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.)

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

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

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

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)

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...

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

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...

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

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

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.)

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

Directory of Open Access Journals (Sweden)

Yifeng Yun

2015-03-01

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

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

Science.gov (United States)

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

2015-03-01

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

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

Science.gov (United States)

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

2018-01-01

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

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

Directory of Open Access Journals (Sweden)

Hongjia Zhang

2018-03-01

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

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

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)

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

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.

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

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)

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)

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.

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...

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

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.)

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...

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.

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)

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...

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

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.

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.

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

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...

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.

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

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.)

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)

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....

IL 12: Femtosecond x-ray powder diffraction

International Nuclear Information System (INIS)

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

2010-01-01

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

X-ray powder 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.)

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)

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)

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

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

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

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...

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.

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.)

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.)

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.

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.

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.

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

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].

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

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

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.

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

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

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.)

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.

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)

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...

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)

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.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-07-01

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

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.

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 ...

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.

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.

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)

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

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.

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....

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.

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

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

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

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)

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

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

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

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.

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.

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.

Pulsed Neutron Powder Diffraction for Materials Science

Science.gov (United States)

Kamiyama, T.

2008-03-01

The accelerator-based neutron diffraction began in the end of 60's at Tohoku University which was succeeded by the four spallation neutron facilities with proton accelerators at the High Energy Accelerator Research Organization (Japan), Argonne National Laboratory and Los Alamos Laboratory (USA), and Rutherford Appleton Laboratory (UK). Since then, the next generation source has been pursued for 20 years, and 1MW-class spallation neutron sources will be appeared in about three years at the three parts of the world: Japan, UK and USA. The joint proton accelerator project (J-PARC), a collaborative project between KEK and JAEA, is one of them. The aim of the talk is to describe about J-PARC and the neutron diffractometers being installed at the materials and life science facility of J-PARC. The materials and life science facility of J-PARC has 23 neutron beam ports and will start delivering the first neutron beam of 25 Hz from 2008 May. Until now, more than 20 proposals have been reviewed by the review committee, and accepted proposal groups have started to get fund. Those proposals include five polycrystalline diffractometers: a super high resolution powder diffractometer (SHRPD), a 0.2%-resolution powder diffractometer of Ibaraki prefecture (IPD), an engineering diffractometers (Takumi), a high intensity S(Q) diffractometer (VSD), and a high-pressure dedicated diffractometer. SHRPD, Takumi and IPD are being designed and constructed by the joint team of KEK, JAEA and Ibaraki University, whose member are originally from the KEK powder group. These three instruments are expected to start in 2008. VSD is a super high intensity diffractometer with the highest resolution of Δd/d = 0.3%. VSD can measure rapid time-dependent phenomena of crystalline materials as well as glass, liquid and amorphous materials. The pair distribution function will be routinely obtained by the Fourier transiformation of S(Q) data. Q range of VSD will be as wide as 0.01 Å-1stress mapping inside

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.

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

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)

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

Final Report for X-ray Diffraction Sample Preparation Method Development

Energy Technology Data Exchange (ETDEWEB)

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

2018-01-30

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

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.)

In-house characterization of protein powder

DEFF Research Database (Denmark)

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

2010-01-01

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

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.

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 ...

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.

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

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

Crystallized solids characterization by X-ray diffraction

International Nuclear Information System (INIS)

Broll, N.

1996-01-01

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

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

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)

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

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

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.

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

Tailoring diffraction technique Rietveld method on residual stress measurements of cold-can oiled 304 stainless steel plates

International Nuclear Information System (INIS)

Parikin; Killen, P.; Anis, M.

2003-01-01

Tailoring of diffraction technique-Rietveld method on residual stress measurements of cold-canailed stainless steel 304 plates assuming the material is isotopic, the residual stress measurements using X-ray powder diffraction is just performed for a plane lying in a large angle. For anisotropic materials, the real measurements will not be represented by the methods. By Utilizing of all diffraction peaks in the observation region, tailoring diffraction technique-Rietveld analysis is able to cover the limitations. The residual stress measurement using X-ray powder diffraction tailored by Rietveld method, in a series of cold-canailed stainless steel 304 plates deforming; 0, 34, 84, 152, 158, 175, and 196 % reduction in thickness, have been reported. The diffraction data were analyzed by using Rietveld structure refinement method. Also, for all cold-canailed stainless steel 304 plates cuplikans, the diffraction peaks are broader than the uncanailed one, indicating that the strains in these cuplikans are inhomogeneous. From an analysis of the refined peak shape parameters, the average root-mean square strain, which describes the distribution of the inhomogeneous strain field, was calculated. Finally, the average residual stresses in cold-canailed stainless steel 304 plates were shown to be a combination effect of hydrostatic stresses of martensite particles and austenite matrix. The average residual stresses were evaluated from the experimentally determined average lattice strains in each phase. It was found the tensile residual stress in a cuplikan was maximum, reaching 442 MPa, for a cuplikan reducing 34% in thickness and minimum for a 196% cuplikan

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...

NiTiO3 powders obtained by polymeric precursor method: Synthesis and characterization

International Nuclear Information System (INIS)

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

2009-01-01

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

Ti₃SiC₂ Synthesis by Powder Metallurgical Methods

OpenAIRE

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

2007-01-01

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

Method to blend separator powders

Science.gov (United States)

Guidotti, Ronald A.; Andazola, Arthur H.; Reinhardt, Frederick W.

2007-12-04

A method for making a blended powder mixture, whereby two or more powders are mixed in a container with a liquid selected from nitrogen or short-chain alcohols, where at least one of the powders has an angle of repose greater than approximately 50 degrees. The method is useful in preparing blended powders of Li halides and MgO for use in the preparation of thermal battery separators.

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

International Nuclear Information System (INIS)

Kassem, M.

2009-07-01

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

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 ...

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...

X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

Energy Technology Data Exchange (ETDEWEB)

Brown, Allan

1970-12-15

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

X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

International Nuclear Information System (INIS)

Brown, Allan

1970-12-01

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

Acemetacin cocrystal structures by powder X-ray diffraction

Science.gov (United States)

Bolla, Geetha

2017-01-01

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

Acemetacin cocrystal structures by powder X-ray diffraction

Directory of Open Access Journals (Sweden)

Geetha Bolla

2017-05-01

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

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

High Pressure X-Ray Diffraction Studies on Nanocrystalline Materials

Science.gov (United States)

Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Pielaszek, R.; Bismayer, U.; Werner, S.; Palosz, W.

2003-01-01

Application of in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2 to 30 nrn diameter in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (nanoparticles of different grain size.

Synthesis of alumina powders by precipitation method and solvothermal treatment

International Nuclear Information System (INIS)

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

2012-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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.

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.

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

International Nuclear Information System (INIS)

Rybak, Jens-Christoph

2012-01-01

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

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...

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…

Solving crystal structures from powder data. I. The role of the prior information in the two-stage method

International Nuclear Information System (INIS)

Altomare, A.; Carrozzini, B.; Giacovazzo, C.; Guagliardi, A.; Moliterni, A.G.G.; Rizzi, R.

1996-01-01

For pt.II see ibid., p.674-81, 1996. The principal limitation of the diffraction methods for crystal structure analysis from powder data is originated by the collapse of the three-dimensional reciprocal space into the one dimension of the powder diffraction pattern. The degradation of the information can make difficult even the solution of small crystal structures and can generate inefficiencies in the least-squares methods devoted to crystal structure refinement. In this paper, the current two-stage procedures, the first stage dedicated to powder-pattern decomposition and the second to direct phasing of powder data, are analysed. It is shown that in the first stage such procedures disregard a large amount of information that can become available during the process of crystal structure solution and analysis. The use of such information is essential for making direct-methods procedures more robust and for improving the accuracy of the least-squares techniques. The performances of EXTRA [Altomare, Burla, Cascarano, Giacovazzo, Guagliardi, Moliterni and Polidori (1995). J. Appl. Cryst. 28, 842-846], a program for full-pattern decomposition based on the Le Bail algorithm, and of SIRPOW.92 [Altomare, Burla, Cascarano, Giacovazzo, Guagliardi, Polidori and Camalli (1994). J. Appl. Cryst. 27, 435-436], a direct-methods program optimized for powder data, are discussed in order to offer to the reader a logical pathway for the analysis of the traditional techniques and for the proposition of a new approach. It is shown that pattern-decomposition programs based on the Le Bail algorithm are able to exploit the prior information in a more effective way than Pawley-method-based decomposition programs. (orig.)

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

International Nuclear Information System (INIS)

Kang, S.; Nam, T.

2001-01-01

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

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

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...

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)

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

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...

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)

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

International Nuclear Information System (INIS)

Ghasemi, Leila; Jafari, Hassan

2017-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-11-15

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

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.

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.

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

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

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.

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

Science.gov (United States)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

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

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

OpenAIRE

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

2009-01-01

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

Food powders flowability characterization: theory, methods, and applications.

Science.gov (United States)

Juliano, Pablo; Barbosa-Cánovas, Gustavo V

2010-01-01

Characterization of food powders flowability is required for predicting powder flow from hoppers in small-scale systems such as vending machines or at the industrial scale from storage silos or bins dispensing into powder mixing systems or packaging machines. This review covers conventional and new methods used to measure flowability in food powders. The method developed by Jenike (1964) for determining hopper outlet diameter and hopper angle has become a standard for the design of bins and is regarded as a standard method to characterize flowability. Moreover, there are a number of shear cells that can be used to determine failure properties defined by Jenike's theory. Other classic methods (compression, angle of repose) and nonconventional methods (Hall flowmeter, Johanson Indicizer, Hosokawa powder tester, tensile strength tester, powder rheometer), used mainly for the characterization of food powder cohesiveness, are described. The effect of some factors preventing flow, such as water content, temperature, time consolidation, particle composition and size distribution, is summarized for the characterization of specific food powders with conventional and other methods. Whereas time-consuming standard methods established for hopper design provide flow properties, there is yet little comparative evidence demonstrating that other rapid methods may provide similar flow prediction.

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)

Stress measurement by neutron diffraction method. Standard method using angular dispersion method and trial of using neutron IP

International Nuclear Information System (INIS)

Sasaki, Toshihiko; Takago, Shigeki

2016-01-01

This paper outlined a stress measurement method using neutrons, and introduced the application examples to stress measurement for metal-based composite materials. In the angular dispersion type measurement using a steady-state reactor type neutron source, the white beams taken out from a nuclear reactor are monochromatized (wavelength λ is a constant value) with a single crystal monochromator and utilized. As an example of measurement, there was the case as follows: the stress of a sintered material which has been put to practical use as valve seat part for automobiles was measured by the neutron method, and the deformation behavior during load was studied. This study performed neutron diffraction measurement using a residual stress analyzer (RESA: Diffractometer for Residual Stress Analysis) installed at JAEA's experimental reactor JRR-3. As a result, it was found that the stress state of the sintered composite material of Fe-Cr and TiN can be predicted with a micromechanics model. A neutron diffraction ring can be obtained using a neutron image plate (IP), where fine powder of gadolinium (Gd) was incorporated into IP for X-rays, and it can be used as an IP reader in the same way as the case of X-rays. A report has been introduced on the examination results of the highly accurate stress measurement by applying the cos α method devised for X-ray stress measurement to neutron diffraction ring. (A.O.)

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-06-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

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.

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.

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

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...

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

Directory of Open Access Journals (Sweden)

Coralia Osorio

2011-01-01

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

Quantitative determination of phases by X-ray diffraction

International Nuclear Information System (INIS)

Azevedo, A.L.T.

1979-01-01

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

Study of crystallite size of yttria-stabilized zirconia powders by Rietveld method

International Nuclear Information System (INIS)

Leite, Wellington Claiton; Brinatti, Andre Mauricio; Ribeiro, Mauricio Aparecido; Andrade, Andre Vitor Chaves de; Chinelatto, Adriana Scoton Antonio; Chinelatto, Adilson Luiz

2009-01-01

The yttria-stabilized zirconia (YSZ) is used in a great variety of applications, for example, electrolytes of solid oxide fuel cells and oxygen sensors. In the study of YSZ, the particle size powders and sintering processes are important to define the final properties of the zirconia products. The objectives of this work were to determine the phases and the crystalline size using X-Ray Diffraction (XRD) data and the Rietveld Method (RM) of the YSZ powders obtained by chemical synthesis based on the Pechini method. It was used ZrOCl 2.8 H 2 O and Y(NO 3 ) 3.5 H 2 O as precursors reagents. After calcination at 550 deg C during 24 hours, the powder was analyzed by XRD and scanning electronic microscopy (SEM). From XRD and using Rietveld method were verified that there is only cubic phase with lattice parameter a = 5.1307(1) Å and the space group Fm3m. Due to substitution of the Zr atoms in the Y atoms sites, there were vacancies in 17.72 % of O atoms sites. However, the percentage of substitution of Zr atoms in Y atoms sites in the structure not was determinate because the curves of atomic scattering of them are very similar. Using Scherrer equation and considering anisotropy effect, the average crystalline size was determinate: 10,43 nm (c axis) and 10,39 (b axis). This spherical symmetry also observed for SEM. (author)

Characterization of Metal Powders Used for Additive Manufacturing.

Science.gov (United States)

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

2014-01-01

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

Characterization of Metal Powders Used for Additive Manufacturing

Science.gov (United States)

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

2014-01-01

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

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

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.)

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

Directory of Open Access Journals (Sweden)

Katharina Fucke

2010-07-01

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

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

Science.gov (United States)

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

2004-01-01

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

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.)

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...

Structural and morphological characterization of TiO2-ZrO2 powders obtained by the polymeric precursors method

International Nuclear Information System (INIS)

Ribeiro, M.A.; Gama, L.; Bispo, A.; Neiva, L.S.; Bernardi, M.I.B.; Kiminami, R.H.G.A.

2010-01-01

This work aims to characterize the structure and morphology of TiO 2 -ZrO 2 powders obtained by polymeric precursor method. For this we studied the following compositions: 0.25, 0.5 and 0.75 moles of Zr and calcined at 800 deg C for one hour. The powders obtained were characterized by XRD, SEM and nitrogen adsorption (BET). The analysis of X-ray diffraction showed that the powders had a phase of TiO 2 in the anatase form and a tetragonal phase of ZrO 2 . The crystallite size was between 8, 13 and 11 nm respectively. The analysis of scanning electron microscopy showed the growth of ZrO 2 nanoparticles and that these comprise spherical agglomerates of less than 100 nm. Particle size determined by the BET ranging 28.1-29.5 nm, showing thereby the character of nanosized powders. (author)

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)

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

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

International Nuclear Information System (INIS)

Eidson, A.F.

1982-01-01

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

Effects of milling method and calcination condition on phase and morphology characteristics of Mg4Nb2O9 powders

International Nuclear Information System (INIS)

Wongmaneerung, R.; Sarakonsri, T.; Yimnirun, R.; Ananta, S.

2006-01-01

Magnesium niobate, Mg 4 Nb 2 O 9 , powders has been synthesized by a solid-state reaction. Both conventional ball- and rapid vibro-milling have been investigated as milling methods, with the formation of the Mg 4 Nb 2 O 9 phase investigated as a function of calcination conditions by DTA and XRD. The particle size distribution of the calcined powders was determined by laser diffraction technique, while morphology, crystal structure and phase composition were determined via a combination of SEM, TEM and EDX techniques. The type of milling method together with the designed calcination condition was found to show a considerable effect on the phase and morphology evolution of the calcined Mg 4 Nb 2 O 9 powders. It is seen that optimization of calcination conditions can lead to a single-phase Mg 4 Nb 2 O 9 in both milling methods. However, the formation temperature and dwell time for single-phase Mg 4 Nb 2 O 9 powders were lower with the rapid vibro-milling technique

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

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)

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.

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

Revisit to diffraction anomalous fine structure

International Nuclear Information System (INIS)

Kawaguchi, T.; Fukuda, K.; Tokuda, K.; Shimada, K.; Ichitsubo, T.; Oishi, M.; Mizuki, J.; Matsubara, E.

2014-01-01

The diffraction anomalous fine structure method has been revisited by applying this measurement technique to polycrystalline samples and using an analytical method with the logarithmic dispersion relation. The diffraction anomalous fine structure (DAFS) method that is a spectroscopic analysis combined with resonant X-ray diffraction enables the determination of the valence state and local structure of a selected element at a specific crystalline site and/or phase. This method has been improved by using a polycrystalline sample, channel-cut monochromator optics with an undulator synchrotron radiation source, an area detector and direct determination of resonant terms with a logarithmic dispersion relation. This study makes the DAFS method more convenient and saves a large amount of measurement time in comparison with the conventional DAFS method with a single crystal. The improved DAFS method has been applied to some model samples, Ni foil and Fe 3 O 4 powder, to demonstrate the validity of the measurement and the analysis of the present DAFS method

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.

Molten salt synthesis of ZnNb2O6 powder

International Nuclear Information System (INIS)

Guo Liangzhai; Dai Jinhui; Tian Jintao; Zhu Zhibin; He Tian

2007-01-01

Pure ZnNb 2 O 6 powder was successfully prepared by the molten salt synthesis method using Nb 2 O 5 and ZnO as raw materials and a mixture of NaCl and KCl as the solvent. The phase form and morphology of the prepared powder were characterized by X-ray diffraction and scanning electron microscopy. The effect of reacting temperature on phase formation was investigated. The results indicated that the single phase ZnNb 2 O 6 powder can be obtained by the molten salt synthesis method at 600 deg. C, and the SEM photographs show that the grains of the powder are rod-like particles

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.

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.)

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.

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

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.

Process Parameters on the Crystallization and Morphology of Hydroxyapatite Powders Prepared by a Hydrolysis Method

Science.gov (United States)

Wang, Moo-Chin; Hon, Min-Hsiung; Chen, Hui-Ting; Yen, Feng-Lin; Hung, I.-Ming; Ko, Horng-Huey; Shih, Wei-Jen

2013-07-01

The effects of process parameters on the crystallization and morphology of hydroxyapatite (Ca10(PO4)6(OH)2, HA) powders synthesized from dicalcium phosphate dihydrate (CaHPO4·2H2O, DCPD) using a hydrolysis method have been investigated. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were used to characterize the synthesized powders. When DCPD underwent hydrolysis in 2.5 NaOH solution (Na(aq)) at 303 K to 348 K (30 °C to 75 °C) for 1 hour, the XRD results revealed that HA was obtained for all the as-dried samples. The SEM morphology of the HA powders for DCPD hydrolysis produced at 348 K (75 °C) shows regular alignment and a short rod shape with a size of 200 nm in length and 50 nm in width. With DCPD hydrolysis in 2.5 M NaOH(aq) holding at 348 K (75 °C) for 1 to 24 hours, XRD results demonstrated that all samples were HA and no other phases could be detected. Moreover, the XRD results also show that all the as-dried powders still maintained the HA structure when DCPD underwent hydrolysis in 0.1 to 5 M NaOH(aq) at 348 K (75 °C) for 1 hour. Otherwise, the full transformation from HA to octa-calcium phosphate (OCP, Ca8H2(PO4)6·5H2O) occurred when hydrolysis happened in 10 M NaOH(aq). FT-IR spectra analysis revealed that some carbonated HA (Ca10(PO4)6(CO3), CHA) had formed. The SEM morphology results show that the 60 to 65 nm width of the uniformly long rods with regular alignment formed in the HA powder aggregates when DCPD underwent hydrolysis in 2.5 M NaOH(aq) at 348 K (75 °C) for 1 hour.

Methods for production of aluminium powders and their application fields

Energy Technology Data Exchange (ETDEWEB)

Gopienko, V.G.; Kiselev, V.P.; Zobnina, N.S. (Vsesoyuznyj Nauchno-Issledovatel' skij i Proektnyj Inst. Alyuminievoj, magnievoj i ehlektrodnoj promyshlennosti (USSR))

1984-12-01

Different types of powder products made of alluminium and its alloys (powder, fine powders, granules and pastes) as well as their basic physicochemical properties are briefly characterized. The principle methods for alluminium powder production are outlined: physicochemical methods, the melt spraying by compressed gas being the mostly developed among them, and physico-mechanical ones. Main application spheres for powder productions of aluminium and its alloys are reported in short.

Methods for production of aluminium powders and their application fields

International Nuclear Information System (INIS)

Gopienko, V.G.; Kiselev, V.P.; Zobnina, N.S.

1984-01-01

Different types of powder products made of alluminium and its alloys (powder, fine powders, granules and pastes) as well as their basic physicochemical properties are briefly characterized. The principle methods for alluminium powder production are outlined: physicochemical methods, the melt spraying by compressed gas being the mostly developed among them, and physico-mechanical ones. Main application spheres for powder productions of aluminium and its alloys are reported in short

Synthesis of magnetite octahedrons from iron powders through a mild hydrothermal method

International Nuclear Information System (INIS)

Mao Baodong; Kang Zhenhui; Wang Enbo; Lian Suoyuan; Gao Lei; Tian Chungui; Wang Chunlei

2006-01-01

Magnetite (Fe 3 O 4 ) octahedral particles were fabricated from iron powders through a simple one-step alkali-assisted hydrothermal process. The crystallinity, morphology, and structural features of the as-prepared magnetite particles were investigated using powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The values of saturation magnetization (M s ) and coercivity (H) of the magnetite octahedrons characterized on a vibrating sample magnetometer (VSM) are 89.81 emu/g and 70.6 Oe, respectively. The concentration of NaOH and the reaction temperature played a key role in the formation of the magnetite octahedrons

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)

Low-Pressure and Low-Temperature Hydriding-Pulverization-Dehydriding Method for Producing Shape Memory Alloy Powders

Science.gov (United States)

Murguia, Silvia Briseño; Clauser, Arielle; Dunn, Heather; Fisher, Wendy; Snir, Yoav; Brennan, Raymond E.; Young, Marcus L.

2018-04-01

Shape memory alloys (SMAs) are of high interest as active, adaptive "smart" materials for applications such as sensors and actuators due to their unique properties, including the shape memory effect and pseudoelasticity. Binary NiTi SMAs have shown the most desirable properties, and consequently have generated the most commercial success. A major challenge for SMAs, in particular, is their well-known compositional sensitivity. Therefore, it is critical to control the powder composition and morphology. In this study, a low-pressure, low-temperature hydriding-pulverization-dehydriding method for preparing well-controlled compositions, size, and size distributions of SMA powders from wires is presented. Starting with three different diameters of as-drawn martensitic NiTi SMA wires, pre-alloyed NiTi powders of various well-controlled sizes are produced by hydrogen charging the wires in a heated H3PO4 solution. After hydrogen charging for different charging times, the wires are pulverized and subsequently dehydrided. The wires and the resulting powders are characterized using scanning electron microscopy, differential scanning calorimetry, and X-ray diffraction. The relationship between the wire diameter and powder size is investigated as a function of hydrogen charging time. The rate of diameter reduction after hydrogen charging of wire is also examined. Finally, the recovery behavior due to the shape memory effect is investigated after dehydriding.

D2B, a new high resolution neutron powder diffractometer at ILL Grenoble

International Nuclear Information System (INIS)

Hewat, A.W.

1987-01-01

Applications of high resolution neutron powder diffraction to materials science have grown rapidly in the past 10 years, with the development of Rietveld methods of profile refinement, and new high resolution diffractometers and multidetectors. Materials studied range from catalysts to zeolites, and from battery electrodes to prestressed superconducting wires. Although the techniques have now been adapted for X-ray and synchrotron radiation, neutron powder diffraction retains unique advantages. In this paper we describe the design and first test measurements on the latest high resolution powder diffractometer D2B at ILL Grenoble. A review of the applications is published in Chemica Scripta (1986). (author) 9 refs., 6 figs., 2 tabs

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...

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)

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-03-01

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

Black powder in gas pipelines

Energy Technology Data Exchange (ETDEWEB)

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

2009-07-01

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

Method of solidifying powderous wastes

International Nuclear Information System (INIS)

Kakimoto, Akira; Miyake, Takashi; Sato, Shuichi; Inagaki, Yuzo.

1985-01-01

Purpose: To improve the properties of solidification products, in the case of solidifying powderous wastes with thermosetting resins. Method. A solvent for the solution of the thermosetting resin is admixed with the powderous wastes into a paste-like form prior to adding the resin to the wastes, which are then mixed with the resin solution. As the result, those solidification products having the specific gravity and the compression strength more excellent than those of the conventional ones, and much higher than the reference values can be obtained. (Kamimura, M.)

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

Directory of Open Access Journals (Sweden)

Marta Bettoni

2009-01-01

Full Text Available Some TiO2 powders, prepared from titanium(IVtetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl alcohol in CH3CN as the test reaction. The decrease of ka have been related to the decrease of the BET surface area, the micropore volume, and the external surface area of the TiO2 powders, but a satisfactory linear correlation is observed only for the last superficial parameter.

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.

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

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.

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

Neutron diffraction studies of high-T/sub c/ superconductors

International Nuclear Information System (INIS)

Jorgensen, J.D.

1988-03-01

Neutron powder diffraction techniques have been used extensively for the study of high-T/sub c/ oxide superconductors because of the need to locate oxygen atoms and accurately determine the oxygen site occupancies, and the difficulty in obtaining single crystals. For example, in the case of YBa 2 Cu 3 O/sub 7-δ/, neutron powder diffraction and Rietveld structural refinement were used to obtain the first complete structural information. Subsequent experiments focussed on determining the relationship of superconducting properties to the number and distribution of oxygen vacancies on the Cu-O sublattice with measurements being done on samples in thermodynamic equilibrium, at high temperature in controlled oxygen atmospheres, and on metastable, oxygen-deficient samples produced by quenching. Neutron powder diffraction has also been used to determine the structures of compounds in which the properties have been modified by substitution on the Y, Ba, or Cu sites. This paper briefly reviews some of the neutron powder diffraction results in these areas. 17 refs

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.

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

International Nuclear Information System (INIS)

Louer, Daniel

1969-01-01

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

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)

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.

Thermal plasma spheroidization and spray deposition of barium titanate powder and characterization of the plasma sprayable powder

Energy Technology Data Exchange (ETDEWEB)

Pakseresht, A.H., E-mail: amirh_pak@yahoo.com [Department of Ceramics, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Rahimipour, M.R. [Department of Ceramics, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Vaezi, M.R. [Department of Nanotechnology and Advanced Materials, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Salehi, M. [Department of Materials Engineering, Isfahan University of Technology, P.O. Box 84156-83111, Isfahan (Iran, Islamic Republic of)

2016-04-15

In this paper, atmospheric plasma spray method was used to produce dense plasma sprayable powder and thick barium titanate film. In this regard, the commercially feedstock powders were granulated and spheroidized by the organic binder and the thermal spray process, respectively. Scanning electron microscopy was used to investigate the microstructure of the produced powders and the final deposits. X-ray diffraction was also implemented to characterize phase of the sprayed powder. The results indicated that spheroidized powder had suitable flowability as well as high density. The micro-hardness of the film produced by the sprayed powders was higher than that of the film deposited by the irregular granules. Additionally, relative permittivity of the films was increased by decreasing the defects from 160 to 293 for film deposited using spheroidized powder. The reduction in the relative permittivity of deposits, in comparison with the bulk material, was due to the existence of common defects in the thermal spray process. - Highlights: • We prepare sprayable BaTiO{sub 3} powder with no or less inside voids for plasma spray application for first time. • The sprayable powder has good flow characteristics and high density. • Powder spheroidization via plasma spray improves the hardness and dielectric properties of the deposited film.

Thermal plasma spheroidization and spray deposition of barium titanate powder and characterization of the plasma sprayable powder

International Nuclear Information System (INIS)

Pakseresht, A.H.; Rahimipour, M.R.; Vaezi, M.R.; Salehi, M.

2016-01-01

In this paper, atmospheric plasma spray method was used to produce dense plasma sprayable powder and thick barium titanate film. In this regard, the commercially feedstock powders were granulated and spheroidized by the organic binder and the thermal spray process, respectively. Scanning electron microscopy was used to investigate the microstructure of the produced powders and the final deposits. X-ray diffraction was also implemented to characterize phase of the sprayed powder. The results indicated that spheroidized powder had suitable flowability as well as high density. The micro-hardness of the film produced by the sprayed powders was higher than that of the film deposited by the irregular granules. Additionally, relative permittivity of the films was increased by decreasing the defects from 160 to 293 for film deposited using spheroidized powder. The reduction in the relative permittivity of deposits, in comparison with the bulk material, was due to the existence of common defects in the thermal spray process. - Highlights: • We prepare sprayable BaTiO_3 powder with no or less inside voids for plasma spray application for first time. • The sprayable powder has good flow characteristics and high density. • Powder spheroidization via plasma spray improves the hardness and dielectric properties of the deposited film.

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....

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

Science.gov (United States)

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

2017-11-01

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

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.

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

Influence of Ultrafine 2CaO·SiO₂ Powder on Hydration Properties of Reactive Powder Concrete.

Science.gov (United States)

Sun, Hongfang; Li, Zishanshan; Memon, Shazim Ali; Zhang, Qiwu; Wang, Yaocheng; Liu, Bing; Xu, Weiting; Xing, Feng

2015-09-17

In this research, we assessed the influence of an ultrafine 2CaO·SiO₂ powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM), mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength) with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO₂. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO₂ powder has the potential to improve the performance of a reactive powder cementitious system.

Powder preparation technics for SnO2 with submycrometrics particles

International Nuclear Information System (INIS)

Hiratsuka, R.S.; Pulcinelli, S.H.; Santilli, C.V.; Masetto, S.R.

1989-01-01

Preparation of SnO 2 fine powders is a pointer research because of this application as gas detecting sensors. This work shows basicaly two powder preparation methods: i) from metalic tin oxidation with nitric acid, ii) from SnCl 4 hydrolysis in aquous solution of amonia hydroxides. It was analysed the concentration of nitric acid and the pH of precipitation influency of the structural and morphologic characteristics of the obtained powders. The materials were characterized by X-ray diffraction, infra-red spectroscopy and specific surface area [pt

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

Characteristics of nano Ti-doped SnO2 powders prepared by sol-gel method

International Nuclear Information System (INIS)

Liu, X.M.; Wu, S.L.; Chu, Paul K.; Zheng, J.; Li, S.L.

2006-01-01

Ti 4+ -doped SnO 2 nano-powders were prepared by the sol-gel process using tin tetrachloride and titanium tetrachloride as the starting materials. The crystallinity and purity of the powders were analyzed by X-ray diffraction (XRD) and the size and distribution of Ti 4+ -doped SnO 2 grains were studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results show that Ti 4+ has been successfully incorporated into the SnO 2 crystal lattice and the electrical conductivity of the doped materials improves significantly

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-12-01

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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 )

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-07-01

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

Preparation of cauliflower-like shaped Ba0.6Sr0.4TiO3 powders by modified oxalate co-precipitation method

International Nuclear Information System (INIS)

Li Mingli; Xu Mingxia

2009-01-01

The quantitative barium-strontium titanyl oxalate (Ba 0.6 Sr 0.4 TiO(C 2 O 4 ) 2 .4H 2 O, BSTO) precursor powders were prepared by the modified oxalate co-preparation method. It was based on the cation-exchange reaction between the stoichiometric solutions of oxalotitanic acid (H 2 TiO(C 2 O 4 ) 2 , HTO) and barium + strontium nitrate solution containing stoichiometric quantities of Ba and Sr ions. The pyrolysis of BSTO at 800 deg. C/4 h in air produced the homogeneous cauliflower-like shaped barium-strontium titanate (Ba 0.6 Sr 0.4 TiO 3 , BST) powders. The effect of polyethylene glycol (PEG) on morphology of BSTO and BST powders was also investigated. The characterization studies were carried on the as-dried BSTO and calcined BST powders by various physicochemical techniques, IR, X-ray diffraction (XRD), scanning electron microscopy (SEM), etc. The BSTO and BST powders obtained by aforementioned technique without PEG were homogeneous with spherical shape. The particles grew into spindle shape with the effect of PEG

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)

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

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

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

Influence of Ultrafine 2CaO·SiO2 Powder on Hydration Properties of Reactive Powder Concrete

Directory of Open Access Journals (Sweden)

Hongfang Sun

2015-09-01

Full Text Available In this research, we assessed the influence of an ultrafine 2CaO·SiO2 powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM, mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO2. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO2 powder has the potential to improve the performance of a reactive powder cementitious system.

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.

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

The Diffraction Response Interpolation Method

DEFF Research Database (Denmark)

Jespersen, Søren Kragh; Wilhjelm, Jens Erik; Pedersen, Peder C.

1998-01-01

Computer modeling of the output voltage in a pulse-echo system is computationally very demanding, particularly whenconsidering reflector surfaces of arbitrary geometry. A new, efficient computational tool, the diffraction response interpolationmethod (DRIM), for modeling of reflectors in a fluid...... medium, is presented. The DRIM is based on the velocity potential impulseresponse method, adapted to pulse-echo applications by the use of acoustical reciprocity. Specifically, the DRIM operates bydividing the reflector surface into planar elements, finding the diffraction response at the corners...

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...

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

Combined wet-chemical process to synthesize 65PMN-35PT nanosized powders

International Nuclear Information System (INIS)

Santos, Luis P.S.; Longo, Elson; Leite, Edson R.; Camargo, Emerson R.

2004-01-01

Columbite MgNb 2 O 6 precursors were synthesized by a wet-chemical method by means of the dissolution of Nb 2 O 5 .5H 2 O and magnesium carbonate in a solution of oxalic acid. Pure 65PMN-35PT powders could be obtained by the columbite method with the use of the partial oxalate and oxidant peroxo methods. Powders were characterized by X-ray diffraction and FT-Raman spectroscopy showing that pure 65PMN-35PT are obtained when the powders are calcined up to 800 deg. C, without any trace of Pb-Nb pyrochlore. Cubic Pb 1,86 Mg 0.24 Nb 1.76 O 6.5 pyrochlore phase is formed by lead loss in the powders calcined at 900 deg. C and higher temperatures as undoubtedly characterized by Raman spectroscopy

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

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

Science.gov (United States)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

Directory of Open Access Journals (Sweden)

Apinpus Rujiwatra

2011-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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.

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.

Structural and electrical properties of copper-nickel-aluminum alloys obtained by conventional powder metallurgy method

International Nuclear Information System (INIS)

Monteiro, Waldemar A.; Carrio, Juan A.G.; Silveira, C.R. da; Pertile, H.K.S.

2009-01-01

This work looked for to search out systematically, in scale of laboratory, copper-nickel-aluminum alloys (Cu-Ni-Al) with conventional powder metallurgy processing, in view of the maintenance of the electric and mechanical properties with the intention of getting electric connectors of high performance or high mechanical damping. After cold uniaxial pressing (1000 kPa), sintering (780 deg C) and convenient homogenization treatments (500 deg C for different times) under vacuum (powder metallurgy), the obtained Cu-Ni-Al alloys were characterized by optical microscopy, electrical conductivity, Vickers hardness. X rays powder diffraction data were collected for the sintered samples in order to a structural and microstructural analysis. The comparative analysis is based on the sintered density, hardness, macrostructures and microstructures of the samples. (author)

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...

Nanosized lead lanthanum titanate (PLT) ceramic powders synthesized by the oxidant peroxo method

Energy Technology Data Exchange (ETDEWEB)

Camargo, Emerson R. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Department of Chemistry, UFSCar-Federal University of Sao Carlos, Rod.Washingtin Luis km 235, CP 676, Sao Carlos SP 13565-9905 (Brazil)], E-mail: camargo@ufscar.br; Barrado, Cristiano M. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Department of Chemistry, UFSCar-Federal University of Sao Carlos, Rod.Washingtin Luis km 235, CP 676, Sao Carlos SP 13565-9905 (Brazil); Ribeiro, Caue [EMBRAPA Instrumentacao Agropecuaria, Rua XV de Novembro 1452, Sao Carlos SP 13560-970 (Brazil)], E-mail: caue@cnpdia.embrapa.br; Longo, Elson [Department of Biochemistry, Chemistry Institute of Araraquara, UNESP-Sao Paulo State University, Rua Francisco Degni, CP 355, Araraquara SP 14801-907 (Brazil)], E-mail: elson@iq.unesp.br; Leite, Edson R. [LIEC-Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Department of Chemistry, UFSCar-Federal University of Sao Carlos, Rod.Washingtin Luis km 235, CP 676, Sao Carlos SP 13565-9905 (Brazil)], E-mail: derl@power.ufscar.br

2009-05-05

For the first time it is reported the synthesis of lead titanate modified with rare earth by the oxidant-peroxo method (OPM). Lanthanum was added up to 20% in mol through the dissolution of lanthanum oxide in nitric acid, followed by the addition of a solution of lead and lanthanum nitrate into an aqueous solution of titanium peroxo complexes. The amorphous precipitate formed was heat-treated at different temperatures in the range from 400 to 900 deg. C for crystallization. Powders were characterized by Raman spectroscopy and X-ray diffraction. Tetragonal perovskite structure was observed for the samples up to 15% of lanthanum substitution and cubic perovskite for sample with 20% of lanthanum. Crystallographic domains calculated by Scherrer equation showing a probable suppression of the crystallite growth in function of lanthanum content. It was observed shifting to lower frequencies of Raman modes in the range between 100 and 400 cm{sup -1} and the vanishing of the A1(2TO) and E(1LO) modes could be attributed to transition phase from tetragonal to cubic. Electronic microscopy image revealed that the powders annealed at height temperature are spherical with sharp size distribution.

Nanosized lead lanthanum titanate (PLT) ceramic powders synthesized by the oxidant peroxo method

International Nuclear Information System (INIS)

Camargo, Emerson R.; Barrado, Cristiano M.; Ribeiro, Caue; Longo, Elson; Leite, Edson R.

2009-01-01

For the first time it is reported the synthesis of lead titanate modified with rare earth by the oxidant-peroxo method (OPM). Lanthanum was added up to 20% in mol through the dissolution of lanthanum oxide in nitric acid, followed by the addition of a solution of lead and lanthanum nitrate into an aqueous solution of titanium peroxo complexes. The amorphous precipitate formed was heat-treated at different temperatures in the range from 400 to 900 deg. C for crystallization. Powders were characterized by Raman spectroscopy and X-ray diffraction. Tetragonal perovskite structure was observed for the samples up to 15% of lanthanum substitution and cubic perovskite for sample with 20% of lanthanum. Crystallographic domains calculated by Scherrer equation showing a probable suppression of the crystallite growth in function of lanthanum content. It was observed shifting to lower frequencies of Raman modes in the range between 100 and 400 cm -1 and the vanishing of the A1(2TO) and E(1LO) modes could be attributed to transition phase from tetragonal to cubic. Electronic microscopy image revealed that the powders annealed at height temperature are spherical with sharp size distribution.

Spheroidization of molybdenum powder by radio frequency thermal plasma

Science.gov (United States)

Liu, Xiao-ping; Wang, Kuai-she; Hu, Ping; Chen, Qiang; Volinsky, Alex A.

2015-11-01

To control the morphology and particle size of dense spherical molybdenum powder prepared by radio frequency (RF) plasma from irregular molybdenum powder as a precursor, plasma process parameters were optimized in this paper. The effects of the carrier gas flow rate and molybdenum powder feeding rate on the shape and size of the final products were studied. The molybdenum powder morphology was examined using high-resolution scanning electron microscopy. The powder phases were analyzed by X-ray diffraction. The tap density and apparent density of the molybdenum powder were investigated using a Hall flow meter and a Scott volumeter. The optimal process parameters for the spherical molybdenum powder preparation are 50 g/min powder feeding rate and 0.6 m3/h carrier gas rate. In addition, pure spherical molybdenum powder can be obtained from irregular powder, and the tap density is enhanced after plasma processing. The average size is reduced from 72 to 62 µm, and the tap density is increased from 2.7 to 6.2 g/cm3. Therefore, RF plasma is a promising method for the preparation of high-density and high-purity spherical powders.

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.)

Simple method of preparing nitrogen - doped nanosized TiO2 powders of high photocatalytic activity under visible light

International Nuclear Information System (INIS)

Nguyen Van Hung; Dang Thi Thanh Le

2014-01-01

Nitrogen-doped nanosized TiO 2 powders were prepared by a simple thermal treatment method of the mixture of titanium dioxide and urea. The prepared products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra (UV-Vis-DRS) and Fourier transform infrared (FT-IR) spectroscopy. The results showed that the crystal structure of N-TiO 2 was a mixture of anatase and rutile phases, and the average particle size was 31 nm calculated from XRD results. The UV-vis spectra indicate an increase in absorption of visible light when compared to undoped TiO 2 . The photocatalytic activity of nitrogen-doped TiO 2 powder was evaluated by the decomposition of methylene blue under visible light irradiation. And it was found that nitrogen-doped TiO 2 powders exhibited much higher photocatalytic activity than undoped TiO 2 . Moreover, the study also showed that, the doping N atoms improve the growth of the TiO 2 crystal and phase transformation. (author)

Review of the Methods for Production of Spherical Ti and Ti Alloy Powder

Science.gov (United States)

Sun, Pei; Fang, Zhigang Zak; Zhang, Ying; Xia, Yang

2017-10-01

Spherical titanium alloy powder is an important raw material for near-net-shape fabrication via a powder metallurgy (PM) manufacturing route, as well as feedstock for powder injection molding, and additive manufacturing (AM). Nevertheless, the cost of Ti powder including spherical Ti alloy has been a major hurdle that prevented PM Ti from being adopted for a wide range of applications. Especially with the increasing importance of powder-bed based AM technologies, the demand for spherical Ti powder has brought renewed attention on properties and cost, as well as on powder-producing processes. The performance of Ti components manufactured from powder has a strong dependence on the quality of powder, and it is therefore crucial to understand the properties and production methods of powder. This article aims to provide a cursory review of the basic techniques of commercial and emerging methods for making spherical Ti powder. The advantages as well as limitations of different methods are discussed.

Comprehensive characterization of ball-milled powders simulating a tribofilm system

Energy Technology Data Exchange (ETDEWEB)

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de; Dietrich, P.M., E-mail: Paul.dietrich@yahoo.de; Unger, W.E.S., E-mail: Wolfgang.Unger@bam.de; Österle, W., E-mail: Werner.Oesterle@bam.de

2016-01-15

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.

Synthesis and characterization of scandia ceria stabilized zirconia powders prepared by polymeric precursor method for integration into anode-supported solid oxide fuel cells

Science.gov (United States)

Tu, Hengyong; Liu, Xin; Yu, Qingchun

2011-03-01

Scandia ceria stabilized zirconia (10Sc1CeSZ) powders are synthesized by polymeric precursor method for use as the electrolyte of anode-supported solid oxide fuel cell (SOFC). The synthesized powders are characterized in terms of crystalline structure, particle shape and size distribution by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). 10Sc1CeSZ electrolyte films are deposited on green anode substrate by screen-printing method. Effects of 10Sc1CeSZ powder characteristics on sintered films are investigated regarding the integration process for application as the electrolytes in anode-supported SOFCs. It is found that the 10Sc1CeSZ films made from nano-sized powders with average size of 655 nm are very porous with many open pores. In comparison, the 10Sc1CeSZ films made from micron-sized powders with average size of 2.5 μm, which are obtained by calcination of nano-sized powders at higher temperatures, are much denser with a few closed pinholes. The cell performances are 911 mW cm-2 at the current density of 1.25 A cm-2 and 800 °C by application of Ce0.8Gd0.2O2 (CGO) barrier layer and La0.6Sr0.4CoO3 (LSC) cathode.

A new method of Debye-Scherrer pattern integration on two-dimensional detectors, demonstrated for the new structure powder diffractometer (SPODI) at the FRM-II in Garching

CERN Document Server

Elf, F; Artus, G R J; Roth, S

2002-01-01

The expected diffraction patterns of the new powder diffractometer SPODI, currently under construction at the FRM-II in Garching, will be smeared Debye-Scherrer rings as depicted by Monte Carlo (MC) simulations. To overcome this disadvantage, a concept based on the combination of MC simulations and empirical approximation methods is developed to reverse the smearing by deconvolution and then summing up along the rings, including corrections for different arc lengths, resulting in conventional one-dimensional diffraction patterns suitable for Rietveld-refinement programs without further processing. (orig.)

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

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

Grain growth studies on nanocrystalline Ni powder

International Nuclear Information System (INIS)

Rane, G.K.; Welzel, U.; Mittemeijer, E.J.

2012-01-01

The microstructure of nanocrystalline Ni powder produced by ball-milling and its thermal stability were investigated by applying different methods of X-ray diffraction line-profile analysis: single-line analysis, whole powder-pattern modelling and the (modified) Warren–Averbach method were employed. The kinetics of grain growth were investigated by both ex-situ and in-situ X-ray diffraction measurements. With increasing milling time, the grain-size reduction is accompanied by a considerable narrowing of the size distribution and an increase in the microstrain. Upon annealing, initial, rapid grain growth occurs, accompanied by the (almost complete) annihilation of microstrain. For longer annealing times, the grain-growth kinetics depend on the initial microstructure: a smaller microstrain with a broad grain-size distribution leads to linear grain growth, followed by parabolic grain growth, whereas a larger microstrain with a narrow grain-size distribution leads to incessant linear grain growth. These effects have been shown to be incompatible with grain-boundary curvature driven growth. The observed kinetics are ascribed to the role of excess free volume at the grain boundaries of nanocrystalline material and the prevalence of an “abnormal grain-growth” mechanism.

Mechanochemical preparation of nanocrystalline TiO2 powders and their behavior at high temperatures

International Nuclear Information System (INIS)

Gajovic, A.; Furic, K.; Tomasic, N.; Popovic, S.; Skoko, Z.; Music, S.

2005-01-01

Nanocrystalline TiO 2 powders were prepared by high-energy ball-milling using zirconia vial and balls. The changes of microstructure caused by material processing were studied using Raman spectroscopy, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The milling of the starting TiO 2 powder (anatase + rutile in traces) induced phase transitions to high-pressure polymorph, TiO 2 II, and rutile. We found that the phase transition to TiO 2 II was initiated at the surface of the small particles, while transition to rutile started in their center. Changes in crystallite size during milling process were obtained by the Scherrer method, while the particle size changes were monitored by TEM. The kinetics of phase changes, a decrease in crystallite/particle size, as well as zirconia contamination depended on the powder-to-ball weight ratio. The starting powder and some selected ball-milled samples were investigated in situ by Raman spectroscopy and XRD at high temperatures (up to 1300 deg. C) to examine their behavior during the sintering process. A difference in the results obtained by these two techniques was explained in frame of basic physical properties characterizing both methods. The morphology of the final sinters was monitored by scanning electron microscopy (SEM)

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)

Microstructural and electrical investigation of Cu-Ni-Cr alloys obtained by powder metallurgy method

International Nuclear Information System (INIS)

Carrio, Juan A.G.; Carvalhal, M.A.; Ayabe, L.M.; Monteiro, W.A.

2009-01-01

The aim of this work, using the powder metallurgy process, is to synthesize metallic alloys with high mechanical strength and high electric conductivity, after melting optimizing and thermal treatments. The Cu-Ni-Cr (wt%) alloys are characterized in their mechanical and electrical properties as well as the obtained microstructure. Through the process of powder metallurgy, contacts and structural parts can be obtained. The alloys elements are added to copper with the intention to improve their strength, ductility and thermal stability, without causing considerable damages in their form, electrical and thermal conductivity, and corrosion resistance. The metallic powders were mixed for a suitable time and then they were pressed in a cold uniaxial pressing (1000 kPa). Afterwards, the specimens were sintered in temperatures varying from 700 up to 800 deg C under vacuum. At last, the samples were homogenized at 550 deg C under vacuum, for special times. The comparative analysis is based on the sintered density, densification parameter, hardness, macrostructures and microstructures of the samples. The alloys were characterized by optical microscopy, X-rays powder diffraction, electrical conductivity and Vickers hardness. (author)

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.

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.

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

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.

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.

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.

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

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders

International Nuclear Information System (INIS)

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-01-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

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

A method of combining STEM image with parallel beam diffraction and electron-optical conditions for diffractive imaging

International Nuclear Information System (INIS)

He Haifeng; Nelson, Chris

2007-01-01

We describe a method of combining STEM imaging functionalities with nanoarea parallel beam electron diffraction on a modern TEM. This facilitates the search for individual particles whose diffraction patterns are needed for diffractive imaging or structural studies of nanoparticles. This also lays out a base for 3D diffraction data collection

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

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)>>>>

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.

Powder injection molding of Stellite 6 powder: Sintering, microstructural and mechanical properties

International Nuclear Information System (INIS)

Gülsoy, H. Özkan; Özgün, Özgür; Bilketay, Sezer

2016-01-01

The purpose of this study was to produce Co-based Stellite 6 superalloy components by using the method of Powder Injection Molding (PIM) and to characterize the microstructural and mechanical properties of the produced components. The experimental studies were started through the formation of feedstock by mixing Stellite 6 powder with a multicomponent binder system. Prepared feedstock was formed by utilizing powder injection molding technique. Then the molded samples were subjected to the solvent and thermal debinding processes. Different sintering cycles were applied to the raw components for the purpose of determining the optimum sintering conditions. The densities of the sintered components were determined in accordance with the Archimedes' principle. The microstructural characterization was performed through scanning electron microscope (SEM) analysis, energy dispersive spectrometry (EDS) analyses, and X-ray diffraction (XRD) analysis. Hardness measurement and tensile test were conducted in order to determine the mechanical properties. The results illustrated that the injection molded Stellite 6 components were composed of fine and equiaxed grains, plenty of carbide precipitates exhibiting homogenous distribution throughout the microstructure formed at the grain boundaries and thus the mechanical properties were considerably high.

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.

Synthesis of ultrafine alumina powders using egg white as complexing medium

International Nuclear Information System (INIS)

Salem, R.E.P.; Guilherme, K. A.; Chinelatto, A.S.A.; Chinelatto, A.L.

2011-01-01

Synthesis of alumina powders through chemical methods has been attracting much attention of researchers in the past few years, due to the ability to produce powders in nanometric scale with high degree of purity. In this work, there were synthesized alumina powders through a chemical route, using egg white as a complexing medium and aluminium nitrate as the source of Al 3+ cations. Egg white contains ovalbumin, a protein which acts effectively on the isolation of aluminium cations during the mixing process, enabling the formation of ultrafine alumina powders in a relatively economic and environmentally friendly way. The powders obtained by calcinations of the precursor resin were characterized by X-ray diffraction, specific surface area measurements, infrared spectroscopy and scanning electron microscopy. It was observed that the egg white, present at the reaction medium, allowed obtaining transition alumina powders, with high degree of purity. (author)

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.

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/

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.

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

Ternary ceramic thermal spraying powder and method of manufacturing thermal sprayed coating using said powder

Energy Technology Data Exchange (ETDEWEB)

Vogli, Evelina; Sherman, Andrew J.; Glasgow, Curtis P.

2018-02-06

The invention describes a method for producing ternary and binary ceramic powders and their thermal spraying capable of manufacturing thermal sprayed coatings with superior properties. Powder contain at least 30% by weight ternary ceramic, at least 20% by weight binary molybdenum borides, at least one of the binary borides of Cr, Fe, Ni, W and Co and a maximum of 10% by weight of nano and submicro-sized boron nitride. The primary crystal phase of the manufactured thermal sprayed coatings from these powders is a ternary ceramic, while the secondary phases are binary ceramics. The coatings have extremely high resistance against corrosion of molten metal, extremely thermal shock resistance and superior tribological properties at low and at high temperatures.

A pseudospectral collocation time-domain method for diffractive optics

DEFF Research Database (Denmark)

Dinesen, P.G.; Hesthaven, J.S.; Lynov, Jens-Peter

2000-01-01

We present a pseudospectral method for the analysis of diffractive optical elements. The method computes a direct time-domain solution of Maxwell's equations and is applied to solving wave propagation in 2D diffractive optical elements. (C) 2000 IMACS. Published by Elsevier Science B.V. All rights...

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 ...

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.

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.)

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

International Nuclear Information System (INIS)

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

1979-07-01

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

An In-situ method for the study of strain broadening usingsynchrotronx-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Tang, Chiu C.; Lynch, Peter A.; Cheary, Robert W.; Clark, Simon M.

2006-12-15

A tensonometer for stretching metal foils has beenconstructed for the study of strain broadening in x-ray diffraction lineprofiles. This device, which is designed for use on the powderdiffractometer in Station 2.3 at Daresbury Laboratory, allows in-situmeasurements to be performed on samples under stress. It can be used fordata collection in either transmission or reflection modes using eithersymmetric or asymmetric diffraction geometries. As a test case,measurements were carried out on a 18mum thick copper foil experiencingstrain levels of up to 5 percent using both symmetric reflection andsymmetric transmission diffraction. All the diffraction profilesdisplayed peak broadening and asymmetry which increased with strain. Themeasured profiles were analysed by the fundamental parameters approachusing the TOPAS peak fitting software. All the observed broadenedprofiles were modelled by convoluting a refineable diffraction profile,representing the dislocation and crystallite size broadening, with afixed instrumental profile pre-determined usinghigh quality LaB6reference powder. The de-convolution process yielded "pure" sampleintegral breadths and asymmetry results which displayed a strongdependence on applied strain and increased almost linearly with appliedstrain. Assuming crystallite size broadening in combination withdislocation broadening arising from fcc a/2<110>111 dislocations,we have extracted the variation of mechanic al property with strain. Theobservation of both peak asymmetry and broadening has been interpreted asa manifestation of a cellular structure with cell walls and cellinteriors possessing high and low dislocation densities.

Crushing method for nuclear fuel powder

International Nuclear Information System (INIS)

Hasegawa, Shin-ichi; Tsuchiya, Haruo.

1997-01-01

A crushing medium is contained in mill pots disposed at the circumferential periphery of a main axis. The diameter of each mill pot is determined such that powdery nuclear fuels containing aggregated powders and ground and mixed powders do not reach criticality. A plurality of mill pots are revolved in the direction of the main axis while each pots rotating on its axis. Powdery nuclear fuels containing aggregated powders are conveyed to a supply portion of the moll pot, and an inert gas is supplied to the supply portion. The powdery nuclear fuels are supplied from the supply portion to the inside of the mill pots, and the powdery nuclear fuels containing aggregated powders are crushed by centrifugal force caused by the rotation and the revolving of the mill pots by means of the crushing medium. UO 2 powder in uranium oxide fuels can be crushed continuously. PuO 2 powder and UO 2 powder in MOX fuels can be crushed and mixed continuously. (I.N.)

Synthesis of ceramic powder of TiO_2 doped with Zr by the Pechini Method applied in ceramic membranes for water treatment

International Nuclear Information System (INIS)

Farias, R.F.V.; Fernandes, M.S.M.; Silva, R.S.; Franca, K.B.; Lira, H.L.; Bonifacio, M.A.R.

2016-01-01

This paper describes the synthesis of ceramic powder of TiO2 doped with Zr by the polymeric precursor method, also known as Pechini method applied in ceramic membranes for water treatment. Three compositions were synthesized according to the molar ratio Ti_x-1Zr_xO_2 (x = 0.25, 0.50 and 0.75 moles), calcined at 700° C/1h. The samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and microbiological analysis. The presence of the doping element was not decisive in the average size of crystallite, which ranged from 5.5 to 11.3 nm. The SEM images showed clusters with uniform surface and granular aspect, it is still possible to see a clearly porous structure formed by clusters of uniform size for all samples. The microbiological analyses of powders have revealed that they have bactericidal properties. (author)

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)

The influence of dislocation defects on the sintering kinetics of ferrite powders

International Nuclear Information System (INIS)

Fadeeva, I.V.; Portnoi, K.V.; Oleinikov, N.N.; Tretyakov, D.Yu.

1976-01-01

In the presented paper are given the results of the X-ray investigations of non-equilibrium defects in powders of nickel-zinc ferrites. The block size, the crystal lattice microdistortions and stacking faults of two types were determined by the method of Fourier's analysis of diffraction line profiles. The influence of similar defects on sintering of ferrite powders was shown. The kinetics data on densification processes occurring during sintering of active powders can adequately be described in terms of the equations which describe reactions in the solid phase, where the interaction limit is on the border of the phases with different geomtery of the border. The correlation between the behaviour of compacts and dislocation defects in powders during sintering is established

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

MECHANICAL ALLOYING SYNTHESIS OF FORSTERITE-DIOPSIDE NANOCOMPOSITE POWDER FOR USING IN TISSUE ENGINEERING

Directory of Open Access Journals (Sweden)

Sorour Sadeghzade

2015-03-01

Full Text Available In present study the pure forsterite-diopside nanocomposite powder was successfully synthesized by the economical method of mechanical alloying and subsequence sintering, for the first time. The starting economical materials were talc (Mg3Si4H2O12, magnesium carbonate (MgCO3 and calcium carbonate (CaCO3 powders. The prepared powder was characterized by thermo gravimetric analysis (TGA, X-ray diffraction (XRD, and scanning electron microscopy (SEM. The results showed preparation of forsterite- diopside nanocomposite powder after 10 h mechanical alloying and sintering at 1200oC for 1 h. The powder crystallite sizes and agglomerated particle sizes were measured about 73 +/- 4 nm and 0.3 - 4 μm, respectively. Absence of enstatite that causes a reduction in mechanical and bioactivity properties of forsterite ceramic, is an important feature of produced powder.

User guide for the POLARIS powder diffractometer at ISIS

International Nuclear Information System (INIS)

Hull, S.; Mayers, J.

1989-11-01

The POLARIS spectrometer at ISIS is currently being scheduled for use as a high intensity, medium resolution powder diffractometer. The particularly high neutron flux on POLARIS enables experiments to be performed with comparatively short counting times or on small sample volumes. This ability has been exploited during kinetic experiments of phase changes, where diffraction data is collected whilst the furnace is heating up. The provision of a large detector bank at 2 θ ∼ 90 0 is particularly important for studies of powder samples at high pressures. This scattering geometry has significant advantages for experiments of this kind, as suitable collimation of the incident and outgoing beams eliminates scattering from the surrounding pressure transmitting medium. This guide is intended to give a short description of the POLARIS powder diffractometer and to provide the basic information required to perform a powder diffraction experiment. (author)

Green biosynthesis of silver nanoparticles using Curcuma longa tuber powder

Science.gov (United States)

Shameli, Kamyar; Ahmad, Mansor Bin; Zamanian, Ali; Sangpour, Parvanh; Shabanzadeh, Parvaneh; Abdollahi, Yadollah; Zargar, Mohsen

2012-01-01

Green synthesis of noble metal nanoparticles is a vastly developing area of research. Metallic nanoparticles have received great attention from chemists, physicists, biologists, and engineers who wish to use them for the development of a new-generation of nanodevices. In this study, silver nanoparticles were biosynthesized from aqueous silver nitrate through a simple and eco-friendly route using Curcuma longa tuber-powder extracts, which acted as a reductant and stabilizer simultaneously. Characterizations of nanoparticles were done using different methods, which included ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray fluorescence spectrometry, and Fourier-transform infrared spectroscopy. The ultraviolet-visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 415 nm. Transmission electron microscopy showed that mean diameter and standard deviation for the formation of silver nanoparticles was 6.30 ± 2.64 nm. Powder X-ray diffraction showed that the particles are crystalline in nature, with a face-centered cubic structure. The most needed outcome of this work will be the development of value-added products from C. longa for biomedical and nanotechnology-based industries. PMID:23341739

Preparation of cauliflower-like shaped Ba{sub 0.6}Sr{sub 0.4}TiO{sub 3} powders by modified oxalate co-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Li Mingli [School of Materials Science and Engineering, Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education, Tianjin University, Tianjin 300072 (China)], E-mail: lml@tju.edu.cn; Xu Mingxia [School of Materials Science and Engineering, Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education, Tianjin University, Tianjin 300072 (China)

2009-04-17

The quantitative barium-strontium titanyl oxalate (Ba{sub 0.6}Sr{sub 0.4}TiO(C{sub 2}O{sub 4}){sub 2}.4H{sub 2}O, BSTO) precursor powders were prepared by the modified oxalate co-preparation method. It was based on the cation-exchange reaction between the stoichiometric solutions of oxalotitanic acid (H{sub 2}TiO(C{sub 2}O{sub 4}){sub 2}, HTO) and barium + strontium nitrate solution containing stoichiometric quantities of Ba and Sr ions. The pyrolysis of BSTO at 800 deg. C/4 h in air produced the homogeneous cauliflower-like shaped barium-strontium titanate (Ba{sub 0.6}Sr{sub 0.4}TiO{sub 3}, BST) powders. The effect of polyethylene glycol (PEG) on morphology of BSTO and BST powders was also investigated. The characterization studies were carried on the as-dried BSTO and calcined BST powders by various physicochemical techniques, IR, X-ray diffraction (XRD), scanning electron microscopy (SEM), etc. The BSTO and BST powders obtained by aforementioned technique without PEG were homogeneous with spherical shape. The particles grew into spindle shape with the effect of PEG.

Effect of synthesis conditions on the preparation of YIG powders via co-precipitation method

International Nuclear Information System (INIS)

Rashad, M.M.; Hessien, M.M.; El-Midany, A.; Ibrahim, I.A.

2009-01-01

Yttrium iron garnet (YIG) (Y 3 Fe 5 O 12 ) powders have been synthesized through a co-precipitation method in the presence of sodium bis(2-ethylhexylsulfosuccinate), AOT as an anionic surfactant. The garnet precursors produced were obtained from aqueous iron and yttrium nitrates mixtures using 5 M sodium hydroxide at pH 10. A statistical Box-Behnken experimental design was used to investigate the effect of the main parameters (i.e. AOT surfactant concentration, annealing time and temperature) on YIG powder formation, crystallite size, morphology and magnetic properties. YIG particles were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometer. XRD revealed that the formation of single cubic phase of YIG was temperature dependent and increased by increasing the annealing temperature from 800 to 1200 o C. SEM micrographs showed that the addition of AOT surfactant promoted the microstructure of YIG in crystalline cubic-like structure. The magnetic properties were sensitive to the synthesis variables of annealing temperature, time and AOT surfactant concentration. The maximum saturation magnetization (28.13 emu/g), remanence magnetization (21.57 emu/g) and coercive force (703 Oe) were achieved at an annealing temperature of 1200 o C, time 2 h and 500 ppm of AOT surfactant concentration.

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).

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...

Method for preparing a sinterable uranium dioxide powder

International Nuclear Information System (INIS)

Thornton, T.A.; Holaday, V.D. Jr.

1985-01-01

This invention provides an improved method for preparing a sinterable uranium dioxide powder for the preparation of nuclear fuel, using microwave radiation in a microwave induction furnace. The starting compound may be uranyl nitrate hexahydrate, ammonium diuranate or ammonium uranyl carbonate. The starting compound is heated in a microwave induction furnace for a period of time sufficient for compound decomposition. The decomposed compound is heated in a microwave induction furnace in a reducing atmosphere for a period of time sufficient to reduce the decomposed compound to uranium dioxide powder

Preparation of powders Ag3PO4 and study of their photocatalytic activity

International Nuclear Information System (INIS)

Badurova, K.

2014-01-01

In our thesis we dealt with preparing powders of Ag 3 PO 4 by using Na 2 HPO 4 ·12H 2 O and Na 3 PO 4 ·12H 2 O as two different precursors. Samples were prepared by precipitation and mechanochemical methods. Photocatalytic efficiency of individual samples was studied by irradiation of suspensions of prepared powders with methylene blue (MB) solution and with phenol solution using source of light similar to solar light. Photocatalytic efficiency was determined via method of determination of total organic carbon (TOC) as the time dependence of phenol concentration and also via monitoring spectrophotometric parameters of solution as the time dependence of MB solution colouring intensity. Effect of sample preparation method on photocatalytic efficiency and morphology of particles was studied. After that, samples were characterised by X-ray powder diffraction method (XRD), scanning electron microscopy (SEM) and Raman spectroscopy (authors)

Effect of fabrication conditions on the properties of indium tin oxide powders

International Nuclear Information System (INIS)

Xie Wei

2008-01-01

This paper reports that indium tin oxide (ITO) crystalline powders are prepared by coprecipitation method. Fabrication conditions mainly as sintering temperature and Sn doping content are correlated with the phase, microstructure, infrared emissivity in and powder resistivity of indium tin oxides by means of x-ray diffraction, Fourier transform infrared, and transmission electron microscope. The optimum sintering temperature of 1350°C and Sn doping content 6∼8wt% are determined. The application of ITO in the military camouflage field is proposed. (condensed matter: electronic structure, electrical, magnetic, and optical properties)

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

Energy Technology Data Exchange (ETDEWEB)

Rybak, Jens-Christoph

2012-07-01

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

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

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

Directory of Open Access Journals (Sweden)

Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

2009-01-01

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

NANOCOMPOSITE POWDERS FOR NEW CONTACT MATERIALS BASED ONCOPPER AND ALUMINA

Directory of Open Access Journals (Sweden)

Marija Korać

2008-11-01

Full Text Available This paper is a contribution to characterization of Cu-Al2O3 powders with nanostructure designed for the production of dispersion strengthened contact materials. New materials with predetermined properties can be successfully synthesized by utilizing the principles of hydrometallurgy and powder metallurgy. The results show a development of a new procedure for the synthesis. The applied characterization methods were differential thermal and thermogravimetric analysis (DTA-TGA, X-ray diffraction (XRD, scanning electron microscopy (SEM, Transmission Electron Microscopy (TEM: Focused Ion Beam (FIB and Analytical Electron Microscopy (AEM. Nanostructure characteristics, particle size in range 20-50 nm, and uniform distribution of dispersoide in copper matrix were validated.

Preparation of lanthanum ferrite powder at low temperature

Energy Technology Data Exchange (ETDEWEB)

Andoulsi, R.; Horchani-Naifer, K.; Ferid, M., E-mail: karima_horchani@yahoo.com [Physical Chemistry Laboratory of Mineral Materials and their Applications, Hammam-Lif (Tunisia)

2012-01-15

Single lanthanum ferrite phase was successfully prepared at low processing temperature using the polymerizable complex method. To implement this work, several techniques such as differential scanning calorimetry, X-ray diffraction, Fourier Transform Infrared Spectroscopy, scanning electron microscopy and BET surface area measurements were used. Throw the obtained results, it was shown that steps of preparing the powder precursor and temperature of its calcination are critical parameters for avoiding phase segregation and obtaining pure lanthanum ferrite compound. Thus, a single perovskite phase was obtained at 600 deg C. At this temperature, the powder was found to be fine and homogeneous with an average crystallite size of 13 nm and a specific surface area of 12.5 m{sup 2}.g{sup -1}. (author)

The high resolution powder diffractometer (HRPD) at ISIS - a user guide

International Nuclear Information System (INIS)

Ibberson, R.M.; David, W.I.F.; Knight, K.S.

1992-05-01

This guide is intended to give a short description of the High Resolution Powder Diffractometer, HRPD, at ISIS and to provide the basic information required in order to perform a routine powder diffraction experiment. (Author)

New manufacturing method for Fe-Si magnetic powders using modified pack-cementation process

Science.gov (United States)

Byun, Ji Young; Kim, Jang Won; Han, Jeong Whan; Jang, Pyungwoo

2013-03-01

This paper describes a new method for making Fe-Si magnetic powders using a pack-cementation process. It was found that Fe-Si alloy powders were formed by a reaction of the pack mixture of Fe, Si, NaF, and Al2O3 powders at 900 °C for 24 h under a hydrogen atmosphere. Separation of the Fe-Si alloy powders was dependent on the particle size of the Fe powders in the pack. For small Fe powders, magnetic separation in a medium of strong alkali solution was recommended. But, for relatively larger Fe powders, the Fe-Si alloy powders were easily separated from Al2O3 powders using a magnet in air atmosphere. The Si content in the Fe-Si magnetic powders were easily controlled by changing the weight ratio of Si to (Si+Fe) in the pack.

Electrodeposition fabrication of Co-based superhydrophobic powder coatings in non-aqueous electrolyte

Science.gov (United States)

Chen, Zhi; Hao, Limei; Duan, Mengmeng; Chen, Changle

2013-05-01

A rapid, facile, one-step process was developed to fabricate Co-based superhydrophobic powder coatings on the stainless steel surfaces with a nonaqueous electrolyte by the electrodeposition method. The structure and composition of the superhydrophobic surfaces were characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and contact angle measurement. The results show that the special hierarchical structures along with the low surface energy lead to the high superhydrophobicity of the substrate surface. The shortest process of constructing the superhydrophobic surface is only 30 seconds, the high contact angle is greater than 160°, and the rolling angle is less than 2°. The method can be used to fabricate the superhydrophobic powder coatings at any conductive cathodic surface, and the as-prepared superhydrophobic powder coatings have advantages of transferability, repairability, and durability. It is expected that this facile method will accelerate the large-scale production of superhydrophobic material.

Processing of tungsten scrap into powders by electroerosion disintegration

International Nuclear Information System (INIS)

Fominskii, L.P.; Leuchuk, M.V.; Myuller, A.S.; Tarabrina, V.P.

1985-01-01

Utilization of tungsten and tungsten alloy swarf and other waste and also of rejected and worn parts is a matter of great importance in view of the shortage of this metal. The authors examine the electroerosion (EE) disintegration of tungsten in water as a means of utilizing swarf and other loose waste. Unlike chemical methods, EE disintegration ensures ecological purity since there are no effluent waters or toxic discharges. Swarf and trimmings of rods of diameters up to 20 mm obtained after the lathe-turning of tungsten bars sintered from PVN and PVV tungsten powders were disintegrated in water at room temperature between tungsten electrodes. The phase composition of the powder was studied using FeK /SUB alpha/ radiation, by x-ray diffraction methods in a DRON-2 diffractometer with a graphite monochromator on the secondary beam. When tungsten is heated to boiling during EE disintegration, the impurities present in it can evaporate and burn out. Thus, tungsten powder produced by EE disintegration can be purer than the starting metal

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.

Synthesis and Cell Seeding Assessment of Novel Biphasic Nano Powder in the CaO–MgO–SiO2 System for Bone Implant Application

Directory of Open Access Journals (Sweden)

Kazem Marzban

2017-02-01

Full Text Available Objective(s: CaO–MgO–SiO2 system bioceramics possess good characteristics for hard tissue engineering applications. The aim of the study was to synthesize the nano powder by using a sol-gel method and evaluate of bioactivity in the cells culture. Methods: To characterize of powder X-ray diffraction (XRD, transmission electron microscopy (TEM and to evaluate the bioactivity sample cell seeding and methylthiazol tetrazolium (MTT assay were performed. Results: X-ray diffraction (XRD analysis showed that the biphasic powder was obtained at 1300°C for 2 h by using a sol-gel method. Transmission electron microscopy (TEM image showed that powder particle size was about 45 nm. Besides, cell culture results indicated that the percentage of viability values was increased by the extension of period. Conclusions: found that the sample is cytocompatible and has cell proliferation potential in culture medium. The present study demonstrates that, the biphasic CaO–MgO–SiO2 system can be used to achieve novel bioactive materials for bone implant application.

[Determination method of polysorbates in powdered soup by HPLC].

Science.gov (United States)

Takeda, Y; Abe, Y; Ishiwata, H; Yamada, T

2001-04-01

A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.

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.

Characterization of composite materials based on cement-ceramic powder blended binder

Science.gov (United States)

Kulovaná, Tereza; Pavlík, Zbyšek

2016-06-01

Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO2 emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzed by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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.

NIST/Sandia/ICDD Electron Diffraction Database: A Database for Phase Identification by Electron Diffraction.

Science.gov (United States)

Carr, M J; Chambers, W F; Melgaard, D; Himes, V L; Stalick, J K; Mighell, A D

1989-01-01

A new database containing crystallographic and chemical information designed especially for application to electron diffraction search/match and related problems has been developed. The new database was derived from two well-established x-ray diffraction databases, the JCPDS Powder Diffraction File and NBS CRYSTAL DATA, and incorporates 2 years of experience with an earlier version. It contains 71,142 entries, with space group and unit cell data for 59,612 of those. Unit cell and space group information were used, where available, to calculate patterns consisting of all allowed reflections with d -spacings greater than 0.8 A for ~ 59,000 of the entries. Calculated patterns are used in the database in preference to experimental x-ray data when both are available, since experimental x-ray data sometimes omits high d -spacing data which falls at low diffraction angles. Intensity data are not given when calculated spacings are used. A search scheme using chemistry and r -spacing (reciprocal d -spacing) has been developed. Other potentially searchable data in this new database include space group, Pearson symbol, unit cell edge lengths, reduced cell edge length, and reduced cell volume. Compound and/or mineral names, formulas, and journal references are included in the output, as well as pointers to corresponding entries in NBS CRYSTAL DATA and the Powder Diffraction File where more complete information may be obtained. Atom positions are not given. Rudimentary search software has been written to implement a chemistry and r -spacing bit map search. With typical data, a full search through ~ 71,000 compounds takes 10~20 seconds on a PDP 11/23-RL02 system.

Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

International Nuclear Information System (INIS)

Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

2009-01-01

Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

Application of physical and chemical characterization techniques to metallic powders

International Nuclear Information System (INIS)

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

2014-01-01

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

Thermally induced phase transformation of pearl powder

International Nuclear Information System (INIS)

Zhang, Guoqing; Guo, Yili; Ao, Ju; Yang, Jing; Lv, Guanglie; Shih, Kaimin

2013-01-01

The polymorphic phase transformation of thermally treated pearl powder was investigated by X-ray diffraction and thermoanalytical techniques. The phase transformation was based on quantification of the calcite content at various temperatures using Rietveld refinement analysis. The results show that the phase transformation of pearl aragonite occurred within a temperature range of 360–410 °C, which is 50–100 °C lower than the range for non-biomineralized aragonite. These thermoanalytical results suggest that the phase transformation of pearl aragonite may occur immediately after the thermal decomposition of the organic matrix in the pearl powder. An important finding is that decomposition of the organic matrix may greatly facilitate such transformation by releasing additional space for an easier structural reconstruction during the phase transformation process. - Highlights: ► Providing a new method to describe the polymorphic transition of pearl powder ► The phase transition sketch was exhibited by XRD phase quantitative analysis. ► There are dozens of degrees in advance comparing to natural aragonite. ► The phase transition occurs following the thermal decomposition of organism

Mechanochemical effects on high-Tc superconductor powders

International Nuclear Information System (INIS)

Yamada, Taichi; Nagai, Ryoji; Takeuchi, Manabu; Minehara, Eisuke.

1991-03-01

We have investigated the mechanochemical effects on high-Tc superconductor (YBa 2 Cu 3 O 7 -δ) powders. The powder was mechanically ground in air using an agate mortar with a pestle. The grinding time was varied from 2 to 100 min. The mean particle sizes of the powders were measured by a sedimentation method. The degradation of superconductivity was evaluated by the measurements of the crystallinity and volume fraction of the superconducting phase. The crystallinity was estimated from X-ray diffraction patterns. The volume fraction of the superconducting phase was estimated from the diamagnetization. The results of these changes of 2 min. and 100 min. grinding are respectively as follows; 1) mean particle size: 10.8 μm and 7.2 μm, 2) crystallinity: 40.0 % and 24.8 %, 3) volume fraction of superconducting phase: 91.5 % and 30.0 %. Recovery of the crystallinity and superconductivity of the ground specimens by re-sintering and re-annealing was also studied. It was found that the recovery of both of the characteristics was not complete. (author)

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)

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

Preparation methods of U3O8 powder for MTR fuel elements

International Nuclear Information System (INIS)

Leal Neto, R.M.; Riella, H.G.

1990-01-01

Three preparation methods of U 3 O 8 powder have been studied with the aim of finding a simple and economic processing route: grinding of sintered U 3 O 8 pellets (Method-1); sintering of U 3 O 8 calcined granules (Method-2); and sintering of ammonium diuranate (ADU) granules (Method-3). Granulometric yield, powder characteristics and processing steps and difficulties have been taken into account for comparison purposes. Method-2 have been found to give the best results. Method-3 gives also good results, but there were some difficulties with ADU handling. (author) [pt

Method of producing radioactive carbon powder

International Nuclear Information System (INIS)

Imamura, Y.

1980-01-01

Carbon powder, placed in a hermetically closed apparatus under vacuum together with radium ore, adsorbs radon gas emanating from the radium ore thus producing a radioactive carbonaceous material, the radioactivity of which is due to the presence of adsorbed radon. The radioactive carbon powder thus obtained has excellent therapeutical efficacy and is suitable for a variety of applications because of the mild radioactivity of radon. Radium ore permits substantially limitlessly repeated production of the radioactive carbon powder

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

DEFF Research Database (Denmark)

Frankær, Christian Grundahl

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

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

Science.gov (United States)

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

2012-04-01

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

Structural 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.

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

Measurements of Residual Stresses In Cold-Rolled 304 Stainless Steel Plates Using X-Ray Diffraction with Rietveld Refinement Method

International Nuclear Information System (INIS)

Parikin; Killen, P; Rafterry, A.

2009-01-01

The determination of the residual stresses using X-ray powder diffraction in a series of cold-rolled 304 stainless steel plates, deforming 0, 34, 84, 152, 158, 175 and 196 % reduction in thickness has been carried out. The diffraction data were analyzed using the Rietveld structure refinement method. The analysis shows that for all specimens, the martensite particles are closely in compression and the austenite matrix is in tension. Both the martensite and austenite, for a sample reducing 34% in thickness (containing of about 1% martensite phase) the average lattice strains are anisotropic and decrease approximately exponential with an increase in the corresponding percent reduction (essentially phase content). It is shown that this feature can be qualitatively understood by taking into consideration the thermal expansion mismatch between the martensite and austenite grains. Also, for all cold-rolled stainless steel specimens, the diffraction peaks are broader than the unrolled one (instrumental resolution), indicating that the strains in these specimens are inhomogeneous. From an analysis of the refined peak shape parameters, the average root-mean square strain, which describes the distribution of the inhomogeneous strain field, was predicted. The average residual stresses in cold-rolled 304 stainless steel plates showed a combination effect of hydrostatic stresses of the martensite particles and the austenite matrix. (author)

Method for forming biaxially textured articles by powder metallurgy

Science.gov (United States)

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2002-01-01

A method of preparing a biaxially textured alloy article comprises the steps of preparing a mixture comprising Ni powder and at least one powder selected from the group consisting of Cr, W, V, Mo, Cu, Al, Ce, YSZ, Y, Rare Earths, (RE), MgO, CeO.sub.2, and Y.sub.2 O.sub.3 ; compacting the mixture, followed by heat treating and rapidly recrystallizing to produce a biaxial texture on the article. In some embodiments the alloy article further comprises electromagnetic or electro-optical devices and possesses superconducting properties.

Experimental method for testing diffraction properties of reflection waveguide holograms.

Science.gov (United States)

Xie, Yi; Kang, Ming-Wu; Wang, Bao-Ping

2014-07-01

Waveguide holograms' diffraction properties include peak wavelength and diffraction efficiency, which play an important role in determining their display performance. Based on the record and reconstruction theory of reflection waveguide holograms, a novel experimental method for testing diffraction properties is introduced and analyzed in this paper, which uses a plano-convex lens optically contacted to the surface of the substrate plate of the waveguide hologram, so that the diffracted light beam can be easily detected. Then an experiment is implemented. The designed reconstruction wavelength of the test sample is 530 nm, and its diffraction efficiency is 100%. The experimental results are a peak wavelength of 527.7 nm and a diffraction efficiency of 94.1%. It is shown that the tested value corresponds well with the designed value.

Synthesis of Black and Red Mercury Sulfide Nano-Powder by Traditional Indian Method for Biomedical Application

International Nuclear Information System (INIS)

Padhi, Payodhar; Sahoo, G.; Das, K.; Ghosh, Sudipto; Panigrahi, S. C.

2008-01-01

physicians could get rid of free mercury by milling and proper choice of the ratio of ingredients as is shown in the investigation by X-ray diffraction studies. In the traditional method for synthesis of mercury sulfide, mercury and pure sulfur were taken and milled in a mortar and pastel. During milling process, the white mercury and yellow sulfur yielded to a gray black colored sulfide. Synthesis of red sulfide of mercury required additional steps of heating and subsequent milling. For therapeutically application, the sulfide thus obtained needed detoxification, which was done using organic extracts. In the present investigation, the same method was followed to synthesize the sapphires and the product was characterized using modern methods like XRD, SEM and HRTEM. With increase in milling time the fineness of the powder increases, which increases the efficacy of the medicine, and free mercury, which is not desirable for medicinal application is found to decrease. The powder obtained at the end of 48 hours of milling is found to be of a size finer than l0nm.

Synthesis of Black and Red Mercury Sulfide Nano-Powder by Traditional Indian Method for Biomedical Application

Science.gov (United States)

Padhi, Payodhar; Sahoo, G.; Das, K.; Ghosh, Sudipto; Panigrahi, S. C.

2008-10-01

physicians could get rid of free mercury by milling and proper choice of the ratio of ingredients as is shown in the investigation by X-ray diffraction studies. In the traditional method for synthesis of mercury sulfide, mercury and pure sulfur were taken and milled in a mortar and pastel. During milling process, the white mercury and yellow sulfur yielded to a gray black colored sulfide. Synthesis of red sulfide of mercury required additional steps of heating and subsequent milling. For therapeutically application, the sulfide thus obtained needed detoxification, which was done using organic extracts. In the present investigation, the same method was followed to synthesize the sapphires and the product was characterized using modern methods like XRD, SEM and HRTEM. With increase in milling time the fineness of the powder increases, which increases the efficacy of the medicine, and free mercury, which is not desirable for medicinal application is found to decrease. The powder obtained at the end of 48 hours of milling is found to be of a size finer than l0nm.

Method and apparatus for the production of metal oxide powder

Science.gov (United States)

Harris, Michael T.; Scott, Timothy C.; Byers, Charles H.

1992-01-01

The present invention provides a method for preparing metal oxide powder. A first solution, which is substantially organic, is prepared. A second solution, which is an aqueous solution substantially immiscible in the first solution, is prepared and delivered as drops to the first solution. The drops of the second solution are atomized by a pulsed electric field forming micro-drops of the second solution. Reagents in the first solution diffuse into and react with reactants in the micro-drops of the second solution forming metal hydroxide or oxalate particles. The metal hydroxide or metal oxalate particles are then recovered and dried to produce the metal oxide powder. An apparatus for preparing a metal oxide powder is also disclosed.

Studies on powder processing and sintering behaviour of ZrO2-9.0 mol% Y2O3 ceramics

International Nuclear Information System (INIS)

Ghosh, A.; Gonal, M.R.; Upadhyaya, D.D.; Ram Prasad

1998-01-01

In the present investigation the synthesis and densification behaviour of ZrO 2 -9.0 mol% Y 2 O 3 ceramics has been described. Powder preparation was based on the co-precipitation method. It was found that variation in the precipitation conditions and washing steps of the precipitated gels resulted in powder of different agglomerate sizes. The effect of different precipitations and washing conditions on the crystallite size of the 600 deg C calcined powders were examined by x-ray diffraction. The powders produced were essentially of the cubic fluorite phase. The ball-milled powders were analyzed for particle size distribution. Densification behaviour of the bodies made by slip casting has also been studied. (author)

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)

Synthesis method for ultrananocrystalline diamond in powder employing a coaxial arc plasma gun

Science.gov (United States)

Naragino, Hiroshi; Tominaga, Aki; Hanada, Kenji; Yoshitake, Tsuyoshi

2015-07-01

A new method that enables us to synthesize ultrananocrystalline diamond (UNCD) in powder is proposed. Highly energetic carbon species ejected from a graphite cathode of a coaxial arc plasma gun were provided on a quartz plate at a high density by repeated arc discharge in a compact vacuum chamber, and resultant films automatically peeled from the plate were aggregated and powdered. The grain size was easily controlled from 2.4 to 15.0 nm by changing the arc discharge energy. It was experimentally demonstrated that the proposed method is a new and promising method that enables us to synthesize UNCD in powder easily and controllably.

Synthesis method for ultrananocrystalline diamond in powder employing a coaxial arc plasma gun

International Nuclear Information System (INIS)

Naragino, Hiroshi; Tominaga, Aki; Yoshitake, Tsuyoshi; Hanada, Kenji

2015-01-01

A new method that enables us to synthesize ultrananocrystalline diamond (UNCD) in powder is proposed. Highly energetic carbon species ejected from a graphite cathode of a coaxial arc plasma gun were provided on a quartz plate at a high density by repeated arc discharge in a compact vacuum chamber, and resultant films automatically peeled from the plate were aggregated and powdered. The grain size was easily controlled from 2.4 to 15.0 nm by changing the arc discharge energy. It was experimentally demonstrated that the proposed method is a new and promising method that enables us to synthesize UNCD in powder easily and controllably. (author)

Comparative study about hydrogen sorption in sponge and powder titanium

International Nuclear Information System (INIS)

Vasut, Felicia; Preda, Anisoara; Zamfirache, Marius; Ducu, Catalin; Malinovschi, Viorel

2005-01-01

Currently, hydrogen may be stored as a compressed gas or a cryogenic liquid. Neither method appears to be practical for many applications in which hydrogen use would otherwise be attractive. For example, gaseous storage of stationary fuel is not feasible because of the large volume or weight of the storage vessels. Liquid hydrogen could be use extensively but the liquefaction process is relatively expensive. The hydrogen can be stored for a long term with a high separation factor, as a solid metal hydride. Using hydride-forming metals and intermetallic compounds, for example, recovery, purification and storage of heavy isotopes in tritium containing system, can solve many problems arising in the nuclear-fuel cycle. The paper presents a comparative study about hydrogen sorption on two titanium structures: powder and sponge. Also, it is presented the characterization, by X-Ray diffraction, of two structures, before and after sorption process. From our results, one can conclude that sorption method is efficient for both samples. Kinetic curves indicates that sorption rate for titanium powder is lower than for sponge titanium. This is the effect of reaction surface, which is larger for powder titanium. Sorption capacity for hydrogen is lower in powder titanium for identical experimental conditions. The difference between storage capacities could be explained by activation temperature, which was lower for titanium powder than for sponge. (authors)

Measurement of residual stress in textured Al alloy by neutron diffraction method

International Nuclear Information System (INIS)

Okido, S.; Hayashi, M.; Tanaka, K.; Akiniwa, Y.; Minakawa, N.; Morii, Y.

1999-01-01

Residual stress generated in a shrunken aluminum alloy specimen, which was prepared for the round robin test conducted by VAMAS (Versailles Project on Advanced Materials and Standards) TWA-20 organized for the purpose of standardizing residual stress measurement methods, was evaluated by a neutron diffraction method. The main purpose of the round robin test was to assess the reproducibility of data obtained with the measurement facilities of the participants. The general standard of the Residual Stress Analyzer (RESA) constructed in the Japan Atomic Energy Research Institute was verified from the measured residual strains, which were equivalent to the values calculated by FEM and values measured by the research facilities in North America. Residual stress was calculated from residual strain in three perpendicular directions. The diffraction intensities were dependent on measurement directions since the prepared specimen possessed texture. Diffraction profiles in directions having a weak diffraction intensity caused an inaccurate evaluation of the residual stress. To solve this problem, a new method for evaluating residual stress with respect to diffraction plane dependency of the elastic constant was applied. The diffraction plane giving the highest intensity among 110, 200, and 220 diffraction was used to evaluate the residual strain in each of three directions. The residual strain obtained on the used diffraction plane was converted to the equivalent strain for the defined diffraction plane using the ratio of elastic constants of these two planes. The developed evaluation method achieved highly accurate measurement and remarkable efficiency in the measurement process. (author)

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)

XRD and neutron diffraction analyses of heat treated U-Mo/Al dispersion fuel

Energy Technology Data Exchange (ETDEWEB)

Nam, Ji Min; Kim, Woo Jeong; Ryu, Ho Jin; Lee, Kyu Hong; Park, Jong Man [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2012-10-15

High density U Mo alloys are regarded as promising candidates for advanced research reactor fuel because they have shown stable irradiation performance when compared to other uranium alloys and compounds. However, interaction layer formation between the U Mo alloys and Al matrix degrades the irradiation performance of U Mo dispersion fuel. Therefore, addition of Ti in U Mo alloys, addition of Si in Al matrix and silicide or nitride coating on the surface of U Mo particles have been proposed in order to inhibit the interaction layer growth. In order to analyze the mechanisms of interaction layer growth inhibition by adding Ti in U Mo alloys or Si in Al matrix, accurate phase characterization of the interaction layers is required. While previous studies using X ray diffraction have been reported, laboratory X ray diffraction method has limitations such as low resolution and small measurement volume. Neutron diffraction method can be a more accurate analysis when compared with X ray diffraction method due to the large penetration depth of neutron. In this study, X ray diffraction and neutron diffraction experiments have been performed by using the laboratory X ray diffractometer and high resolution powder diffractometer (HRPD) of the HANARO research reactor in KAERI.

Preparation and Characterization of Nano-structured Ceramic Powders Synthesized by Emulsion Combustion Method

International Nuclear Information System (INIS)

Takatori, Kazumasa; Tani, Takao; Watanabe, Naoyoshi; Kamiya, Nobuo

1999-01-01

The emulsion combustion method (ECM), a novel powder production process, was originally developed to synthesize nano-structured metal-oxide powders. Metal ions in the aqueous droplets were rapidly oxidized by the combustion of the surrounding flammable liquid. The ECM achieved a small reaction field and a short reaction period to fabricate the submicron-sized hollow ceramic particles with extremely thin wall and chemically homogeneous ceramic powder. Alumina, zirconia, zirconia-ceria solid solutions and barium titanate were synthesized by the ECM process. Alumina and zirconia powders were characterized to be metastable in crystalline phase and hollow structure. The wall thickness of alumina was about 10 nm. The zirconia-ceria powders were found to be single-phase solid solutions for a wide composition range. These powders were characterized as equiaxed-shape, submicron-sized chemically homogeneous materials. The powder formation mechanism was investigated through the synthesis of barium titanate powder with different metal sources

Influence of Homogenization and Micro/Nano Source of Starting Powders on Format Ion of the Single YAP Phase

Directory of Open Access Journals (Sweden)

Michalik D.

2016-12-01

Full Text Available Manufacturing high purity polycrystalline YAlO3 (YAP ceramics could replace monocrystalline YAP thus recently it is an interesting task for low cost producers of scintillators. The paper presents influence of different source of initial oxide powders (micro/nano powders of Y2O3 and Al2O3 and the method of their homogenization on the formation of a YAP phase. The solid state reaction method was used to prepare YAP powder or ceramic pellets. After preheating, all samples in the form of powders and pellets were heat-treated in the temperature range of 1050-1650 °C. DTA method was applied for examination of the phase crystallization in the tested system. X-ray diffraction method (XRD was used for characterization of the phase composition. X-ray microanalysis (EDS was used to control homogeneity in the small areas. Morphology of the resultant samples are presented on SEM pictures. The results show a significant influence of the starting powders on the homogeneity, purity and temperature of formation of the main phase.

Studies of deformation-induced texture development in sheet materials using diffraction techniques

International Nuclear Information System (INIS)

Banovic, S.W.; Vaudin, M.D.; Gnaeupel-Herold, T.H.; Saylor, D.M.; Rodbell, K.P

2004-01-01

Crystallographic texture measurements were made on a series of rolled aluminum sheet specimens deformed in equi-biaxial tension up to a strain level of 0.11. The measurement techniques used were neutron diffraction with a 4-circle goniometer, electron backscatter diffraction, conventional powder X-ray diffraction (XRD), and XRD using an area detector. Results indicated a complex texture orientation distribution function which altered in response to the applied plastic deformation. Increased deformation caused the {1 1 0} planes, to align parallel to the plane of the sheet. The different techniques produced results that were very consistent with each other. The advantages and disadvantages of the various methods are discussed, with particular consideration of the time taken for each method, the range of orientation space accessible, the density of data that can be obtained, and the statistical significance of each data set with respect to rolled sheet product

Evaluation of gamma prime volume fractions and lattice misfits in a nickel base superalloy using the external standard X-ray diffraction method

Energy Technology Data Exchange (ETDEWEB)

Tiley, J., E-mail: jaimie.tiley@wpafb.af.mil [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Viswanathan, G.B. [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Hwang, J.Y. [Materials Engineering Department, University of North Texas, Denton, TX (United States); Shiveley, A. [Air Force Research Laboratory, Materials and Manufacturing Directorate, WPAFB, OH (United States); Banerjee, R. [Materials Engineering Department, University of North Texas, Denton, TX (United States)

2010-11-25

The unconstrained lattice parameters and volume fractions of {gamma}' for a low misfit nickel based superalloy were evaluated using X-ray diffraction techniques. Extraction techniques were used to provide unconstrained {gamma}' powders for both water quenched and slow cooled samples that were aged at 760 deg. C for 0, 25, 50, 100, and 200 h. The external standard method was used to determine the volume fraction for the unaged water quenched sample and the slow cooled sample aged for 200 h. These two extremes in processing conditions provided an increase in the total volume fraction of {gamma}'.

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)

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)

Evaluation of drug-carrier interactions in quaternary powder mixtures containing perindopril tert-butylamine and indapamide.

Science.gov (United States)

Voelkel, Adam; Milczewska, Kasylda; Teżyk, Michał; Milanowski, Bartłomiej; Lulek, Janina

2016-04-30

Interactions occurring between components in the quaternary powder mixtures consisting of perindopril tert-butylamine, indapamide (active pharmaceutical ingredients), carrier substance and hydrophobic colloidal silica were examined. Two grades of lactose monohydrate: Spherolac(®) 100 and Granulac(®) 200 and two types of microcrystalline cellulose: M101D+ and Vivapur(®) 102 were used as carriers. We determined the size distribution (laser diffraction method), morphology (scanning electron microscopy) and a specific surface area of the powder particles (by nitrogen adsorption-desorption). For the determination of the surface energy of powder mixtures the method of inverse gas chromatography was applied. Investigated mixtures were characterized by surface parameters (dispersive component of surface energy, specific interactions parameters, specific surface area), work of adhesion and cohesion as well as Flory-Huggins parameter χ23('). Results obtained for all quaternary powder mixtures indicate existence of interactions between components. The strongest interactions occur for both blends with different types of microcrystalline cellulose (PM-1 and PM-4) while much weaker ones for powder mixtures with various types of lactose (PM-2 and PM-3). Published by Elsevier B.V.

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)

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.)

Method and apparatus for the production of metal oxide powder

Science.gov (United States)

Harris, M.T.; Scott, T.C.; Byers, C.H.

1992-06-16

The present invention provides a method for preparing metal oxide powder. A first solution, which is substantially organic, is prepared. A second solution, which is an aqueous solution substantially immiscible in the first solution, is prepared and delivered as drops to the first solution. The drops of the second solution are atomized by a pulsed electric field forming micro-drops of the second solution. Reagents in the first solution diffuse into and react with reactants in the micro-drops of the second solution forming metal hydroxide or oxalate particles. The metal hydroxide or metal oxalate particles are then recovered and dried to produce the metal oxide powder. An apparatus for preparing a metal oxide powder is also disclosed. 2 figs.

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).

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.

The influence of direct compression powder blend transfer method from the container to the tablet press on product critical quality attributes: a case study.

Science.gov (United States)

Teżyk, Michał; Jakubowska, Emilia; Milczewska, Kasylda; Milanowski, Bartłomiej; Voelkel, Adam; Lulek, Janina

2017-06-01

The aim of this article is to compare the gravitational powder blend loading method to the tablet press and manual loading in terms of their influence on tablets' critical quality attributes (CQA). The results of the study can be of practical relevance to the pharmaceutical industry in the area of direct compression of low-dose formulations, which could be prone to content uniformity (CU) issues. In the preliminary study, particle size distribution (PSD) and surface energy of raw materials were determined using laser diffraction method and inverse gas chromatography, respectively. For trials purpose, a formulation containing two pharmaceutical ingredients (APIs) was used. Tablet samples were collected during the compression progress to analyze their CQAs, namely assay and CU. Results obtained during trials indicate that tested direct compression powder blend is sensitive to applied powder handling method. Mild increase in both APIs content was observed during manual scooping. Gravitational approach (based on discharge into the drum) resulted in a decrease in CU, which is connected to a more pronounced assay increase at the end of tableting than in the case of manual loading. The correct design of blend transfer over single unit processes is an important issue and should be investigated during the development phase since it may influence the final product CQAs. The manual scooping method, although simplistic, can be a temporary solution to improve the results of API's content and uniformity when compared to industrial gravitational transfer.

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.

A drop penetration method to measure powder blend wettability.

Science.gov (United States)

Wang, Yifan; Liu, Zhanjie; Muzzio, Fernando; Drazer, German; Callegari, Gerardo

2018-03-01

Water wettability of pharmaceutical blends affects important quality attributes of final products. We investigate the wetting properties of a pharmaceutical blend lubricated with Magnesium Stearate (MgSt) as a function of the mechanical shear strain applied to the blend. We measure the penetration dynamics of sessile drops deposited on slightly compressed powder beds. We consider a blend composed of 9% Acetaminophen 90% Lactose and 1% MgSt by weight. Comparing the penetration time of water and a reference liquid Polydimethylsiloxane (silicon oil) we obtain an effective cosine of the contact angle with water, based on a recently developed drop penetration method. We repeat the experiments for blends exposed to increasing levels of shear strain and demonstrate a significant decrease in water wettability (decrease in the cosine of the contact angle). The results are consistent with the development of a hydrophobic film coating the powder particles as a result of the increased shear strain. Finally, we show that, as expected dissolution times increase with the level of shear strain. Therefore, the proposed drop penetration method could be used to directly assess the state of lubrication of a pharmaceutical blend and act as a quality control on powder blend attributes before the blend is tableted. Copyright © 2017 Elsevier B.V. All rights reserved.

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

International Nuclear Information System (INIS)

Freyer, Benjamin

2013-01-01

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

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

Synthesis of Uranium nitride powders using metal uranium powders

International Nuclear Information System (INIS)

Yang, Jae Ho; Kim, Dong Joo; Oh, Jang Soo; Rhee, Young Woo; Kim, Jong Hun; Kim, Keon Sik

2012-01-01

Uranium nitride (UN) is a potential fuel material for advanced nuclear reactors because of their high fuel density, high thermal conductivity, high melting temperature, and considerable breeding capability in LWRs. Uranium nitride powders can be fabricated by a carbothermic reduction of the oxide powders, or the nitriding of metal uranium. The carbothermic reduction has an advantage in the production of fine powders. However it has many drawbacks such as an inevitable engagement of impurities, process burden, and difficulties in reusing of expensive N 15 gas. Manufacturing concerns issued in the carbothermic reduction process can be solved by changing the starting materials from oxide powder to metals. However, in nitriding process of metal, it is difficult to obtain fine nitride powders because metal uranium is usually fabricated in the form of bulk ingots. In this study, a simple reaction method was tested to fabricate uranium nitride powders directly from uranium metal powders. We fabricated uranium metal spherical powder and flake using a centrifugal atomization method. The nitride powders were obtained by thermal treating those metal particles under nitrogen containing gas. We investigated the phase and morphology evolutions of powders during the nitriding process. A phase analysis of nitride powders was also a part of the present work

Fundamental parameters approach applied to focal construct geometry for X-ray diffraction

International Nuclear Information System (INIS)

Rogers, K.; Evans, P.; Prokopiou, D.; Dicken, A.; Godber, S.; Rogers, J.

2012-01-01

A novel geometry for the acquisition of powder X-ray diffraction data, referred to as focal construct geometry (FCG), is presented. Diffraction data obtained by FCG have been shown to possess significantly enhanced intensity due to the hollow tube beam arrangement utilized. In contrast to conventional diffraction, the detector is translated to collect images along a primary axis and record the location of Bragg maxima. These high intensity condensation foci are unique to FCG and appear due to the convergence of Debye cones at single points on the primary axis. This work focuses on a two dimensional, fundamental parameter's approach to simulate experimental data and subsequently aid with interpretation. This convolution method is shown to favorably reproduce the experimental diffractograms and can also accommodate preferred orientation effects in some circumstances.

The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

DEFF Research Database (Denmark)

Wragg, David S.; Johnsen, Rune; Norby, Poul

2010-01-01

The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...

Synchrotron diffraction studies of TiC/FeTi cermets obtained by SHS

International Nuclear Information System (INIS)

Contreras, L.; Turrillas, X.; Mas-Guindal, M.J.; Vaughan, G.B.M.; Kvick, A.; Rodriguez, M.A.

2005-01-01

TiC/FeTi composites have been obtained in situ by Self-propagating High-temperature Synthesis (SHS) of an intimate mixture of compacted powders of elemental carbon, titanium and iron. The reaction has been followed in real time by X-ray diffraction at the ESRF. The mechanism of the reaction is discussed in terms of the formation of a liquid phase corresponding to the eutectic of the Fe/Ti system prior to the TiC synthesis. Temperatures of reaction have been estimated by correlating thermal expansion coefficients with diffraction peaks shifts. The microstructures obtained by this method, suitable for cutting tools and wear resistant applications, are presented

Profiling pleural effusion cells by a diffraction imaging method

Science.gov (United States)

Al-Qaysi, Safaa; Hong, Heng; Wen, Yuhua; Lu, Jun Q.; Feng, Yuanming; Hu, Xin-Hua

2018-02-01

Assay of cells in pleural effusion (PE) is an important means of disease diagnosis. Conventional cytology of effusion samples, however, has low sensitivity and depends heavily on the expertise of cytopathologists. We applied a polarization diffraction imaging flow cytometry method on effusion cells to investigate their features. Diffraction imaging of the PE cell samples has been performed on 6000 to 12000 cells for each effusion cell sample of three patients. After prescreening to remove images by cellular debris and aggregated non-cellular particles, the image textures were extracted with a gray level co-occurrence matrix (GLCM) algorithm. The distribution of the imaged cells in the GLCM parameters space was analyzed by a Gaussian Mixture Model (GMM) to determine the number of clusters among the effusion cells. These results yield insight on textural features of diffraction images and related cellular morphology in effusion samples and can be used toward the development of a label-free method for effusion cells assay.

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.

Evaluation of fine ceramics raw powders with particle size analyzers having different measuring principle and its problem

International Nuclear Information System (INIS)

Hayakawa, Osamu; Nakahira, Kenji; Tsubaki, Junichiro.

1995-01-01

Many kinds of analyzers based on various principles have been developed for measuring particle size distribution of fine ceramics powders. But the reproducibility of the results, interchangeability of the models, reliability of the ends of the measured distribution have not been investigated for each principle. In this paper, these important points for particle size analysis were clarified by measuring raw material powders of fine ceramics. (1) in the case of laser diffraction and scattering method, the reproducibility in the same model is good, however, interchangeability of the different models is not so good, especially at the ends of the distribution. Submicron powders having high refractive index show such a tendency remarkably. (2) the photo sedimentation method has some problems to be conquered, especially in measuring submicron powders having high refractive index or flaky shape particles. The reproducibility of X-ray sedimentation method is much better than that of photo sedimentation. (3) the light obscuration and electrical sensing zone methods, show good reproducibility, however, sometime bad interchangeability is affected by calibration and so on. (author)

Enhanced method of magnetic powder alignment for production of PLP Nd-Fe-B magnets

International Nuclear Information System (INIS)

Popov, A.G.; Golovnia, O.A.; Protasov, A.V.

2017-01-01

It is demonstrated how the high degree of powder alignment in PLP magnets can be achieved by loading the powder into a container placed in a magnetic field of moderate strength. The strip-cast alloy with a composition of 30.00 Nd, 1.95 Dy, 66.42 Fe, 0.99 B, 0.54 Co, 0.1 Ga (wt%) was subjected to hydrogen decrepitation and then milled in a vibratory mill in toluene to an average particle size of 2.9 µm determined by the FSSS method. The powder was compacted in the magnetic field of 0.2 – 1.2 T to the filling density 2.6 – 3.2×10 3 kg/m 3 . It is shown that loading the powder into a container placed in a magnetic field enhances the degree of powder alignment in sintered Nd-Fe-B magnets produced from non-pressed powder. At the filling density less than 3.2×10 3 kg/m 3 , the density of magnets is high but insufficient, because of the formation of magnetostatic chains of particles, which impedes the powder compaction. The simulation by the discrete-element method qualitatively proves that the magnetostatic interaction of the chains of particles that are formed in the course of loading in the magnetic field stimulates a decrease in the density of the sintered magnets and its non-uniform distribution over the sample. As a result of the optimization of the parameters of the alignment and compaction of the powder loaded in a magnetic field, PLP magnets with B r ≥1.34 T, H c ≥950 kA/m, (BH) max ≥340 kJ/m 3 , and the degree of alignment exceeding 96% were produced. - Highlights: • The pressless process (PLP) in magnet production is studied. • A new method of the loading of powder in an applied DC magnetic field is suggested. • The method allows achieving higher degree of alignment in moderate magnetic field. • Density of sintered magnets is studied experimentally and via DEM simulation. • Low density is caused by the formation of magnetostatic chains of powder particles.

Enhanced method of magnetic powder alignment for production of PLP Nd-Fe-B magnets

Energy Technology Data Exchange (ETDEWEB)

Popov, A.G. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, Str. S. Kovalevskoy, 18, 620137 Ekaterinburg (Russian Federation); Institute of Natural Sciences and Mathematics, Ural Federal University, Av. Mira, 19, 620002 Ekaterinburg (Russian Federation); Golovnia, O.A., E-mail: golovnya@imp.uran.ru [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, Str. S. Kovalevskoy, 18, 620137 Ekaterinburg (Russian Federation); Institute of Natural Sciences and Mathematics, Ural Federal University, Av. Mira, 19, 620002 Ekaterinburg (Russian Federation); Protasov, A.V. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, Str. S. Kovalevskoy, 18, 620137 Ekaterinburg (Russian Federation); Institute of Natural Sciences and Mathematics, Ural Federal University, Av. Mira, 19, 620002 Ekaterinburg (Russian Federation)

2017-04-15

It is demonstrated how the high degree of powder alignment in PLP magnets can be achieved by loading the powder into a container placed in a magnetic field of moderate strength. The strip-cast alloy with a composition of 30.00 Nd, 1.95 Dy, 66.42 Fe, 0.99 B, 0.54 Co, 0.1 Ga (wt%) was subjected to hydrogen decrepitation and then milled in a vibratory mill in toluene to an average particle size of 2.9 µm determined by the FSSS method. The powder was compacted in the magnetic field of 0.2 – 1.2 T to the filling density 2.6 – 3.2×10{sup 3} kg/m{sup 3}. It is shown that loading the powder into a container placed in a magnetic field enhances the degree of powder alignment in sintered Nd-Fe-B magnets produced from non-pressed powder. At the filling density less than 3.2×10{sup 3} kg/m{sup 3}, the density of magnets is high but insufficient, because of the formation of magnetostatic chains of particles, which impedes the powder compaction. The simulation by the discrete-element method qualitatively proves that the magnetostatic interaction of the chains of particles that are formed in the course of loading in the magnetic field stimulates a decrease in the density of the sintered magnets and its non-uniform distribution over the sample. As a result of the optimization of the parameters of the alignment and compaction of the powder loaded in a magnetic field, PLP magnets with B{sub r} ≥1.34 T, H{sub c} ≥950 kA/m, (BH){sub max} ≥340 kJ/m{sup 3}, and the degree of alignment exceeding 96% were produced. - Highlights: • The pressless process (PLP) in magnet production is studied. • A new method of the loading of powder in an applied DC magnetic field is suggested. • The method allows achieving higher degree of alignment in moderate magnetic field. • Density of sintered magnets is studied experimentally and via DEM simulation. • Low density is caused by the formation of magnetostatic chains of powder particles.

Nanocrystalline AL2 O2 powders produced by laser induced gas phase reactions

International Nuclear Information System (INIS)

Borsella, E.; Botti, S.; Martelli, S.; Zappa, G.; Giorgi, R.; Turt, S.

1993-01-01

Nanocrystalline Al 2 O 3 powders were successfully synthesized by a CO 2 laser-driven gas-phase reaction involving trimethylaluminium (Al(CH 3 ) 3 ) and nitrous-oxide (N 2 O). Ethylene (C 2 H 4 ) was added as gas sensitizer. The as-synthesized powder particles showed a considerable carbon contamination and an amorphous-like structure. After thermal treatment at 1200-1400 degrees C, the powder was transformed to hexagonal a-Al 2 O 3 with very low carbon contamination as confirmed by X-ray diffraction, X-ray photo-electron spectroscopy and chemical analysis. The calcinated powders resulted to be spherical single crystal nanoparticles with a mean size of 15-20 nm, as determined by X-ray diffraction, electron microscopy and B.E.T. specific surface measurements. The laser synthesized Al 2 O 3 particles are well suited dispersoids for intermetallic alloy technology

A method for preparing a sintered glass powder for manufacturing microspheres

International Nuclear Information System (INIS)

Budrick, R.G.; King, F.T.; Nolen, R.L. Jr.; Solomon, D.E.

1975-01-01

The invention relates to the manufacture of sintered glass-powder. It relates to a method comprising the step of forming a vitreous gel so that it contains an occluded substance adapted to expand when heated, said gel being subsequently dried, then crushed and sorted prior to being washed and dried again. Application to the manufacture of sintered glass-powder for forming microspheres adapted to contain a thermonuclear fuel [fr

Potassium Disorder in the Defect Pyrochlore KSbTeO6: A Neutron Diffraction Study

Directory of Open Access Journals (Sweden)

José Antonio Alonso

2017-01-01

Full Text Available KSbTeO6 defect pyrochlore has been prepared from K2C2O4, Sb2O3, and 15% excess TeO2 by solid-state reaction at 850 °C. Direct methods implemented in the software EXPO2013 allowed establishing the basic structural framework. This was followed by a combined Rietveld refinement from X-ray powder diffraction (XRD and neutron powder diffraction (NPD data, which unveiled additional structural features. KSbTeO6 is cubic, a = 10.1226(7 Å, space group F d 3 ¯ m , Z = 8 and it is made of a mainly covalent framework of corner-sharing (Sb,TeO6 octahedra, with weakly bonded K+ ions located within large cages. The large K-O distances, 3.05(3–3.07(3 Å, and quite large anisotropic atomic displacement parameters account for the easiness of K+ exchange for other cations of technological importance.

Effect of surface coating with magnesium stearate via mechanical dry powder coating approach on the aerosol performance of micronized drug powders from dry powder inhalers.

Science.gov (United States)

Zhou, Qi Tony; Qu, Li; Gengenbach, Thomas; Larson, Ian; Stewart, Peter J; Morton, David A V

2013-03-01

The objective of this study was to investigate the effect of particle surface coating with magnesium stearate on the aerosolization of dry powder inhaler formulations. Micronized salbutamol sulphate as a model drug was dry coated with magnesium stearate using a mechanofusion technique. The coating quality was characterized by X-ray photoelectron spectroscopy. Powder bulk and flow properties were assessed by bulk densities and shear cell measurements. The aerosol performance was studied by laser diffraction and supported by a twin-stage impinger. High degrees of coating coverage were achieved after mechanofusion, as measured by X-ray photoelectron spectroscopy. Concomitant significant increases occurred in powder bulk densities and in aerosol performance after coating. The apparent optimum performance corresponded with using 2% w/w magnesium stearate. In contrast, traditional blending resulted in no significant changes in either bulk or aerosolization behaviour compared to the untreated sample. It is believed that conventional low-shear blending provides insufficient energy levels to expose host micronized particle surfaces from agglomerates and to distribute guest coating material effectively for coating. A simple ultra-high-shear mechanical dry powder coating step was shown as highly effective in producing ultra-thin coatings on micronized powders and to substantially improve the powder aerosolization efficiency.

Phase quantification of mullite-zirconia and zircon commercial powders using PAC and XRD techniques

Energy Technology Data Exchange (ETDEWEB)

Rendtorff, Nicolas M.; Conconi, Maria S.; Aglietti, Esteban F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC: CONICET-CIC) (Argentina); Chain, Cecilia Y.; Pasquevich, Alberto F. [Universidad Nacional de La Plata, Departamento de Fisica, IFLP, Facultad de Ciencias Exactas (Argentina); Rivas, Patricia C. [CONICET (Argentina); Martinez, Jorge A., E-mail: toto@fisica.unlp.edu.ar; Caracoche, Maria C. [Universidad Nacional de La Plata, Departamento de Fisica, IFLP, Facultad de Ciencias Exactas (Argentina)

2010-06-15

The short range technique of the Perturbed Angular Correlation (PAC) and x-ray diffraction (Rietveld) methods have been employed to determine the phase content in commercial mullite-zirconia and zircon raw materials that are ordinarily used to produce ceramic materials. The PAC technique, which probes zirconium-containing compounds at nanoscopic level, showed that zircon contains crystalline ZrSiO{sub 4} and an important amount of a structurally distorted zircon, which is also observed accompanying monoclinic zirconia in mullite-zirconia. This particular zircon phase was not detected by the long range x-ray diffraction-Rietveld technique. After an annealing treatment, important changes in crystalline contents of the powders allow confirming, by the x-ray diffraction-Rietveld method, the preexistence of this particular zircon phase. This fact must be taken into account when preparing multicomposites based on the present raw materials.

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...

Chemical compositions of spherical titanium powders prepared by RF induction plasma

International Nuclear Information System (INIS)

Gu Zhongtao; Jin Yuping; Ye Gaoying

2012-01-01

Spherical titanium powders were prepared by RF induction plasma technology. The particle size is essentially un- changed, while the particle size distribution is relatively narrow after spheroidization processing. X-ray diffraction (XRD) random testing of the spherical titanium powders shows no structure and phase changes. The content of O, H, N and C decreases, while the content of Ti increases slightly. It indicates that spheroidization with RF plasma can enhance powder purity. (authors)

Gas-Phase Combustion Synthesis of Aluminum Nitride Powder

Science.gov (United States)

Axelbaum, R. L.; Lottes, C. R.; Huertas, J. I.; Rosen, L. J.

1996-01-01

Due to its combined properties of high electrical resistivity and high thermal conductivity aluminum nitride (AlN) is a highly desirable material for electronics applications. Methods are being sought for synthesis of unagglomerated, nanometer-sized powders of this material, prepared in such a way that they can be consolidated into solid compacts having minimal oxygen content. A procedure for synthesizing these powders through gas-phase combustion is described. This novel approach involves reacting AlCl3, NH3, and Na vapors. Equilibrium thermodynamic calculations show that 100% yields can be obtained for these reactants with the products being AlN, NaCl, and H2. The NaCl by-product is used to coat the AlN particles in situ. The coating allows for control of AlN agglomeration and protects the powders from hydrolysis during post-flame handling. On the basis of thermodynamic and kinetic considerations, two different approaches were employed to produce the powder, in co-flow diffusion flame configurations. In the first approach, the three reactants were supplied in separate streams. In the second, the AlCl3 and NH3 were premixed with HCl and then reacted with Na vapor. X-ray diffraction (XRD) spectra of as-produced powders show only NaCl for the first case and NaCl and AlN for the second. After annealing at 775 C tinder dynamic vacuum, the salt was removed and XRD spectra of powders from both approaches show only AlN. Aluminum metal was also produced in the co-flow flame by reacting AlCl3 with Na. XRD spectra of as-produced powders show the products to be only NaCl and elemental aluminum.

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

Characterization of nano-powder grown ultra-thin film p-CuO/n-Si hetero-junctions by employing vapour-liquid-solid method for photovoltaic applications

Energy Technology Data Exchange (ETDEWEB)

Sultana, Jenifar; Das, Anindita [Centre for Research in Nanoscience and Nanotechnology (CRNN), Kolkata 700098 (India); Das, Avishek [Department of Electronic Science, University of Calcutta, Kolkata 700009 (India); Saha, Nayan Ranjan [Department of Polymer Science and Technology, University of Calcutta, Kolkata 700009 (India); Karmakar, Anupam [Department of Electronic Science, University of Calcutta, Kolkata 700009 (India); Chattopadhyay, Sanatan, E-mail: scelc@caluniv.ac.in [Department of Electronic Science, University of Calcutta, Kolkata 700009 (India)

2016-08-01

In this work, the CuO nano-powder has been synthesized by employing chemical bath deposition technique for its subsequent use to grow ultrathin film (20 nm) of p-CuO on n-Si substrate for the fabrication of p-CuO/n-Si hetero-junction diodes. The thin CuO film has been grown by employing vapour-liquid-solid method. The crystalline structure and chemical phase of the film are characterized by employing field-emission scanning electron microscopy and X-ray diffraction studies. Chemical stoichiometry of the film has been confirmed by using energy dispersive X-ray spectroscopy. The potential for photovoltaic applications of such films is investigated by measuring the junction current-voltage characteristics and by extracting the relevant parameters such as open circuit photo-generated voltage, short circuit current density, fill-factor and energy conversion efficiency. - Highlights: • Synthesis of CuO nano-powder by CBD method • Growth of ultra-thin film of CuO by employing VLS method for the first time • Physical and electrical characterization of such films for photovoltaic applications • Estimation of energy conversion efficiency of the p-CuO/n-Si p-n junction solar cell.

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

Science.gov (United States)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

TOF neutron diffraction study of archaeological ceramics

International Nuclear Information System (INIS)

Kockelmann, W.; Kirfel, A.

1999-01-01

Complete text of publication follows. The time-of flight (TOF) neutron diffractometer ROTAX [1] at ISIS has been used for identification and quantitative phase analysis of archaeological pottery. Neutron diffraction yields mineral phase fractions which, in parallel with information obtained from other archaeometric examination techniques, can provide a fingerprint that can be used to identify provenance and reconstruct methods of manufacturing of an archaeological ceramic product. Phase fractions obtained from a 13th century Rhenish stoneware jar compare well with those obtained from a powder sample prepared from the same fragment. This indicates that reliable results can be obtained by illuminating a large piece or even an intact ceramic object making TOF neutron diffraction a truly non-destructive examination technique. In comparison to X-ray diffraction, information from the bulk sample rather than from surface regions is obtained. ROTAX allows for a simple experimental set-up, free of sample movements. Programmes of archaeological study on ROTAX involve Russian samples (Upper-Volga culture, 5000-2000 BC), Greek pottery, (Agora/Athens, 500-300 BC), and medieval German earthenware and stoneware ceramics (Siegburg waster heap, 13-15th century). (author)

Neutron diffraction technique as a method for material studies

International Nuclear Information System (INIS)

Belhorma, B.; Labrim, H.; Gandou, Z.

2010-01-01

The Morocco's first Nuclear Research has been constructed in CNESTEN. The reactor divergence has been tested, and the nominal power of 2MW was successfully achieved. The reactor has 4 beam ports two of them are projected for neutron scattering. Such technique allows studying the crystallographic and magnetic structures of materials using the thermal neutrons produced in the reactor. the powder diffractometer has been designed. Component reception and installation procedures are in progress. The second experiment consists on small angle neutron scattering that allows the study of soft matter and polymers in the range of 1-50 nm. The third technique that can complete the two previous is the 4-circle neutron spectrometry which is designed mainly to study structural properties of the mono-crystalline material and texture.This technique is complementary to the X-ray diffraction already available in CNESTEN. Some applications of this technique are: --to determine the crystallographic and magnetic structure of polycrystalline materials.-- to study the texture in metals and alloys.-- to perform holography measurement

Direct methods for surface X-ray diffraction

International Nuclear Information System (INIS)

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

2000-01-01

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

ALADIN - Advanced Laue Diffraction Instruments using Neutrons

International Nuclear Information System (INIS)

Lemee-Cailleau, M.H.; Ouladdiaf, B.; McIntyre, G.J.

2011-01-01

Laue diffraction techniques have proven to be very attractive to a broad user community interested in obtaining detailed structural information on very small single-crystal samples or needing data collection speeds comparable to those available with the powder diffraction technique. However our experience has clearly demonstrated the negative effect of up-stream monochromatic instruments on the quality of Laue data. In order to obtain Laue diffraction data with a statistical accuracy similar to that achieved on a monochromatic instrument (neutron or X-rays), the project ALADIN (for Advanced Laue Diffraction Instruments using Neutrons) aims to: -) construct a Laue-dedicated thermal neutron guide, with m=2 super-mirror coating, providing access to the desirable wavelength bandwidth; -) installation of one of the ILL Laue diffractometers (VIVALDI or CYCLOPS) on this new guide. (authors)

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

Application of the Rietveld method in powders of strontium-doped lanthanum manganite calcined in different temperatures

International Nuclear Information System (INIS)

Chiba, R.; Vargas, R.A.; Martinez, L.G.; Andreoli, M.; Seo, E.S.M.

2010-01-01

The strontium-doped lanthanum manganite (LSM) is a ceramic material used as cathode in device called High Temperature Solid Oxide Fuel Cell. In this work, the LSM was synthesized by the citrate technique with the objective to get powders without the formation of secondary phases, such as lanthanum oxide and the lanthanum hydroxide, harmful for the functional performance of the device. The definitive calcination temperatures had been 700, 900 and 1100 deg C, due the decomposition of the polymeric precursors to present stabilization from 480 deg C. The analysis by X-ray diffraction of the calcined powders in different temperatures shows the formation only of phase LSM of hexagonal crystalline structure, type pseudo-perovskite. Using the refinement of Rietveld was determined the parameters and volumes of unity cells, atomic positions and occupations. These results confirm that the chemical compositions obtained are similar to the nominal. (author)

Yttrium orthoferrite powder obtained by the mechanochemical synthesis

Directory of Open Access Journals (Sweden)

Lazarević Zorica Ž.

2017-01-01

Full Text Available Yttrium orthoferrite (YFeO3 powder was prepared by a mechanochemical synthesis from a mixture of Y2O3 and α-Fe2O3 powders in a planetary ball mill for 2.5 h. The obtained YFeO3 powder sample was characterized by X-ray diffraction (XRD, Raman and infrared spectroscopy. The average crystallite size calculated by the Scherrer equation was 12 nm. The Mössbauer spectroscopy at room temperature confirms the superparamagnetic character of YFeO3 orthoferrite sample. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. III 45003, Grant no. III 45015, Grant no. III 45018

An efficient and accurate method for calculating nonlinear diffraction beam fields

Energy Technology Data Exchange (ETDEWEB)

Jeong, Hyun Jo; Cho, Sung Jong; Nam, Ki Woong; Lee, Jang Hyun [Division of Mechanical and Automotive Engineering, Wonkwang University, Iksan (Korea, Republic of)

2016-04-15

This study develops an efficient and accurate method for calculating nonlinear diffraction beam fields propagating in fluids or solids. The Westervelt equation and quasilinear theory, from which the integral solutions for the fundamental and second harmonics can be obtained, are first considered. A computationally efficient method is then developed using a multi-Gaussian beam (MGB) model that easily separates the diffraction effects from the plane wave solution. The MGB models provide accurate beam fields when compared with the integral solutions for a number of transmitter-receiver geometries. These models can also serve as fast, powerful modeling tools for many nonlinear acoustics applications, especially in making diffraction corrections for the nonlinearity parameter determination, because of their computational efficiency and accuracy.

Mechanochemical synthesis of ultrafine Ce2S3 powder

International Nuclear Information System (INIS)

Tsuzuki, T.; McCormick, P.G.

1998-01-01

Full text: Rare earth sulphides have been receiving an increasing attraction for various applications including infrared window materials and magneto-optical devices. In particular, Ce 2 S 3 has been under intensive study for use as a red pigment to replace toxic cadmium sulfoselenide. The conventional method for synthesising Ce 2 S 3 is the sulphidization of the element or sesquioxide with hydrogen sulphide gas. However, the method usually requires a high-temperature process (>1000 deg C), and hence coarse particles larger than the optimal size of ∼ 2 S 3 powder by mechanochemical processing using X-ray diffraction spectroscopy, BET surface area analysis and transmission electron microscopy. Mechanical milling of the mixture of a cerium salt and an alkali/alkali-earth sulphide powders led to a solid state displacement reaction in a steady-state manner, forming Ce 2 S 3 nanoparticles in a salt by-product matrix. After a simple washing process to remove the salt by-product, ultrafine Ce 2 S 3 particles with sizes of 20 - 200 nm having an orthorhombic structure were obtained. Using a diluent and mechanically alloyed CaS nanoparticles in the starting powder, particles of only a cubic γ-Ce 2 S 3 phase with sizes of 10 - 80 nm were formed

Obtainment of TiO2 powders solar cells photo electrodes dye sensitized

International Nuclear Information System (INIS)

Forbeck, Guilherme; Folgueras, Marilena V.; Chinelatto, Adilson L.

2012-01-01

Titanium dioxide in its polymorphic anatase phase, presents interesting properties for solar cells photo electrodes dye sensitized such as the forbidden energy band, high refractive index and high constant dielectric. In this study, powders of nanometric titanium dioxide were produced with predominantly the anatase phase and high surface area. We used the sol-gel method, and titanium tetraisopropoxide as a precursor, which was hydrolyzed in nitric acid solution. The obtained powder was heated to 450 ° C, varying the time for each lot (0, 20 or 120 minutes). The powders were characterized by X-ray diffraction, atomic force microscopy and surface area analysis. For all lots nanosized crystallites predominated. It was observed that in the batch with 120min heating an increase rutile content. The TiO 2 with 20min heating showed high surface area, greater than that of TiO 2 as taken reference

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.

Influence of starting powder milling on magnetic properties of Mn-Zn ferrite

Directory of Open Access Journals (Sweden)

Miodrag M. Milutinov

2017-06-01

Full Text Available In this paper, the influence of additional sieving and milling of starting industrial Mn-Zn powders on magnetic properties was investigated. The starting powder was milled for 60 minutes, followed by sieving through 325 and 400 meshes. The starting and milled powders were used to fabricate toroid shaped samples sintered at 1200°C for 2 hours. Structural parameters of the fabricated samples were analysed by X-ray diffraction and scanning electron microscopy. Complex permeability, core loss density, and hysteresis were measured using the modified watt-meter method. The complex permeability and hysteresis loop were modelled with a new model proposed in the paper. The core loss density was modelled with the Steinmetz empirical equation. The experimental results and calculations show the significance of the additional milling and sieving process on magnetic properties of Mn-Zn ferrite in the frequency range 0.1-10MHz. These processes increase the relative permeability about 3 times and decrease the core loss 4 times by milling of the starting powder.

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.

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

NARCIS (Netherlands)

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

1994-01-01

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

Probing the structure of heterogeneous diluted materials by diffraction tomography.

Science.gov (United States)

Bleuet, Pierre; Welcomme, Eléonore; Dooryhée, Eric; Susini, Jean; Hodeau, Jean-Louis; Walter, Philippe

2008-06-01

The advent of nanosciences calls for the development of local structural probes, in particular to characterize ill-ordered or heterogeneous materials. Furthermore, because materials properties are often related to their heterogeneity and the hierarchical arrangement of their structure, different structural probes covering a wide range of scales are required. X-ray diffraction is one of the prime structural methods but suffers from a relatively poor detection limit, whereas transmission electron analysis involves destructive sample preparation. Here we show the potential of coupling pencil-beam tomography with X-ray diffraction to examine unidentified phases in nanomaterials and polycrystalline materials. The demonstration is carried out on a high-pressure pellet containing several carbon phases and on a heterogeneous powder containing chalcedony and iron pigments. The present method enables a non-invasive structural refinement with a weight sensitivity of one part per thousand. It enables the extraction of the scattering patterns of amorphous and crystalline compounds with similar atomic densities and compositions. Furthermore, such a diffraction-tomography experiment can be carried out simultaneously with X-ray fluorescence, Compton and absorption tomographies, enabling a multimodal analysis of prime importance in materials science, chemistry, geology, environmental science, medical science, palaeontology and cultural heritage.

A detailed study of the amorphisation reaction in NiMo alloys by diffraction and scattering methods

International Nuclear Information System (INIS)

Rose, P.

1995-01-01

X-ray and neutron diffraction and neutron small angle scattering (SAS) measurements have been made on NiMo specimens prepared by mechanical alloying (MA). We have extended our earlier studies and measured a new series of MA treated NiMo samples. Molybdenum scatters X-rays more strongly than nickel, but with neutrons, the reverse is the case. Analysis of the X-ray and neutron diffraction patterns together, therefore provides an accurate measurement of the consumption of both constituents in the reaction. The diffraction data on the new samples confirm that the consumption of the parent crystalline materials follows an exponential dependence with the time of MA treatment and also provides evidence of a ''delayed start'' to the reaction. This is consistent with an initial period of mixing of the constituents before the onset of (atomic) interdiffusion and amorphisation. The neutron SAS experiments have been made on Ni 47.7 Mo 52.3 MA treated specimens, which can be ''contrast-matched'' to reduce the scattering from the external surfaces of the powder grains. The new neutron SAS data confirm the presence of fractal surfaces between the alloy constituents, for samples in the early stages of the MA process. (orig.)

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

Energy Technology Data Exchange (ETDEWEB)

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

2001-07-01

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

Nonvolatile RRAM cells from polymeric composites embedding recycled SiC powders.

Science.gov (United States)

De Girolamo Del Mauro, Anna; Nenna, Giuseppe; Miscioscia, Riccardo; Freda, Cesare; Portofino, Sabrina; Galvagno, Sergio; Minarini, Carla

2014-10-21

Silicon carbide powders have been synthesized from tires utilizing a patented recycling process. Dynamic light scattering, Raman spectroscopy, SEM microscopy, and X-ray diffraction have been carried out to gather knowledge about powders and the final composite structure. The obtained powder has been proven to induce resistive switching in a PMMA polymer-based composite device. Memory effect has been detected in two-terminal devices having coplanar contacts and quantified by read-write-erase measurements in terms of level separation and persistence.

Effect of cryogenic milling on Al7075 prepared by spark plasma sintering method.

Czech Academy of Sciences Publication Activity Database

Lukáč, František; Chráska, Tomáš; Molnárová, O.; Málek, P.; Cinert, Jakub

2017-01-01

Roč. 32, S1 (2017), S221-S224 ISSN 0885-7156. [European Powder Diffraction Conference (EPDIC) /15./. Bari, 12.06.2016-15.06.2016] R&D Projects: GA ČR(CZ) GA15-15609S Institutional support: RVO:61389021 Keywords : Intermetallic precipitates * cryogenic milling * powder metallurgy * ultrafine-grained materials * Al7075 alloy Subject RIV: JG - Metallurgy OBOR OECD: Materials engineering Impact factor: 0.674, year: 2016 https://www.cambridge.org/core/journals/powder-diffraction/ article /effect-of-cryogenic-milling-on-al7075-prepared-by-spark-plasma-sintering-method/17E9F722BAFD428BA7310194FEE551C6

Chemical Reduction Synthesis of Iron Aluminum Powders

Science.gov (United States)

Zurita-Méndez, N. N.; la Torre, G. Carbajal-De; Ballesteros-Almanza, L.; Villagómez-Galindo, M.; Sánchez-Castillo, A.; Espinosa-Medina, M. A.

In this study, a chemical reduction synthesis method of iron aluminum (FeAl) nano-dimensional intermetallic powders is described. The process has two stages: a salt reduction and solvent evaporation by a heat treatment at 1100°C. The precursors of the synthesis are ferric chloride, aluminum foil chips, a mix of Toluene/THF in a 75/25 volume relationship, and concentrated hydrochloric acid as initiator of the reaction. The reaction time was 20 days, the product obtained was dried at 60 °C for 2 h and calcined at 400, 800, and 1100 °C for 4 h each. To characterize and confirm the obtained synthesis products, X-Ray Diffraction (XRD), and Scanning Electron Microscopy (SEM) techniques were used. The results of morphology and chemical characterization of nano-dimensional powders obtained showed a formation of agglomerated particles of a size range of approximately 150 nm to 1.0 μm. Composition of powders was identified as corundum (Al2O3), iron aluminide (FeAl3), and iron-aluminum oxides (Fe0. 53Al0. 47)2O3 phases. The oxide phases formation were associated with the reaction of atmospheric concentration-free oxygen during synthesis and sintering steps, reducing the concentration of the iron aluminum phase.

Effect of drying method on the adsorption isotherms and isosteric heat of passion fruit pulp powder

Directory of Open Access Journals (Sweden)

Maria Angélica Marques Pedro

2010-12-01

Full Text Available The sorption behavior of dry products is generally affected by the drying method. The sorption isotherms are useful to determine and compare thermodynamic properties of passion fruit pulp powder processed by different drying methods. The objective of this study is to analyze the effects of different drying methods on the sorption properties of passion fruit pulp powder. Passion fruit pulp powder was dehydrated using different dryers: vacuum, spray dryer, vibro-fluidized, and freeze dryer. The moisture equilibrium data of Passion Fruit Pulp (PFP powders with 55% of maltodextrin (MD were determined at 20, 30, 40 and 50 ºC. The behavior of the curves was type III, according to Brunauer's classification, and the GAB model was fitted to the experimental equilibrium data. The equilibrium moisture contents of the samples were little affected by temperature variation. The spray dryer provides a dry product with higher adsorption capacity than that of the other methods. The vibro-fluidized bed drying showed higher adsorption capacity than that of vacuum and freeze drying. The vacuum and freeze drying presented the same adsorption capacity. The isosteric heats of sorption were found to decrease with increasing moisture content. Considering the effect of drying methods, the highest isosteric heat of sorption was observed for powders produced by spray drying, whereas powders obtained by vacuum and freeze drying showed the lowest isosteric heats of sorption.

The Influence of Duration of Mechanical Activation of Titanium Powder on its Morphology, Microstructure, and Microhardness

Science.gov (United States)

Ditenberg, I. A.; Korchagin, M. A.; Pinzhin, Yu. P.; Melnikov, V. V.; Tyumentsev, A. N.; Grinyaev, K. V.; Smirnov, I. V.; Radishevskii, V. L.; Tsverova, A. S.; Sukhanov, I. I.

2017-10-01

Using the methods of X-ray diffraction analysis and scanning and transmission electron microscopy, an investigation of the influence of duration of mechanical activation on morphology and structure of titanium powder is performed. In the course of processing the following stages of material transformation are revealed: fragmentation of the initial powder, conglomeration, and ovalization of the conglomerates. It is found that when the duration of mechanical activation increases, the characteristic size of coherent scattering regions is significantly decreased, which is accompanied by an increase in the value of microdistortions and intensive fragmentation of the crystal lattice inside powder particles followed by the formation of highly defective nanostructured states. The transformation of microstructure is accompanied by a considerable increase in microhardness.

Upconversion luminescence of Er3+/Yb3+ doped Sr5(PO4)3OH phosphor powders

Science.gov (United States)

Mokoena, P. P.; Swart, H. C.; Ntwaeaborwa, O. M.

2018-04-01

Sr5(PO4)3OH co-doped with Er3+and Yb3+ powder phosphors were synthesized by urea combustion method. The crystal structure was analyzed using X-ray diffraction (XRD). Particle morphology was analyzed using a Jeol JSM 7800F thermal field emission scanning electron microscope (FE-SEM) and the chemical composition analysis was carried out using an Oxford Instruments AzTEC energy dispersive spectrometer (EDS) attached to the FE-SEM. Upconversion emission was measured by using a FLS980 Spectrometer equipped with a 980 nm NIR laser as the excitation source, and a photomultiplier (PMT) detector. The XRD data of the Sr5(PO4)3OH powder exhibited characteristic diffraction patterns of the hexagonal structure referenced in the standard JCPDS card number 00-033-1348. The sharp peaks revealed the formation of crystalline Sr5(PO4)3OH. The powders were made up of hexagonal nanospheres. The enhanced red emission due to the 4F9/2 → 4I15/2 transitions of Er3+ was observed and was attributed to up conversion (UC) energy transfer from Yb3+. The upconversion energy transfer mechanism from Yb3+ to Er3+ is discussed.

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.

Effect of Gallium and Indium Co-Substituting on Upconversion Properties of Er/Yb:Yttrium Aluminum Garnet Powders Prepared by the Co-Precipitation Method.

Science.gov (United States)

Zhang, Wei; Liang, Yun-Ling; Hu, Zheng-Fa; Feng, Zu-Yong; Lun, Ma; Zhang, Xiu-ping; Sheng, Xia; Liu, Qian; Luo, Jie

2016-04-01

Gallium and Indium co-substituted Yb, Er:YAG was fabricated through the chemical co-precipitation method. The formation process and structure of the Ga3+ and In3+ substituted phosphor powders were characterized by the X-ray diffraction, thermo-gravimetry analyzer, infrared spectra, and X-ray photoelectron spectroscopy, and the effects of Ga3+ and In3+ concentration on the luminescence properties were investigated by spectrum. The results showed that the blue shift occurred after the substitution of Ga3+ and In3+ for Al3+ in matrix, and the intensity of emission spectrum was affected by the concentration of Ga3+ and In3+.

Superconducting properties of in situ powder-in-tube-processed MgB2 tapes fabricated with sub-micrometre Mg powder prepared by an arc-plasma method

International Nuclear Information System (INIS)

Yamada, H; Uchiyama, N; Matsumoto, A; Kitaguchi, H; Kumakura, H

2007-01-01

We fabricated in situ powder-in-tube-processed MgB 2 /Fe tapes using sub-micrometre Mg powder prepared by applying an arc-plasma method. We found that the use of this sub-micrometre Mg powder was very effective in increasing the J c values. The transport J c value of 10 mol% SiC-added tapes fabricated with this sub-micrometre Mg powder reached 275 A mm -2 at 4.2 K and 10 T. This value was about six times that of 5 mol% SiC-added tapes fabricated with commercial Mg powder. Microstructure analyses suggest that this J c enhancement is primarily due to the smaller MgB 2 grain size

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...

Synthesis and Characterization of Nanocrystalline Al-20 at. % Cu Powders Produced by Mechanical Alloying

Directory of Open Access Journals (Sweden)

Molka Ben Makhlouf

2016-06-01

Full Text Available Mechanical alloying is a powder processing technique used to process materials farther from equilibrium state. This technique is mainly used to process difficult-to-alloy materials in which the solid solubility is limited and to process materials where nonequilibrium phases cannot be produced at room temperature through conventional processing techniques. This work deals with the microstructural properties of the Al-20 at. % Cu alloy prepared by high-energy ball milling of elemental aluminum and copper powders. The ball milling of powders was carried out in a planetary mill in order to obtain a nanostructured Al-20 at. % Cu alloy. The obtained powders were characterized using scanning electron microscopy (SEM, differential scanning calorimetry (DSC and X-ray diffraction (XRD. The structural modifications at different stages of the ball milling are investigated with X-ray diffraction. Several microstructure parameters such as the crystallite sizes, microstrains and lattice parameters are determined.

Synthesis and characterization of bismuth alkaline titanate powders

Energy Technology Data Exchange (ETDEWEB)

Torres-Huerta, A.M., E-mail: atorresh@ipn.mx [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Dominguez-Crespo, M.A. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Hernandez-Perez, M.A. [ESIQIE, Metalurgia, Instituto Politecnico Nacional, Mexico, D. F (Mexico); Garcia-Zaleta, D.S. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Brachetti-Sibaja, S.B. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Instituto Tecnologico de Ciudad Madero, Av. 1o. de Mayo esq. Sor Juana Ines de la Cruz s/n Col. Los Mangos C.P.89440 Cd. Madero Tamaulipas (Mexico)

2011-06-15

In this work, samples of bismuth alkaline titanate, (K{sub 0.5}Na{sub 0.5}){sub (2-x/2)}Bi{sub (x/6)}TiO{sub 3}, (x = 0.05-0.75) have been prepared by conventional ceramic technique and molten salts. Metal oxides or carbonates powders were used as starting raw materials. The crystalline phase of the synthesized powders was identified by the X-ray diffraction (XRD) and particle morphology was characterized by scanning electron microscopy (SEM). Solid state reaction method was unsuccessful to obtain pellets. From XRD results, a rhombohedral structure was detected and the parameter lattice were estimated to be a = 5.5478 A and {alpha} = 59.48{sup o}. These parameters were used to refine the structure by Rietveld analysis. SEM results showed several morphologies. Apparently, bismuth is promoting the grain growth whose sizes vary from 30 nm to 180 nm It is expected that these materials can be utilized in practical applications as substitutes for lead zirconatetitanate (PZT)-based ceramics.

A method of eliminating the surface defect in low-temperature oxidation powder added UO2 pellet

International Nuclear Information System (INIS)

Yoo, H. S.; Lee, S. J.; Kim, J. I.; Jeon, K. R.; Kim, J. W.

2002-01-01

A study on methods to eliminate surface defect shown in low-temperature oxidation powder added UO 2 pellet has been performed. Powders oxidized at 350 .deg. C for 4 hrs were prepared and mixed with UO 2 powder after crushing them. After being sintered, surfaces of the pellet were inspected both visually and optically. A large number of defects were observed on the surface of the specimens in which low-temperature oxidation powders were directly mixed or master mixed with UO 2 powder while both specimens produced from mixed powders including milled oxidation powders and powders that were milled totally after mixing had clean surfaces. However, optical examination showed considerably large defected pores in the milled oxidation powder added pellet and it was confirmed that the inner defects can be eliminated completely only when milling the entire mixture on UO 2 and low-temperature oxidation powder, but not by crushing only oxidation powder

New titrimetric method for oxygen to metal ratio in uranium oxide powders

International Nuclear Information System (INIS)

Ray, Vinod Kumar; Brahmananda Reddy, G.; Balaji Rao, Y.; Subba Rao, Y.

2015-01-01

O/U ratio is of high importance to both U 3 O 8 and UO 2 powders for different reasons. In UO 2 powder it is a guiding parameter for sintering process where as for U 3 O 8 , it indicates efficiency of ammonium di-uranate (ADU) to U 3 O 8 conversion process. In the present method for O/U determination, UO 2 and U 3 O 8 powders are dissolved in 4.5 M sulphuric acid and little HF by heating on hot plate. Subsequently, optimized quantity of phosphoric acid is added on cooling, for getting sharp end point. The resultant solution is titrated with standard potassium dichromate using barium diphenylamine sulphonate (BDS) as an indicator. The expanded uncertainties calculated for UO 2 and U 3 O 8 powders are ±0.004 and ±0.006 O/U ratio units respectively at 95 % confidence level. (author)

International Centre for Diffraction Data (ICDD)