution contains Cu 2 (OH) 3 Cl prevailing over CuCl 2 and Cu 2 O was not identified

  5. 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.

  6. [Comparative analysis between origin of cooked traditional Chinese medicine powder and modern formula granules].

    Science.gov (United States)

    Li, Rui; Zhai, Hua-Qiang; Tian, Wei-Lan; Hou, Ji-Ru; Jin, Shi-Yuan; Wang, Yong-Yan

    2016-03-01

    In this study, the origin and causes of cooked traditional Chinese medicine powder were reviewed, and a comprehensive analysis was made for the time background of modern traditional Chinese medicine formula granules and the future development trend, in order to provide reference for application and promotion of traditional Chinese medicine formula granules. By reference to ancient medical books of previous dynasties, a system review was conducted for infancy, formation, maturity and transition of cooked traditional Chinese medicine powder, and a comprehensive analysis was made for the six factors of cooked traditional Chinese medicine powder's maturity in the Song Dynasty. Efforts were made to collect domestic and foreign research literatures of modern formula granules, understand the detailed development, and conduct an objective analysis of the current clinical application of modern formula granules. According to the comparative analysis for the application characteristics of cooked traditional Chinese medicine powder and modern formula granules, ①the popularity of cooked traditional Chinese medicine powder in the Song Dynasty has six factors: soaring numbers of medical students and medical practitioners, high medical expenses due to huge army, rapid population growth, frequent epidemics and increasing diseases, and insufficient finances of central and local governments. ②On the basis of clinical application characteristics of traditional Chinese medicine formula granules, traditional Chinese medicine formula granules contain extracted and concentrated effective components, which guarantee the curative effect, meet modern people's demands for "quick, simple and convenience" traditional Chinese medicine decoctions, show a relatively high cost performance; however, formula granules are restricted by their varieties and lack unified quality control standards, and single-extract formula granules have not synergy and attenuation effects of combined traditional

  7. Microstructural Analysis of Sintered Gradient Materials Based on Distaloy SE Powder

    Directory of Open Access Journals (Sweden)

    Zarębski K.

    2016-06-01

    Full Text Available The study describes the microstructural analysis of cylindrically-shaped functionally graded products sintered from iron powder with scheduled graded structure on the cross-section running from the core to the surface layer of the sinter. Different types of structure were produced using Distaloy SE powder in two compositions - one without the addition of carbon, and another with 0.6wt% C. Two methods were used to fill the die cavity and shape the products. The first method involving a two-step compaction of individual layers. The second method using an original technique of die filling enabled the formation of transition zone between the outer layer and the core still at the stage of product shaping. As part of microstructural analysis, structural constituents were identified and voids morphology was examined. Studies covered the effect of the type of the applied method on properties of the graded zone obtained in the manufactured products

  8. Identification of low amount of irradiated spices (red pepper, garlic, ginger powder) with luminescence analysis

    Science.gov (United States)

    Kim, Byeong-Keun; Akram, Kashif; Kim, Cheong-Tae; Kang, Na-Roo; Lee, Jin-Won; Ryang, Jun-Hwan; Kwon, Joong-Ho

    2012-08-01

    For the identification of irradiated food, current analysis methods have limitations regarding presence and stability of radiation-induced markers. In this study, different spice blends with small quantity of different irradiated (0, 1 and 10 kGy) spice powders, such as red pepper, garlic or ginger, were investigated using PSL and TL techniques. In PSL-based screening analysis, the spice blends containing 10% of irradiated materials (1 or 10 kGy) were determined as intermediate or positive. In TL results, the blends containing 1% of 1 or 10 kGy-irradiated spices showed the typical TL glow curves that could be interpreted as positive. The blends with irradiated garlic powder provided more good results where identification was possible at 0.5% mixing of irradiated sample. However, the TL ratios of all spice blends were <0.1 and only TL glow curve shape and intensity may be used to discriminate the samples having irradiated component.

  9. Development of high performance liquid chromatography method for miconazole analysis in powder sample

    Science.gov (United States)

    Hermawan, D.; Suwandri; Sulaeman, U.; Istiqomah, A.; Aboul-Enein, H. Y.

    2017-02-01

    A simple high performance liquid chromatography (HPLC) method has been developed in this study for the analysis of miconazole, an antifungal drug, in powder sample. The optimized HPLC system using C8 column was achieved using mobile phase composition containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220 nm. The calibration graph was linear in the range from 10 to 50 mg/L with r 2 of 0.9983. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47 mg/L, respectively. The present HPLC method is applicable for the determination of miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The developed HPLC method provides short analysis time, high reproducibility and high sensitivity.

  10. Structure determination of β- and γ-BaAlF 5 by X-ray and neutron powder diffraction: A model for the α → β γ transitions

    Science.gov (United States)

    Le Bail, Armel; Ferey, Gérard; Mercier, Anne-Marie; De Kozak, Ariel; Samouél, Maurice

    1990-12-01

    β-BaAlF 5 is monoclinic (space group {P2 1}/{n}): a = 5.1517(1), Å, b = 19.5666(4), Å, c = 7.5567(2), Å, β = 92.426(1)°, Z = 8. γ-BaAlF 5 is monoclinic (space group P2 1): a = 5.2584(1), Å, b = 9.7298(2), Å, c = 7.3701(2), Å, β = 90.875(1)°, Z = 4. Both structures are determined ab initio from X-ray powder data; final results are given from neutron powder data refinements ( RI = 0.038, RP = 0.072, and RWP = 0.087 and RI = 0.048, RP = 0.083, and RWP = 0.101 for the β and γ phases, respectively). Like α-BaAlF 5, the β and γ phases are built up from isolated infinite (AlF 5) 2 n- n chains with AlF 6 octahedra sharing corners in a cis-position. Close structural relationships are shown to exist between the BaAl cationic subnetwork of: α-BaAlF 5 and the CrB-type structure; β-BaAlF 5 and the SrAg-type; γ-BaAlF 5 and the FeB-type. The polymorphic transitions are proposed to be topotactic and a displacive mechanism is suggested.

  11. Analysis of soft magnetic materials by electron backscatter diffraction as a powerful tool

    Science.gov (United States)

    Schuller, David; Hohs, Dominic; Loeffler, Ralf; Bernthaler, Timo; Goll, Dagmar; Schneider, Gerhard

    2018-04-01

    The current work demonstrates that electron backscatter diffraction (EBSD) is a powerful and versatile characterization technique for investigating soft magnetic materials. The properties of soft magnets, e.g., magnetic losses strongly depend on the materials chemical composition and microstructure, including grain size and shape, texture, degree of plastic deformation and elastic strain. In electrical sheet stacks for e-motor applications, the quality of the machined edges/surfaces of each individual sheet is of special interest. Using EBSD, the influence of the punching process on the microstructure at the cutting edge is quantitatively assessed by evaluating the crystallographic misorientation distribution of the deformed grains. Using an industrial punching process, the maximum affected deformation depth is determined to be 200 - 300 μm. In the case of laser cutting, the affected deformation depth is determined to be approximately zero. Reliability and detection limits of the developed EBSD approach are evaluated on non-affected sample regions and model samples containing different indentation test bodies. A second application case is the investigation of the recrystallization process during the annealing step of soft magnetic composites (SMC) toroids produced by powder metallurgy as a function of compaction pressure, annealing parameters and powder particle size. With increasing pressure and temperature, the recrystallized area fraction (e.g., grains with crystallographic misorientations particle boundaries or areas with existing plastic deformation. The progress of recrystallization is visualized as a function of time and of different particle to grain size distributions. Here, large particles with coarse internal grain structures show a favorable recrystallization behavior which results in large bulk permeability of up to 600 - 700 and lower amount of residual misorientations (>3°).

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

    International Nuclear Information System (INIS)

    YangDai, Tianyi; Zhang, Li

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-02-01

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

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

    Science.gov (United States)

    YangDai, Tianyi; Zhang, Li

    2016-02-01

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

  15. Oxygen stoichiometry and the structure of Tl[sub 2]Ba[sub 2]Ca[sub 2]Cu[sub 3]O[sub 10-y]. A high-resolution powder neutron diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Ogborne, D.M.; Weller, M.T.; Lanchester, P.C. (Dept. of Chemistry and Physics, Univ. of Southampton (United Kingdom))

    1992-09-15

    Samples of Tl[sub 2]Ba[sub 2]Ca[sub 2]Cu[sub 3]O[sub 10-y] have been prepared with three different oxygen stoichiometries by reaction under various oxygen gas partial pressures. Powder neutron diffraction studies on these materials show that for y > 0 oxygen vacancies exist in the thallium-oxygen layer; filling this site results in a contraction of the lattice with concomitant reduction in the apical Cu-O bond length but with an expansion of the copper-oxygen interlayer distance. These structural changes which occur as a function of oxygen content are discussed in terms of the superconducting properties of these materials. (orig.).

  16. Neutron powder diffraction investigation on the crystal and magnetic structure of (Ho{sub 0.50+x}Ca{sub 0.50-x})(Mn{sub 1-x}Cr{sub x})O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Martinelli, A; Ferretti, M [SPIN-CNR, Corso Perrone 24, 16152 Genova (Italy); Castellano, C [Dipartimento di Chimica Strutturale e Stereochimica Inorganica, Universita degli Studi di Milano, Via C Venezian 21, 20133 Milano (Italy); Cimberle, M R; Masini, R [IMEM-CNR, Via Dodecaneso 33, 16146 Genova (Italy); Ritter, C, E-mail: alberto.martinelli@spin.cnr.it [Institute Laue-Langevin, 6 rue Jules Horowitz, 38042 Grenoble Cedex 9 (France)

    2011-10-19

    The crystal and magnetic structure of (Ho{sub 0.50+x}Ca{sub 0.50-x})(Mn{sub 1-x}Cr{sub x})O{sub 3} (x = 0.00, 0.01, 0.02, 0.03) has been investigated between 5 and 300 K by means of neutron powder diffraction followed by Rietveld refinement and dc magnetic measurements. During cooling an orthorhombic to monoclinic phase transition occurs on account of the charge and orbital ordering taking place in the Mn sub-lattice; at low temperature phase separation takes place and the main monoclinic phase coexists with a secondary orthorhombic phase, whose amount slightly increases with the increase of Cr content. Cr{sup 3+} is not involved in orbital ordering or superexchange interactions. The charge and magnetic ordering are decoupled: the Mn moments order according to a CE-type structure in all samples. (paper)

  17. Magnetic ordering in the monoclinic structure of Nd5Si1.45Ge2.55 and Pr5Si1.5Ge2.5 studied by means of neutron powder diffraction

    International Nuclear Information System (INIS)

    Magen, C; Ritter, C; Morellon, L; Algarabel, P A; Ibarra, M R

    2004-01-01

    The compounds Nd 5 Si 1.45 Ge 2.55 and Pr 5 Si 1.5 Ge 2.5 have been investigated by means of magnetization measurements and neutron powder diffraction techniques. These alloys present a room-temperature monoclinic Gd 5 Si 2 Ge 2 -type crystallographic structure and, on cooling, both systems order ferromagnetically, at T C = 56 and 32 K, respectively, from a high-temperature paramagnetic to a low-temperature complex canted ferromagnetic state. The monoclinic crystallographic structure remains unchanged upon cooling down to 4 K, demonstrating the existence of a monoclinic ferromagnetic phase, and the possibility of a full decoupling of magnetic and crystallographic degrees of freedom in the 5:4 lanthanide intermetallic compounds

  18. Measurement and QCD analysis of the diffractive deep-inelastic scattering cross section at HERA

    International Nuclear Information System (INIS)

    Aktas, A.; Andreev, V.; Anthonis, T.

    2006-05-01

    A detailed analysis is presented of the diffractive deep-inelastic scattering process ep→eXY, where Y is a proton or a low mass proton excitation carrying a fraction 1-x P >0.95 of the incident proton longitudinal momentum and the squared four-momentum transfer at the proton vertex satisfies t 2 . Using data taken by the H1 experiment, the cross section is measured for photon virtualities in the range 3.5 ≤Q 2 ≤1600 GeV 2 , triple differentially in x P , Q 2 and β=x/x P , where x is the Bjorken scaling variable. At low x P , the data are consistent with a factorisable x P dependence, which can be described by the exchange of an effective pomeron trajectory with intercept α P (0)=1.118 ±0.008(exp.) +0.029 -0.010 (model). Diffractive parton distribution functions and their uncertainties are determined from a next-to-leading order DGLAP QCD analysis of the Q 2 and β dependences of the cross section. The resulting gluon distribution carries an integrated fraction of around 70% of the exchanged momentum in the Q 2 range studied. Total and differential cross sections are also measured for the diffractive charged current process e + p → anti ν e XY and are found to be well described by predictions based on the diffractive parton distributions. The ratio of the diffractive to the inclusive neutral current ep cross sections is studied. Over most of the kinematic range, this ratio shows no significant dependence on Q 2 at fixed x P and x or on x at fixed Q 2 and β. (Orig.)

  19. Measurement and QCD analysis of the diffractive deep-inelastic scattering cross section at HERA

    Science.gov (United States)

    Aktas, A.; Andreev, V.; Anthonis, T.; Antunovic, B.; Aplin, S.; Asmone, A.; Astvatsatourov, A.; Babaev, A.; Backovic, S.; Baghdasaryan, A.; Baranov, P.; Barrelet, E.; Bartel, W.; Baudrand, S.; Baumgartner, S.; Beckingham, M.; Behnke, O.; Behrendt, O.; Belousov, A.; Berger, N.; Bizot, J. C.; Boenig, M.-O.; Boudry, V.; Bracinik, J.; Brandt, G.; Brisson, V.; Bruncko, D.; Büsser, F. W.; Bunyatyan, A.; Buschhorn, G.; Bystritskaya, L.; Campbell, A. J.; Cassol-Brunner, F.; Cerny, K.; Cerny, V.; Chekelian, V.; Contreras, J. G.; Coughlan, J. A.; Coppens, Y. R.; Cox, B. E.; Cozzika, G.; Cvach, J.; Dainton, J. B.; Dau, W. D.; Daum, K.; de Boer, Y.; Delcourt, B.; Del Degan, M.; de Roeck, A.; de Wolf, E. A.; Diaconu, C.; Dodonov, V.; Dubak, A.; Eckerlin, G.; Efremenko, V.; Egli, S.; Eichler, R.; Eisele, F.; Eliseev, A.; Elsen, E.; Essenov, S.; Falkewicz, A.; Faulkner, P. J. W.; Favart, L.; Fedotov, A.; Felst, R.; Feltesse, J.; Ferencei, J.; Finke, L.; Fleischer, M.; Flucke, G.; Fomenko, A.; Franke, G.; Frisson, T.; Gabathuler, E.; Garutti, E.; Gayler, J.; Gerlich, C.; Ghazaryan, S.; Ginzburgskaya, S.; Glazov, A.; Glushkov, I.; Goerlich, L.; Goettlich, M.; Gogitidze, N.; Gorbounov, S.; Grab, C.; Greenshaw, T.; Gregori, M.; Grell, B. R.; Grindhammer, G.; Gwilliam, C.; Haidt, D.; Hansson, M.; Heinzelmann, G.; Henderson, R. C. W.; Henschel, H.; Herrera, G.; Hildebrandt, M.; Hiller, K. H.; Hoffmann, D.; Horisberger, R.; Hovhannisyan, A.; Hreus, T.; Hussain, S.; Ibbotson, M.; Ismail, M.; Jacquet, M.; Janssen, X.; Jemanov, V.; Jönsson, L.; Johnson, C. L.; Johnson, D. P.; Jung, A. W.; Jung, H.; Kapichine, M.; Katzy, J.; Kenyon, I. R.; Kiesling, C.; Klein, M.; Kleinwort, C.; Klimkovich, T.; Kluge, T.; Knies, G.; Knutsson, A.; Korbel, V.; Kostka, P.; Krastev, K.; Kretzschmar, J.; Kropivnitskaya, A.; Krüger, K.; Landon, M. P. J.; Lange, W.; Laštovička-Medin, G.; Laycock, P.; Lebedev, A.; Leibenguth, G.; Lendermann, V.; Levonian, S.; Lindfeld, L.; Lipka, K.; Liptaj, A.; List, B.; List, J.; Lobodzinska, E.; Loktionova, N.; Lopez-Fernandez, R.; Lubimov, V.; Lucaci-Timoce, A.-I.; Lueders, H.; Lux, T.; Lytkin, L.; Makankine, A.; Malden, N.; Malinovski, E.; Marage, P.; Marshall, R.; Marti, L.; Martisikova, M.; Martyn, H.-U.; Maxfield, S. J.; Mehta, A.; Meier, K.; Meyer, A. B.; Meyer, H.; Meyer, J.; Michels, V.; Mikocki, S.; Milcewicz-Mika, I.; Milstead, D.; Mladenov, D.; Mohamed, A.; Moreau, F.; Morozov, A.; Morris, J. V.; Mozer, M. U.; Müller, K.; Murín, P.; Nankov, K.; Naroska, B.; Naumann, T.; Newman, P. R.; Niebuhr, C.; Nikiforov, A.; Nowak, G.; Nowak, K.; Nozicka, M.; Oganezov, R.; Olivier, B.; Olsson, J. E.; Osman, S.; Ozerov, D.; Palichik, V.; Panagoulias, I.; Papadopoulou, T.; Pascaud, C.; Patel, G. D.; Peng, H.; Perez, E.; Perez-Astudillo, D.; Perieanu, A.; Petrukhin, A.; Pitzl, D.; Plačakytė, R.; Portheault, B.; Povh, B.; Prideaux, P.; Rahmat, A. J.; Raicevic, N.; Reimer, P.; Rimmer, A.; Risler, C.; Rizvi, E.; Robmann, P.; Roland, B.; Roosen, R.; Rostovtsev, A.; Rurikova, Z.; Rusakov, S.; Salvaire, F.; Sankey, D. P. C.; Sauter, M.; Sauvan, E.; Schilling, F.-P.; Schmidt, S.; Schmitt, S.; Schmitz, C.; Schoeffel, L.; Schöning, A.; Schultz-Coulon, H.-C.; Sefkow, F.; Shaw-West, R. N.; Sheviakov, I.; Shtarkov, L. N.; Sloan, T.; Smirnov, P.; Soloviev, Y.; South, D.; Spaskov, V.; Specka, A.; Steder, M.; Stella, B.; Stiewe, J.; Stoilov, A.; Straumann, U.; Sunar, D.; Tchoulakov, V.; Thompson, G.; Thompson, P. D.; Toll, T.; Tomasz, F.; Traynor, D.; Trinh, T. N.; Truöl, P.; Tsakov, I.; Tsipolitis, G.; Tsurin, I.; Turnau, J.; Tzamariudaki, E.; Urban, K.; Urban, M.; Usik, A.; Utkin, D.; Valkárová, A.; Vallée, C.; van Mechelen, P.; Vargas Trevino, A.; Vazdik, Y.; Veelken, C.; Vinokurova, S.; Volchinski, V.; Wacker, K.; Weber, G.; Weber, R.; Wegener, D.; Werner, C.; Wessels, M.; Wessling, B.; Wissing, C.; Wolf, R.; Wünsch, E.; Xella, S.; Yan, W.; Yeganov, V.; Žáček, J.; Zálešák, J.; Zhang, Z.; Zhelezov, A.; Zhokin, A.; Zhu, Y. C.; Zimmermann, J.; Zimmermann, T.; Zohrabyan, H.; Zomer, F.

    2006-12-01

    A detailed analysis is presented of the diffractive deep-inelastic scattering process ep→eXY, where Y is a proton or a low mass proton excitation carrying a fraction 1-xIP>0.95 of the incident proton longitudinal momentum and the squared four-momentum transfer at the proton vertex satisfies |t|<1 GeV2. Using data taken by the H1 experiment, the cross section is measured for photon virtualities in the range 3.5≤Q2≤1600 GeV2, triple differentially in xIP, Q2 and β=x/xIP, where x is the Bjorken scaling variable. At low xIP, the data are consistent with a factorisable xIP dependence, which can be described by the exchange of an effective pomeron trajectory with intercept αIP(0)=1.118±0.008(exp.)+0.029 -0.010(model). Diffractive parton distribution functions and their uncertainties are determined from a next-to-leading order DGLAP QCD analysis of the Q2 and β dependences of the cross section. The resulting gluon distribution carries an integrated fraction of around 70% of the exchanged momentum in the Q2 range studied. Total and differential cross sections are also measured for the diffractive charged current process e+p→ν¯eXY and are found to be well described by predictions based on the diffractive parton distributions. The ratio of the diffractive to the inclusive neutral current ep cross sections is studied. Over most of the kinematic range, this ratio shows no significant dependence on Q2 at fixed xIP and x or on x at fixed Q2 and β.

  20. Preparation and pattern recognition of metallic Ni ultrafine powders by electroless plating

    International Nuclear Information System (INIS)

    Zhang, H.J.; Zhang, H.T.; Wu, X.W.; Wang, Z.L.; Jia, Q.L.; Jia, X.L.

    2006-01-01

    Using hydrazine hydrate as reductant, metallic Ni ultrafine powders were prepared from NiSO 4 aqueous solution by electroless plating method. The factors including concentration of NiSO 4 , bathing temperature, ratio of hydrazine hydrate to NiSO 4 , the pH of the solution, etc., on influence of the yield and average particle size of metallic Ni ultrafine powders were studied in detail. X-ray powders diffraction patterns show that the nickel powders are cubic crystallite. The average crystalline size of the ultrafine nickel powders is about 30 nm. The dielectric and magnetic loss of ultrafine Ni powders-paraffin wax composites were measured by the rectangle waveguide method in the range 8.2-12.4 GHz. The factors for Ni ultrafine powders preparation are optimized by computer pattern recognition program based on principal component analysis, the optimum factors regions with higher yield of metallic Ni ultrafine powders are indicated by this way

  1. Circular Hough transform diffraction analysis: A software tool for automated measurement of selected area electron diffraction patterns within Digital MicrographTM

    International Nuclear Information System (INIS)

    Mitchell, D.R.G.

    2008-01-01

    A software tool (script and plugin) for computing circular Hough transforms (CHT) in Digital Micrograph TM has been developed, for the purpose of automated analysis of selected area electron diffraction patterns (SADPs) of polycrystalline materials. The CHT enables the diffraction pattern centre to be determined with sub-pixel accuracy, regardless of the exposure condition of the transmitted beam or if a beam stop is present. Radii of the diffraction rings can also be accurately measured with sub-pixel precision. If the pattern is calibrated against a known camera length, then d-spacings with an accuracy of better than 1% can be obtained. These measurements require no a priori knowledge of the pattern and very limited user interaction. The accuracy of the CHT is degraded by distortion introduced by the projector lens, and this should be minimised prior to pattern acquisition. A number of optimisations in the CHT software enable rapid processing of patterns; a typical analysis of a 1kx1k image taking just a few minutes. The CHT tool appears robust and is even able to accurately measure SADPs with very incomplete diffraction rings due to texture effects. This software tool is freely downloadable via the Internet

  2. Circular Hough transform diffraction analysis: A software tool for automated measurement of selected area electron diffraction patterns within Digital Micrograph{sup TM}

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, D.R.G. [Institute of Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia)], E-mail: drm@ansto.gov.au

    2008-03-15

    A software tool (script and plugin) for computing circular Hough transforms (CHT) in Digital Micrograph{sup TM} has been developed, for the purpose of automated analysis of selected area electron diffraction patterns (SADPs) of polycrystalline materials. The CHT enables the diffraction pattern centre to be determined with sub-pixel accuracy, regardless of the exposure condition of the transmitted beam or if a beam stop is present. Radii of the diffraction rings can also be accurately measured with sub-pixel precision. If the pattern is calibrated against a known camera length, then d-spacings with an accuracy of better than 1% can be obtained. These measurements require no a priori knowledge of the pattern and very limited user interaction. The accuracy of the CHT is degraded by distortion introduced by the projector lens, and this should be minimised prior to pattern acquisition. A number of optimisations in the CHT software enable rapid processing of patterns; a typical analysis of a 1kx1k image taking just a few minutes. The CHT tool appears robust and is even able to accurately measure SADPs with very incomplete diffraction rings due to texture effects. This software tool is freely downloadable via the Internet.

  3. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    International Nuclear Information System (INIS)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N; Sowa, H; Ahsbahs, H; Chernyshev, V V; Dmitriev, V P

    2008-01-01

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, β-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions

  4. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N [Research and Education Center ' Molecular Design and Ecologically Safe Technologies' , REC-008, Novosibirsk State University (Russian Federation); Sowa, H [Goettingen University (Germany); Ahsbahs, H; Chernyshev, V V [Marburg University (Germany); Dmitriev, V P [Swiss-Norwegian Beamline ESRF, Grenoble (France)], E-mail: boldyrev@nsu.ru

    2008-07-15

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, {beta}-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions.

  5. Line profile analysis of ODS steels Fe20Cr5AlTiY milled powders at different Y2O3 concentrations

    Science.gov (United States)

    Afandi, A.; Nisa, R.; Thosin, K. A. Z.

    2017-04-01

    Mechanical properties of material are largely dictated by constituent microstructure parameters such as dislocation density, lattice microstrain, crystallite size and its distribution. To develop ultra-fine grain alloys such as Oxide Dispersion Strengthened (ODS) alloys, mechanical alloying is crucial step to introduce crystal defects, and refining the crystallite size. In this research the ODS sample powders were mechanically alloyed with different Y2O3 concentration respectively of 0.5, 1, 3, and 5 wt%. MA process was conducted with High Energy Milling (HEM) with the ball to powder ratio of 15:1. The vial and the ball were made of alumina, and the milling condition is set 200 r.p.m constant. The ODS powders were investigated by X-Ray Diffractions (XRD), Bragg-Brentano setup of SmartLab Rigaku with 40 KV, and 30 mA, step size using 0.02°, with scanning speed of 4°min-1. Line Profile Analysis (LPA) of classical Williamson-Hall was carried out, with the aim to investigate the different crystallite size, and microstrain due to the selection of the full wide at half maximum (FWHM) and integral breadth.

  6. Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

    Science.gov (United States)

    Ng, Khim Hui; Heng, Audrey; Osborne, Murray

    2012-03-01

    Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Detection of Yersinia enterocolitica in milk powders by cross-priming amplification combined with immunoblotting analysis.

    Science.gov (United States)

    Zhang, Hongwei; Feng, Shaolong; Zhao, Yulong; Wang, Shuo; Lu, Xiaonan

    2015-12-02

    Yersinia enterocolitica (Y. enterocolitica) is frequently isolated from a wide variety of foods and can cause human yersiniosis. Biochemical and culture-based assays are common detection methods, but require a long incubation time and easily misidentify Y. enterocolitica as other non-pathogenic Yersinia species. Alternatively, cross-priming amplification (CPA) under isothermal conditions combined with immunoblotting analysis enables a more sensitive detection in a relatively short time period. A set of specific displacement primers, cross primers and testing primers was designed on the basis of six specific sequences in Y. enterocolitica 16S-23S rDNA internal transcribed spacer. Under isothermal condition, amplification and hybridization were conducted simultaneously at 63°C for 60 min. The specificity of CPA was tested for 96 different bacterial strains and 165 commercial milk powder samples. Two red lines were developed on BioHelix Express strip for all of the Y. enterocolitica strains, and one red line was shown for non-Y. enterocolitica strains. The limit of detection of CPA was 10(0)fg for genomic DNA (1000 times more sensitive than PCR assay), 10(1) CFU/ml for pure bacterial culture, and 10(0) CFU per 100 g milk powder with pre-enrichment at 37°C for 24 h. CPA combined with immunoblotting analysis can achieve highly specific and sensitive detection of Y. enterocolitica in milk powder in 90 min after pre-enrichment. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Crystallization and preliminary X-ray diffraction analysis of red clover necrotic mosaic virus

    International Nuclear Information System (INIS)

    Martin, Stanton L.; Guenther, Richard H.; Sit, Tim L.; Swartz, Paul D.; Meilleur, Flora; Lommel, Steven A.; Rose, Robert B.

    2010-01-01

    Virions of red clover necrotic mosaic virus have been purified and crystallized. The space group was determined to be I23, with unit-cell parameter a = 377.8 Å. The crystals diffracted to 4 Å resolution. Red clover necrotic mosaic virus (RCNMV) is a species that belongs to the Tombusviridae family of plant viruses with a T = 3 icosahedral capsid. RCNMV virions were purified and were crystallized for X-ray analysis using the hanging-drop vapor-diffusion method. Self-rotation functions and systematic absences identified the space group as I23, with two virions in the unit cell. The crystals diffracted to better than 4 Å resolution but were very radiation-sensitive, causing rapid decay of the high-resolution reflections. The data were processed to 6 Å in the analysis presented here

  9. Multielemental analysis of Brazilian milk powder and bread samples by neutron activation

    International Nuclear Information System (INIS)

    Maihara, V.A.; Vasconcellos, M.B.A.

    1988-01-01

    The concentrations of Na, Cl, Mn, Br, Fe, Zn, Rb, Sb, Sc, Cr, Al and Mg were determined in some types of bread and in some brands of milk powder consumed in the city of Sao Paulo (SP - Brasil), by instrumental neutron activation analysis. Radiochemical separations were carried out by means of retention of 24 Na on hydrated antimony pentoxide (HAP) from a 8N HCl solution, after digestion of the organic matter. Thus the radioisotopes 64 Cu, 69m Zn and 140 La could be determined in the effluent solution. The detection limits of the trace elements analyzed in bread and milk powder samples were determined using the Currie and Girardi criterions. (author) 22 refs.; 2 figs.; 7 tabs

  10. Analysis of powdered milk by PIXE (Proton Induced X-ray Emission)

    International Nuclear Information System (INIS)

    Desales Galeana, G.

    1990-01-01

    The purpose of this work was to establish the conditions to analyze elements of Z>15 in powdered milk samples using the PIXE technique. Ten different commercial samples were analyzed: 2 full-cream, 3 half-cream and 5 for infant feeding. They were all purchased in Toluca City, Mexico. Thick targets were prepared and irradiated with 1.5 and 3 MeV protons beam in Mexico's Nuclear Center Tandem Van de Graff Accelerator. The obtained data were analyzed by two computers programs. Iron, the reference element was analyzed by atomic absorption spectrometry. Concentrations of the following elements: phosphorus, chlorine, potassium, calcium, chrome, iron, cobalt, nickel, copper, zinc, bromine, rubidium, molybdenum and cadmium were evaluated. The concentrations of the first four elements were usually high, whereas those of the other elements remained in some ppm. The experimental conditions set up in this work were suitable for the analysis of powdered milk and can be applied to other organic samples (Author)

  11. Residual Stress Analysis for Engineering Applications by Means of Neutron Diffraction

    International Nuclear Information System (INIS)

    Gndupel-Herold, Thomas; Brand, Paul C.; Prask, Henry J.

    1999-01-01

    The economic and scientific importance of neutron diffraction residual stress analysis has led to an increasing number of suitable instruments worldwide. Recently, a dedicated state-of-the-art diffractometer has been installed at the National Institute of Standards and Technology reactor. It has been used for a variety of measurements on basic and engineering stress problems. Among the most prominent examples that have been investigated are residual stresses in rails, weldments, and plasma-sprayed coatings

  12. Effectiveness of local vancomycin powder to decrease surgical site infections: a meta-analysis.

    Science.gov (United States)

    Chiang, Hsiu-Yin; Herwaldt, Loreen A; Blevins, Amy E; Cho, Edward; Schweizer, Marin L

    2014-03-01

    Some surgeons use systemic vancomycin to prevent surgical site infections (SSIs), but patients who do not carry methicillin-resistant Staphylococcus aureus have an increased risk of SSIs when given vancomycin alone for intravenous prophylaxis. Applying vancomycin powder to the wound before closure could increase the local tissue vancomycin level without significant systemic levels. However, the effectiveness of local vancomycin powder application for preventing SSIs has not been established. Our objective was to systematically review and evaluate studies on the effectiveness of local vancomycin powder for decreasing SSIs. Meta-analysis. We included observational studies, quasi-experimental studies, and randomized controlled trials of patients undergoing surgical procedures that involved vancomycin powder application to surgical wounds, reported SSI rates, and had a comparison group that did not use local vancomycin powder. The primary outcome was postoperative SSIs. The secondary outcomes included deep incisional SSIs and S. aureus SSIs. We performed systematic literature searches in PubMed, the Cochrane Database of Systematic Reviews, the Database of Abstracts of Reviews of Effects, the Cochrane Central Register of Controlled Trials via Wiley, Scopus (including EMBASE abstracts), Web of Science, ClinicalTrials.gov, BMC Proceedings, ProQuest Dissertation, and Thesis in Health and Medicine, and conference abstracts from IDWeek, the Interscience Conference on Antimicrobial Agents and Chemotherapy, the Society for Healthcare Epidemiology of America, and the American Academy of Orthopedic Surgeons annual meetings, and also the Scoliosis Research Society Annual Meeting and Course. We ran the searches from inception on May 9, 2013 with no limits on date or language. After reviewing 373 titles or abstracts and 22 articles in detail, we included 10 independent studies and used a random-effects model when pooling risk estimates to assess the effectiveness of local

  13. Electron diffraction analysis of an AB{sub 2}-type Laves phase for hydrogen battery applications

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Z.; Chumbley, S.; Laabs, F.C. [Iowa State Univ., Ames, IA (United States). Ames Lab.

    2000-11-16

    A multicomponent AB{sub 2} type nickel-metal hydride (Ni-MH) battery alloy prepared by high-pressure gas atomization (HPGA) was investigated by transmission electron microscopy (TEM) in both the as-atomized and heat treated condition. TEM examination showed a heavily faulted dendritic growth structure in as-atomized powder. Selected area diffraction (SAD) showed that this region consisted of both a cubic C15 structure with lattice constant a=7.03 A and an hexagonal C14 structure with lattice parameter a=4.97 A, c=8.11 A. The orientation relationship (OR) between the C14 and C15 structures was determined to be (111)[1 anti 10]{sub C15}//(0001)[11 anti 20]C{sub 14}. An interdendritic phase possessing the C14 structure was also seen. There was also a very fine grain region consisting of the C14 structure. Upon heat treatment, the faulted structure became more defined and appeared as intercalation layers within the grains. Spherical particles rich in Zr and Ni appeared scattered at the grain boundries instead of the C14 interdendritic phase. The polycrystalline region also changed to a mixture of C14 and C15 structures. The phase stability of the C15 and C14 structures based on a consideration of atomic size factor and the average electron concentration is discussed. (orig.)

  14. X-ray diffraction analysis of a severely plastically deformed aluminum alloy

    International Nuclear Information System (INIS)

    Ortiz, A.L.; Shaw, L.

    2004-01-01

    The crystallite size, lattice microstrain, lattice parameter, and formation of solid solutions of a nanocrystalline Al 93 Fe 3 Cr 2 Ti 2 alloy prepared via mechanical alloying (MA) starting from elemental powders have been investigated using the Rietveld method of X-ray diffraction (XRD) in conjunction with line-broadening analyses through the variance, Warren-Averbach, and Stokes and Wilson methods. Detailed analyses using transmission electron microscopy (TEM), scanning electron microscopy (SEM), and inductively coupled plasma-optical emission spectroscopy (ICP) have also been conducted in order to corroborate the formation of solid solutions and the grain size measurement determined from the XRD analyses. The results from the exhaustive XRD analyses are in excellent agreement with those derived from the investigation of TEM, SEM, and ICP. The lattice microstrains of the nanocrystalline Al solid solution determined from the XRD analyses are isotropic along different crystallographic directions and high, exhibiting the same order of magnitude as the ratio of the tensile strength to the elastic modulus of the Al crystal. Implications resulting from the comparison between the present study and the simplified XRD analyses are discussed

  15. Crystal structure and charge density analysis of Li2NH by synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Noritake, T.; Nozaki, H.; Aoki, M.; Towata, S.; Kitahara, G.; Nakamori, Y.; Orimo, S.

    2005-01-01

    Complex hydrides, such as lithium amide (LiNH 2 ) and lithium imide (Li 2 NH), have recently been noticed as one of the most promising materials for reversible hydrogen storage. In this paper, we reveal the bonding nature of hydrogen in Li 2 NH crystal by synchrotron powder X-ray diffraction measurement at room temperature. The crystal structure was refined by Rietveld method and the charge density distribution was analyzed by maximum entropy method (MEM). The Li 2 NH crystal is anti-fluorite type structure (space group Fm3-bar m) consisting of Li and NH. Hydrogen atom occupies randomly the 48h (Wyckoff notation) sites around N atom. The refined lattice constant is a=5.0742(2)A. The charge density distribution around NH anion in Li 2 NH is almost spherical. The number of electrons within the sphere around the Li and NH is estimated from the obtained charge density distribution. As the result, the ionic charge is expressed as [Li 0.99+ ] 2 [NH] 1.21- . Therefore, it is confirmed experimentally that Li 2 NH is ionically bonded

  16. Integrated Data Collection Analysis (IDCA) Program — Bullseye® Smokeless Powder

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Phillips, Jason J. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Shelley, Timothy J. [Bureau of Alcohol, Tobacco and Firearms, Redstone Arsenal, AL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-05-30

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of Bullseye® smokeless powder (Gunpowder). The participants found the Gunpowder: 1) to have a range of sensitivity to impact, from less than RDX to almost as sensitive as PETN, 2) to be moderately sensitive to BAM and ABL friction, 3) have a range for ESD, from insensitive to more sensitive than PETN, and 4) to have thermal sensitivity about the same as PETN and RDX.

  17. XRD analysis and microstructure of milled and sintered V, W, C, and Co powders

    CSIR Research Space (South Africa)

    Bolokang, AS

    2011-01-01

    Full Text Available on the starting compositions of pure elements, their lattice coherency according to Hume-Rothery rules on crystal structure and atomic size, and enough milling time that provides adequate kinetics. Keywords ? X-ray analysis; ? (V,W)C; ? Co15W8C6...-1 International Journal of Refractory Metals and Hard Materials Volume 29, Issue 1, January 2011, Pages 108?111 XRD analysis and microstructure of milled and sintered V, W, C, and Co powders ? A.S. Bolokang ? M.J. Phasha ? C. Oliphant ? D. Motaung ? a...

  18. Elucidating the breathing of the metal-organic framework MIL-53(Sc) with ab initio molecular dynamics simulations and in situ X-ray powder diffraction experiments.

    Science.gov (United States)

    Chen, Linjiang; Mowat, John P S; Fairen-Jimenez, David; Morrison, Carole A; Thompson, Stephen P; Wright, Paul A; Düren, Tina

    2013-10-23

    Ab initio molecular dynamics (AIMD) simulations have been used to predict structural transitions of the breathing metal-organic framework (MOF) MIL-53(Sc) in response to changes in temperature over the range 100-623 K and adsorption of CO2 at 0-0.9 bar at 196 K. The method has for the first time been shown to predict successfully both temperature-dependent structural changes and the structural response to variable sorbate uptake of a flexible MOF. AIMD employing dispersion-corrected density functional theory accurately simulated the experimentally observed closure of MIL-53(Sc) upon solvent removal and the transition of the empty MOF from the closed-pore phase to the very-narrow-pore phase (symmetry change from P2(1)/c to C2/c) with increasing temperature, indicating that it can directly take into account entropic as well as enthalpic effects. We also used AIMD simulations to mimic the CO2 adsorption of MIL-53(Sc) in silico by allowing the MIL-53(Sc) framework to evolve freely in response to CO2 loadings corresponding to the two steps in the experimental adsorption isotherm. The resulting structures enabled the structure determination of the two CO2-containing intermediate and large-pore phases observed by experimental synchrotron X-ray diffraction studies with increasing CO2 pressure; this would not have been possible for the intermediate structure via conventional methods because of diffraction peak broadening. Furthermore, the strong and anisotropic peak broadening observed for the intermediate structure could be explained in terms of fluctuations of the framework predicted by the AIMD simulations. Fundamental insights from the molecular-level interactions further revealed the origin of the breathing of MIL-53(Sc) upon temperature variation and CO2 adsorption. These simulations illustrate the power of the AIMD method for the prediction and understanding of the behavior of flexible microporous solids.

  19. Determination of metal impurities in MOX powder by direct current arc atomic emission spectroscopy. Application of standard addition method for direct analysis of powder sample

    International Nuclear Information System (INIS)

    Furuse, Takahiro; Taguchi, Shigeo; Kuno, Takehiko; Surugaya, Naoki

    2016-12-01

    Metal impurities in MOX powder obtained from uranium and plutonium recovered from reprocessing process of spent nuclear fuel have to be determined for its characterization. Direct current arc atomic emission spectroscopy (DCA-AES) is one of the useful methods for direct analysis of powder sample without dissolving the analyte into aqueous solution. However, the selection of standard material, which can overcome concerns such as matrix matching, is quite important to create adequate calibration curves for DCA-AES. In this study, we apply standard addition method using the certified U_3O_8 containing known amounts of metal impurities to avoid the matrix problems. The proposed method provides good results for determination of Fe, Cr and Ni contained in MOX samples at a significant quantity level. (author)

  20. Analysis of diffuse scattering in neutron powder diagrams. Application to glassy carbon

    International Nuclear Information System (INIS)

    Boysen, H.

    1985-01-01

    From the quantitative analysis of the diffuse scattered intensity in powder diagrams valuable information about the disorder in crystals may be obtained. According to the dimensionality of this disorder (0D, 1D, 2D or 3D corresponding to diffuse peaks, streaks, planes or volume in reciprocal space) a characteristic modulation of the background is observed, which is described by specific functions. These are derived by averaging the appropriate cross sections over all crystallite orientations in the powder and folding with the resolution function of the instrument. If proper account is taken of all proportionality factors different components of the background can be put on one relative scale. The results are applied to two samples of glassy carbon differing in their degree of disorder. The neutron powder patterns contain contributions from 0D (00l peaks due to the stacking of graphitic layers), 1D (hkzeta streaks caused by the random orientation of these layers) and 3D (incoherent scattering, averaged thermal diffuse scattering, multiple scattering). From the fit to the observed data various parameters of the disorder like domain sizes, strains, interlayer distances, amount of incorporated hydrogen, pore sizes etc. are determined. It is shown that the omission of resolution corrections leads to false parameters. (orig.)

  1. Microstructural analysis of sinterized aluminum powder obtained by the high energy milling of beverage cans

    International Nuclear Information System (INIS)

    Souza, Jose Raelson Pereira de; Peres, Mauricio Mhirdaui

    2016-01-01

    The objective is the study of the effect of high energy milling on the sintering of aluminum from beverage cans. The selected aluminum cans were cut and subjected to high energy milling under a common atmosphere (in the air). In milling, three grams of aluminum was used to maintain the ratio of 10/1 between the mass of the beads and the material. The milling time was varied in 1h, 1.5h and 2h, keeping the other variables constant. The particle size distribution was measured by laser granulometry, for further compaction and sintering at a temperature of 600 ° C for 2 h. The samples were characterized by scanning electron microscopy (SEM). The granulometric analysis of the powders found that higher milling times produced finer particles. Powders with granulometry of less than 45 μm were obtained at 1 h, 1.5 h and 2 h times. The times of 1.5h and 2h promoted finer particles with better distribution of size. The SEM analyzes showed little variation in the shape of the particles as a function of the variation of the grinding times, presenting irregularities in the platelet geometry. The sintering time and temperature were effective in the densification of the powder particles, which were influenced by the average particle size

  2. Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction--a benchmark structure-property study.

    Science.gov (United States)

    Lock, Nina; Jensen, Ellen M L; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B

    2013-07-14

    Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0-2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water-isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5-7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300-1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

  3. Influence of Ba/Fe mole ratios on magnetic properties, crystallite size and shifting of X-ray diffraction peaks of nanocrystalline BaFe12O19 powder, prepared by sol gel auto combu

    Science.gov (United States)

    Suastiyanti, Dwita; Sudarmaji, Arif; Soegijono, Bambang

    2012-06-01

    Barium hexaferrite BaFe12O19 (BFO) is of great importance as permanent magnets, particularly for magnetic recording as well as in microwave devices. Nano-crystalline BFO powders were prepared by sol gel auto combustion method in citric acid - metal nitrates system. Hence the mole ratios of Ba/Fe were variated at 1:12; 1:11.5 and 1:11. Ratio of cation to fuel was fixed at 1:1. An appropriate amount of amonia solution was added dropwise to this solution with constant stirring until the PH reached 7 in all cases. Heating at 850oC for 10 hours for each sample to get final formation of BFO nanocrystalline. The data from XRD showing the lattice parameters a,c and the unit-cell volume V, confirm that BFO with ratio 1:12 has same crystall parameters with ratio 1:11. Ratio of Ba/Fe 1:12 and 1:11 have diffraction pattern similarly at almost each 2 θ for each samples. Ratio of Ba/Fe 1: 11.5 has the finest crystallite size 22 nm. Almost diffraction pattern peaks of Ba/Fe 1:11.5 move to the left from of Ba/Fe 1:12 then return to diffraction pattern of Ba/Fe 1:12 for Ba/Fe 1:11. SEM observations show the particle size less than 100 nm and the same shape for each sample. Ratio of Ba/Fe 1: 12 gives the highest intrinsic coercive Hc = 427.3 kA/m. The highest remanent magnetization is at ratio 1:11 with Mr = 0.170 T. BFO with mole ratio 1:11.5 has the finest grain 22 nm, good magnetic properties and the highest value of best FoM 89%.

  4. Crystals of DhaA mutants from Rhodococcus rhodochrous NCIMB 13064 diffracted to ultrahigh resolution: crystallization and preliminary diffraction analysis

    International Nuclear Information System (INIS)

    Stsiapanava, Alena; Koudelakova, Tana; Lapkouski, Mikalai; Pavlova, Martina; Damborsky, Jiri; Kuta Smatanova, Ivana

    2008-01-01

    Three mutants of the haloalkane dehalogenase DhaA derived from R. rhodochrous NCIMB 13064 were crystallized and diffracted to ultrahigh resolution. The enzyme DhaA from Rhodococcus rhodochrous NCIMB 13064 belongs to the haloalkane dehalogenases, which catalyze the hydrolysis of haloalkanes to the corresponding alcohols. The haloalkane dehalogenase DhaA and its variants can be used to detoxify the industrial pollutant 1,2,3-trichloropropane (TCP). Three mutants named DhaA04, DhaA14 and DhaA15 were constructed in order to study the importance of tunnels connecting the buried active site with the surrounding solvent to the enzymatic activity. All protein mutants were crystallized using the sitting-drop vapour-diffusion method. The crystals of DhaA04 belonged to the orthorhombic space group P2 1 2 1 2 1 , while the crystals of the other two mutants DhaA14 and DhaA15 belonged to the triclinic space group P1. Native data sets were collected for the DhaA04, DhaA14 and DhaA15 mutants at beamline X11 of EMBL, DESY, Hamburg to the high resolutions of 1.30, 0.95 and 1.15 Å, respectively

  5. AUSPEX: a graphical tool for X-ray diffraction data analysis.

    Science.gov (United States)

    Thorn, Andrea; Parkhurst, James; Emsley, Paul; Nicholls, Robert A; Vollmar, Melanie; Evans, Gwyndaf; Murshudov, Garib N

    2017-09-01

    In this paper, AUSPEX, a new software tool for experimental X-ray data analysis, is presented. Exploring the behaviour of diffraction intensities and the associated estimated uncertainties facilitates the discovery of underlying problems and can help users to improve their data acquisition and processing in order to obtain better structural models. The program enables users to inspect the distribution of observed intensities (or amplitudes) against resolution as well as the associated estimated uncertainties (sigmas). It is demonstrated how AUSPEX can be used to visually and automatically detect ice-ring artefacts in integrated X-ray diffraction data. Such artefacts can hamper structure determination, but may be difficult to identify from the raw diffraction images produced by modern pixel detectors. The analysis suggests that a significant portion of the data sets deposited in the PDB contain ice-ring artefacts. Furthermore, it is demonstrated how other problems in experimental X-ray data caused, for example, by scaling and data-conversion procedures can be detected by AUSPEX.

  6. The purification, crystallization and preliminary X-ray diffraction analysis of dihydrodipicolinate synthase from Clostridium botulinum

    International Nuclear Information System (INIS)

    Dobson, Renwick C. J.; Atkinson, Sarah C.; Gorman, Michael A.; Newman, Janet M.; Parker, Michael W.; Perugini, Matthew A.

    2008-01-01

    Dihydrodipicolinate synthase (DHDPS), an enzyme in the lysine-biosynthetic pathway, is a promising target for antibiotic development against pathogenic bacteria. Here, the expression, purification, crystallization and preliminary diffraction analysis of DHDPS from C. botulinum are reported. In recent years, dihydrodipicolinate synthase (DHDPS; EC 4.2.1.52) has received considerable attention from both mechanistic and structural viewpoints. This enzyme, which is part of the diaminopimelate pathway leading to lysine, couples (S)-aspartate-β-semialdehyde with pyruvate via a Schiff base to a conserved active-site lysine. In this paper, the expression, purification, crystallization and preliminary X-ray diffraction analysis of DHDPS from Clostridium botulinum, an important bacterial pathogen, are presented. The enzyme was crystallized in a number of forms, predominantly using PEG precipitants, with the best crystal diffracting to beyond 1.9 Å resolution and displaying P4 2 2 1 2 symmetry. The unit-cell parameters were a = b = 92.9, c = 60.4 Å. The crystal volume per protein weight (V M ) was 2.07 Å 3 Da −1 , with an estimated solvent content of 41%. The structure of the enzyme will help guide the design of novel therapeutics against the C. botulinum pathogen

  7. Crystallization and preliminary X-ray diffraction analysis of diaminopimelate epimerase from Escherichia coli

    International Nuclear Information System (INIS)

    Hor, Lilian; Dobson, Renwick C. J.; Dogovski, Con; Hutton, Craig A.; Perugini, Matthew A.

    2009-01-01

    Diaminopimelate (DAP) epimerase, an enzyme in the lysine-biosynthetic pathway, is a promising target for antibiotic development against pathogenic bacteria. Here, the cloning, expression, purification, crystallization and preliminary diffraction analysis of DAP epimerase from E. coli are reported. Diaminopimelate (DAP) epimerase (EC 5.1.1.7) catalyzes the penultimate step of lysine biosynthesis in bacteria and plants, converting l,l-diaminopimelate to meso-diaminopimelate. Here, the cloning, expression, purification, crystallization and preliminary X-ray diffraction analysis of DAP epimerase from Escherichia coli are presented. Crystals were obtained in space group P4 1 2 1 2 and diffracted to 2.0 Å resolution, with unit-cell parameters a = b = 89.4, c = 179.6 Å. Molecular replacement was conducted using Bacillus anthracis DAP epimerase as a search model and showed the presence of two molecules in the asymmetric unit, with an initial R free of 0.456 and R work of 0.416

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

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi

    2010-01-01

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

  9. Applications of the Warren-Averbach method of X-ray diffraction line profile analysis

    International Nuclear Information System (INIS)

    Ichikawa, Rodrigo Uchida

    2013-01-01

    The objective of this work was to develop and implement a methodology of X-ray Line Profile Analysis (XLPA) for the study and determination of the mean crystallite sizes and microstrains in materials. A computer program was developed to speed up the treatment of diffraction peaks and perform the deconvolution utilizing the Stokes method to correct the instrumental contribution in the X-ray diffraction measurements. The XLPA methods used were the Scherrer, Williamson-Hall and Single-Line methods, which can be called real space methods, and the Fourier space method of Warren-Averbach. Furthermore, considering a mathematical modelling it was possible to calculate the crystallite size distribution, considering the log-normal distribution and spherical crystallites. It was possible to demonstrate the proposed theory can provide reliable results evaluating a dispersion parameter. The methodologies described above were applied in two distinct materials: in the alloy Zircaloy-4 and in ZnO. (author)

  10. Atomic-layer-resolved analysis of surface magnetism by diffraction spectroscopy

    International Nuclear Information System (INIS)

    Matsui, Fumihiko; Matsushita, Tomohiro; Daimon, Hiroshi

    2010-01-01

    X-ray absorption near edge structure (XANES) and X-ray magnetic circular dichroism (XMCD) measurements by Auger-electron-yield detection are powerful analysis tools for the electronic and magnetic structures of surfaces, but all the information from atoms within the electron mean-free-path range is summed into the obtained spectrum. In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, diffraction spectroscopy, which is the combination of X-ray absorption spectroscopy and Auger electron diffraction (AED). From a series of measured thickness dependent AED patterns, we deduced a set of atomic-layer-specific AED patterns arithmetically. Based on these AED patterns, we succeeded in disentangling obtained XANES and XMCD spectra into those from different atomic layers.

  11. High temperature neutron diffraction study of LaPO4

    International Nuclear Information System (INIS)

    Mishra, S.K.; Mittal, R.; Ningthoujam, R.S.; Vatsa, R.K.; Hansen, T.

    2016-01-01

    We report high temperature powder neutron diffractions study in LaPO 4 using high-flux D20 neutron diffractometer in the Institut Laue-Langevin, France. The measurements were carried out in high resolution mode (incident neutron wavelength 1.36 A) at various temperature upto 900°C. CarefuI inspection of temperature dependence of diffraction data showed appearance and disappearance of certain Bragg's reflections above 1273 K. It is a signature of structural phase transition. Rietveld refinement of the powder diffraction data revealed that diffraction patterns at and above 800°C could be indexed using the monoclinic structure with P21/n space group. Detail analysis for identify the water molecules is under investigation. (author)

  12. Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data

    DEFF Research Database (Denmark)

    Gorelik, Tatiana E; van de Streek, Jacco; Kilbinger, Andreas F M

    2012-01-01

    Ab-initio crystal structure analysis of organic materials from electron diffraction data is presented. The data were collected using the automated electron diffraction tomography (ADT) technique. The structure solution and refinement route is first validated on the basis of the known crystal stru...

  13. X-ray diffraction analysis and in vitro characterization of the UAM2 protein from Oryza sativa

    DEFF Research Database (Denmark)

    Welner, Ditte Hededam; Tsai, Alex Yi-Lin; DeGiovanni, Andy M.

    2017-01-01

    protein from Oryza sativa (OsUAM2) were undertaken. Here, X-ray diffraction data are reported, as well as analysis of the oligomeric state in the crystal and in solution. OsUAM2 crystallizes readily but forms highly radiation-sensitive crystals with limited diffraction power, requiring careful low......, a requirement for a structural metal ion....

  14. Spectrochemical analysis of powder using 355 nm Nd-YAG laser-induced low-pressure plasma.

    Science.gov (United States)

    Lie, Zener S; Pardede, M; Hedwig, R; Suliyanti, M M; Kurniawan, Koo Hendrik; Munadi; Lee, Yong-Inn; Kagawa, Kiichiro; Hattori, Isamu; Tjia, May On

    2008-04-01

    The applicability of spectrochemical analysis of minute amounts of powder samples was investigated using an ultraviolet Nd-YAG laser (355 nm) and low-pressure ambient air. A large variety of chemical powder samples of different composition were employed in the experiment. These included a mixture of copper(II) sulfate pentahydrate, zinc sulfide, and chromium(III) sulfate n-hydrate powders, baby powder, cosmetic powders, gold films, zinc supplement tablet, and muds and soils from different areas. The powder samples were prepared by pulverizing the original samples to an average size of around 30 microm in order to trap them in the tiny micro holes created on the surface of the quartz subtarget. It was demonstrated that in all cases studied, good quality spectra were obtained with low background, free from undesirable contamination by the subtarget elements and featuring ppm sensitivity. A further measurement revealed a linear calibration curve with zero intercept. These results clearly show the potential application of this technique for practical qualitative and quantitative spectrochemical analysis of powder samples in various fields of study and investigation.

  15. Phase identification and internal stress analysis of steamside oxides on superheater tubes by means of X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Pantleon, Karen; Montgomery, Melanie [Technical Univ. of Denmark, Lyngby (Denmark). Inst. of Manufacturing Engineering and Management

    2005-05-01

    For superheater tubes, the adherence of the inner steamside oxide is especially important as spallation of this oxide results in a) blockage of loops which cause insufficient steam flow through the superheaters and subsequently overheating and tube failure and b) spalled oxide can cause erosion of turbine blades. Oxide spallation is a serious problem for austenitic steels where the significant differences of the thermal expansion coefficients of steel and oxide cause relatively high thermal stresses. Usually, various oxides layered within the scale are suggested from microscopical observations of the morphology and/or topography of the oxide scale accompanied by the analysis of chemical elements present. Reports about the application of X-ray diffraction on the study of steamside oxide formation are very scarce in literature. If applied at all, XRD-studies are restricted to ideally flat samples oxidized under laboratory conditions, but relation to real operating conditions and the effect of the real sample geometry is missing. Within the frame of the project, steamside oxides on plant exposed components of ferritic/ martensitic X20CrMoV12-1 as well as fine- and coarse-grained austenitic TP347H were studied by means of X-ray diffraction. Depth dependent phase analysis on sample segments cut from the tubes was carried out by means of grazing incidence diffraction and, in order to obtain information from a larger depth, conventional XRD was combination with stepwise mechanical removal of the steamside oxides. After each removal step phase analysis was performed both on the segments and on the removed powders. Phase specific stress analysis was carried out on rings cut from the tube. Results show that steamside oxides on X20CrMoV12-1 consist of pure Hematite at the surface followed by a relatively thick layer of pure Magnetite. Both phases are under relatively high tensile stresses. While the phase composition of the Hematite layer appears to be the same for all

  16. Barium strontium titanate powders prepared by spray pyrolysis

    International Nuclear Information System (INIS)

    Brankovic, G.; Brankovic, Z.; Goes, M.S.; Paiva-Santos, C.O.; Cilense, M.; Varela, J.A.; Longo, E.

    2005-01-01

    Ultasonic spray pyrolysis (SP) has been investigated for the production of the barium strontium titanate (BST) powders from the polymeric precursors. The processing parameters, such as flux of aerosol and temperature profile inside the furnace, were optimized to obtain single phase BST. The powders were characterized by the methods of X-ray diffraction analysis, SEM, EDS and TEM. The obtained powders were submicronic, consisting of spherical, polycrystalline particles, with internal nanocrystalline structure. Crystallite size of 10 nm, calculated using Rietveld refinement, is in a good agreement with results of HRTEM

  17. The effect of polymorphism on powder compaction and dissolution properties of chemically equivalent oxytetracycline hydrochloride powders.

    Science.gov (United States)

    Liebenberg, W; de Villiers, M M; Wurster, D E; Swanepoel, E; Dekker, T G; Lötter, A P

    1999-09-01

    In South Africa, oxytetracycline is identified as an essential drug; many generic products are on the market, and many more are being developed. In this study, six oxytetracycline hydrochloride powders were obtained randomly from manufacturers, and suppliers were compared. It was found that compliance to a pharmacopoeial monograph was insufficient to ensure the optimum dissolution performance of a simple tablet formulation. Comparative physicochemical raw material analysis showed no major differences with regard to differential scanning calorimetry (DSC), infrared (IR) spectroscopy, powder dissolution, and particle size. However, the samples could be divided into two distinct types with respect to X-ray powder diffraction (XRD) and thus polymorphism. The two polymorphic forms had different dissolution properties in water or 0.1 N hydrochloride acid. This difference became substantial when the dissolution from tablets was compared. The powders containing form A were less soluble than that containing form B.

  18. Assessment of firing conditions in old fired-clay bricks: The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Energy Technology Data Exchange (ETDEWEB)

    Viani, Alberto, E-mail: viani@itam.cas.cz [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Sotiriadis, Konstantinos [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Len, Adél [Wigner Research Centre for Physics HAS, Konkoly-Thege 29-33, 1121 Budapest (Hungary); Šašek, Petr; Ševčík, Radek [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic)

    2016-06-15

    Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

  19. Garlic powder intake and cardiovascular risk factors: a meta-analysis of randomized controlled clinical trials.

    Science.gov (United States)

    Kwak, Jin Sook; Kim, Ji Yeon; Paek, Ju Eun; Lee, You Jin; Kim, Haeng-Ran; Park, Dong-Sik; Kwon, Oran

    2014-12-01

    Although preclinical studies suggest that garlic has potential preventive effects on cardiovascular disease (CVD) risk factors, clinical trials and reports from systematic reviews or meta-analyses present inconsistent results. The contradiction might be attributed to variations in the manufacturing process that can markedly influence the composition of garlic products. To investigate this issue further, we performed a meta-analysis of the effects of garlic powder on CVD risk factors. We searched PubMed, Cochrane, Science Direct and EMBASE through May 2014. A random-effects meta-analysis was performed on 22 trials reporting total cholesterol (TC), 17 trials reporting LDL cholesterol (LDL-C), 18 trials reporting HDL cholesterol (HDL-C), 4 trials reporting fasting blood glucose (FBG), 9 trials reporting systolic blood pressure (SBP) and 10 trials reporting diastolic blood pressure (DBP). The overall garlic powder intake significantly reduced blood TC and LDL-C by -0.41 mmol/L (95% confidence interval [CI], -0.69, -0.12) (-15.83 mg/dL [95% CI, -26.64, -4.63]) and -0.21 mmol/L (95% CI, -0.40, -0.03) (-8.11 mg/dL [95% CI, -15.44, -1.16]), respectively. The mean difference in the reduction of FBG levels was -0.96 mmol/L (95% CI, -1.91, -0.01) (-17.30 mg/dL [95% CI, -34.41, -0.18]). Evidence for SBP and DBP reduction in the garlic supplementation group was also demonstrated by decreases of -4.34 mmHg (95% CI, -8.38, -0.29) and -2.36 mmHg (95% CI, -4.56, -0.15), respectively. This meta-analysis provides consistent evidence that garlic powder intake reduces the CVD risk factors of TC, LDL-C, FBG and BP.

  20. A X-ray diffraction analysis on graphene layers of Assam coal

    Energy Technology Data Exchange (ETDEWEB)

    Saikia, B.K.; Boruah, R.K.; Gogoi, P.K. [CSIR, Jorhat (India)

    2009-01-15

    The so-called turbostatic structure of carbons in coal with randomly oriented stacking of the lamellae (graphene) produces intense peaks, which are the dominant features in its X-ray diffraction profiles. The diffractogram may be conveniently divided into two regions of reciprocal space, the medium S region (1 < S < 3 {angstrom}) and a high S region (S > 3 {angstrom}) where S = 4 {pi} {lambda} {sup -1}sin{theta}. To better understand the molecular level structure of high sulphur Assam coal, two coal samples (Tirap-1 and Tirap-2) from Tirap colliery of Makum coalfield, Assam (India) has been interpreted in this study by using the X-ray diffraction profiles. Random layered (graphene) structural parameters of these coals were determined by using X-ray diffraction technique, which showed that the L{sub a} and L{sub c} are 64.99 angstrom and 22.63 angstrom for Tirap-2 and 55.54 angstrom and 23.80 angstrom for that of Tirap-1 coals respectively. The position of {gamma} band was found to be at 4.34 {angstrom} and 4.13 angstrom for Tirap-2 and Tirap-1 coals respectively. The number of layers and average number of carbon atoms (N) per aromatic graphene were found to be 21 and 8 for both the coal samples. Proximate, ultimate and ash analysis of the two coal samples were also carried out in this investigation.

  1. The materials science synchrotron beamline EDDI for energy-dispersive diffraction analysis

    International Nuclear Information System (INIS)

    Genzel, Ch.; Denks, I.A.; Gibmeier, J.; Klaus, M.; Wagener, G.

    2007-01-01

    In April 2005 the materials science beamline EDDI (Energy Dispersive DIffraction) at the Berlin synchrotron storage ring BESSY started operation. The beamline is operated in the energy-dispersive mode of diffraction using the high energy white photon beam provided by a superconducting 7 T multipole wiggler. Starting from basic information on the beamline set-up, its measuring facilities and data processing concept, the wide range of applications for energy-dispersive diffraction is demonstrated by a series of examples coming from different fields in materials sciences. It will be shown, that the EDDI beamline is especially suitable for the investigation of structural properties and gradients in the near surface region of polycrystalline materials. In particular, this concerns the analysis of multiaxial residual stress fields in the highly stressed surface zone of technical parts. The high photon flux further facilitates fast in situ experiments at room as well as high temperature to monitor for example the growth kinetics and reaction in thin film growth

  2. Glove powder's carrying capacity for latex protein: analysis using the ASTM ELISA test.

    Science.gov (United States)

    Beezhold, D; Horton, K; Hickey, V; Daddona, J; Kostyal, D

    2003-01-01

    Glove donning powders carry latex proteins and disperse them into the workplace environment. We have used the ASTM D6499 ELISA to quantify the amount of latex antigen bound to and carried by glove powders. We could differentiate between a small amount of protein actually bound to the powders and a larger amount carried by the powder. Enhanced binding of a major allergen, Hev b 5, to the starch powders was demonstrated by Western blot. The D6499 ELISA is able to measure total latex antigen, soluble and powder bound, simultaneously without the need to centrifuge the samples.

  3. An improved method for obtaining small pressed powder pellets for the analysis by XRF

    International Nuclear Information System (INIS)

    D'Angelo, J.; Marchevsky, E.; Strasser, E.; Perino, E.

    2002-01-01

    A rapid, very low cost of instrumentation and simple approach to specimen preparation for the analysis by X-ray fluorescence spectrometry is presented. This technique requires a few mg of powders samples, Which are compressed to produce pellets. This procedure is employed for determining major and trace elements in muscovites and K-feldspars. Factors affecting measured intensities, such as particle size and distribution, surface texture, pelletizing pressure, etc, are considered. A description of new sample preparation device, including technical characteristics, is also given. It is demonstrated that suitable specimen presentation to the X-ray beam is obtained by using our procedure. (author)

  4. Crystal optimization and preliminary diffraction data analysis of the SCAN domain of Zfp206

    International Nuclear Information System (INIS)

    Liang, Yu; Choo, Siew Hua; Rossbach, Michael; Baburajendran, Nithya; Palasingam, Paaventhan; Kolatkar, Prasanna R

    2012-01-01

    Crystals of the SCAN domain of Zfp206 are tetragonal, belonging to space group I422 with unit-cell parameters a = 67.57, c = 87.54 Å and one molecule in the asymmetric unit, and diffract to 1.85 Å resolution. Zfp206 (also named Zscan10) is a transcription factor that plays an important role in maintaining the pluripotent state of embryonic stem cells. Zfp206 is a member of the SCAN-domain family of C 2 H 2 zinc-finger transcription factors. The SCAN domain is a highly conserved motif of 84 residues which mediates the self-association of and heterodimerization between SCAN-domain family transcription factors. The SCAN domain may therefore be the key to the selective oligomerization of and may combinatorially enhance the regulatory versatility of C 2 H 2 zinc fingers. This paper describes crystallization attempts with the SCAN domain of Zfp206 (Zfp206SCAN) and optimization strategies to obtain diffraction-quality crystals. The best diffracting crystal was grown in a solution consisting of 0.3 M ammonium sulfate, 0.1 M Tris–HCl pH 8.6, 25% PEG 3350, 0.1 M ethylenediaminetetraacetic acid disodium salt dehydrate (EDTA) using the hanging-drop vapour-diffusion technique. Optimized crystals diffracted to 1.85 Å resolution and belonged to space group I422, with unit-cell parameters a = 67.57, c = 87.54 Å. A Matthews analysis indicated the presence of one Zfp206SCAN molecule per asymmetric unit

  5. Comparison of dissimilarity measures for cluster analysis of X-ray diffraction data from combinatorial libraries

    Science.gov (United States)

    Iwasaki, Yuma; Kusne, A. Gilad; Takeuchi, Ichiro

    2017-12-01

    Machine learning techniques have proven invaluable to manage the ever growing volume of materials research data produced as developments continue in high-throughput materials simulation, fabrication, and characterization. In particular, machine learning techniques have been demonstrated for their utility in rapidly and automatically identifying potential composition-phase maps from structural data characterization of composition spread libraries, enabling rapid materials fabrication-structure-property analysis and functional materials discovery. A key issue in development of an automated phase-diagram determination method is the choice of dissimilarity measure, or kernel function. The desired measure reduces the impact of confounding structural data issues on analysis performance. The issues include peak height changes and peak shifting due to lattice constant change as a function of composition. In this work, we investigate the choice of dissimilarity measure in X-ray diffraction-based structure analysis and the choice of measure's performance impact on automatic composition-phase map determination. Nine dissimilarity measures are investigated for their impact in analyzing X-ray diffraction patterns for a Fe-Co-Ni ternary alloy composition spread. The cosine, Pearson correlation coefficient, and Jensen-Shannon divergence measures are shown to provide the best performance in the presence of peak height change and peak shifting (due to lattice constant change) when the magnitude of peak shifting is unknown. With prior knowledge of the maximum peak shifting, dynamic time warping in a normalized constrained mode provides the best performance. This work also serves to demonstrate a strategy for rapid analysis of a large number of X-ray diffraction patterns in general beyond data from combinatorial libraries.

  6. Computation of X-ray powder diffractograms of cement components ...

    Indian Academy of Sciences (India)

    Computation of X-ray powder diffractograms of cement components and its application to phase analysis and hydration performance of OPC cement. Rohan Jadhav N C Debnath. Volume 34 Issue 5 August 2011 pp 1137- ... Keywords. Portland cement; X-ray diffraction; crystal structure; characterization; Rietveld method.

  7. Authentication of Whey Protein Powders by Portable Mid-Infrared Spectrometers Combined with Pattern Recognition Analysis.

    Science.gov (United States)

    Wang, Ting; Tan, Siow Ying; Mutilangi, William; Aykas, Didem P; Rodriguez-Saona, Luis E

    2015-10-01

    The objective of this study was to develop a simple and rapid method to differentiate whey protein types (WPC, WPI, and WPH) used for beverage manufacturing by combining the spectral signature collected from portable mid-infrared spectrometers and pattern recognition analysis. Whey protein powders from different suppliers are produced using a large number of processing and compositional variables, resulting in variation in composition, concentration, protein structure, and thus functionality. Whey protein powders including whey protein isolates, whey protein concentrates and whey protein hydrolysates were obtained from different suppliers and their spectra collected using portable mid-infrared spectrometers (single and triple reflection) by pressing the powder onto an Attenuated Total Reflectance (ATR) diamond crystal with a pressure clamp. Spectra were analyzed by soft independent modeling of class analogy (SIMCA) generating a classification model showing the ability to differentiate whey protein types by forming tight clusters with interclass distance values of >3, considered to be significantly different from each other. The major bands centered at 1640 and 1580 cm(-1) were responsible for separation and were associated with differences in amide I and amide II vibrations of proteins, respectively. Another important band in whey protein clustering was associated with carboxylate vibrations of acidic amino acids (∼1570 cm(-1)). The use of a portable mid-IR spectrometer combined with pattern recognition analysis showed potential for discriminating whey protein ingredients that can help to streamline the analytical procedure so that it is more applicable for field-based screening of ingredients. A rapid, simple and accurate method was developed to authenticate commercial whey protein products by using portable mid-infrared spectrometers combined with chemometrics, which could help ensure the functionality of whey protein ingredients in food applications. © 2015

  8. Data analysis of a polycrystalline nickel sample obtained with neutron diffraction

    International Nuclear Information System (INIS)

    Parente, C.B.R.; Mazzochi, V.L.; Araujo Kaschny, J.R. de; Costa, M.S. da; Rizzo, P.; Campos, W.M.S.

    1990-01-01

    A simple analysis of the nickel structure was made. Neutron diffraction data were used, obtained with polycrystalline nickel placed in a cylindrical sample-holder with dimensions of 1,5cm of diameter and 5cm of height. The theoretical intensities were calculated of 3 forms: 1. without considering the temperature and obsorption effects, 2. considering only the temperature effect and 3. considering both the temperature and absorption effects. The disagreement factors found in this 3 cases were, respectively, R 1 = 13.4%, R 2 = 7,7% e R 3 = 7,5%. (L.C.)

  9. Accurate measurement of the orientation relationship of lath martensite and bainite by electron backscatter diffraction analysis

    International Nuclear Information System (INIS)

    Miyamoto, G.; Takayama, N.; Furuhara, T.

    2009-01-01

    A new method to determine the orientation relationship between martensite and bainite with the parent austenite is developed based on electron backscatter diffraction analysis. This method can determine the orientation relationship accurately without the presence of retained austenite, and is applicable to lath martensite and bainite in low-alloyed carbon steels. The angles between close-packed directions are about 3 o for lath martensite regardless of the carbon content, while the angles between close-packed planes become smaller with increasing carbon content.

  10. Measurement and analysis of field-induced crystallographic texture using curved position-sensitive diffraction detectors

    DEFF Research Database (Denmark)

    Simons, Hugh; Daniels, John E.; Studer, Andrew J.

    2014-01-01

    This paper outlines measurement and analysis methodologies created for determining the structural responses of electroceramics to an electric field. A sample stage is developed to apply electric fields to ceramic materials at elevated temperatures during neutron diffraction experiments. The tested...... employing a curved positive sensitive detector. Methodologies are proposed to account for the geometrical effects when vector fields are applied to textured materials with angularly dispersive detector geometries. Representative results are presented for the ferroelectric (Bi1/2Na1/2)TiO3-6%BaTiO3 (BNT-6BT...

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

    International Nuclear Information System (INIS)

    Braun, G.E.

    1986-01-01

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

  12. Suitable pellets standards development for LA-ICPMS analysis of Al2O3 powders

    International Nuclear Information System (INIS)

    Ferraz, Israel Elias; Sousa, Talita Alves de; Silva, Ieda de Souza; Gomide, Ricardo Goncalves; Oliveira, Luis Claudio de

    2013-01-01

    Chemical and physical characterization of aluminium oxides has a special interest for the nuclear industry, despite arduous chemical digestion process. Therefore, laser ablation inductively coupled plasma mass spectrometry is an attractive method for analysis. However, due to the lack of suitable matrix-matched certified reference materials (MRC) for such powders and ceramic pellets analysis, LA-ICPMS has not yet been fully applied. Furthermore, establishing calibrate curves to trace element quantification using external standards raises a significant problem. In this context, the development of suitable standard pellets to have calibration curves for chemical determination of the impurities onto aluminium oxide powders by LA-ICPMS analytical technique was aimed in this work. It was developed using two different analytical strategies: (I) boric acid pressed pellets and (II) lithium tetra-borate melted pellets, both spiked with high purity oxides of Si, Mg, Ca, Na,Fe, Cr and Ni. The analytical strategy (II) which presented the best analytical parameters was selected, a reference certificated material was analyzed and the results compared. The limits of detection, linearity, precision, accuracy and recovery study results are presented and discussed. (author)

  13. Identification of low amount of irradiated spices (red pepper, garlic, ginger powder) with luminescence analysis

    International Nuclear Information System (INIS)

    Kim, Byeong-Keun; Akram, Kashif; Kim, Cheong-Tae; Kang, Na-Roo; Lee, Jin-Won; Ryang, Jun-Hwan; Kwon, Joong-Ho

    2012-01-01

    For the identification of irradiated food, current analysis methods have limitations regarding presence and stability of radiation-induced markers. In this study, different spice blends with small quantity of different irradiated (0, 1 and 10 kGy) spice powders, such as red pepper, garlic or ginger, were investigated using PSL and TL techniques. In PSL-based screening analysis, the spice blends containing 10% of irradiated materials (1 or 10 kGy) were determined as intermediate or positive. In TL results, the blends containing 1% of 1 or 10 kGy-irradiated spices showed the typical TL glow curves that could be interpreted as positive. The blends with irradiated garlic powder provided more good results where identification was possible at 0.5% mixing of irradiated sample. However, the TL ratios of all spice blends were <0.1 and only TL glow curve shape and intensity may be used to discriminate the samples having irradiated component. - Highlights: ► Sample blends with small quantities of irradiated spices were evaluated. ► The PSL was inappropriate to detect irradiated ingredient in small quantity. ► TL glow curve shape and intensity could be used as conclusive evidence of irradiation. ► TL ratios of all irradiated and nonirradiated samples were <0.1.

  14. Understanding deformation mechanisms during powder compaction using principal component analysis of compression data.

    Science.gov (United States)

    Roopwani, Rahul; Buckner, Ira S

    2011-10-14

    Principal component analysis (PCA) was applied to pharmaceutical powder compaction. A solid fraction parameter (SF(c/d)) and a mechanical work parameter (W(c/d)) representing irreversible compression behavior were determined as functions of applied load. Multivariate analysis of the compression data was carried out using PCA. The first principal component (PC1) showed loadings for the solid fraction and work values that agreed with changes in the relative significance of plastic deformation to consolidation at different pressures. The PC1 scores showed the same rank order as the relative plasticity ranking derived from the literature for common pharmaceutical materials. The utility of PC1 in understanding deformation was extended to binary mixtures using a subset of the original materials. Combinations of brittle and plastic materials were characterized using the PCA method. The relationships between PC1 scores and the weight fractions of the mixtures were typically linear showing ideal mixing in their deformation behaviors. The mixture consisting of two plastic materials was the only combination to show a consistent positive deviation from ideality. The application of PCA to solid fraction and mechanical work data appears to be an effective means of predicting deformation behavior during compaction of simple powder mixtures. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Optimal methodologies for terahertz time-domain spectroscopic analysis of traditional pigments in powder form

    Science.gov (United States)

    Ha, Taewoo; Lee, Howon; Sim, Kyung Ik; Kim, Jonghyeon; Jo, Young Chan; Kim, Jae Hoon; Baek, Na Yeon; Kang, Dai-ill; Lee, Han Hyoung

    2017-05-01

    We have established optimal methods for terahertz time-domain spectroscopic analysis of highly absorbing pigments in powder form based on our investigation of representative traditional Chinese pigments, such as azurite [blue-based color pigment], Chinese vermilion [red-based color pigment], and arsenic yellow [yellow-based color pigment]. To accurately extract the optical constants in the terahertz region of 0.1 - 3 THz, we carried out transmission measurements in such a way that intense absorption peaks did not completely suppress the transmission level. This required preparation of pellet samples with optimized thicknesses and material densities. In some cases, mixing the pigments with polyethylene powder was required to minimize absorption due to certain peak features. The resulting distortion-free terahertz spectra of the investigated set of pigment species exhibited well-defined unique spectral fingerprints. Our study will be useful to future efforts to establish non-destructive analysis methods of traditional pigments, to construct their spectral databases, and to apply these tools to restoration of cultural heritage materials.

  16. Mechanism of nanostructure formation in ball-milled Cu and Cu–3wt%Zn studied by X-ray diffraction line profile analysis

    International Nuclear Information System (INIS)

    Khoshkhoo, M. Samadi; Scudino, S.; Bednarcik, J.; Kauffmann, A.; Bahmanpour, H.; Freudenberger, J.; Scattergood, R.; Zehetbauer, M.J.; Koch, C.C.; Eckert, J.

    2014-01-01

    Highlights: • Nanostructured powders of Cu and Cu–3wt%Zn were produced using ball milling. • During cryomilling, nanostructure was formed by structural decomposition. • Dynamic recrystallization happened in room–temperature milling of Cu–3wt%Zn. • Structural decomposition took place during room–temperature milling of Cu. -- Abstract: The mechanism of nanostructure formation during cryogenic and room-temperature milling of Cu and Cu–3wt%Zn was investigated using X-ray diffraction line profile analysis. For that, the whole powder pattern modeling approach (WPPM) was used to analyze the evolution of microstructural features including coherently scattering domain size, dislocation density, and density of planar faults. It was found that for all sets of experiments, structural decomposition is the dominant mechanism of nanostructure formation during cryomilling. During subsequent RT-milling, grain refinement still occurs by structural decomposition for pure copper. On the other hand, discontinuous dynamic recrystallization is responsible for nanostructure formation during RT-milling of Cu–3wt%Zn. This is attributed to lower stacking-fault energy of Cu–3wt%Zn compared to pure copper. Finally, room temperature milling reveals the occurrence of a detwinning phenomenon

  17. [Analysis and characterization of Belamcanda chinensis with space mutagenesis breeding by X-ray fluorescence analysis and X-ray diffraction].

    Science.gov (United States)

    Guan, Ying; Ding, Xi-Feng; Wang, Wen-Jing; Guo, Xi-Hua; Zhu, Yan-Ying

    2008-02-01

    The contents of various elements in the fourth generation Belamcanda chinensis (L.) DC. with space mutagenesis breeding were analyzed and characterized. X-ray fluorescence spectrum analysis (XRF) and powder X-ray diffraction (PXRD) were applied jointly. It was found that the content of K element in the space flight mutagenesis increases 1.03 and 0.31 times, Mg enhances 1.44 and 0.06 times, but Al reduces 38.5% and 85.5% respectively compared to the contents in the ground group and the comparison group, while those of Ca, Mn and Fe enhance 0.95, 0.30 and 0.29 times respectively contrasted to the ground group. Besides, there was discovered the crystal of whewellite in the Belamcanda chinensis (L.) DC. and the content in the ground group is less than that of the outer space and the outer space group, which in turn is less than that of the comparison group. It is concluded that the contents of mineral elements indispensable to body in the space group are closer or superior to the comparison, group as compared to the ground group. In the present paper, a quick and simple appraising method is offered, which may be of great significance to the popularization of the planting outer space Chinese traditional medicine to filtrate more excellent breed and set up norm of quality appraisal.

  18. Analysis of rocks involving the x-ray diffraction, infrared and thermal gravimetric techniques

    International Nuclear Information System (INIS)

    Ikram, M.; Rauf, M.A.; Munir, N.

    1998-01-01

    Chemical analysis of rocks and minerals are usually obtained by a number of analytical techniques. The purpose of present work is to investigate the chemical composition of the rock samples and also to find that how far the results obtained by different instrumental methods are closely related. Chemical tests wee performed before using the instrumental techniques in order to determined the nature of these rocks. The chemical analysis indicated mainly the presence of carbonate and hence the carbonate nature of these rocks. The x-ray diffraction, infrared spectroscopy and thermal gravimetric analysis techniques were used for the determination of chemical composition of these samples. The results obtained by using these techniques have shown a great deal of similarities. (author)

  19. Characterization of the Roraima savanna across of X-ray diffraction, thermomagnetic analysis and Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Gilmar A.; Araujo, R.C.; Sergio, C.S. [Universidade Federal de Roraima (UFRR), Boa Vista, RR (Brazil)

    2012-07-01

    Full text: The technique of X-ray diffraction has great resolving power to determine the phases present in crystalline material, thereby enabling it to determine the elements present in the materials as well as changes in structure that they can suffer when subjected to various physical processes and/or chemical means. The research had as objective to characterize the mineralogy of iron oxides, silicon, aluminum and other minerals in the soil of five points of the Roraima savannah. The points where samples were collected are five municipalities in the state of Roraima. The area of sampling is part of the savanna in Roraima. The samples were collected. We analyzed samples from five points from the collection of natural soil in the locations listed. The samples were placed in a mill to a uniform grain size. After the milling process, the magnetic material was separated using a permanent magnet. Then the samples were analyzed by x-ray diffraction, thermomagnetic analysis and Moessbauer spectroscopy. Preliminary results of XRD showed the occurrence of phases of oxides of iron, silicon, aluminum and other phases less. Thermomagnetic analysis show that the magnetic phases are magnetite and hematite. The results of the Moessbauer spectroscopy indicates the reliability in the two prior art and confirmed the presence of the phases of oxides of iron present in the soil analyzed. (author)

  20. X-ray diffraction analysis of synthesized silver nanohexagon for the study of their mechanical properties

    Energy Technology Data Exchange (ETDEWEB)

    Das, Ratan, E-mail: dasratanphy@gmail.com; Sarkar, Sumit, E-mail: sarkarsumit07phy@gmail.com

    2015-11-01

    Silver nanohexagons have been prepared through the chemical reduction method using poly(vinyl pyrrolidone) (PVP) as a capping agent. High Resolution Transmission Electron Microscopic (HRTEM) study shows that average size of the prepared silver nanoparticles is 45 nm approximately with nearly hexagon shape. The peaks in the X-Ray Diffraction (XRD) pattern are in good agreement with that of face centered cubic structure. Williamson–Hall plots (W–H plot) have been analyzed to study the crystalline size and lattice strain considering the peak broadening of the AgNHs. The mechanical properties such as strain, stress and energy density of prepared nanohexagon have been calculated assuming uniform deformation model (UDM), uniform stress deformation model (USDM), and uniform deformation energy density model (UDEDM) and size–strain plot method (SSP). From all these results, it is found that the size and strain estimated from W–H analysis and SSP method are in good agreement. - Highlights: • PVP capped silver nanohexagons have been synthesized by chemical reduction method. • HRTEM images show that the average size of the prepared nanohexagons is 45 nm. • X-ray diffraction study confirms the crystallinity of silver nanohexagons. • Elastic properties have been calculated by W–H analysis using different models. • Further, the results from UDM, USDM, and UDEDM matches with SSP method.