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.

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...

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.

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.)

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

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

International Nuclear Information System (INIS)

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

1991-01-01

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

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.

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

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)

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

International Nuclear Information System (INIS)

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

2003-01-01

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

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.

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...

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.

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

International Nuclear Information System (INIS)

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

2003-01-01

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

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...

Comparison between powder and slices diffraction methods in teeth samples

Energy Technology Data Exchange (ETDEWEB)

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

2011-07-01

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

Comparison between powder and slices diffraction methods in teeth samples

International Nuclear Information System (INIS)

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

2011-01-01

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

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 new synchrotron powder diffraction techniques to anomalous scattering from glasses

International Nuclear Information System (INIS)

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

1995-01-01

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

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.

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.

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...

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

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.

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.)

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

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.

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)

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

International Nuclear Information System (INIS)

Tanaka, Masahiko; Katsuya, Yoshio; Sakata, Osami

2016-01-01

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

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....

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-27

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

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)

Thermal evolution of CaO-doped HfO{sub 2} films and powders

Energy Technology Data Exchange (ETDEWEB)

Barolin, S A; Sanctis, O A de [Lab. Materiales Ceramicos, FCEIyA, Universidad Nacional de Rosario, IFIR-CONICET (Argentina); Caracoche, M C; Martinez, J A; Taylor, M A; Pasquevich, A F [Departamento de Fisica, FCE, Universidad Nacional de La Plata, IFLP-CONICET (Argentina); Rivas, P C, E-mail: oski@fceia.unr.edu.a [Facultad de Ciencias Agronomicas y Forestales, Universidad Nacional de La Plata, IFLP (Argentina)

2009-05-01

Solid solutions of ZrO2 and HfO2 are potential electrolyte materials for intermediate-temperature SOFC because both are oxygen-ion conductors. The main challenge for these compounds is to reduce the relatively high value of the activation energies vacancies diffusion, which is influenced by several factors. In this work the thermal evolution of CaO-HfO{sub 2} materials have been investigated. (CaO)y-Hf(1-y)O(2-y) (y = 0.06, 0.14 y 0.2) coatings and powders were synthesized by chemical solution deposition (CSD). Films were deposited onto alumina substrates by Dip Coating technique, the burning of organic waste was carried out at 500 deg. C under normal atmosphere and then the films were thermally treated at intervals of temperature rising to a maximum temperature of 1250 deg. C. By means Glazing Incidence X-ray Diffraction (rho-2theta configuration) the phases were studied in the annealed films. On the other hand, the thermal evolution and crystallization process of powders were analyzed in-situ by HT-XRD. The phenomena crystallization occurred in films and powders were analyzed. The activation energies of diffusion of oxygen vacancies of HfO2-14 mole% CaO and HfO2-20 mole% CaO films were measured from the thermal evolution of the relaxation constant measured by Perturbed Angular Correlation Technique.

Structural and thermal behaviour of carious and sound powders of human tooth enamel and dentine

International Nuclear Information System (INIS)

Tiznado-Orozco, Gaby E; Garcia-Garcia, R; Reyes-Gasga, J

2009-01-01

Powder from carious human tooth enamel and dentine were structurally, chemically and thermally analysed and compared against those from sound (healthy) teeth. Structural and chemical analyses were performed using x-ray diffraction, energy-dispersive x-ray spectroscopy and transmission electron microscopy. Thermal analysis was carried out by thermogravimetric analysis, Fourier transform infrared spectroscopy and x-ray diffraction. Results demonstrate partially dissolved crystals of hydroxyapatite (HAP) with substitutions of Na, Mg, Cl and C, and a greater weight loss in carious dentine as compared with carious enamel. A greater amount of thermal decomposition is observed in carious dentine as compared with sound dentine, with major variations in the a-axis of the HAP unit cell than in the c-axis. Variations in shape and intensity of the OH - , CO 3 2- and PO 4 3- FTIR bands were also found.

Crystallization behaviour and thermal stability of two aluminium-based metallic glass powder materials

Energy Technology Data Exchange (ETDEWEB)

Li, X.P.; Yan, M. [University of Queensland, School of Mechanical and Mining Engineering, ARC Centre of Excellence for Design in Light Metals, Brisbane, QLD 4072 (Australia); Yang, B.J. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Wang, J.Q., E-mail: jqwang@imr.ac.cn [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Schaffer, G.B. [University of Queensland, School of Mechanical and Mining Engineering, ARC Centre of Excellence for Design in Light Metals, Brisbane, QLD 4072 (Australia); Qian, M., E-mail: ma.qian@uq.edu.au [University of Queensland, School of Mechanical and Mining Engineering, ARC Centre of Excellence for Design in Light Metals, Brisbane, QLD 4072 (Australia)

2011-12-15

Highlights: Black-Right-Pointing-Pointer The crystallization paths and products of Al{sub 86}Ni{sub 7}Y{sub 4.5}Co{sub 1}La{sub 1.5} powder have been identified. Black-Right-Pointing-Pointer The thermal stability of Al{sub 86}Ni{sub 7}Y{sub 4.5}Co{sub 1}La{sub 1.5} powder has been assessed. Black-Right-Pointing-Pointer The Al{sub 86}Ni{sub 7}Y{sub 4.5}Co{sub 1}La{sub 1.5} powder shows a wide processing window of 75 K. Black-Right-Pointing-Pointer The powder has the potential to be consolidated into thick BMG components based on the findings. Black-Right-Pointing-Pointer The Al{sub 85}Ni{sub 5}Y{sub 6}Co{sub 2}Fe{sub 2} powder shows similar characteristics but inferior thermal stability. - Abstract: The crystallization behaviour and thermal stability of two Al-based metallic glass powder materials, Al{sub 85}Ni{sub 5}Y{sub 6}Co{sub 2}Fe{sub 2} and Al{sub 86}Ni{sub 6}Y{sub 4.5}Co{sub 2}La{sub 1.5}, have been investigated using differential scanning calorimetry (DSC), X-ray diffraction (XRD) and electron microscopy. Both alloy powders show a distinct three-stage crystallization process with a similar gap of {approx}75 K between the onset crystallization temperature (T{sub x}) and the second crystallization temperature. Crystallization occurs by the precipitation and growth of fcc-Al, without intermetallic formation. The apparent activation energy for each stage of crystallization was determined from DSC analyses and the phases resulting from each crystallization stage were identified by XRD and electron microscopy. The critical cooling rate for each alloy powder was calculated from the DSC data. These results are necessary to inform the consolidation of amorphous powder particles of Al{sub 85}Ni{sub 5}Y{sub 6}Co{sub 2}Fe{sub 2} or Al{sub 86}Ni{sub 6}Y{sub 4.5}Co{sub 2}La{sub 1.5} into thick (>1 mm) metallic glass components.

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

Anisotropic thermal expansion of MgSiN2 from 10 to 300 K as measured by neutron diffraction

NARCIS (Netherlands)

Bruls, R.J.; Hintzen, H.T.J.M.; Metselaar, R.; Loong, C.K.

2000-01-01

The lattice parameters of orthorhombic MgSiN2 as a function of the temperature have been determined from time-of-flight neutron powder diffraction. The results indicate that MgSiN2, just like several other adamantine-type crystals, exhibits a relatively small thermal expansion coefficient at low

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...

Thermal expansion and phase transformations of nitrogen-expanded austenite studied with in situ synchrotron X-ray diffraction

DEFF Research Database (Denmark)

Brink, Bastian; Ståhl, Kenny; Christiansen, Thomas Lundin

2014-01-01

Nitrogen-expanded austenite, _N, with high and low nitrogen contents was produced from AISI 316 grade stainless steel powder by gaseous nitriding in ammonia/hydrogen gas mixtures. In situ synchrotron X-ray diffraction was applied to investigate the thermal expansion and thermal stability...... as a fitting parameter. The stacking fault density is constant for temperatures up to 680 K, whereafter it decreases to nil. Surprisingly, a transition phase with composition M4N (M = Fe, Cr, Ni, Mo) appears for temperatures above 770 K. The linear coefficient of thermal expansion depends on the nitrogen...

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.)

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...

Competing orbital ordering in RVO3 compounds: High-resolution x-ray diffraction and thermal expansion

International Nuclear Information System (INIS)

Sage, M. H.; Blake, G. R.; Palstra, T. T. M.; Marquina, C.

2007-01-01

We report evidence for the phase coexistence of orbital orderings of different symmetry in RVO 3 compounds with intermediate-size rare earths. Through a study by high-resolution x-ray powder diffraction and thermal expansion, we show that the competing orbital orderings are associated with the magnitude of the VO 6 octahedral tilting and magnetic exchange striction in these compounds and that the phase-separated state is stabilized by lattice strains

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 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...

Morphology control and negative thermal expansion in cubic ZrWMoO8 powders

International Nuclear Information System (INIS)

Liu, Qinqin; Yang, Juan; Sun, Xiujuan; Cheng, Xiaonong

2008-01-01

Cubic ZrWMoO 8 powders with rod-like aggregate and thin fasciculus-like and flower-like rod cluster morphologies have been successfully fabricated with different amounts of (NH 4 ) 2 HPO 4 as surfactant using a hydrothermal method. X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and differential scanning calorimetry were utilized to investigate the influence of the addition of (NH 4 ) 2 HPO 4 on the crystallization process and crystal morphology of the resulting products. The results show that the purity and the thermal expansion property of the resulting products are not influenced by the addition of (NH 4 ) 2 HPO 4 . The cubic ZrWMoO 8 powders with both rod-like aggregate and flower-like rod cluster morphologies show a positive thermal expansion property in the temperature range from room temperature to 120 C, while they show a negative thermal expansion property in the temperature range from 120 C to 700 C. The abnormal thermal expansion property of cubic ZrWMoO 8 below 120 C is caused by the presence of water molecules. Investigations also show that the essence of the different morphologies of the ZrWMoO 8 particles obtained is the result of the different aggregation modes of the nanorods, which act as nuclei, and the corresponding aggregation process is dominated by the addition of (NH 4 ) 2 HPO 4 and its amount. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Thermal stability of retained austenite in TRIP steels studied by synchrotron X-ray diffraction during cooling

International Nuclear Information System (INIS)

Dijk, N.H. van; Butt, A.M.; Zhao, L.; Sietsma, J.; Offerman, S.E.; Wright, J.P.; Zwaag, S. van der

2005-01-01

We have performed in situ X-ray diffraction measurements at a synchrotron source in order to study the thermal stability of the retained austenite phase in transformation induced plasticity steels during cooling from room temperature to 100 K. A powder analysis of the diffraction data reveals a martensitic transformation of part of the retained austenite during cooling. The fraction of austenite that transforms during cooling is found to depend strongly on the bainitic holding time and the composition of the steel. It is shown that that austenite grains with a lower average carbon concentration have a lower stability during cooling

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.

Thermal conductivity model for powdered materials under vacuum based on experimental studies

Directory of Open Access Journals (Sweden)

N. Sakatani

2017-01-01

Full Text Available The thermal conductivity of powdered media is characteristically very low in vacuum, and is effectively dependent on many parameters of their constituent particles and packing structure. Understanding of the heat transfer mechanism within powder layers in vacuum and theoretical modeling of their thermal conductivity are of great importance for several scientific and engineering problems. In this paper, we report the results of systematic thermal conductivity measurements of powdered media of varied particle size, porosity, and temperature under vacuum using glass beads as a model material. Based on the obtained experimental data, we investigated the heat transfer mechanism in powdered media in detail, and constructed a new theoretical thermal conductivity model for the vacuum condition. This model enables an absolute thermal conductivity to be calculated for a powder with the input of a set of powder parameters including particle size, porosity, temperature, and compressional stress or gravity, and vice versa. Our model is expected to be a competent tool for several scientific and engineering fields of study related to powders, such as the thermal infrared observation of air-less planetary bodies, thermal evolution of planetesimals, and performance of thermal insulators and heat storage powders.

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.

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

The Measurement of Thermal Conductivities of Silica and Carbon Black Powders at Different pressures by Thermal COnductivity Probe

Institute of Scientific and Technical Information of China (English)

X.G.Liang; X.S.Ge; 等

1992-01-01

This investigation was done to study the gas filled powder insulation and thermal conductivity probe for the measurent of thermal conductivity of powders.The mathematical analysis showed that the heat capacity of the probe itself and the thermal rsistance between the probe and powder must be considered .The authors developed a slender probe and measured the effective thermal conductivity of sillca and carbon black powders under a variety of conditions.

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...

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.)

Fourier diffraction theorem for diffusion-based thermal tomography

International Nuclear Information System (INIS)

Baddour, Natalie

2006-01-01

There has been much recent interest in thermal imaging as a method of non-destructive testing and for non-invasive medical imaging. The basic idea of applying heat or cold to an area and observing the resulting temperature change with an infrared camera has led to the development of rapid and relatively inexpensive inspection systems. However, the main drawback to date has been that such an approach provides mainly qualitative results. In order to advance the quantitative results that are possible via thermal imaging, there is interest in applying techniques and algorithms from conventional tomography. Many tomography algorithms are based on the Fourier diffraction theorem, which is inapplicable to thermal imaging without suitable modification to account for the attenuative nature of thermal waves. In this paper, the Fourier diffraction theorem for thermal tomography is derived and discussed. The intent is for this thermal-diffusion based Fourier diffraction theorem to form the basis of tomographic reconstruction algorithms for quantitative thermal imaging

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)

The effect of thermal pre-treatment of titanium hydride (TiH2) powder in argon condition

Science.gov (United States)

Franciska P., L.; Erryani, Aprilia; Annur, Dhyah; Kartika, Ika

2018-04-01

Titanium hydride (TiH2) powders are used to enhance the foaming process in the formation of a highly porous metallic material with a cellular structure. But, the low temperature of hydrogen release is one of its problems. The present study, different thermal pre-treatment temperatures were employed to investigate the decomposition behavior of TiH2 to retard or delay a hydrogen gas release process during foaming. As a foaming agent, TiH2 was subjected to various heat treatments prior at 450 and 500°C during 2 hours in argon condition. To study the formation mechanism, the thermal behavior of titanium hydride and hydrogen release are investigated by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The morphology of pre-treated titanium hydride powders were examined using Scanning Electron Microscope (SEM) while unsure mapping and elemental composition of the pre-treated powders processed by Energy Dispersive Spectroscopy (EDS). To study the phase formation was characterized by X-ray diffraction analysis (XRD). In accordance with the results, an increase in pre-treatment temperature of TiH2 to higher degrees are changing the process of releasing hydrogen from titanium hydride powder. DTA/TGA results showed that thermal pre-treatment TiH2 at 450°C, released the hydrogen gas at 560°C in heat treatment when foaming process. Meanwhile, thermal pre-treatment in TiH2 at 500°C, released the hydrogen gas at 670°C when foaming process. There is plenty of direct evidence for the existence of oxide layers that showed by EDS analysis obtained in SEM. As oxygen is a light element and qualitative proof shows that the higher pre-treatment temperature produces more and thicker oxygen layers on the surface of the TiH2 powder particles. It might the thickness of oxide layer are different from different pre-treatment temperatures, which leading to the differences in the decomposition temperature. But from SEM result that oxidation of the powder does not

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

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

International Nuclear Information System (INIS)

Tanaka, M; Katsuya, Y; Matsushita, Y

2013-01-01

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

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

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

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....

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

International Nuclear Information System (INIS)

Rybak, Jens-Christoph

2012-01-01

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

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.

Gas-thermal coating of powdered materials. Communication 2

International Nuclear Information System (INIS)

Ermakov, S.S.

1986-01-01

This paper investigates the microstructure, microhardness, chemical composition of the transition zone, and also the strength characteristics of gas-thermal coatings including their adhesive power to the substrate (iron brand NC 100.24) and the residual stresses in the coatings. The microstructure of the transition zone was investigated; it was established that on the side of the substrate its density is greater than the mean density of both types of coating. It is shown that the porosity of the substrate has a competing effect on the thermal interaction of materials. Discovered regularities lead to the conclusion that the process of gas-thermal coating of powdered materials is more effective than when compact materials are coated; most effective is the combination of gas-thermal coating with processes of heat treatment of powder-metallurgy products

Effects of pressure on thermal transport in plutonium oxide powder

International Nuclear Information System (INIS)

Bielenberg, Patricia; Prenger, F. Coyne; Veirs, Douglas Kirk; Jones, Jerry

2004-01-01

Radial temperature profiles in plutonium oxide (PuO 2 ) powder were measured in a cylindrical vessel over a pressure range of 0.055 to 334.4 kPa with two different fill gases, helium and argon. The fine PuO 2 powder provides a very uniform self-heating medium amenable to relatively simple mathematical descriptions. At low pressures ( 2 powder has small particle sizes (on the order of 1 to 10 μm), random particle shapes, and high porosity so a more general model was required for this system. The model correctly predicts the temperature profiles of the powder over the wide pressure range for both argon and helium as fill gases. The effective thermal conductivity of the powder bed exhibits a pressure dependence at higher pressures because the pore sizes in the interparticle contact area are relatively small (less than 1 μm) and the Knudsen number remains above the continuum limit at these conditions for both fill gases. Also, the effective thermal conductivity with argon as a fill gas is higher than expected at higher pressures because the solid pathways account for over 80% of the effective powder conductivity. The results obtained from this model help to bring insight to the thermal conductivity of very fine ceramic powders with different fill gases.

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

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

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

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

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.)

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.

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

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

Fabrication of TiC-TiO{sub 2} composite powders by thermal plasma oxidation of titanium carbide powder; Tanka chitan funmatsu no plasma sanka hanno ni yori seiseishita TiC-TiO{sub 2} fukugo funmatsu

Energy Technology Data Exchange (ETDEWEB)

Ishigaki, T.; Li, Y.; Haneda, H. [National institute for Research Inorganic materials, Tsukuba (Japan); Kataoka, E. [Showa Cabot Supermetals K.K., Tokyo (Japan)

2000-09-15

TiC-TiO{sub 2} composite powders were prepared by in-flight oxidation of titanium carbide powder in RF induction thermal plasmas. Original titanium carbide powder of 20 - 38 {mu}m in particle size was axially injected into the center of argon-oxygen plasma. The powders were partially spheroidized and evaporated through the plasma treatment. X-ray diffraction of plasma-treated powders showed the formation of titanium dioxides, both rutile and anatase phases. The phase content of the plasma-prepared powders strongly depended on the plasma conditions, such as the plasma generating pressure and the oxygen flow rate in plasma generating gas. Especially, the increase of oxygen flow rate in plasma gas gave rise to the increase of heat transfer from plasma to powder particles, exothermic heat of oxidation reaction and cooling rate of plasma, giving the increase of spheroidization ratio, formation ratio of titanium dioxides, and content of anatase phases. (author)

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.)

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.)

Powder metallurgy and mechanical alloying effects on the formation of thermally induced martensite in an FeMnSiCrNi SMA

Directory of Open Access Journals (Sweden)

Pricop Bogdan

2015-01-01

Full Text Available By ingot metallurgy (IM, melting, alloying and casting, powder metallurgy (PM, using as-blended elemental powders and mechanical alloying (MA of 50 % of particle volume, three types of FeMnSiCrNi shape memory alloy (SMA specimens were fabricated, respectively. After specimen thickness reduction by hot rolling, solution treatments were applied, at 973 and 1273 K, to thermally induce martensite. The resulting specimens were analysed by X-ray diffraction (XRD and scanning electron microscopy (SEM, in order to reveal the presence of ε (hexagonal close-packed, hcp and α’ (body centred cubic, bcc thermally induced martensites. The reversion of thermally induced martensites, to γ (face centred cubic, fcc austenite, during heating, was confirmed by dynamic mechanical analysis (DMA, which emphasized marked increases of storage modulus and obvious internal friction maxima on DMA thermograms. The results proved that the increase of porosity degree, after PM processing, increased internal friction, while MA enhanced crystallinity degree.

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

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 ...

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

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.

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

Powder processing and spheroidizing with thermal inductively coupled plasma

International Nuclear Information System (INIS)

Nutsch, G.; Linke, P.; Zakharian, S.; Dzur, B.; Weiss, K.-H.

2001-01-01

Processing of advanced powder materials for the spraying industry is one of the most promising applications of the thermal RF inductively coupled plasma. By selecting the feedstock carefully and adjusting the RF plasma parameters, unique materials with high quality can be achieved. Powders injected in the hot plasma core emerge with modified shapes, morphology, crystal structure and chemical composition. Ceramic oxide powders such as Al 2 O 3 , ZrO 2 , SiO 2 are spheroidized with a high spheroidization rate. By using the RF induction plasma spheroidizing process tungsten melt carbide powders are obtained with a high spheroidization rate at high feeding rates by densification of agglomerated powders consisting of di-tungsten carbide and monocarbide with a definite composition. This kind of ball-like powders is particularly suited for wear resistant applications. (author)

Metal-Matrix Hardmetal/Cermet Reinforced Composite Powders for Thermal Spray

Directory of Open Access Journals (Sweden)

Dmitri GOLJANDIN

2012-03-01

Full Text Available Recycling of materials is becoming increasingly important as industry response to public demands, that resources must be preserved and environment protected. To produce materials competitive in cost with primary product, secondary producers have to pursue new technologies and other innovations. For these purposes different recycling technologies for composite materials (oxidation, milling, remelting etc are widely used. The current paper studies hardmetal/cermet powders produced by mechanical milling technology. The following composite materials were studied: Cr3C2-Ni cermets and WC-Co hardmetal. Different disintegrator milling systems for production of powders with determined size and shape were used. Chemical composition of produced powders was analysed.  To estimate the properties of recycled hardmetal/cermet powders, sieving analysis, laser granulometry and angularity study were conducted. To describe the angularity of milled powders, spike parameter–quadric fit (SPQ was used and experiments for determination of SPQ sensitivity and precision to characterize particles angularity were performed. Images used for calculating SPQ were taken by SEM processed with Omnimet Image Analyser 22. The graphs of grindability and angularity were composed. Composite powders based on Fe- and Ni-self-fluxing alloys for thermal spray (plasma and HVOF were produced. Technological properties of powders and properties of thermal sprayed coatings from studied powders were investigated. The properties of spray powders reinforced with recycled hardmetal and cermet particles as alternatives for cost-sensitive applications were demonstrated.DOI: http://dx.doi.org/10.5755/j01.ms.18.1.1348

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

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

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.

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.

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

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

Wear Resistant Thermal Sprayed Composite Coatings Based on Iron Self-Fluxing Alloy and Recycled Cermet Powders

Directory of Open Access Journals (Sweden)

Heikki SARJAS

2012-03-01

Full Text Available Thermal spray and WC-Co based coatings are widely used in areas subjected to abrasive wear. Commercial  cermet thermal spray powders for HVOF are relatively expensive. Therefore applying these powders in cost-sensitive areas like mining and agriculture are hindered. Nowadays, the use of cheap iron based self-fluxing alloy powders for thermal spray is limited. The aim of this research was to study properties of composite powders based on self-fluxing alloys and recycled cermets and to examine the properties of thermally sprayed (HVOF coatings from composite powders based on iron self-fluxing alloy and recycled cermet powders (Cr3C2-Ni and WC-Co. To estimate the properties of  recycled cermet powders, the sieving analysis, laser granulometry and morphology were conducted. For deposition of coatings High Velocity Oxy-Fuel spray was used. The structure and composition of powders and coatings were estimated by SEM and XRD methods. Abrasive wear performance of coatings was determined and compared with wear resistance of coatings from commercial powders. The wear resistance of thermal sprayed coatings from self-fluxing alloy and recycled cermet powders at abrasion is comparable with wear resistance of coatings from commercial expensive spray powders and may be an alternative in tribological applications in cost-sensitive areas.DOI: http://dx.doi.org/10.5755/j01.ms.18.1.1338

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

International Nuclear Information System (INIS)

Mazumdar, S.

1999-01-01

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

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...

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.)

Investigation of the oxidative processes in intermetallic Sm Co5 powder during heat treatment

International Nuclear Information System (INIS)

Talijan, Nadezda M.; Milutinovic-Nikolic, Aleksandra; Stajic-Trosic, Jasna T.; Jovanovic, Zarko D.

1996-01-01

Understanding of the thermal stability of intermetallic Sm Co 5 powder is essential for designing the working atmosphere in all phases of the technological procedure in the production of sintered Sm Co 5 magnets to obtain maximal magnetic properties. The thermal stability of the Sm Co 5 powder with defined chemical composition and particle size was investigated in the interval from 20 to 900 deg C. Commercial Sm Co 5 powder was used in this experiment. The powder was milled in anhydrous toluene in an agate mortar to fine powder of quality used in the production of sintered magnets. All the experiments were carried out with powder of an average particle size of 7.23μm, established by SEM. THe thermal stability of the Sm Co 5 powder in static air atmosphere was investigated by thermogravimetric analysis (TGA) using a DuPont Thermal Analyzer. Investigation of the behaviour of Sm Co 5 powder during heating was carried out using new samples of Sm Co 5 powder for each of the investigated temperature cycles. It was found by TGA that up to 200 deg C, the oxidation of Sm Co 5 was negligible. X-ray diffraction of the thermogravimetric experimental residue of the Sm Co 5 powder, heated at 240 deg C, yielded only the presence of the Sm Co 5 phase. By X-ray diffraction different crystal forms were identified depending on the maximal heating temperature. The following phases were identified: Sm 2 O 3 , Co, Co O, Co 3 O 4 and Sm Co O 3 . According to TG and X-ray results, for each of the investigated temperatures, the corresponding chemical reactions were established. The experimental data from both the thermal and X-ray investigations confirm that the phases of pressing and aligning the Sm Co 5 powder, in the process of producing sintered Sm Co 5 magnets, may be performed without a protective atmosphere. (author)

Thermal behavior and phase transformation of ZrO2–10%SiO2 precursor powder prepared by a co-precipitation route without adding stability agent

International Nuclear Information System (INIS)

Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Cheng-Li; Wang, Moo-Chin; Lee, Kuen-Chan; Huang, Hong-Hsin; Lee, Huey-Er

2014-01-01

Highlights: • The precursor powders contained about 68.3 wt% ZrO 2 , which corresponds to ZrO 2 ·1/8 H 2 O. • The exothermic peak temperature of tetragonal ZrO 2 formation occurred at 1014 K. • The activation energy of ZrO 2 –10%SiO 2 precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO 2 formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO 2 fully converted to monoclinic ZrO 2 . - Abstract: Thermal behavior and phase transformation of ZrO 2 –10%SiO 2 precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO 2 freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO 2 crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO 2 appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO 2 fully converted to monoclinic ZrO 2 occurred

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...

Thermal conductivity of 238PuO2 powder, intermediates, and dense fuel forms

International Nuclear Information System (INIS)

Bickford, D.F.; Crain, B. Jr.

1975-10-01

The thermal conductivities of porous 238 PuO 2 powder (calcined oxalate), milled powder, and high-density granules were calculated from direct measurements of steady-state temperature profiles resulting from self-heating. Thermal conductivities varied with density, temperature, and gas content of the pores. Errors caused by thermocouple heat conduction were less than 5 percent when the dimensions of the thermal conductivity cell and the thermocouple were properly selected

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 ...

LSA glass-ceramic tiles made by powder pressing

International Nuclear Information System (INIS)

Figueira, F.C.; Bertan, F.M.; Riella, H.G.; Uggioni, E.; Bernardin, A.M.

2009-01-01

A low cost alternative for the production of glass-ceramic materials is the pressing of the matrix glass powders and its consolidation simultaneously with crystallization in a single stage of sintering. The main objective of this work was to obtain LSA glass ceramics with low thermal expansion, processed by pressing and sintering a ceramic frit powder. The raw materials were homogenized and melted (1480 deg C, 80min), and the melt was poured in water. The glass was chemically (XRF and AAS) and thermally (DTA, 10 deg C/min, air) characterized, and then ground (60min and 120min). The ground powders were characterized (laser diffraction) and compressed (35MPa and 45MPa), thus forming four systems. The compacts were dried (150 deg C, 24h) and sintered (1175 deg C and 1185 deg C, 10 deg C/min). Finally, the glass-ceramics were characterized by microstructural analysis (SEM and XRD), mechanical behavior (σbending) and thermal analysis (α). The best results for thermal expansion were those for the glass-ceramics processed with smaller particle size and greater compaction pressure. (author)

Processing line for industrial radiation-thermal synthesis of doped lithium ferrite powders

Science.gov (United States)

Surzhikov, A. P.; Galtseva, O. V.; Vasendina, E. A.; Vlasov, V. A.; Nikolaev, E. V.

2016-02-01

The paper considers the issues of industrial production of doped lithium ferrite powders by radiation-thermal method. A technological scheme of the processing line is suggested. The radiation-thermal technological scheme enables production of powders with technical characteristics close to the required ones under relatively low temperature annealing conditions without intermediate mixing. The optimal conditions of the radiation-thermal synthesis are achieved isothermally under irradiation by the electron beam with energy of 2.5 MeV in the temperature range of 700-750 0C within- 120 min.

The mechanical and thermal characteristics of phenolic foam reinforced with kaolin powder and glass fiber fabric

Science.gov (United States)

Xiao, Wenya; Huang, Zhixiong; Ding, Jie

2017-12-01

In this work, kaolin powder and glass fiber fabric were added to PF in order to improve its thermal stability and mechanical property. Micro-structures of carbonized PF with kaolin powder were inspected by scanning electron microscopy (SEM) to demonstrate the filler’s pinning effect. SEM results illustrated modified PF had well morphology after high-temperature heat treatment. The Fourier transform infrared spectrometer (FTIR) test was carried out and found that kaolin powder only physically dispersed in PF. The compression test and thermal weight loss test were done on two groups of modified PF (Group A: add powder and fabric; Group B: add powder only). Results showed that all modified PF were better than pure PF, while foams with powder and fabric showed better mechanical characteristic and thermal stability compared with foams with powder only.

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

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

Effect of Powder-Suspended Dielectric on the EDM Characteristics of Inconel 625

Science.gov (United States)

Talla, Gangadharudu; Gangopadhyay, S.; Biswas, C. K.

2016-02-01

The current work attempts to establish the criteria for powder material selection by investigating the influence of various powder-suspended dielectrics and machining parameters on various EDM characteristics of Inconel 625 (a nickel-based super alloy) which is nowadays regularly used in aerospace, chemical, and marine industries. The powders include aluminum (Al), graphite, and silicon (Si) that have significant variation in their thermo-physical characteristics. Results showed that powder properties like electrical conductivity, thermal conductivity, density, and hardness play a significant role in changing the machining performance and the quality of the machined surface. Among the three powders, highest material removal rate was observed for graphite powder due to its high electrical and thermal conductivities. Best surface finish and least radial overcut (ROC) were attained using Si powder. Maximum microhardness was found for Si due to its low thermal conductivity and high hardness. It is followed by graphite and aluminum powders. Addition of powder to the dielectric has increased the crater diameter due to expansion of plasma channel. Powder-mixed EDM (PMEDM) was also effective in lowering the density of surface cracks with least number of cracks obtained with graphite powder. X-ray diffraction analysis indicated possible formation of metal carbides along with grain growth phenomenon of Inconel 625 after PMEDM.

Electron diffraction patterns with thermal diffuse scattering maxima around Kikuchi lines

International Nuclear Information System (INIS)

Karakhanyan, R. K.; Karakhanyan, K. R.

2011-01-01

Transmission electron diffraction patterns of silicon with thermal diffuse maxima around Kikuchi lines, which are analogs of the maxima of thermal diffuse electron scattering around point reflections, have been recorded. Diffuse maxima are observed only around Kikuchi lines with indices that are forbidden for the silicon structure. The diffraction conditions for forming these maxima are discussed.

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.

Properties of polyester based powder coating containing Cloisite®30B modified with silane 3-aminopropyltriethoxysilane

International Nuclear Information System (INIS)

Bertuoli, P.T.; Frizzo, V.P.; Zattera, A.J.; Scienza, L.C.

2014-01-01

The incorporation of clay into a polymer matrix results in nanocomposites with mechanical strength, thermal and barrier properties superior to the free filler matrix. With the aim to obtain a powder coating with better thermal properties than the coating free of filler, the organoclay Cloisite®30B was modified with 3-aminopropyltriethoxysilane (APS) and incorporated to a polyester based powder coating, on proportions of 2 to 8 wt% in the melt state. The powder coatings were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The powder coating containing clay showed no alteration in the basal spacing compared to that basal spacing of the clay. Compared to the powder coating free of the clay, powder coatings containing clay had lower thermal stability due to the presence of the organic modifier. The presence of clay reduced the crosslinking temperature and the incorporation of 2 wt% of the clay caused the increase in the energy released in the crosslinking process. (author)

Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent

Energy Technology Data Exchange (ETDEWEB)

Chu, Hsueh-Liang [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Cheng-Li [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Lee, Kuen-Chan [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Huang, Hong-Hsin [Department of Electrical Engineering, Cheng Shiu University, 840 Cheng Ching Road, Niaosong, Kaohsiung 83347, Taiwan (China); Lee, Huey-Er, E-mail: huerle@kmu.edu.tw [School of Dentistry, College of Dental Medicine, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, 100 Tzyou 1st Road, Kaohsiung 807, Taiwan (China)

2014-12-15

Highlights: • The precursor powders contained about 68.3 wt% ZrO{sub 2}, which corresponds to ZrO{sub 2}·1/8 H{sub 2}O. • The exothermic peak temperature of tetragonal ZrO{sub 2} formation occurred at 1014 K. • The activation energy of ZrO{sub 2}–10%SiO{sub 2} precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO{sub 2} formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2}. - Abstract: Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO{sub 2} freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO{sub 2} crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO{sub 2} appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2} occurred.

Crystal structure and thermal expansion of Mn(1-x)Fe(x)Ge.

Science.gov (United States)

Dyadkin, Vadim; Grigoriev, Sergey; Ovsyannikov, Sergey V; Bykova, Elena; Dubrovinsky, Leonid; Tsvyashchenko, Anatoly; Fomicheva, L N; Chernyshov, Dmitry

2014-08-01

A series of temperature-dependent single-crystal and powder diffraction experiments has been carried out using synchrotron radiation in order to characterize the monogermanides of Mn, Fe and their solid solutions. The MnGe single crystal is found to be enantiopure and we report the absolute structure determination. The thermal expansion, parametrized with the Debye model, is discussed from the temperature-dependent powder diffraction measurements for Mn(1-x)Fe(x)Ge (x = 0, 0.1, 0.2, 0.25, 0.3, 0.4, 0.5, 0.6, 0.7, 0.75, 0.8, 0.9). Whereas the unit-cell dimension and the Debye temperature follow a linear trend as a function of composition, the thermal expansion coefficient deviates from linear dependence with increasing Mn content. No structural phase transformations have been observed for any composition in the temperature range 80-500 K for both single-crystal and powder diffraction, indicating that the phase transition previously observed with neutron powder diffraction most probably has a magnetic origin.

Characterization of prealloyed copper powders treated in high energy ball mill

International Nuclear Information System (INIS)

Rajkovic, Viseslava; Bozic, Dusan; Jovanovic, Milan T.

2006-01-01

The inert gas atomised prealloyed copper powders containing 3.5 wt.% Al were milled up to 20 h in the planetary ball mill in order to oxidize aluminium in situ with oxygen from the air. In the next procedure compacts from milled powder were synthesized by hot-pressing in argon atmosphere. Compacts from as-received Cu-3.5 wt.% Al powder and electrolytic copper powder were also prepared under the same conditions. Microstructural and morphological changes of high energy milled powder as well as changes of thermal stability and electrical conductivity of compacts were studied as a function of milling time and high temperature exposure at 800 deg. C. Optical, scanning electron microscopy (SEM) and X-ray diffraction analysis were performed for microstructural characterization, whereas thermal stability and electrical conductivity were evaluated by microhardness measurements and conductometer Sigmatest, respectively. The prealloyed 5 h-milled and compacted powder showed a significant increase in microhardness reaching the value of 2600 MPa, about 4 times greater than that of compacts synthesized from as-received electrolytic copper powder (670 MPa). The electrical conductivity of compacts from 5 h-milled powder was 52% IACS. The results were discussed in terms of the effect of small grain size and finely distributed alumina dispersoids on hardening and thermal stability of compacts

Enhancement of thermal neutron shielding of cement mortar by using borosilicate glass powder.

Science.gov (United States)

Jang, Bo-Kil; Lee, Jun-Cheol; Kim, Ji-Hyun; Chung, Chul-Woo

2017-05-01

Concrete has been used as a traditional biological shielding material. High hydrogen content in concrete also effectively attenuates high-energy fast neutrons. However, concrete does not have strong protection against thermal neutrons because of the lack of boron compound. In this research, boron was added in the form of borosilicate glass powder to increase the neutron shielding property of cement mortar. Borosilicate glass powder was chosen in order to have beneficial pozzolanic activity and to avoid deleterious expansion caused by an alkali-silica reaction. According to the experimental results, borosilicate glass powder with an average particle size of 13µm showed pozzolanic activity. The replacement of borosilicate glass powder with cement caused a slight increase in the 28-day compressive strength. However, the incorporation of borosilicate glass powder resulted in higher thermal neutron shielding capability. Thus, borosilicate glass powder can be used as a good mineral additive for various radiation shielding purposes. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

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

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)

Synthesis of yttria powders by electrospray pyrolysis

International Nuclear Information System (INIS)

Rulison, A.J.; Flagan, R.C.

1994-01-01

Electrospray atomization of high-concentration (∼400 g/L) chemical precursor solutions was applied to the synthesis of yttria powders. Conditions were found which led to high-quality powders, composed of dense, spheroidal, submicrometer, and nanocrystalline oxide particles. The precursor solutions were hydrated yttrium nitrates dissolved in n-propyl alcohol at concentrations ranging from 44.1 to 455 g/L. Electrospray atomization produced submicrometer precursor droplets which were dispersed in air and carried through an electric furnace for thermal decomposition at 500 C for several seconds residence time. X-ray powder diffraction patterns indicated the expected cubic phase. Transmission electron micrographs showed that the particle structure varied with solution composition, ranging from hollow, inflated spheres for 6-hydrated nitrates to dense spheroids for 5-hydrated nitrates. The use of 6-hydrated nitrates in the solutions appeared to form particle surfaces which were impermeable to alcohol vapor evolved during thermal decomposition, leading to hollow, inflated spheres

Tailoring the thermal conductivity of the powder bed in Electron Beam Melting (EBM) Additive Manufacturing.

Science.gov (United States)

Smith, C J; Tammas-Williams, S; Hernandez-Nava, E; Todd, I

2017-09-05

Metallic powder bed additive manufacturing is capable of producing complex, functional parts by repeatedly depositing thin layers of powder particles atop of each other whilst selectively melting the corresponding part cross-section into each layer. A weakness with this approach arises when melting overhanging features, which have no prior melted material directly beneath them. This is due to the lower thermal conductivity of the powder relative to solid material, which as a result leads to an accumulation of heat and thus distortion. The Electron Beam Melting (EBM) process alleviates this to some extent as the powder must first be sintered (by the beam itself) before it is melted, which results in the added benefit of increasing the thermal conductivity. This study thus sought to investigate to what extent the thermal conductivity of local regions in a titanium Ti-6Al-4V powder bed could be varied by imparting more energy from the beam. Thermal diffusivity and density measurements were taken of the resulting sintered samples, which ranged from being loosely to very well consolidated. It was found that the calculated thermal conductivity at two temperatures, 40 and 730 °C, was more than doubled over the range of input energies explored.

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

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…

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)

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.

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

Directory of Open Access Journals (Sweden)

Svіtlana HAVENKO

2015-03-01

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

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...

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

Sintering of B4C powder obtained by a modified carbo-thermal reaction

International Nuclear Information System (INIS)

Rocha, R.M.; Kazumi, M.H.; Goncalves, D.P.; Melo, F.C.L.

2005-01-01

Boron carbide is one of the hardest materials and a highly refractory material that is of great interest for structural, electronic and nuclear applications. B 4 C is commercially manufactured by the carbo-thermal reduction of a mixture of boron oxide (B 2 O 3 ) in an batch electric arc furnace process. However the carbo-thermal reaction on the stoichiometric starting composition results an excess carbon residue because of the boron loss in the form of B 2 O 2 . Thus, a modified carbo-thermal reaction is applied with an excess B 2 O 3 to compensate the loss and to obtain stoichiometric powders. The aim of this work is to study the sinterability of this powder with the lower carbon residue acting as sintering additive. Pressureless sintering in the temperatures of 1900 deg. C/30 min and 2100 deg. C/30 min in argon atmosphere were applied. The synthesized powders were analysed by XRD and SEM. Density of 94% of theoretical density was achieved for sample prepared with the powder obtained with 50% B 2 O 3 excess synthesized at 1700 deg. C/15 min. (authors)

Interstitial pressure dependence of the thermal conductivity of some rare earth oxide powders

International Nuclear Information System (INIS)

Pradeep, P.

1997-01-01

Thermal transport properties of powdered materials depend upon interstitial gas pressure. The present study reports the experimental results for the effective thermal conductivity of three rare earth oxide powders viz. yttrium oxide, samarium oxide, and gadolinium oxide, at various interstitial pressures by using transient plane source (TPS) method. A theoretical model is also proposed for the interpretation of the variation of the effective thermal conductivity with interstitial gas pressure. Its validity is found to be good in low pressure range of 45 mm Hg to normal pressure when compared with the experimental results. Also an attempt has been made to calculate the variation of thermal conductivity with interstitial pressure in the high pressure range up to 2 kbar using the proposed model. (author)

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

Thermal diffuse scattering in angular-dispersive neutron diffraction

International Nuclear Information System (INIS)

Popa, N.C.; Willis, B.T.M.

1998-01-01

The theoretical treatment of one-phonon thermal diffuse scattering (TDS) in single-crystal neutron diffraction at fixed incident wavelength is reanalysed in the light of the analysis given by Popa and Willis [Acta Cryst. (1994), (1997)] for the time-of-flight method. Isotropic propagation of sound with different velocities for the longitudinal and transverse modes is assumed. As in time-of-flight diffraction, there exists, for certain scanning variables, a forbidden range in the one-phonon TDS of slower-than-sound neutrons, and this permits the determination of the sound velocity in the crystal. A fast algorithm is given for the TDS correction of neutron diffraction data collected at a fixed wavelength: this algorithm is similar to that reported earlier for the time-of-flight case. (orig.)

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)

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 ...

Influence of pin and hammer mill on grinding characteristics, thermal and antioxidant properties of coriander powder.

Science.gov (United States)

Barnwal, P; Singh, K K; Sharma, Alka; Choudhary, A K; Saxena, S N

2015-12-01

In present study, influence of grinding (hammer and pin mills) and moisture content (range: 6.4-13.6 % dry basis) on the quality traits of coriander powder were investigated. These include grinding parameters, colour parameters, specific heat, thermal conductivity, thermal diffusivity, glass transition temperature, essential oil, total phenolic content, total flavonoid content and DPPH scavenging (%) of coriander powder. For coriander seed, the geometric properties such as major, medium, minor dimensions, geometric mean diameter, arithmetic mean diameter, sphericity, surface area and volume of coriander seeds increased significantly with increasing moisture (6.4-13.6 % db). For coriander powder, the grinding parameters such as average particle size, volume surface mean diameter and volume mean diameter increased significantly with increasing moisture (6.4-13.6 % db). With the grinding method, the colour attributes of coriander powder such as L-value, a-value, b-value, hue angle and browning index varied significantly. It was observed that the specific heat followed second order polynomial relationship with temperature and moisture whereas thermal conductivity varied linearly with temperature and moisture content. The variation of glass transition temperature with moisture can be best represented in quadratic manner. Total flavonoid content (mg QE/g crude seed extract) and DPPH scavenging % activity of coriander powder is significantly affected by grinding methods. A lower value of specific heat was observed for hammer ground coriander powder as compared to pin mill ground coriander powder. The thermal conductivity of hammer mill ground coriander powder was higher as compared to pin mill ground coriander. It was observed that hammer mill yields more fine coriander powder in comparison to pin mill. The browning index was more in hammer mill ground coriander powder.

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.

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

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

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

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

Sintering of B{sub 4}C powder obtained by a modified carbo-thermal reaction

Energy Technology Data Exchange (ETDEWEB)

Rocha, R.M.; Kazumi, M.H.; Goncalves, D.P.; Melo, F.C.L. [Centro Tecnico Aeroespacial (CTA) - Instituto de Aeronautica e Espaco, Praca Marechal Eduardo Gomes, 50 Campus do CTA - Vila das Acacias, 12228-904 Sao Jose dos Campos-SP (Brazil)

2005-07-01

Boron carbide is one of the hardest materials and a highly refractory material that is of great interest for structural, electronic and nuclear applications. B{sub 4}C is commercially manufactured by the carbo-thermal reduction of a mixture of boron oxide (B{sub 2}O{sub 3}) in an batch electric arc furnace process. However the carbo-thermal reaction on the stoichiometric starting composition results an excess carbon residue because of the boron loss in the form of B{sub 2}O{sub 2}. Thus, a modified carbo-thermal reaction is applied with an excess B{sub 2}O{sub 3} to compensate the loss and to obtain stoichiometric powders. The aim of this work is to study the sinterability of this powder with the lower carbon residue acting as sintering additive. Pressureless sintering in the temperatures of 1900 deg. C/30 min and 2100 deg. C/30 min in argon atmosphere were applied. The synthesized powders were analysed by XRD and SEM. Density of 94% of theoretical density was achieved for sample prepared with the powder obtained with 50% B{sub 2}O{sub 3} excess synthesized at 1700 deg. C/15 min. (authors)

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 ...

Response to Thermal Exposure of Ball-Milled Aluminum-Borax Powder Blends

Science.gov (United States)

Birol, Yucel

2013-04-01

Aluminum-borax powder mixtures were ball milled and heated above 873 K (600 °C) to produce Al-B master alloys. Ball-milled powder blends reveal interpenetrating layers of deformed aluminum and borax grains that are increasingly refined with increasing milling time. Thermal exposure of the ball-milled powder blends facilitates a series of thermite reactions between these layers. Borax, dehydrated during heating, is reduced by Al, and B thus generated reacts with excess Al to produce AlB2 particles dispersed across the aluminum grains starting at 873 K (600 °C). AlB2 particles start to form along the interface of the aluminum and borax layers. Once nucleated, these particles grow readily to become hexagonal-shaped crystals that traverse the aluminum grains with increasing temperatures as evidenced by the increase in the size as well as in the number of the AlB2 particles. Ball milling for 1 hour suffices to achieve a thermite reaction between borax and aluminum. Ball milling further does not impact the response of the powder blend to thermal exposure. The nucleation-reaction sites are multiplied, however, with increasing milling time and thus insure a higher number of smaller AlB2 particles. The size of the AlB2 platelets may be adjusted with the ball milling time.

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-08-15

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

Low-temperature densification and excellent thermal properties of W–Cu thermal-management composites prepared from copper-coated tungsten powders

International Nuclear Information System (INIS)

Zhang, Lianmeng; Chen, Wenshu; Luo, Guoqiang; Chen, Pingan; Shen, Qiang; Wang, Chuanbin

2014-01-01

Highlights: • High-density (98.4%) W–20 wt.%Cu composites were low-temperature fabricated. • A highly pure Cu network and a homogenous microstructure formed in the composites. • The interfaces between W and Cu are well bonded with no spaces. • The composites have excellent thermal properties. -- Abstract: High-density W–20 wt.%Cu composites containing a Cu-network structure and exhibiting good thermal properties were fabricated by low-temperature hot-press sintering from high-purity copper-coated tungsten powders. The relative density of W–20 wt.%Cu composites sintered at 950 °C–100 MPa–2 h was 98.4%. The low-temperature densification of W–Cu composites occurs because the sintering mode of the coated particles involves only sintering of Cu to Cu, rather than both Cu to W and Cu to Cu, as required for conventional powder particles. The microstructure shows that a network of high-purity Cu extends throughout the composites, and that the W is distributed homogeneously; the interfaces between W and Cu show good contact. The composites have excellent thermal conductivity (239 W/(m K)) and a relatively low coefficient of thermal expansion (7.4 × 10 −6 /K), giving them some of the best properties reported to date for thermal-management materials. The excellent performance is mainly because of their structure, which arises from the characteristics of the high-purity copper-coated tungsten powders

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)

Evaluation of Energy Consumption in the Mercury Treatment of Phosphor Powder from Spent Fluorescent Lamps Using a Thermal Process

Directory of Open Access Journals (Sweden)

Yong Choi

2017-11-01

Full Text Available In a pilot-plant-scale thermal mercury treatment of phosphor powder from spent fluorescent lamps, energy consumption was estimated to control mercury content by the consideration of reaction kinetics. Mercury content was analyzed as a function of treatment temperature and time. The initial mercury content of the phosphor powder used in the thermal process was approximately 3500 mg/kg. The target mercury content in the phosphor powder thermal process of the phosphor powder was 5 mg/kg or less at 400 °C or higher because the target mercury content was recommended by Minamata Convention and Basel Convention. During thermal processing, the reaction rate was represented by a first order reaction with the Arrhenius equation. The reaction rate constant increased with temperature from 0.0112 min−1 at 350 °C to 0.0558 min−1 at 600 °C. The frequency factor was 2.51 min−1, and the activation energy was 6509.11 kcal/kg. Reaction rate constants were used to evaluate the treatment time required to reduce mercury content in phosphor powder to be less than 5 mg/kg. The total energy consumption in a pilot-plant-scale thermal process was evaluated to determine the optimal temperature for removing mercury in phosphor powder.

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...

Recovery Of Electrodic Powder From Spent Lithium Ion Batteries (LIBs

Directory of Open Access Journals (Sweden)

Shin S.M.

2015-06-01

Full Text Available This study was focused on recycling process newly proposed to recover electrodic powder enriched in cobalt (Co and lithium (Li from spent lithium ion battery. In addition, this new process was designed to prevent explosion of batteries during thermal treatment under inert atmosphere. Spent lithium ion batteries (LIBs were heated over the range of 300°C to 600°C for 2 hours and each component was completely separated inside reactor after experiment. Electrodic powder was successfully recovered from bulk components containing several pieces of metals through sieving operation. The electrodic powder obtained was examined by X-ray diffraction (XRD, energy dispersive X-ray spectroscopy (EDS, and atomic absorption spectroscopy (AA and furthermore image of the powder was taken by scanning electron microscopy (SEM. It was finally found that cobalt and lithium were mainly recovered to about 49 wt.% and 4 wt.% in electrodic powder, respectively.

Modelling and Characterization of Effective Thermal Conductivity of Single Hollow Glass Microsphere and Its Powder.

Science.gov (United States)

Liu, Bing; Wang, Hui; Qin, Qing-Hua

2018-01-14

Tiny hollow glass microsphere (HGM) can be applied for designing new light-weighted and thermal-insulated composites as high strength core, owing to its hollow structure. However, little work has been found for studying its own overall thermal conductivity independent of any matrix, which generally cannot be measured or evaluated directly. In this study, the overall thermal conductivity of HGM is investigated experimentally and numerically. The experimental investigation of thermal conductivity of HGM powder is performed by the transient plane source (TPS) technique to provide a reference to numerical results, which are obtained by a developed three-dimensional two-step hierarchical computational method. In the present method, three heterogeneous HGM stacking elements representing different distributions of HGMs in the powder are assumed. Each stacking element and its equivalent homogeneous solid counterpart are, respectively, embedded into a fictitious matrix material as fillers to form two equivalent composite systems at different levels, and then the overall thermal conductivity of each stacking element can be numerically determined through the equivalence of the two systems. The comparison of experimental and computational results indicates the present computational modeling can be used for effectively predicting the overall thermal conductivity of single HGM and its powder in a flexible way. Besides, it is necessary to note that the influence of thermal interfacial resistance cannot be removed from the experimental results in the TPS measurement.

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.

Diamond Thermal Expansion Measurement Using Transmitted X-ray Back-diffraction.

OpenAIRE

Giles, Carlos; Adriano, Cris; Lubambo, Adriana Freire; Cusatis, Cesar; Mazzaro, Irineu; Hönnicke, Marcelo Goncalves

2015-01-01

The linear thermal expansion coefficient of diamond has been measured using forward-diffracted profiles in X-ray backscattering. This experimental technique is presented as an alternative way of measuring thermal expansion coefficients of solids in the high-resolution Bragg backscattering geometry without the intrinsic difficulty of detecting the reflected beam. The temperature dependence of the lattice parameter is obtained from the high sensitivity of the transmitted profiles to the Bragg a...

Thermal decomposition of ammonium hexachloroosmate

DEFF Research Database (Denmark)

Asanova, T I; Kantor, Innokenty; Asanov, I. P.

2016-01-01

Structural changes of (NH4)2[OsCl6] occurring during thermal decomposition in a reduction atmosphere have been studied in situ using combined energy-dispersive X-ray absorption spectroscopy (ED-XAFS) and powder X-ray diffraction (PXRD). According to PXRD, (NH4)2[OsCl6] transforms directly to meta...

Optimizing Compliance and Thermal Conductivity of Plasma Sprayed Thermal Barrier Coatings via Controlled Powders and Processing Strategies

Science.gov (United States)

Tan, Yang; Srinivasan, Vasudevan; Nakamura, Toshio; Sampath, Sanjay; Bertrand, Pierre; Bertrand, Ghislaine

2012-09-01

The properties and performance of plasma-sprayed thermal barrier coatings (TBCs) are strongly dependent on the microstructural defects, which are affected by starting powder morphology and processing conditions. Of particular interest is the use of hollow powders which not only allow for efficient melting of zirconia ceramics but also produce lower conductivity and more compliant coatings. Typical industrial hollow spray powders have an assortment of densities resulting in masking potential advantages of the hollow morphology. In this study, we have conducted process mapping strategies using a novel uniform shell thickness hollow powder to control the defect microstructure and properties. Correlations among coating properties, microstructure, and processing reveal feasibility to produce highly compliant and low conductivity TBC through a combination of optimized feedstock and processing conditions. The results are presented through the framework of process maps establishing correlations among process, microstructure, and properties and providing opportunities for optimization of TBCs.

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

Extruded Al-Al2O3 composites formed in situ during consolidation of ultrafine Al powders: Effect of the powder surface area

International Nuclear Information System (INIS)

Balog, Martin; Simancik, Frantisek; Walcher, Martin; Rajner, Walter; Poletti, Cecilia

2011-01-01

Highlights: → 25 gas atomised Al 99.5% powders with particle size 2 O 3 dispersoids. → Compacts showed good thermal stability due to grain pinning of Al 2 O 3 dispersoids. - Abstract: Twenty-five samples of commercially available, gas-atomised Al (99.5%) powders with particle sizes 2 O 3 composites formed in situ during extrusion. The effect of particle size, surface area, oxygen content and atomisation atmosphere of the powder on the microstructure and mechanical properties of the extruded compacts were studied by Brunauer, Emmett, Teller (BET) analysis, hot gas extraction, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and tensile tests. Thermal stability of the compacts and the individual strengthening mechanisms operating in the compacts were discussed. It was found that the properties of the compacts stemmed from the extraordinary grain boundary strengthening effect of the ultrafine-grained compacts due to their microstructures. The efficiency of the grain boundary strengthening was significantly enhanced by the presence of nano-metric Al 2 O 3 dispersoids introduced in situ. The strength of the compacts was closely related to the surface area of the powder particles. In addition, the entrapped gasses and chemically bonded humidity had a negative effect on the mechanical properties of the compacts.

Fabrication of spherical high-nitrogen stainless steel powder alloys by mechanical alloying and thermal plasma spheroidization

Science.gov (United States)

Razumov, Nikolay G.; Wang, Qing Sheng; Popovich, Anatoly A.; Shamshurin, Aleksey I.

2018-04-01

This paper describes the results of experimental studies on the treatment of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, synthesized by the mechanical alloying (MA) of elemental powders in the flow of a radio frequency thermal plasma. The as-milled powder with irregular particles were successfully converted into spherical high-nitrogen stainless steel powder alloy. Measurement of the residual nitrogen content in the obtained powder, shown that during the plasma spheroidization process, part of the nitrogen escapes from the alloy.

Thermal expansion studies on Inconel-600[reg] by high temperature X-ray diffraction

International Nuclear Information System (INIS)

Raju, S.; Sivasubramanian, K.; Divakar, R.; Panneerselvam, G.; Banerjee, A.; Mohandas, E.; Antony, M.P.

2004-01-01

The lattice thermal expansion characteristics of Inconel-600[reg] have been studied by high temperature X-ray diffraction (HT-XRD) technique in the temperature range 298-1200 K. Altogether four experimental runs were conducted on thin foils of about 75-100 μm thickness. The diffraction profiles have been accurately calibrated to offset the shift in 2θ values introduced by sample buckling at elevated temperatures. The corrected lattice parameter data have been used to estimate the instantaneous and mean linear thermal expansion coefficients as a function of temperature. The thermal expansion values estimated in the present study show a fair degree of agreement with other existing dilatometer based bulk thermal expansion estimates. The lattice parameter for this alloy at 300 K is found to be 0.3549(1) nm. The mean linear thermal expansivity is found to be 11.4 x 10 -6 K -1

Preparation, Characterization and application of Alumina Powder Produced by advanced Preparation Techniques

International Nuclear Information System (INIS)

Khalil, T.; Abou El Nour, F.; Bossert, J.; Ashor, A.H.

2000-01-01

Aluminum oxide powders were prepared by advanced chemical techniques. The morphology of the produced powders were examined using scanning electron microscopy (SEM). Surface characteristics of the powders were measured through nitrogen gas adsorption and application of the BET equation at 77 K, through the use of nitrogen gas adsorption at liquid nitrogen temperature and application of the Brunauer-Emett-Teller (BET) equation. The total surface area, total pore volume and pore radius of the powders were calculated through the construction of the plots relating the amount of nitrogen gas adsorbed V 1 and the thickness of the adsorbed layer t(V 1 -t plots). The thermal behaviour of the powders were studied with the help of differential thermal analysis (DTA) and thermogravimetry (TG). Due to the presence of some changes in the DTA base lines, possibly as a result of phase transformations, X-ray diffraction was applied to identify these phases. The sintering behaviour of the compact powders after isostatic pressing was evaluated using dilatometry. The sintering temperature of the studied samples were also determined using heating microscopy. The effect of changing sintering temperature and of applying different isostatic pressures on the density and porosity of the compacts was investigated

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....

Influence of reagents mixture density on the radiation-thermal synthesis of lithium-zinc 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

Influence of Li2CO3-ZnO-Fe2O3 powder reagents mixture density on the synthesis efficiency of lithium-zinc ferrites in the conditions of thermal heating or pulsed electron beam heating was studied by X-Ray diffraction and magnetization analysis. The results showed that the including a compaction of powder reagents mixture in ferrite synthesis leads to an increase in concentration of the spinel phase and decrease in initial components content in lithium-substituted ferrites synthesized by thermal or radiation-thermal heating.

Thermal expansion study of simulated DUPIC fuel using neutron diffraction

International Nuclear Information System (INIS)

Kang, Kweon Ho; Ryu, H. J.; Bae, J. H.; Kim, H. S.; Song, K. C.; Yang, M. S.; Choi, Y. N.; Han, Y. S.; Oh, H. S.

2001-07-01

The lattice parameters of simulated DUPIC fuel and UO2 were measured from room temperature to 1273 K using neutron diffraction to investigate the thermal expansion and density variation with temperature. The lattice parameter of simulated DUPIC fuel is lower than that of UO2 and the linear thermal expansion of simulated DUPIC fuel is higher than that of UO2. For the temperature range from 298 to 1273 K, the average linear thermal expansion coefficients for UO2 and simulated DUPIC fuel are 10.471 ''10-6 and 10.751 ''10-6 K-1, respectively

Thermal evolution of the crystal structure of the orthorhombic perovskite LaFeO3

International Nuclear Information System (INIS)

Dixon, Charlotte A.L.; Kavanagh, Christopher M.; Knight, Kevin S.; Kockelmann, Winfried; Morrison, Finlay D.; Lightfoot, Philip

2015-01-01

The thermal evolution of the crystal structure of the prototypical orthorhombic perovskite LaFeO 3 has been studied in detail by powder neutron diffraction in the temperature range 25thermal behavior to be understood. In particular, the largest-amplitude symmetry modes (viz. in-phase and out-of-phase octahedral tilts, and A-site cation displacements) are shown to display relatively ‘normal’ behavior, increasing with decreasing temperature, which contrasts with the anomalous behavior previously shown by the derivative Bi 0.5 La 0.5 FeO 3 . However, an unexpected behavior is seen in the nature of the intra-octahedral distortion, which is used to rationalize the unique occurrence of a temperature dependent crossover of the a and c unit cell metrics in this compound. - Graphical abstract: The unusual thermal evolution of lattice metrics in the perovskite LaFeO 3 is rationalized from a detailed powder neutron diffraction study. - Highlights: • Crystal structure of the perovskite LaFeO 3 studied in detail by powder neutron diffraction. • Unusual thermal evolution of lattice metrics rationalized. • Contrasting behavior to Bi-doped LaFeO 3 . • Octahedral distortion/tilt parameters explain unusual a and c lattice parameter behavior

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...

Thermal expansion coefficient measurement from electron diffraction of amorphous films in a TEM.

Science.gov (United States)

Hayashida, Misa; Cui, Kai; Malac, Marek; Egerton, Ray

2018-05-01

We measured the linear thermal expansion coefficients of amorphous 5-30 nm thick SiN and 17 nm thick Formvar/Carbon (F/C) films using electron diffraction in a transmission electron microscope. Positive thermal expansion coefficient (TEC) was observed in SiN but negative coefficients in the F/C films. In case of amorphous carbon (aC) films, we could not measure TEC because the diffraction radii required several hours to stabilize at a fixed temperature. Crown Copyright © 2018. Published by Elsevier B.V. All rights reserved.

Direct synthesis of nano-sized glass powders with spherical shape by RF (radio frequency) thermal plasma

International Nuclear Information System (INIS)

Seo, J.H.; Kim, J.S.; Lee, M.Y.; Ju, W.T.; Nam, I.T.

2011-01-01

A new route for obtaining very small, spheroid glass powders is demonstrated using an RF (radio frequency) thermal plasma system. During the process, four kinds of chemicals, here SiO 2 , B 2 O 3 , BaCO 3 , and K 2 CO 3 , were mixed at pre-set weight ratios, spray-dried, calcined at 250 deg. C for 3 h, and crushed into fragments. Then, they were successfully reformed into nano-sized amorphous powders (< 200 nm) with spherical shape by injecting them along the centerline of an RF thermal plasma reactor at ∼ 24 kW. The as-synthesized powders show negligible (< 1%) composition changes when compared with the injected precursors of raw material compounds.

The thermal behaviour and structural stability of nesquehonite, MgCO3.3H2O, evaluated by in situ laboratory parallel-beam X-ray powder diffraction: New constraints on CO2 sequestration within minerals.

Science.gov (United States)

Ballirano, Paolo; De Vito, Caterina; Ferrini, Vincenzo; Mignardi, Silvano

2010-06-15

In order to gauge the appropriateness of CO(2) reaction with Mg chloride solutions as a process for storing carbon dioxide, the thermal behaviour and structural stability of its solid product, nesquehonite (MgCO(3).3H(2)O), were investigated in situ using real-time laboratory parallel-beam X-ray powder diffraction. The results suggest that the nesquehonite structure remains substantially unaffected up to 373 K, with the exception of a markedly anisotropic thermal expansion acting mainly along the c axis. In the 371-390 K range, the loss of one water molecule results in the nucleation of a phase of probable composition MgCO(3).2H(2)O, which is characterized by significant structural disorder. At higher temperatures (423-483 K), both magnesite and MgO.2MgCO(3) coexist. Finally, at 603 K, periclase nucleation starts and the disappearance of carbonate phases is completed at 683 K. Consequently, the structural stability of nesquehonite at high temperatures suggests that it will remain stable under the temperature conditions that prevail at the Earth's surface. These results will help (a) to set constraints on the temperature conditions under which nesquehonite may be safely stored and (b) to develop CO(2) sequestration via the synthesis of nesquehonite for industrial application. Copyright 2010 Elsevier B.V. All rights reserved.

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.

Technical assistance for development of thermally conductive nitride filler for epoxy molding compounds

Energy Technology Data Exchange (ETDEWEB)

Ryu, Ho Jin; Song, Kee Chan; Jung, In Ha

2005-07-15

Technical assistance was carried out to develop nitride filler for thermally conductive epoxy molding compounds. Carbothermal reduction method was used to fabricate silicon nitride powder from mixtures of silica and graphite powders. Microstructure and crystal structure were observed by using scanning electron microscopy and x-ray diffraction technique. Thermal properties of epoxy molding compounds containing silicon nitride were measured by using laser flash method. Fabrication process of silicon nitride nanowire was developed and was applied to a patent.

Hardness and thermal stability of cubic silicon nitride

DEFF Research Database (Denmark)

Jiang, Jianzhong; Kragh, Flemming; Frost, D. J.

2001-01-01

The hardness and thermal stability of cubic spinel silicon nitride (c-Si3N4), synthesized under high-pressure and high-temperature conditions, have been studied by microindentation measurements, and x-ray powder diffraction and scanning electron microscopy, respectively The phase at ambient...

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.

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

Preparation of thermally stable nanocrystalline hydroxyapatite by hydrothermal method.

Science.gov (United States)

Prakash Parthiban, S; Elayaraja, K; Girija, E K; Yokogawa, Y; Kesavamoorthy, R; Palanichamy, M; Asokan, K; Narayana Kalkura, S

2009-12-01

Thermally stable hydroxyapatite (HAp) was synthesized by hydrothermal method in the presence of malic acid. X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA) was done on the synthesized powders. These analyses confirmed the sample to be free from impurities and other phases of calcium phosphates, and were of rhombus morphology along with nanosized particles. IR and Raman analyses indicated the adsorption of malic acid on HAp. Thermal stability of the synthesized HAp was confirmed by DTA and TGA. The synthesized powders were thermally stable upto 1,400 degrees C and showed no phase change. The proposed method might be useful for producing thermally stable HAp which is a necessity for high temperature coating applications.

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)

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

Ultra-low thermal conductivities of hot-pressed attapulgite and its potential as thermal insulation material

Energy Technology Data Exchange (ETDEWEB)

Liu, Yuan; Ren, Zhifeng, E-mail: bohr123@163.com, E-mail: zren@uh.edu [Department of Physics and TcSUH, University of Houston, Houston, Texas 77204 (United States); Wang, Xiuzhang [Department of Physics and TcSUH, University of Houston, Houston, Texas 77204 (United States); Hubei Key Laboratory of Pollutant Analysis and Reuse Technology and School of Physics and Electronic Science, Hubei Normal University, Huangshi, Hubei 435002 (China); Wang, Yumei [Department of Physics and TcSUH, University of Houston, Houston, Texas 77204 (United States); Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China); Tang, Zhongjia; Makarenko, Tatyana; Guloy, Arnold [Department of Chemistry, University of Houston, Houston, Texas 77204 (United States); Zhang, Qinyong, E-mail: bohr123@163.com, E-mail: zren@uh.edu [Center for Advanced Materials and Energy, Xihua University, Chengdu, Sichuan 610039 (China)

2016-03-07

In the past, there have been very few reports on thermal properties of attapulgite which is a widely used clay mineral. In this work, we report on extremely low thermal conductivities in attapulgite samples synthesized by hot-pressing. Attapulgite powder was hot-pressed at different temperatures into bulk samples, and a systematic study was conducted on the microstructures and thermal properties. Differential scanning calorimetry analysis shows that hot-pressing induces a rapid dehydration of the attapulgite powders. X-ray diffraction data and scanning/transmission electron microscopy reveal that the hot-pressed attapulgite features high porosity and complex microstructures, including an amorphous phase. As a result, the hot-pressed attapulgite exhibits thermal conductivity less than 2.5 W m{sup −1} K{sup −1} up to 600 °C. For one sample with porosity of 45.7%, the thermal conductivity is as low as 0.34 W m{sup −1} K{sup −1} at 50 °C. This suggests the potential of hot-pressed attapulgite as a candidate for thermal barrier materials.

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.

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)

X-ray diffraction patterns of thermally-reduced graphenes

International Nuclear Information System (INIS)

Ju, Hae-Mi; Choi, Sung-Ho; Huh, Seung-Hun

2010-01-01

Thermally-reduced graphenes (GPs) from graphene oxides (GOs) in the range of 200 - 800 .deg. C have been investigated by using X-ray diffraction (XRD). The temperature-dependent evolutions of the (002) peaks show that exfoliation of GO sheets occurs, along with wrinkling, at ∼200 .deg. C and that high-quality GPs are produced at ∼ 600 .deg. C (GP 600 ). These phenomena are explained by the vaporization of intercalated water molecules and the effective removal of the oxide groups of GO by thermal annealing, respectively. GP 600 exhibited a clean and sharp (002) peak corresponding to an interlayer distance of 3.392 A, which is close to that of conventional graphene (∼3.4 A). The structure of GP 600 is further discussed.

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.

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.

Studies on the sintering behaviour of uranium dioxide powder compacts

International Nuclear Information System (INIS)

Das, P.; Chowdhury, R.

1988-01-01

Uranium dioxide fuel pellets are normally made from their precursor ammonium diuranate, followed by calcination, subsequent reduction to sinterable grade powders and a post operation treatment of pressing and sintering. The low temperature calcined powders, usually exhibiting non-crystalline behaviour (under X-ray diffraction studies) progressively transforms into a crystalline variety on subsequent heat treatment at higher temperature. It is observed however that powders calcined between 800 to 900 0 C exhibit enhanced densification behaviour when sintered at higher temperatures. The isothermal shrinkage versus time plot of the sintered compacts are well described by a hyperbolic relationship which takes care of the observed shrinkage (λ) as caused due to a cumulative effect from the initial sintering of the powder compacts at zero time (α) and that caused due to the structural transformation from a non-crystalline modification with increased thermal treatment (β). The derived equation is a modification of the sintering mechanism of the viscous flow type proposed by Frenkel, involving sintering of an amorphous phase, the viscosity of the latter is presumed to increase with increasing thermal treatment to assume the final modified form as λ=t/(α+βt), where t = time, λ = shrinkage and α and β are the unknown parameters. (orig.)

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)

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.)

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.

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.

Structural characterization and thermal behaviour of biological hydroxyapatite

Czech Academy of Sciences Publication Activity Database

Kohutová, A.; Honcová, P.; Svoboda, L.; Bezdička, Petr; Maříková, Monika

2012-01-01

Roč. 108, č. 1 (2012), s. 163-170 ISSN 1388-6150 Institutional research plan: CEZ:AV0Z40320502 Keywords : hydroxyapatite * hard tissues * X-ray powder diffraction * scanning electron microscope * thermal analysis * mass spectrometry Subject RIV: CA - Inorganic Chemistry Impact factor: 1.982, year: 2012

Effects of Magnetite Aggregate and Steel Powder on Thermal Conductivity and Porosity in Concrete for Nuclear Power Plant

Directory of Open Access Journals (Sweden)

Han-Seung Lee

2016-01-01

Full Text Available Among many engineering advantages in concrete, low thermal conductivity is an attractive property. Concrete has been widely used for nuclear vessels and plant facilities for its excellent radiation shielding. The heat isolation through low thermal conductivity is actually positive for nuclear power plant concrete; however the property may cause adverse effect when fires and melt-down occur in nuclear vessel since cooling down from outer surface is almost impossible due to very low thermal conductivity. If concrete containing atomic reactor has higher thermal conductivity, the explosion risk of conductive may be partially reduced. This paper presents high thermally conductive concrete development. For the work, magnetite with varying replacements of normal aggregates and steel powder of 1.5% of volume are considered, and the equivalent thermal conductivity is evaluated. Only when the replacement ratio goes up to 30%, thermal conductivity increases rapidly to 2.5 times. Addition of steel powder is evaluated to be effective by 1.08~1.15 times. In order to evaluate the improvement of thermal conductivity, several models like ACI, DEMM, and MEM are studied, and their results are compared with test results. In the present work, the effects of steel powder and magnetite aggregate are studied not only for strength development but also for thermal behavior based on porosity.

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

Mechanically Strain-Induced Modification of Selenium Powders in the Amorphization Process

International Nuclear Information System (INIS)

Fuse, Makoto; Shirakawa, Yoshiyuki; Shimosaka, Atsuko; Hidaka, Jusuke

2003-01-01

For the fabrication of particles designed in the nanoscale structure, or the nanostructural modification of particles using mechanical grinding process, selenium powders ground by a planetary ball mill at various rotational speeds have been investigated. Structural analyses, such as particle size distributions, crystallite sizes, lattice strains and nearest neighbour distances were performed using X-ray diffraction, scanning electron microscopy and dynamical light scattering.By grinding powder particles became spherical composites consisting of nanocrystalline and amorphous phase, and had a distribution with the average size of 2.7 μm. Integral intensities of diffraction peaks of annealed crystal selenium decreased with increasing grinding time, and these peaks broadened due to lattice strains and reducing crystallite size during the grinding. The ground powder at 200 rpm did not have the lattice strain and showed amorphization for the present grinding periods. It indicates that the amorphization of Se by grinding accompanies the lattice strain, and the lattice strain arises from a larger energy concerning intermolecular interaction. In this process, the impact energy is spent on thermal and structural changes according to energy accumulation in macroscopic (the particle size distribution) and microscopic (the crystallite size and the lattice strain) range

Thermal evolution behavior of carbides and γ′ precipitates in FGH96 superalloy powder

International Nuclear Information System (INIS)

Zhang Lin; Liu Hengsan; He Xinbo; Rafi-ud-din; Qu Xuanhui; Qin Mingli; Li Zhou; Zhang Guoqing

2012-01-01

The characteristics of rapidly solidified FGH96 superalloy powder and the thermal evolution behavior of carbides and γ′ precipitates within powder particles were investigated. It was observed that the reduction of powder size and the increase of cooling rate had transformed the solidification morphologies of atomized powder from dendrite in major to cellular structure. The secondary dendritic spacing was measured to be 1.02–2.55 μm and the corresponding cooling rates were estimated to be in the range of 1.4 × 10 4 –4.7 × 10 5 K·s −1 . An increase in the annealing temperature had rendered the phase transformation of carbides evolving from non-equilibrium MC′ carbides to intermediate transition stage of M 23 C 6 carbides, and finally to thermodynamically stable MC carbides. The superfine γ′ precipitates were formed at the dendritic boundaries of rapidly solidified superalloy powder. The coalescence, growth, and homogenization of γ' precipitates occurred with increasing annealing temperature. With decreasing cooling rate from 650 °C·K −1 to 5 °C·K −1 , the morphological development of γ′ precipitates had been shown to proceed from spheroidal to cuboidal and finally to solid state dendrites. Meanwhile, a shift had been observed from dendritic morphology to recrystallized structure between 900 °C and 1050 °C. Moreover, accelerated evolution of carbides and γ' precipitates had been facilitated by the formation of new grain boundaries which provide fast diffusion path for atomic elements. - Highlights: ► Microstructural characteristic of FGH96 superalloy powder was investigated. ► The relation between microstructure, particle size, and cooling rate was studied. ► Thermal evolution behavior of γ′ and carbides in loose FGH96 powder was studied.

Recovery Of Electrodic Powder From Spent Nickel-Metal Hydride Batteries (NiMH

Directory of Open Access Journals (Sweden)

Shin S.M.

2015-06-01

Full Text Available This study was focused on recycling process newly proposed to recover electrodic powder enriched in nickel (Ni and rare earth elements (La and Ce from spent nickel-metal hydride batteries (NiMH. In addition, this new process was designed to prevent explosion of batteries during thermal treatment under inert atmosphere. Spent nickel metal hydride batteries were heated over range of 300°C to 600°C for 2 hours and each component was completely separated inside reactor after experiment. Electrodic powder was successfully recovered from bulk components containing several pieces of metals through sieving operation. The electrodic powder obtained was examined by X-ray diffraction (XRD and energy dispersive X-ray spectroscopy (EDX and image of the powder was taken by scanning electron microscopy (SEM. It was finally found that nickel and rare earth elements were mainly recovered to about 45 wt.% and 12 wt.% in electrodic powder, respectively.

Properties of polyester based powder coating containing Cloisite®30B modified with silane 3-aminopropyltriethoxysilane; Propriedades da tinta em po base poliester contendo Cloisite®30B modificada com 3-aminopropiltrietoxisilano

Energy Technology Data Exchange (ETDEWEB)

Bertuoli, P.T.; Frizzo, V.P.; Zattera, A.J., E-mail: paulabertuoli@hotmail.com [Universidade de Caxias do Sul (UCS), RS (Brazil). Programa de Pos-Graduacao em Engenharia de Processos e Tecnologias; Scienza, L.C. [Universidade Federal do Rio Grande do Sul (UFRGS), RS (Brazil). Departamento de Materiais

2014-07-01

The incorporation of clay into a polymer matrix results in nanocomposites with mechanical strength, thermal and barrier properties superior to the free filler matrix. With the aim to obtain a powder coating with better thermal properties than the coating free of filler, the organoclay Cloisite®30B was modified with 3-aminopropyltriethoxysilane (APS) and incorporated to a polyester based powder coating, on proportions of 2 to 8 wt% in the melt state. The powder coatings were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The powder coating containing clay showed no alteration in the basal spacing compared to that basal spacing of the clay. Compared to the powder coating free of the clay, powder coatings containing clay had lower thermal stability due to the presence of the organic modifier. The presence of clay reduced the crosslinking temperature and the incorporation of 2 wt% of the clay caused the increase in the energy released in the crosslinking process. (author)

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...

Preparation and properties of thermal insulation coatings with a sodium stearate-modified shell powder as a filler

Science.gov (United States)

Tang, Qiang; Zhang, Ya-mei; Zhang, Pei-gen; Shi, Jin-jie; Tian, Wu-bian; Sun, Zheng-ming

2017-10-01

Waste shell stacking with odor and toxicity is a serious hazard to our living environment. To make effective use of the natural resources, the shell powder was applied as a filler of outdoor thermal insulation coatings. Sodium stearate (SS) was used to modify the properties of shell powder to reduce its agglomeration and to increase its compatibility with the emulsion. The oil absorption rate and the spectrum reflectance of the shell powder show that the optimized content of SS as a modifier is 1.5wt%. The total spectrum reflectance of the coating made with the shell powder that is modified at this optimum SS content is 9.33% higher than that without any modification. At the optimum SS content of 1.5wt%, the thermal insulation of the coatings is improved by 1.0°C for the cement mortar board and 1.6°C for the steel plate, respectively. The scouring resistance of the coating with the 1.5wt% SS-modified shell powder is three times that of the coating without modification.

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

Energy Technology Data Exchange (ETDEWEB)

Rybak, Jens-Christoph

2012-07-01

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

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

Science.gov (United States)

Yamamura, Shigeo; Momose, Yasunori

2003-06-18

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

A 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)

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.

Preparation of fine powdered composite for latent heat storage

Energy Technology Data Exchange (ETDEWEB)

Fořt, Jan, E-mail: jan.fort.1@fsv.cvut.cz; Trník, Anton, E-mail: anton.trnik@fsv.cvut.cz; Pavlíková, Milena, E-mail: milena.pavlikova@fsv.cvut.cz; Pavlík, Zbyšek, E-mail: pavlikz@fsv.cvut.cz [Department of Materials Engineering and Chemistry, Faculty of Civil Engineering, Czech Technical University in Prague, Thákurova 7, 166 29 Prague (Czech Republic); Pomaleski, Marina, E-mail: marina-pomaleski@fsv.cvut.cz [Faculty of Civil Engineering, Architecture and Urbanism, University of Campinas, R. Saturnino de Brito 224, 13083-889 Campinas – SP (Brazil)

2016-07-07

Application of latent heat storage building envelope systems using phase-change materials represents an attractive method of storing thermal energy and has the advantages of high-energy storage density and the isothermal nature of the storage process. This study deals with a preparation of a new type of powdered phase change composite material for thermal energy storage. The idea of a composite is based upon the impregnation of a natural silicate material by a reasonably priced commercially produced pure phase change material and forming the homogenous composite powdered structure. For the preparation of the composite, vacuum impregnation method is used. The particle size distribution accessed by the laser diffraction apparatus proves that incorporation of the organic phase change material into the structure of inorganic siliceous pozzolana does not lead to the clustering of the particles. The compatibility of the prepared composite is characterized by the Fourier transformation infrared analysis (FTIR). Performed DSC analysis shows potential of the developed composite for thermal energy storage that can be easily incorporated into the cement-based matrix of building materials. Based on the obtained results, application of the developed phase change composite can be considered with a great promise.

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)

Thermal Plasma Spheroidization of High-Nitrogen Stainless Steel Powder Alloys Synthesized by Mechanical Alloying

Science.gov (United States)

Razumov, Nikolay G.; Popovich, Anatoly A.; Wang, QingSheng

2018-03-01

This paper presents the results of experimental studies on the treatment of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, synthesized by the mechanical alloying (MA) of elemental powders in the flow of a thermal plasma. Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys were prepared by MA in the attritor under an argon atmosphere. For spheroidization of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, the TekSphero 15 plant manufactured by Tekna Plasma Systems Inc was used. The studies have shown the possibility of obtaining Fe-23Cr-11Mn-1N high-nitrogen spherical powders steel alloys from the powder obtained by MA. According to the results of a series of experiments, it was found that the results of plasma spheroidization of powders essentially depend on the size of the fraction due to some difference in the particle shape and flowability, and on the gas regime of the plasma torch. It is established that during the plasma spheroidization process, some of the nitrogen leaves the alloy. The loss rate of nitrogen depends on the size of the initial particles.

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

Synthesis of (Cr,V){sub 2}(C,N) solid solution powders by thermal processing precursors

Energy Technology Data Exchange (ETDEWEB)

Liu, Anrui [School of Materials Science & Engineering, Sichuan University, Chengdu, 610065 (China); Liu, Ying [School of Materials Science & Engineering, Sichuan University, Chengdu, 610065 (China); Key Laboratory of Advanced Special Material & Technology, Ministry of Education, Chengdu, 610065 (China); Ma, Shiqing; Qiu, Yuchong; Rong, Pengcheng; Ye, Jinwen [School of Materials Science & Engineering, Sichuan University, Chengdu, 610065 (China)

2017-06-01

The single-phase (Cr,V){sub 2}(C,N) solid solution powders were fabricated via carbothermal reduction-nitridation (CRN) processing technique. The effects of heat treatment temperature, nitrogen pressure and carbon proportion were experimentally studied in detail by X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and thermal analysis. The chemical transformations of vanadium and chromium compounds were as follows: precursors → V{sub 2}O{sub 3}, Cr{sub 2}O{sub 3} → Cr{sub 3}C{sub 2}, Cr{sub 2}O{sub 3}, (Cr,V){sub 2}(C,N) → (Cr,V){sub 2}(C,N). When the heat-treated temperature was below 1200 °C, chromium oxides didn’t completely react. However, higher temperature ∼1300 °C could not only lead to the segregation of some nitrides and carbon black, but also to the occurrence of fiber-bridged particles. The system nitrogen pressure over 0.03 MPa would cause a subtle transformation of (Cr,V){sub 2}(C,N) to VCrN{sub 2}. When the carbon proportion was below 15 wt%, the oxides could not be completely reduced, while when the carbon proportion was above 15.5 wt%, some undesired carbides, like Cr{sub 23}C{sub 6} and Cr{sub 3}C{sub 2}, would form. Ultimately, the homogeneously distributed pure-phase (Cr,V){sub 2}(C,N) spherical particles with the average size of ∼1.5 μm were obtained at the optimal conditions of the treatment of precursors at 1200 °C for 1 h with the nitrogen pressure of 0.03 MPa and carbon content of 15.5 wt%. The chemical composition of the solid solution with the optimal process could be drawn as (Cr{sub 0.85}V{sub 0.15}){sub 2}(C{sub 0.57}N{sub 0.43}). Thermal processing precursors method shows the advantages of lower synthesis temperature, shorter period and finer particles when comparing with the conventional preparations. - Highlights: • Single phase of (Cr,V){sub 2}(C,N) powders were synthesized for the first time. • Precursors were used to prepared the powders by carbothermal

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

Characterisation of WC-12Co thermal spray powders and HPHVOF wear resistant coatings

CSIR Research Space (South Africa)

Lovelock, HDL

1998-01-01

Full Text Available were selected for the deposition of thermal spray coatings using the JP 5000 high pressure high velocity oxyfuel (HPHVOF) system. Dry sand rubber wheel abrasion tests were performed on the coatings in order to determine the effect of powder...

The incorporation of exhauster powder mass in ceramics atomised

International Nuclear Information System (INIS)

Knop, W.R.; Valentina, L. Dalla; Folgueiras, M.V.; Semptikovski, S.C.

2009-01-01

Inside the context of alternative search for the use of industrial waste as natural raw for the industrial ceramic, this work had the objective to evaluate the possibility of the use of exhauster powder generated in the foundry process. The characterization was performed by scanning electron microscopy, x-ray diffractometry and thermal analysis, noting that it is a powder with a high content of fine and compatible with the composition of ceramic bodies. Formulations were prepared with different exhauster powder content. The sintered materials at 1000, 1100 and 1200 deg C were characterized according technological properties as water absorption, linear shrinkage, bulk density and apparent density. Microstructural analysis was carried out by scanning electron microscopy and X-ray diffraction. The results showed that it is possible to use the waste. It was observed that the waste increase the density in sintering process, and with high levels of waste occurs an increase of the porosity and intensification in the color of the new material. (author)

Quantifying the properties of low-cost powder metallurgy titanium alloys

International Nuclear Information System (INIS)

Bolzoni, L.; Ruiz-Navas, E.M.; Gordo, E.

2017-01-01

The extensive industrial employment of titanium is hindered by its high production costs where reduction of these costs can be achieved using cheap alloying elements and appropriate alternative processing techniques. In this work the feasibility of the production of low-cost titanium alloys is addressed by adding steel to pure titanium and processing the alloys by powder metallurgy. In particular, a spherical 4140 LCH steel powder commonly used in metal injection moulding is blended with irregular hydride-dehydride Ti. The new low-cost alloys are cold uniaxially pressed and sintered under high vacuum and show comparable properties to other wrought-equivalent and powder metallurgy titanium alloys. Differential thermal analysis and X-ray diffraction analyses confirm that Ti can tolerate the employment of iron as primary alloying element without forming detrimental TiFe-based intermetallic phases. Thus, the newly designed α+β alloys could be used for cheaper non-critical components.

Quantifying the properties of low-cost powder metallurgy titanium alloys

Energy Technology Data Exchange (ETDEWEB)

Bolzoni, L., E-mail: bolzoni.leandro@gmail.com [WaiCAM (Waikato Centre for Advanced Materials), The University of Waikato, Private Bag 3105, 3240 Hamilton (New Zealand); Ruiz-Navas, E.M.; Gordo, E. [Department of Materials Science and Engineering, University Carlos III of Madrid, Avda. de la Universidad, 30, 28911 Leganés, Madrid (Spain)

2017-02-27

The extensive industrial employment of titanium is hindered by its high production costs where reduction of these costs can be achieved using cheap alloying elements and appropriate alternative processing techniques. In this work the feasibility of the production of low-cost titanium alloys is addressed by adding steel to pure titanium and processing the alloys by powder metallurgy. In particular, a spherical 4140 LCH steel powder commonly used in metal injection moulding is blended with irregular hydride-dehydride Ti. The new low-cost alloys are cold uniaxially pressed and sintered under high vacuum and show comparable properties to other wrought-equivalent and powder metallurgy titanium alloys. Differential thermal analysis and X-ray diffraction analyses confirm that Ti can tolerate the employment of iron as primary alloying element without forming detrimental TiFe-based intermetallic phases. Thus, the newly designed α+β alloys could be used for cheaper non-critical components.

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.

Synthesis of Nanocrystalline RuO2(60%)-SnO2(40%)Powders by Amorphous Citrate Route

Institute of Scientific and Technical Information of China (English)

无

2007-01-01

Nanometer RuO2-SnO2was synthesized by the citrate-gel method using RuCl3, SnCl4 as cation sources, citric acid as complexing agent and anhydrous ethanol as solvent. The structures of the derived powders were characterized by thermogravimetric and differential thermal analysis, X-ray diffraction, transmission electron microscope, and Brunauer-Emmett-Teller surface area measurement. The pure, fine and amorphous powders was obtained at 160℃. The materials calcined at above 400 ℃ were composed of rutile-type oxide phases having particle sizes of fairly narrow distribution and good thermal resistant properties. By adding SnO2 to RUO2, the Ru metallic phase can be effectively controlled under a traditional temperature of preparation for dimensional stable anode.

Direct Iron Coating onto Nd-Fe-B Powder by Thermal Decomposition of Iron Pentacarbonyl

International Nuclear Information System (INIS)

Yamamuro, S; Okano, M; Tanaka, T; Sumiyama, K; Nozawa, N; Nishiuchi, T; Hirosawa, S; Ohkubo, T

2011-01-01

Iron-coated Nd-Fe-B composite powder was prepared by thermal decomposition of iron pentacarbonyl in an inert organic solvent in the presence of alkylamine. Though this method is based on a modified solution-phase process to synthesize highly size-controlled iron nanoparticles, it is in turn featured by a suppressed formation of iron nanoparticles to achieve an efficient iron coating solely onto the surfaces of rare-earth magnet powder. The Nd-Fe-B magnetic powder was successfully coated by iron shells whose thicknesses were of the order of submicrometer to micrometer, being tuneable by the amount of initially loaded iron pentacarbonyl in a reaction flask. The amount of the coated iron reached to more than 10 wt.% of the initial Nd-Fe-B magnetic powder, which is practically sufficient to fabricate Nd-Fe-B/α-Fe nanocomposite permanent magnets.

Neutron diffraction study, magnetic properties and thermal stability of YMn2D6 synthesized under high deuterium pressure

International Nuclear Information System (INIS)

Paul-Boncour, V.; Filipek, S.M.; Dorogova, M.; Bouree, F.; Andre, G.; Marchuk, I.; Percheron-Guegan, A.; Liu, R.S.

2005-01-01

A new phase YMn 2 D 6 was synthesized by submitting YMn 2 to 1.7kbar deuterium pressure at 473K. According to X-ray and neutron powder diffraction experiments, YMn 2 D 6 crystallizes in the Fm3-bar m space group with a=6.709(1)A at 300K. The Y and half of the Mn atoms occupy statistically the 8c site whereas the other Mn atoms are located in 4a site and surrounded by 6D atoms (24e). This corresponds to a K 2 PtCl 6 -type structure with a partially disordered substructure which can be written as [YMn]MnH 6 . No ordered magnetic moment is observed in the NPD patterns and the magnetization measurements display a paramagnetic behavior. The study of the thermal stability by Differential Scanning Calorimetry and XRD experiments indicates that this phase decomposes in YD 2 and Mn at 625K, and is more stable than YMn 2 H 4.5

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

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

Science.gov (United States)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

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.

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

International Nuclear Information System (INIS)

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

1988-01-01

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

Effect of heat treatment on Fe-B-Si-Nb alloy powder prepared by mechanical alloying

Directory of Open Access Journals (Sweden)

Rodrigo Estevam Coelho

2005-06-01

Full Text Available The effect of heat treatment on crystallization behavior of Fe73.5B15Si10Nb1.5 alloy powder prepared by mechanical alloying was studied. The powder samples were prepared by mechanical alloying (MA and for different milling times (1, 5, 25, 70 and 100 hours. Crystalline powders of iron, boron, silicon and niobium were sealed with tungsten carbide balls in a cylindrical vial under nitrogen atmosphere. The ball-to-powder weight ratio was 20 to 1. A Fritsch Pulverizette 5 planetary ball mill was used for MA the powders at room temperature and at 250 rpm. To study the microstructural evolution, a small amount of powder was collected after different milling times and examined by X-ray diffraction, using CuKalpha radiation (lambda = 0.15418 nm. The crystallization behavior was studied by differential thermal analysis, from 25 up to 1000 °C at a heating rate of 25 °C min-1.

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

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)

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.

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)

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.

LSA glass-ceramic tiles made by powder pressing; Obtencao de placas vitroceramicas do sistema LSA utilizando a prensagem de pos

Energy Technology Data Exchange (ETDEWEB)

Figueira, F.C.; Bertan, F.M. [Colorminas Colorificio e Mineracao, Icara, SC (Brazil); Riella, H.G. [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Programa de Pos-Graduaco em Engenharia Quimica; Uggioni, E. [Universidade do Extremo Sul Catarinense (UFSC), Florianopolis, SC (Brazil). Curso de Engenharia de Materiais; Bernardin, A.M., E-mail: amb@unesc.ne [Servico Nacional de Aprendizagem Industrial (SENAI), Tijucas, SC (Brazil). Dept. de Tecnologia em Ceramica

2009-07-01

A low cost alternative for the production of glass-ceramic materials is the pressing of the matrix glass powders and its consolidation simultaneously with crystallization in a single stage of sintering. The main objective of this work was to obtain LSA glass ceramics with low thermal expansion, processed by pressing and sintering a ceramic frit powder. The raw materials were homogenized and melted (1480 deg C, 80min), and the melt was poured in water. The glass was chemically (XRF and AAS) and thermally (DTA, 10 deg C/min, air) characterized, and then ground (60min and 120min). The ground powders were characterized (laser diffraction) and compressed (35MPa and 45MPa), thus forming four systems. The compacts were dried (150 deg C, 24h) and sintered (1175 deg C and 1185 deg C, 10 deg C/min). Finally, the glass-ceramics were characterized by microstructural analysis (SEM and XRD), mechanical behavior ({sigma}bending) and thermal analysis ({alpha}). The best results for thermal expansion were those for the glass-ceramics processed with smaller particle size and greater compaction pressure. (author)

Extruded Al-Al{sub 2}O{sub 3} composites formed in situ during consolidation of ultrafine Al powders: Effect of the powder surface area

Energy Technology Data Exchange (ETDEWEB)

Balog, Martin, E-mail: martin.balog@savba.sk [Institute of Materials and Machine Mechanics, Slovak Academy of Sciences, Bratislava (Slovakia); Simancik, Frantisek [Institute of Materials and Machine Mechanics, Slovak Academy of Sciences, Bratislava (Slovakia); Walcher, Martin; Rajner, Walter [NMD - New Materials Development GmbH, St. Pantaleon (Austria); Poletti, Cecilia [Institute of Materials Science and Welding, Graz University of Technology, Kopernikusgasse 24/I, A8010 Graz (Austria)

2011-11-25

Highlights: {yields} 25 gas atomised Al 99.5% powders with particle size <10 {mu}m were hot extruded. {yields} The strength of compacts was closely related to powder surface area. {yields} Grain boundary strengthening was enhanced by the presence of in situ Al{sub 2}O{sub 3} dispersoids. {yields} Compacts showed good thermal stability due to grain pinning of Al{sub 2}O{sub 3} dispersoids. - Abstract: Twenty-five samples of commercially available, gas-atomised Al (99.5%) powders with particle sizes <10 {mu}m were hot extruded into Al-Al{sub 2}O{sub 3} composites formed in situ during extrusion. The effect of particle size, surface area, oxygen content and atomisation atmosphere of the powder on the microstructure and mechanical properties of the extruded compacts were studied by Brunauer, Emmett, Teller (BET) analysis, hot gas extraction, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and tensile tests. Thermal stability of the compacts and the individual strengthening mechanisms operating in the compacts were discussed. It was found that the properties of the compacts stemmed from the extraordinary grain boundary strengthening effect of the ultrafine-grained compacts due to their microstructures. The efficiency of the grain boundary strengthening was significantly enhanced by the presence of nano-metric Al{sub 2}O{sub 3} dispersoids introduced in situ. The strength of the compacts was closely related to the surface area of the powder particles. In addition, the entrapped gasses and chemically bonded humidity had a negative effect on the mechanical properties of the compacts.

Effect of composition and heat treatment on the phase formation of mechanically alloyed Cr-B and Mo-B powders

International Nuclear Information System (INIS)

Wu, H M; Hu, C J; Pai, K Y

2009-01-01

Blended elemental Cr-B and Mo-B powders in atomic ratio of 67:33, 50:50, and 20:80 were subjected to mechanical alloying up to 60 h and subsequent heat treatment to investigate effect of composition and heat treatment on the phase formation of Cr-B and Mo-B powders. It was studied by X-ray diffraction and differential thermal analysis. Mechanical alloying these powder mixtures for 60 h leads essentially to a amorphous structure except for the Mo 20 B 80 powder, which creates a partially amorphous MoB 4 structure. Annealing at lower temperatures relieves the strains cumulative in the milled powders and creates no new phase. The structures obtained after annealing the milled powders at higher temperature vary and depend on the overall composition of the powder mixtures. Annealing the milled Mo-B powders having greater Mo content ends up with a dissociation reaction at higher temperature.

Thermal behaviour and microanalysis of coal subbituminus

Science.gov (United States)

Heriyanti; Prendika, W.; Ashyar, R.; Sutrisno

2018-04-01

Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRD) is used to study the thermal behaviour of sub-bituminous coal. The DSC experiment was performed in air atmosphere up to 125 °C at a heating rate of 25 °C min1. The DSC curve showed that the distinct transitional stages in the coal samples studied. Thermal heating temperature intervals, peak and dissociation energy of the coal samples were also determined. The XRD analysis was used to evaluate the diffraction pattern and crystal structure of the compounds in the coal sample at various temperatures (25-350 °C). The XRD analysis of various temperatures obtained compounds from the coal sample, dominated by quartz (SiO2) and corundum (Al2O3). The increase in temperature of the thermal treatment showed a better crystal formation.

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

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

International Nuclear Information System (INIS)

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

1995-01-01

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

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

Influence of Diatomite and Mineral Powder on Thermal Oxidative Ageing Properties of Asphalt

Directory of Open Access Journals (Sweden)

Yongchun Cheng

2015-01-01

Full Text Available Ageing of asphalt affects the performances of asphalt pavement significantly. Therefore, effects of diatomite and mineral powder on ageing properties of asphalt were investigated systematically in order to improve the antiageing property of mixture. Thin film oven test (TFOT was used to conduct the short term ageing in laboratory. Softening points, penetrations, force ductility, low temperature creep properties, and viscosities of asphalt mastics were tested before and after TFOT, respectively. Results indicated that percent retained penetration (PRP increased with the increasing of fillers. Increment of softening point (ΔT, ductility retention rate (DRR, deformation energy ageing index (JAI, and viscosity ageing index (VAI of asphalt mastics nonlinearly decreased with the increasing of fillers. Ageing of asphalt was reduced by diatomite and mineral powder. And the antiageing effect of diatomite was better than that of mineral powder as a result of its porous structure. It is suggested that the mineral powder could be reasonably replaced by diatomite in order to reduce thermal oxidative ageing of asphalt mixture. The optimal content of diatomite 12.8% is also suggested for engineering.

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)

Determination of X-Ray Diffraction on the Phase Transformation of Microwave-Assisted Titanate Nanotubes during Thermal Treatment

Directory of Open Access Journals (Sweden)

Hsin-Hung Ou

2010-01-01

Full Text Available Based on the determination of X-ray powder diffraction, this study aims to investigate the thermal effect on the phase transformation of microwave-assisted titanate nanotubes (MTNTs. The phase transformation is highly dependent on the intercalating amount of Na(I within MTNTs and on the heating atmosphere. In other words, the presence of Na(I favors the transformation of TNTs phase into Na2Ti6O13 whereas anatase phase selectively formed in the case of MTNTs with less Na(I amount. Furthermore, H2 versus O2 is able to form anatase phase and establish a newly transformation pathway. The photocatalytic ability of the calcined MTNTs was also evaluated based on the observed rate constant of trichloroethylene degradation. In addition to anatase phase, the newly phase including Na2Ti6O13 and Ti2O3 with calcined MTNTs is able to photocatalyze trichloroethylene. MTNTs calcined with the presence of H2 also exhibit a superior photocatalytic performance to P25 TiO2.

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)

Water Outgassing from PBX-9502 powder by isoconversional thermal analysis

International Nuclear Information System (INIS)

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

2009-01-01

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

Monitoring alloy formation during mechanical alloying process by x-ray diffraction techniques

International Nuclear Information System (INIS)

Abdul Kadir Masrom; Noraizam Md Diah; Mazli Mustapha

2002-01-01

Monitoring alloying (MA) is a novel processing technique that use high energy impact ball mill to produce alloys with enhanced properties and microscopically homogeneous materials starting from various powder mixtures. Mechanical alloying process was originally developed to produce oxide dispersion strengthened nickel superalloys. In principal, in high-energy ball milling process, alloy is formed by the result of repeated welding, fracturing and rewelding of powder particles in a high energy ball mill. In this process a powder mixture in a ball mill is subjected to high-energy collisions among balls. MA has been shown to be capable of synthesizing a variety of materials. It is known to be capable to prepare equilibrium and non-equilibrium phases starting from blended elemental or prealloyed powders. The process ability to produce highly metastable materials such as amorphous alloys and nanostructured materials has made this process attractive and it has been considered as a promising material processing technique that could be used to produce many advanced materials at low cost. The present study explores the conditions under which aluminum alloys formation occurs by ball milling of blended aluminum and its alloying elements powders. In this work, attempt was made in producing aluminum 2024 alloys by milling of blended elemental aluminum powder of 2024 composition in a stainless steel container under argon atmosphere for up to 210 minutes. X-ray diffraction together with thermal analysis techniques has been used to monitor phase changes in the milled powder. Results indicate that, using our predetermined milling parameters, alloys were formed after 120 minutes milling. The thermal analysis data was also presented in this report. (Author)

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.

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 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

Research on Zr50Al15-xNi10Cu25Yx amorphous alloys prepared by mechanical alloying with commercial pure element powders

International Nuclear Information System (INIS)

Long Woyun; Ouyang Xueqiong; Luo Zhiwei; Li Jing; Lu Anxian

2011-01-01

Amorphous Zr 50 Al 15-x Ni 10 Cu 25 Y x alloy powders were fabricated by mechanical alloying at low vacuum with commercial pure element powders. The effects on glass forming ability of Al partial substituted by Y in Zr 50 Al 15 Ni 10 Cu 25 and thermal stability of Si 3 N 4 powders addition were investigated. The as-milled powders were characterized by X-ray diffraction, scanning electron microscopy and differential scanning calorimeter. The results show that partial substitution of Al can improve the glass forming ability of Zr 50 Al 15 Ni 10 Cu 25 alloy. Minor Si 3 N 4 additions raise the crystallization activation energy of the amorphous phase and thus improve its thermal stability. -- Research Highlights: → ZrAlNiCu amorphous alloys can be synthesized by MA in low cost. → Appropriate amount of Al substituted by Y in ZrAlNiCu alloy can improve its glass forming ability. → A second phase particle addition helps to improve the thermal stability of the amorphous matrix.

Fabrication of Powder Metallurgy Pure Ti Material by Using Thermal Decomposition of TiH2

Science.gov (United States)

Mimoto, Takanori; Nakanishi, Nozomi; Umeda, Junko; Kondoh, Katsuyoshi

Titanium (Ti) and titanium alloys have been interested as an engineering material because they are widely used across various industrial applications, for example, motorcycle, automotive and aerospace industries, due to their light weight, high specific strength and superior corrosion resistance. Ti materials are particularly significant for the aircraft using carbon/carbon (C/C) composites, for example, carbon fiber reinforced plastics (CFRP), because Ti materials are free from the problem of contact corrosion between C/C composites. However, the applications of Ti materials are limited because of their high cost. From a viewpoint of cost reduction, cost effective process to fabricate Ti materials is strongly required. In the present study, the direct consolidation of titanium hydride (TiH2) raw powders in solid-state was employed to fabricate pure Ti bulk materials by using thermal decomposition of TiH2. In general, the production cost of Ti components is expensive due to using commercially pure (CP) Ti powders after dehydrogenation. On the other hand, the novel process using TiH2 powders as starting materials is a promising low cost approach for powder metallurgy (P/M) Ti products. Furthermore, this new process is also attractive from a viewpoint of energy saving because the dehydrogenation is integrated into the sintering process. In this study, TiH2 raw powders were directly consolidated by conventional press technique at 600 MPa to prepare TiH2 powder compacted billets. To thermally decompose TiH2 and obtain sintered pure Ti billets, the TiH2 powder billets were heated in the integrated sintering process including dehydrogenation. The hot-extruded pure Ti material, which was heat treated at 1273 K for 180 min in argon gas atmosphere, showed tensile strength of 701.8 MPa and elongation of 27.1%. These tensile properties satisfied the requirements for JIS Ti Grade 4. The relationship between microstructures, mechanical properties response and heat treatment

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-03-15

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

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...

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)

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

Structure and Thermal Expansion of YSZ and La2Zr2O7 Above 1500°C from Neutron Diffraction on Levitated Samples

International Nuclear Information System (INIS)

Ushakov, Sergey V.; Neuefeind, Joerg C.

2015-01-01

High-temperature time-of-flight neutron diffraction experiments were performed in this paper on cubic yttria-stabilized zirconia (YSZ, 10 mol% YO 1.5 ) and lanthanum zirconate (LZ) prepared by laser melting. Three spheroids of each composition were aerodynamically levitated and rotated in argon flow and heated with a CO 2 laser. Unit cell, positional and atomic displacement parameters were obtained by Rietveld analysis. Below ~1650°C the mean thermal expansion coefficient (TEC) for YSZ is higher than for LZ (13 ± 1 vs. 10.3 ± 0.6) × 10 -6 /K. From ~1650°C to the onset of melting of LZ at ~2250°C, TEC for YSZ and LZ are similar and within (7 ± 2) × 10 -6 /K. LZ retains the pyrochlore structure up to the melting temperature with Zr coordination becoming closer to perfectly octahedral. Congruently melting LZ is La deficient. The occurrence of thermal disordering of oxygen sublattice (Bredig transition) in defect fluorite structure was deduced from the rise in YSZ TEC to ~25 × 10 -6 /K at 2350°C–2550°C with oxygen displacement parameters (U iso ) reaching 0.1 Å 2 , similar to behavior observed in UO 2 . Acquisition of powder-like high-temperature neutron diffraction data from solid-levitated samples is feasible and possible improvements are outlined. Finally, this methodology should be applicable to a wide range of materials for high-temperature applications.

Influence of Al on the magnetic properties of TmCo{sub 4}Al compound, a magnetic and neutron diffraction study

Energy Technology Data Exchange (ETDEWEB)

Laslo, A. [CNRS, Inst. Néel, F-38042 Grenoble (France); Univ. Grenoble Alpes, Inst. Néel, F-38042 Grenoble (France); Babes-Bolyai University, Faculty of Physics, 400084 Cluj-Napoca (Romania); Pop, V. [Babes-Bolyai University, Faculty of Physics, 400084 Cluj-Napoca (Romania); Isnard, O. [CNRS, Inst. Néel, F-38042 Grenoble (France); Univ. Grenoble Alpes, Inst. Néel, F-38042 Grenoble (France)

2015-03-25

Highlights: • The existence of a compensation temperature is found for TmCo{sub 4}Al. • The crystal structure and its thermal evolution are analysed by X-ray and neutron diffraction. • The ferrimagnetic magnetic structure of TmCo{sub 4}Al is established. • Magnetic properties are determined. • Significant coercivity is reported for TmCo{sub 4}Al. - Abstract: The structural and magnetic properties of the TmCo{sub 4}Al compound are presented as deduced from magnetic measurements, X-ray and neutron powder diffraction. The crystal structure is obtained in the light of Rietveld refinement of the neutron powder diffraction pattern. The symmetry of the CaCu{sub 5} structure is preserved and the Al atom is found to substitute the Co one exclusively on the 3g atomic position. Thermal expansion of the crystal lattice is reported, the temperature variation occurring mostly along the basal hexagonal plane. This compound exhibits a ferrimagnetic structure, the Tm and Co magnetic moments being coupled antiparallel. An ordering temperature of 511 K is found. The thermal dependence of the Tm magnetic moment is obtained down to 4 K. A compensation of the two sublattice magnetization is found at 75 K, a feature induced by the Al for Co substitution and not observed in the corresponding TmCo{sub 5} compound. Magnetization curves reveal large coercivity values at low temperature such as 2.48 T at 2 K.

Thermal stability of nanocrystalline ε-Fe2O3

Czech Academy of Sciences Publication Activity Database

Brázda, Petr; Večerníková, Eva; Pližingrová, Eva; Lančok, Adriana; Nižňanský, D.

2014-01-01

Roč. 117, č. 1 (2014), s. 85-91 ISSN 1388-6150 R&D Projects: GA ČR GAP204/10/0035 Institutional support: RVO:61388980 Keywords : ε-Fe2O3 * Differential thermal analysis * Evolved gas analysis * Infrared spectroscopy * Thermogravimetry * X-ray powder diffraction Subject RIV: CA - Inorganic Chemistry Impact factor: 2.042, year: 2014

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.

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.

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.

Synthesis of nanocrystalline magnesium nitride (Mg3N2) powder using thermal plasma

International Nuclear Information System (INIS)

Kim, Dong-Wook; Kim, Tae-Hee; Park, Hyun-Woo; Park, Dong-Wha

2011-01-01

Nanocrystalline magnesium nitride (Mg 3 N 2 ) powder was synthesized from bulk magnesium by thermal plasma at atmospheric pressure. Magnesium vapor was generated through heating the bulk magnesium by DC plasma jet and reacted with ammonia gas. Injecting position and flow rates of ammonia gas were controlled to investigate an ideal condition for Mg 3 N 2 synthesis. The synthesized Mg 3 N 2 was cooled and collected on the chamber wall. Characteristics of the synthesized powders for each experimental condition were analyzed by X-ray diffractometer (XRD), scanning electron microscopy (SEM) and thermogravity analysis (TGA). In absence of NH 3 , magnesium metal powder was formed. The synthesis with NH 3 injection in low temperature region resulted in a formation of crystalline magnesium nitride with trigonal morphology, whereas the mixture of magnesium metal and amorphous Mg 3 N 2 was formed when NH 3 was injected in high temperature region. Also, vaporization process of magnesium was discussed.

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...

Thermal decomposition of lanthanide and actinide tetrafluorides

International Nuclear Information System (INIS)

Gibson, J.K.; Haire, R.G.

1988-01-01

The thermal stabilities of several lanthanide/actinide tetrafluorides have been studied using mass spectrometry to monitor the gaseous decomposition products, and powder X-ray diffraction (XRD) to identify solid products. The tetrafluorides, TbF 4 , CmF 4 , and AmF 4 , have been found to thermally decompose to their respective solid trifluorides with accompanying release of fluorine, while cerium tetrafluoride has been found to be significantly more thermally stable and to congruently sublime as CeF 4 prior to appreciable decomposition. The results of these studies are discussed in relation to other relevant experimental studies and the thermodynamics of the decomposition processes. 9 refs., 3 figs

Thermal expansion of L-ascorbic acid

Science.gov (United States)

Nicolaï, B.; Barrio, M.; Tamarit, J.-Ll.; Céolin, R.; Rietveld, I. B.

2017-04-01

The specific volume of vitamin C has been investigated by X-ray powder diffraction as a function of temperature from 110 K up to complete degradation around 440 K. Its thermal expansion is relatively small in comparison with other organic compounds with an expansivity α v of 1.2(3) × 10-4 K-1. The structure consists of strongly bound molecules in the ac plane through a dense network of hydrogen bonds. The thermal expansion is anisotropic. Along the b axis, the expansion has most leeway and is about 10 times larger than in the other directions.

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)

Combustion synthesis of nanocrystalline ceria (CeO2) powders by a dry route

International Nuclear Information System (INIS)

Hwang, C.-C.; Huang, T.-H.; Tsai, J.-S.; Lin, C.-S.; Peng, C.-H.

2006-01-01

In this study, ceria (CeO 2 ) powders were synthesized with 50 g per batch via a combustion technique using two kinds of starting materials-urea [(NH 2 ) 2 CO] (as a fuel) and ceric ammonium nitrate [Ce(NH 4 ) 2 (NO 3 ) 6 ] (acting as both the source of cerium ion and an oxidizer). The starting materials were mixed thoroughly without adding water, and then ignited in the air at room temperature. It underwent a self-combustion process with a large amount of smoke, a voluminous loose product. The as-synthesized powders were characterized by X-ray diffraction (XRD) analysis, transmission electron microscope (TEM), scanning electron microscope (SEM), CHN elemental analyzer, surface area measurements, and sinterability. Experimental results revealed that the nanocrystalline CeO 2 powders with low impurity content ( 2 /g and ∼25 nm, respectively, through the stoichiometric fuel/oxidizer ratio reaction. The powder, when cold pressed and sintered in the air at 1250 deg. C for 1 h, was measured to attain the sintered density ∼92% of theoretical density having submicron grain size. In addition, the thermal decomposition and combustion process of the reactant mixture were investigated using thermogravimetry (TG), differential scanning calorimetry (DSC), and mass spectrometry (MS) techniques simultaneously. Based on the results of thermal analysis, a possible mechanism concerning the combustion reaction is proposed

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

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...

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

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.

Influence of a microcomposite and a nanocomposite on the properties of an epoxy-based powder coating

International Nuclear Information System (INIS)

Piazza, Diego; Lorandi, Natalia P.; Pasqual, Charles I.; Scienza, Lisete C.; Zattera, Ademir J.

2011-01-01

Highlights: → New materials for using as protective coatings for metal surfaces. → Development of nanostructured powder paints. → Characterization of the new material in the powder and coating form. → Development of a new material for use in the automotive industry, industrial production of appliances, furniture industry. → Development of new material using the process of mixing using a twin-screw extruder, followed by sintering process on a metal plate. - Abstract: The incorporation of nanoclays into coatings has been considered to be commercially favorable due to the improvements obtained in the barrier, thermal, and anticorrosion properties, among others, leading to the development of a new segment in the area of clean technologies: the application of nanocomposites to powder coatings. In this study, in order to compare the performance of a powder coating with the addition of a conventional load (barium sulfate) and a montmorillonite clay (MMT), two mixtures of commercial epoxy-based powder coating were prepared in the melt state, with the addition of 2 and 4% (w/w) of MMT, or 2 and 4% (w/w) of barium sulfate (BaSO 4 ). The thermal properties were investigated through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to evaluate the load dispersion and the morphology of the systems formed. The physical and anticorrosion properties of the coatings were also investigated. The interaction of the MMT with the polymeric matrix, associated to the aspect ratio, resulted in better barrier properties, thermal stability, and adhesion to the metal substrate.

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)

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.

Production and thermal stability of pure and Cr3+ -doped hydroxyapatite

International Nuclear Information System (INIS)

De Araujo, T S; De Souza, S O; De Sousa, E M B; Araujo, M S

2010-01-01

Hydroxyapatite (HAP) have been used as starting material for biomedical applications. The pure and Cr 3+ -doped hydroxyapatite were prepared by chemical precipitation reactions at 100, 500 e 800 0 C in order to investigate the thermal stability of these materials. The characterization of the thermal behavior of this phosphate, especially on the structural changes with heating, is very important for production of sunscreens The powders were characterized using chemical analysis: X-ray diffraction (XRD) and thermal analysis. The present study was successful in the preparation of pure hydroxyapatite and chromium substituted hydroxyapatites with good thermal stability and nanoparticles formation.

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

Structural, optical and photo thermal properties of Er3+:Y2O3 doped PMMA nanocomposite

Science.gov (United States)

Tabanli, Sevcan; Eryurek, Gonul

2018-02-01

Thermal decomposition technique was employed to synthesize of phosphors of yttria (Y2O3) doped with erbium (Er3+) ions. After the synthesized procedure, the nano-sized crystalline powders were annealed at 800oC for 24 h. Annealed powders were embedded in poly(methyl methacrylate) (PMMA) by free radical polymerization to fabricate nanocomposite polymer materials. The crystalline structure of the powder and doped PMMA nanocomposite samples were determined using X-ray diffraction technique. Scherrer's equation and the FW1/5/4/5M method were used to determine average crystalline size and grain size distributions, respectively. The spectroscopic properties of the powders and doped PMMA nanocomposites were studied by measuring the upconversion emission spectra under near-infrared laser excitation at room temperature. The laser-induced photo thermal behaviors of Er3+:Y2O3 nano-powders and doped PMMA nanocomposite were investigated using the fluorescence intensity ratio (FIR) technique.

Influence of controlled atmosphere on thermal inactivation of Escherichia coli ATCC 25922 in almond powder.

Science.gov (United States)

Cheng, Teng; Li, Rui; Kou, Xiaoxi; Wang, Shaojin

2017-06-01

Heat controlled atmosphere (CA) treatments hold potential to pasteurize Salmonella enteritidis PT 30 in almonds. Nonpathogenic Escherichia coli ATCC 25922 was used as a surrogate species of pathogenic Salmonella for validation of thermal pasteurization to meet critical safety requirements. A controlled atmosphere/heating block system (CA-HBS) was used to rapidly determine thermal inactivation of E. coli ATCC 25922. D- and z-values of E. coli ATCC 25922 inoculated in almond powder were determined at four temperatures between 65 °C and 80 °C under different gas concentrations and heating rates. The results showed that D- and z-values of E. coli under CA treatment were significantly (P < 0.05) lower than those under regular atmosphere (RA) treatment at 4 given temperatures. Relatively higher CO 2 concentrations (20%) and lower O 2 concentrations (2%) were more effective to reduce thermal inactivation time. There were no significant differences in D-values of E. coli when heating rates were above 1 °C/min both in RA and CA treatments. But D-values significantly (P < 0.05) increased under RA treatment and decreased under CA treatment at lower heating rates. Combination of rapid heat and CA treatments could be a promising method for thermal inactivation of S. enteritidis PT 30 in almond powder. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

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

Thermal expansion of mullite-type Bi{sub 2}Al{sub 4}O{sub 9}: A study by X-ray diffraction, vibrational spectroscopy and density functional theory

Energy Technology Data Exchange (ETDEWEB)

Mangir Murshed, M., E-mail: murshed@uni-bremen.de [Chemische Kristallographie fester Stoffe, Institut für Anorganische Chemie, Universität Bremens, Leobener Straße, D-28359 Bremen (Germany); Mendive, Cecilia B.; Curti, Mariano [Departamento de Química, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Mar del Plata, Dean Funes 3350, B7600AYL Mar del Plata (Argentina); Šehović, Malik [Chemische Kristallographie fester Stoffe, Institut für Anorganische Chemie, Universität Bremens, Leobener Straße, D-28359 Bremen (Germany); Friedrich, Alexandra [Institut für Geowissenschaften, Abteilung Kristallographie, Goethe-Universität Frankfurt, Altenhöferallee 1, D-60438 Frankfurt am Main (Germany); Fischer, Michael [Kristallographie, FB Geowissenschaften, Universität Bremen, Klagenfurter Straße, D-28359 Bremen (Germany); Gesing, Thorsten M. [Chemische Kristallographie fester Stoffe, Institut für Anorganische Chemie, Universität Bremens, Leobener Straße, D-28359 Bremen (Germany)

2015-09-15

Polycrystalline Bi{sub 2}Al{sub 4}O{sub 9} powder samples were synthesized using the glycerine method. Single crystals were produced from the powder product in a Bi{sub 2}O{sub 3} melt. The lattice thermal expansion of the mullite-type compound was studied using X-ray diffraction, Raman spectroscopy and density functional theory (DFT). The metric parameters were modeled using Grüneisen approximation for the zero pressure equation of state, where the temperature-dependent vibrational internal energy was calculated from the Debye characteristic frequency. Both the first-order and second-order Grüneisen approximations were applied for modeling the volumetric expansion, and the second-order approach provided physically meaningful axial parameters. The phonon density of states as well as phonon dispersion guided to set the characteristic frequency for simulation. The experimental infrared and Raman phonon bands were compared with those calculate from the DFT calculations. Selective Raman modes were analyzed for the thermal anharmonic behaviors using simplified Klemens model. The respective mode Grüneisen parameters were calculated from the pressure-dependent Raman spectra. - Graphical abstract: Crystal structure of mullite-type Bi{sub 2}Al{sub 4}O{sub 9} showing the edge-sharing AlO{sub 6} octahedra running parallel to the c-axis. - Highlights: • Thermal expansion of Bi{sub 2}Al{sub 4}O{sub 9} was studied using XRD, FTIR, Raman and DFT. • Metric parameters were modeled using Grüneisen approximation. • Phonon DOS and phonon dispersion helped to set the Debye frequency. • Mode Grüneisen parameters were calculated from the pressure-dependent Raman spectra. • Anharmonicity was analyzed for some selective Raman modes.

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

Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

International Nuclear Information System (INIS)

Kuo, C.-W.; Lee, Y.-H.; Hung, I-M.; Wang, M.-C.; Wen, S.-B.; Fung, K.-Z.; Shih, C.-J.

2008-01-01

Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl 2 .8H 2 O and Y(NO 3 ) 3 .6H 2 O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO 2 . The activation energy for the crystallization of the cubic ZrO 2 formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO 2 formation. The TEM examination shows that the cubic ZrO 2 has a spherical-like morphology with a size ranging from 10 to 20 nm

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)>>>>

Thermal conductivity enhancement of sodium acetate trihydrate by adding graphite powder and the effect on stability of supercooling

DEFF Research Database (Denmark)

Johansen, Jakob Berg; Dannemand, Mark; Kong, Weiqiang

2015-01-01

. The graphite powder was stabilized using carboxymetyl cellulose and successfully tested in heating and supercooling cycles with no loss of performance. Thermal conductivity enhancing properties of graphite powder was shown in samples. Since the experiments were conducted in small scale, at 200 g per sample......, large scale experiments are required to validate graphite as a thermo conductivity enhancing agent, suitable for use in seasonal heat storage applications utilizing SAT....

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.

Synthesis and characterization of nanocomposite powders of calcium phosphate/titanium oxide for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Delima, S.A.; Camargo, N.H.A.; Souza, J.C.P.; Gemelli, E., E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: souzajulio@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

2009-07-01

The nanostructured bioceramics of calcium phosphate are current themes of research and they are becoming important as bone matrix in regeneration of tissues in orthopedic and dental applications. Nanocomposite powders of calcium phosphate, reinforced with nanometric particles of titanium oxide, silica oxide and alumina oxid ealpha, are being widely studied because they offer new microstructures, nanostructures and interconnected microporosity with high superficial area of micropores that contribute to osteointegration and osteoinduction processes. This study is about the synthesis of nanocomposites powders of calcium phosphate reinforced with 1%, 2%, 3% and 5% in volume of titanium oxide and its characterization through the techniques of X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Differential Thermal Analysis (DTA), Thermogravimetry (TG) and Dilatometry. (author)

Synthesis and characterization of nanocomposite powders of calcium phosphate/titanium oxide for biomedical applications

International Nuclear Information System (INIS)

Delima, S.A.; Camargo, N.H.A.; Souza, J.C.P.; Gemelli, E.

2009-01-01

The nanostructured bioceramics of calcium phosphate are current themes of research and they are becoming important as bone matrix in regeneration of tissues in orthopedic and dental applications. Nanocomposite powders of calcium phosphate, reinforced with nanometric particles of titanium oxide, silica oxide and alumina oxid ealpha, are being widely studied because they offer new microstructures, nanostructures and interconnected microporosity with high superficial area of micropores that contribute to osteointegration and osteoinduction processes. This study is about the synthesis of nanocomposites powders of calcium phosphate reinforced with 1%, 2%, 3% and 5% in volume of titanium oxide and its characterization through the techniques of X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Differential Thermal Analysis (DTA), Thermogravimetry (TG) and Dilatometry. (author)

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

Science.gov (United States)

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

2010-09-01

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

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.

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.

Thermal Properties of Green Fuel Briquettes from Residue Corncobs Materials Mixed Macadamia Shell Charcoal Powder

Science.gov (United States)

Teeta, Suminya; Nachaisin, Mali; Wanish, Suchana

2017-09-01

The objective of this research was to produce green fuel briquettes from corncobs by adding macadamia shell charcoal powder. The study was sectioned into 3 parts: 1) Quality improvement of green fuel briquettes by adding macadamia; 2) Fuel property analysis based on ASTM standards and thermal fuel efficiency; and 3) Economics appropriateness in producing green fuel briquettes. This research produced green fuel briquettes using the ratio of corncobs weight and macadamia shell charcoal powder in 100:0 90:10 80:20 70:30 60:40 and 50:50 and pressing in the cold briquette machine. Fuel property analysis showed that green fuel briquettes at the ratio 50:50 produced maximum heating values at 21.06 Megajoule per kilogram and briquette density of 725.18 kilograms per cubic meter, but the percent of moisture content, volatile matter, ash, and fixed carbon were 10.09, 83.02, 2.17 and 4.72 respectively. The thermal efficiency of green fuel briquettes averaged 20.22%. Economics appropriateness was most effective where the ratio of corncobs weight to macadamia shell charcoal powder was at 50:50 which accounted for the cost per kilogram at 5.75 Baht. The net present value was at 1,791.25 Baht. Internal rate of return was at 8.62 and durations for a payback period of investment was at 1.9 years which was suitable for investment.

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

Influence of a microcomposite and a nanocomposite on the properties of an epoxy-based powder coating

Energy Technology Data Exchange (ETDEWEB)

Piazza, Diego [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Lorandi, Natalia P. [Corrosion and Surface Protection Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Pasqual, Charles I. [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Scienza, Lisete C. [Corrosion and Surface Protection Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil); Zattera, Ademir J., E-mail: ajzattera@terra.com.br [Polymers Laboratory, Caxias do Sul University - Exact Science and Technology Center, Francisco Getulio Vargas Street, 1130, Petropolis, CEP 95070-560 Caxias do Sul, RS (Brazil)

2011-08-25

Highlights: {yields} New materials for using as protective coatings for metal surfaces. {yields} Development of nanostructured powder paints. {yields} Characterization of the new material in the powder and coating form. {yields} Development of a new material for use in the automotive industry, industrial production of appliances, furniture industry. {yields} Development of new material using the process of mixing using a twin-screw extruder, followed by sintering process on a metal plate. - Abstract: The incorporation of nanoclays into coatings has been considered to be commercially favorable due to the improvements obtained in the barrier, thermal, and anticorrosion properties, among others, leading to the development of a new segment in the area of clean technologies: the application of nanocomposites to powder coatings. In this study, in order to compare the performance of a powder coating with the addition of a conventional load (barium sulfate) and a montmorillonite clay (MMT), two mixtures of commercial epoxy-based powder coating were prepared in the melt state, with the addition of 2 and 4% (w/w) of MMT, or 2 and 4% (w/w) of barium sulfate (BaSO{sub 4}). The thermal properties were investigated through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to evaluate the load dispersion and the morphology of the systems formed. The physical and anticorrosion properties of the coatings were also investigated. The interaction of the MMT with the polymeric matrix, associated to the aspect ratio, resulted in better barrier properties, thermal stability, and adhesion to the metal substrate.

Synthesis of carbon nitride powder by selective etching of TiC0.3N0.7 in chlorine-containing atmosphere at moderate temperature

International Nuclear Information System (INIS)

Sui Jian; Lu Jinjun

2010-01-01

We reported the synthesis of carbon nitride powder by extracting titanium from single inorganic precursor TiC 0.3 N 0.7 in chlorine-containing atmosphere at ambient pressure and temperature not exceeding 500 deg. C. The TiC 0.3 N 0.7 crystalline structure acted as a template, supplying active carbon and nitrogen atoms for carbon nitride when it was destroyed in chlorination. X-ray diffraction data showed that the obtained carbon nitride powders were amorphous, which was in good agreement with transmission electron microscope analysis. The composition and structure of carbon nitride powders were analyzed by employing Fourier transform infrared spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. Results indicated that disorder structure was most likely for the carbon nitride powders and the N content depended greatly on the chlorination temperature. Thermal analysis in flowing N 2 indicated that the mass loss started from 300 deg. C and the complete decomposition occurred at around 650 deg. C, confirming the low thermal stability of the carbon nitride material.

Anisotropic lattice thermal expansion of PbFeBO4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

International Nuclear Information System (INIS)

Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

2014-01-01

Highlights: • Mullite-type PbFeBO 4 shows uni-axial negative coefficient of thermal expansion. • Anisotropic thermal expansion of the metric parameters was modeled using modified Grüneisen approximation. • The model includes harmonic, quasi-harmonic and intrinsic anharmonic contributions to the internal energy. • DFT calculation, temperature- and pressure-dependent Raman spectra help understand the phonon decay and associated anharmonicity. - Abstract: The lattice thermal expansion of mullite-type PbFeBO 4 is presented in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. The unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies of the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO 4 , FeO 6 and BO 3 polyhedra as a function of temperature

In situ thermal residual stress evolution in ultrathin ZnO and Ag films studied by synchrotron x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Renault, P.O., E-mail: Pierre.olivier.renault@univ-poitiers.fr [Institut P' , CNRS, Universite de Poitiers, UPR 3346, 86962 Futuroscope (France); Krauss, C.; Le Bourhis, E.; Geandier, G. [Institut P' , CNRS, Universite de Poitiers, UPR 3346, 86962 Futuroscope (France); Benedetto, A. [Saint-Gobain Recherche (SGR), 93303 Aubervilliers (France); Grachev, S.Y.; Barthel, E. [Lab. Surface du Verre et Interfaces (SVI), UMR-CNRS 125, 93303 Aubervilliers (France)

2011-12-30

Residual-stress evolution in sputtered encapsulated ZnO/Ag/ZnO stack has been studied in-situ by synchrotron x-ray diffraction when heat treated. The ZnO/Ag/ZnO stack encapsulated into Si{sub 3}N{sub 4} layers and deposited on (001) Si substrates was thermally heated from 25 Degree-Sign C to 600 Degree-Sign C and cooled down to 25 Degree-Sign C. X-ray diffraction 2D patterns captured continuously during the heat treatment allowed monitoring the diffraction peak shifts of both Ag (15 nm thick) and ZnO (10 nm and 50 nm thick) sublayers. Due to the mismatch between the coefficients of thermal expansion, the silicon substrate induced compressive thermal stresses in the films during heating. We first observed a linear increase of the compressive stress state in both Ag and ZnO films and then a more complex elastic-stress evolution starts to operate from about 100 Degree-Sign C for Ag and about 250 Degree-Sign C for ZnO. Thermal contraction upon cooling seems to dominate so that the initial compressive film stresses relax by about 300 and 700 MPa after thermal treatment for ZnO and Ag, respectively. The overall behavior is discussed in terms of structural changes induced by the heat treatment.

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.)

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.

Thermal annealing of natural, radiation-damaged pyrochlore

Energy Technology Data Exchange (ETDEWEB)

Zietlow, Peter; Beirau, Tobias; Mihailova, Boriana; Groat, Lee A.; Chudy, Thomas; Shelyug, Anna; Navrotsky, Alexandra; Ewing, Rodney C.; Schlüter, Jochen; Škoda, Radek; Bismayer, Ulrich

2017-01-01

Radiation damage in minerals is caused by the α-decay of incorporated radionuclides, such as U and Th and their decay products. The effect of thermal annealing (400–1000 K) on radiation-damaged pyrochlores has been investigated by Raman scattering, X-ray powder diffraction (XRD), and combined differential scanning calorimetry/thermogravimetry (DSC/TG). The analysis of three natural radiation-damaged pyrochlore samples from Miass/Russia [6.4 wt% Th, 23.1·10

Synthesis and characterization of nanocomposite powders of calcium phosphate/silica-gel; Sintese e caracterizacao de pos nanoestruturados de fosfato de calcio/silica-gel

Energy Technology Data Exchange (ETDEWEB)

Muller, D.T.; Delima, S.A. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Dept. de Engenharia Mecanica; Santos, R.B.M.; Camargo, N.H.A., E-mail: dem2nhac@joinville.udesc.b [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais

2009-07-01

In the recent years ceramics of calcium phosphate are pointed out as an outstanding material in substitution and regeneration in defects from osseous tissue, in reason of their similar mineralogical characteristics of apatite of bone structure. However, the challenge with phosphate calcium ceramics find out about the mechanical properties and the development of biomaterials similar of the bone structure, what sometimes is not so easy, about fragile materials. The aim of this work focused in synthesis and characterization nanocomposites powders of calcium phosphate/silica-gel with percentages 1, 2, 3 e 5% of nanometric silica. The method synthesis used for the compositions elaboration was dissolution-precipitation. The presented results are related with the optimization to method elaboration of nanostructured powders, the mineralogical characterization with X-ray diffraction, thermal behavior with thermal differential analysis, differential scanning calorimetry here is ADT and dilatometer. The scanning electronic microscopy was used to help of morphological characterization the nanostructured powders and the surfaces from body test recovered from the mechanical test. (author)

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.

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.

Synthesis and characterization of powders calcium phosphate for biomedical applications

International Nuclear Information System (INIS)

Oliveira, D.M.P. de; Prants, W.T.; Camargo, N.H.A.; Gemelli, E.

2009-01-01

Scientists of different areas research the bioceramics as new materials to substitute parts of the human body. The bioceramics of the calcium phosphate have the advantage present similar chemical composition to the structure of the bony apatite of the human skeleton. In this study, calcium phosphate powder was synthesized chemically using the solution of phosphorus pentoxide (P 2 O 5 ) and calcium oxide (CaO) necessary for molar Ca/P =1.67. These works aim the study of different thermal treatments, physics and of the microstructure properties. For characterization the bony matrix were used the techniques of: X-ray diffraction (DRX); Scanning Electronic Microscopy (SEM) and Differential Scanning Calorimetry (DSC). (author)

Synthesis and thermal behaviour of pauflerite, β-VOSO4, and its α-modification

International Nuclear Information System (INIS)

Paufler, Peter; Filatov, Stanislav K.; Krzhizhanovskaya, Maria G.; Bubnova, Rimma S.; Russian Academy of Sciences, St. Peterburg

2014-01-01

Powder α-VOSO 4 was prepared by dehydration of VOSO 4 . 3H 2 O. β-VOSO 4 was synthesized by boiling of V 2 O 5 in H 2 SO 4 . Thermal behaviour of VOSO 4 . 3H 2 O, α- and β-VOSO 4 modifications is studied by high-temperature powder X-ray diffraction and thermal analysis, including two-step dehydration of VOSO 4 . 3H 2 O, formation of α-VOSO 4 , thermal expansion and decomposition of both modifications into V 2 O 5 . Higher anisotropy of thermal expansion of the tetragonal α-modification α c = 39(2) . 10 -6 K -1 along the vanadyl ion and α a = 2.4(6) . 10 -6 K -1 in the perpendicular direction comparing to the orthorhombic β-modification (α a = 20.2(7), α b = 2.8(8), α c = 17.8(4) . 10 -6 K -1 ) is explained from a crystal chemical point of view.

Crystallite sizes of LiH before and after ball milling and thermal exposure

International Nuclear Information System (INIS)

Ortiz, Angel L.; Osborn, William; Markmaitree, Tippawan; Shaw, Leon L.

2008-01-01

The powder characteristics of lithium hydride (LiH) as a function of high-energy ball milling condition are systematically investigated via quantitative X-ray diffraction (XRD) analysis. The results obtained from the XRD analysis are compared with those attained from scanning electron microscopy (SEM), transmission electron microscopy (TEM), and specific surface area (SSA) analyses. The thermal stability of the ball-milled LiH is also investigated in order to provide physical insights into its cyclic stability in hydrogen sorption and desorption cycles. The results indicate that ball milling is effective in obtaining nano-crystalline LiH powder which is relatively stable with retention of nano-crystals after thermal exposure at 285 deg. C (equivalent to 0.58T m ) for 1 h. The good thermal stability observed is attributed to the presence of many pores in the agglomerates at the ball-milled condition. These pores effectively prevent crystal growth during the thermal exposure

Crystallite sizes of LiH before and after ball milling and thermal exposure

Energy Technology Data Exchange (ETDEWEB)

Ortiz, Angel L. [Departamento de Electronica e Ingenieria Electromecanica, Universidad de Extremadura, Badajoz (Spain); Osborn, William; Markmaitree, Tippawan [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, 97 North Eagleville Road, U-3136 Storrs, CT 06269-3136 (United States); Shaw, Leon L. [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, 97 North Eagleville Road, U-3136 Storrs, CT 06269-3136 (United States)], E-mail: leon.shaw@uconn.edu

2008-04-24

The powder characteristics of lithium hydride (LiH) as a function of high-energy ball milling condition are systematically investigated via quantitative X-ray diffraction (XRD) analysis. The results obtained from the XRD analysis are compared with those attained from scanning electron microscopy (SEM), transmission electron microscopy (TEM), and specific surface area (SSA) analyses. The thermal stability of the ball-milled LiH is also investigated in order to provide physical insights into its cyclic stability in hydrogen sorption and desorption cycles. The results indicate that ball milling is effective in obtaining nano-crystalline LiH powder which is relatively stable with retention of nano-crystals after thermal exposure at 285 deg. C (equivalent to 0.58T{sub m}) for 1 h. The good thermal stability observed is attributed to the presence of many pores in the agglomerates at the ball-milled condition. These pores effectively prevent crystal growth during the thermal exposure.

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

International Nuclear Information System (INIS)

Poblete, V.; Acevedo, R.

1998-01-01

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

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)

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.)

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.

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.

Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

Energy Technology Data Exchange (ETDEWEB)

Kuo, C.-W. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Lee, Y.-H. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Far-East Road, Chung-Li, Taoyuan, Taiwan (China); Wang, M.-C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Wen, S.-B. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: cjshih@kmu.edu.tw

2008-04-03

Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl{sub 2}.8H{sub 2}O and Y(NO{sub 3}){sub 3}.6H{sub 2}O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO{sub 2}. The activation energy for the crystallization of the cubic ZrO{sub 2} formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO{sub 2} formation. The TEM examination shows that the cubic ZrO{sub 2} has a spherical-like morphology with a size ranging from 10 to 20 nm.

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).

Obtaining zircaloy powder through hydriding

International Nuclear Information System (INIS)

Dupim, Ivaldete da Silva; Moreira, Joao M.L.

2009-01-01

Zirconium alloys are good options for the metal matrix in dispersion fuels for power reactors due to their low thermal neutron absorption cross-section, good corrosion resistance, good mechanical strength and high thermal conductivity. A necessary step for obtaining such fuels is producing Zr alloy powder for the metal matrix composite material. This article presents results from the Zircaloy-4 hydrogenation tests with the purpose to embrittle the alloy as a first step for comminuting. Several hydrogenation tests were performed and studied through thermogravimetric analysis. They included H 2 pressures of 25 and 50 kPa and temperatures ranging between from 20 to 670 deg C. X-ray diffraction analysis showed in the hydrogenated samples the predominant presence of ZrH 2 and some ZrO 2 . Some kinetics parameters for the Zircaloy-4 hydrogenation reaction were obtained: the time required to reach the equilibrium state at the dwell temperature was about 100 minutes; the hydrogenation rate during the heating process from 20 to 670 deg C was about 21 mg/h, and at constant temperature of 670 deg C, the hydride rate was about 1.15 mg/h. The hydrogenation rate is largest during the heating process and most of it occurs during this period. After hydrogenated, the samples could easily be comminuted indicating that this is a possible technology to obtain Zircaloy powder. The results show that only few minutes of hydrogenation are necessary to reach the hydride levels required for comminuting the Zircaloy. The final hydride stoichiometry was between 2.7 and 2.8 H for each Zr atom in the sample (author)

Structural and thermal properties of LaMnO3 from neutron diffraction and first principles studies

International Nuclear Information System (INIS)

Wdowik, Urszula D; Ouladdiaf, Bachir; Chatterji, Tapan

2011-01-01

Neutron diffraction experiments have been performed on powder samples of LaMnO 3 below and above the Jahn-Teller transition temperature of 750 K. Experimental investigations are assisted by density functional theory calculations. Theoretical studies are carried out for the orbitally ordered state of LaMnO 3 which allows one to compare the behavior of the orbitally ordered and disordered structures as a function of temperature. The temperature dependences of the structural parameters characterizing the Jahn-Teller distortions are reported and discussed. A gradual departure of the experimental data from theoretical predictions is observed above 650 K. In this range of temperatures, anions surrounding the Jahn-Teller active cations perform more isotropic thermal motion. The onset of structural phase transition induces a reduction of the crystal volume by about 0.4% which follows from the structural transformations yielding more regular oxygen octahedra formed above the phase transformation. It is found that above the Jahn-Teller transition the distortions of the MnO 6 octahedra are not completely removed. The non-vanishing distortions are accompanied by the lifted degeneracy of the Mn e g states. Weak residual distortions can be assigned to the short-range orbital order that persists within a local scale but it seems quenched on average giving rise to a disappearance of the long-range order coherency of the Jahn-Teller effect.

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

Pressurized Anneal of Consolidated Powders

Science.gov (United States)

Nemir, David Charles (Inventor); Rubio, Edward S. (Inventor); Beck, Jan Bastian (Inventor)

2017-01-01

Systems and methods for producing a dense, well bonded solid material from a powder may include consolidating the powder utilizing any suitable consolidation method, such as explosive shockwave consolidation. The systems and methods may also include a post-processing thermal treatment that exploits a mismatch between the coefficients of thermal expansion between the consolidated material and the container. Due to the mismatch in the coefficients, internal pressure on the consolidated material during the heat treatment may be increased.

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.

POWDER INJECTION MOLDING OF SIC FOR THERMAL MANAGEMENT V

Directory of Open Access Journals (Sweden)

Valmikanathan Onbattuvelli

2012-06-01

Full Text Available Silicon carbide (SiC exhibits many functional properties that are relevant to applications in electronics, aerospace, defense and automotive industries. However, the successful translation of these properties into final applications lies in the net-shaping of ceramics into fully dense microstructures. Increasing the packing density of the starting powders is one effective route to achieve high sintered density and dimensional precision. The present paper presents an in-depth study on the effects of nanoparticle addition on the powder injection molding process (PIM of SiC powder-polymer mixtures. In particular, bimodal mixtures of nanoscale and sub-micrometer particles are found to have significantly increased powder packing characteristics (solids loading in the powder-polymer mixtures. The influence of nanoparticle addition on the multi-step PIM process is examined. The above results provide new perspectives which could impact a wide range of materials, powder processing techniques and applications.

Thermal aging of melt-spun NdFeB magnetic powder in hydrogen

Science.gov (United States)

Pinkerton, Frederick E.; Balogh, Michael P.; Ellison, Nicole; Foto, Aldo; Sechan, Martin; Tessema, Misle M.; Thompson, Margarita P.

2016-11-01

High energy product neodymium-iron-boron (NdFeB) magnets are the premier candidate for demanding electrified vehicle traction motor applications. Injection molded (IM) or compression molded (CM) magnets made using NdFeB powders are promising routes to improve motor efficiency, cost, and manufacturability. However, IM and CM NdFeB magnets are susceptible to substantial thermal aging losses at motor operating temperatures when exposed to the automatic transmission fluid (ATF) used as a lubricant and cooling medium. The intrinsic coercivity Hci of NdFeB IM and CM magnets degrades by as much as 18% when aged for 1000 h in ATF at 150 °C, compared to a 3% loss when aged in air. Here we report aging studies of rapidly quenched NdFeB powder in air, ATF, and H2 gas. Expansion of the NdFeB crystal lattice in both ATF and H2 identified hydrogen dissociated from the ATF during aging and diffused into the primary NdFeB phase as the probable cause of the coercivity loss of IM and CM magnets.

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

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)

Sintering and thermal ageing studies of zirconia - yttria ceramics by impedance spectroscopy

International Nuclear Information System (INIS)

Florio, Daniel Zanetti de

1998-01-01

ZrO 2 :8 mol %Y 2 O 3 solid electrolyte ceramic pellets have been prepared with powders of three different origins: a Nissan (Japan) commercial powder, a powder obtained by the coprecipitation technique at IPEN, and the mixing of powder oxides (ZrO 2 produced at a Pilot Plant at IPEN and 99.9% pure Y 2 O 3 of USA origin). These starting powders have been analysed by the following techniques: X-ray fluorescence for yttrium content, X-ray diffraction for structural phase content, sedimentation for particle size distribution, gas adsorption (BET) for surface area determination, and transmission electron microscopy for average particle size determination. Pressed ceramic pellets have been analysed by dilatometry to evaluate the sintering stages. Sintered pellets have been characterized by X-ray diffraction for phase analysis and scanning electron microscopy for grain morphology analysis. Impedance spectroscopy analysis have been carried out to follow thermal ageing of zirconia-yttria solid electrolyte at 600 deg C, the working temperature of permanent oxygen sensor, and to study sintering kinetics. The main results show that ageing at 600 deg C decreases the emf sensor response in the first 100 h to a steady value. Moreover, sintering studies by impedance spectroscopy allowed for finding correlations between electrical parameters, sintering kinetics and grain growth mechanisms. (author)

Thermal and ultrasonic influence in the formation of nanometer scale hydroxyapatite bio-ceramic

Science.gov (United States)

Poinern, GJE; Brundavanam, R; Le, X Thi; Djordjevic, S; Prokic, M; Fawcett, D

2011-01-01

Hydroxyapatite (HAP) is a widely used biocompatible ceramic in many biomedical applications and devices. Currently nanometer-scale forms of HAP are being intensely investigated due to their close similarity to the inorganic mineral component of the natural bone matrix. In this study nano-HAP was prepared via a wet precipitation method using Ca(NO3)2 and KH2PO4 as the main reactants and NH4OH as the precipitator under ultrasonic irradiation. The Ca/P ratio was set at 1.67 and the pH was maintained at 9 during the synthesis process. The influence of the thermal treatment was investigated by using two thermal treatment processes to produce ultrafine nano-HAP powders. In the first heat treatment, a conventional radiant tube furnace was used to produce nano-particles with an average size of approximately 30 nm in diameter, while the second thermal treatment used a microwave-based technique to produce particles with an average diameter of 36 nm. The crystalline structure and morphology of all nanoparticle powders produced were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Both thermal techniques effectively produced ultrafine powders with similar crystalline structure, morphology and particle sizes. PMID:22114473

Growth, optical, thermal and dielectric studies of an amino acid organic nonlinear optical material: L-Alanine

International Nuclear Information System (INIS)

Caroline, M. Lydia; Sankar, R.; Indirani, R.M.; Vasudevan, S.

2009-01-01

Good transparent bulk single crystals of L-alanine (nonlinear optical material) have been grown successfully by slow cooling technique from aqueous solution at pH value of 2.0. Optically transparent crystals with dimensions 2.4 cm x 1.2 cm x 1.6 cm, were grown by optimizing the growth parameters within a growth period of 2 weeks. The crystallinity of L-alanine crystal was confirmed by the powder X-ray diffraction study and diffraction peaks are indexed. The vibrational structure of the molecule is elucidated from FTIR spectra. The thermal behaviour of the grown crystal was investigated by thermogravimetric (TG) and differential thermal analyses (DTA) techniques in a nitrogen atmosphere. The result showed that the material starts decomposing at 297 deg. C. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance between the wavelengths ranging from 200 to 1200 nm. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time

Thermal aging of melt-spun NdFeB magnetic powder in hydrogen

International Nuclear Information System (INIS)

Pinkerton, Frederick E.; Balogh, Michael P.; Ellison, Nicole; Foto, Aldo; Sechan, Martin; Tessema, Misle M.; Thompson, Margarita P.

2016-01-01

High energy product neodymium-iron-boron (NdFeB) magnets are the premier candidate for demanding electrified vehicle traction motor applications. Injection molded (IM) or compression molded (CM) magnets made using NdFeB powders are promising routes to improve motor efficiency, cost, and manufacturability. However, IM and CM NdFeB magnets are susceptible to substantial thermal aging losses at motor operating temperatures when exposed to the automatic transmission fluid (ATF) used as a lubricant and cooling medium. The intrinsic coercivity H ci of NdFeB IM and CM magnets degrades by as much as 18% when aged for 1000 h in ATF at 150 °C, compared to a 3% loss when aged in air. Here we report aging studies of rapidly quenched NdFeB powder in air, ATF, and H 2 gas. Expansion of the NdFeB crystal lattice in both ATF and H 2 identified hydrogen dissociated from the ATF during aging and diffused into the primary NdFeB phase as the probable cause of the coercivity loss of IM and CM magnets. - Highlights: • Injection molded NdFeB magnets age rapidly in automatic transmission fluid (ATF). • Coercivity loss is not due to direct chemical reaction between ATF and the powder. • Chemical reaction with the binder does not play a major role in aging. • Hydrogen dissociates from ATF and diffuses into Nd 2 Fe 14 B, reducing coercivity.

Thermal aging of melt-spun NdFeB magnetic powder in hydrogen

Energy Technology Data Exchange (ETDEWEB)

Pinkerton, Frederick E., E-mail: frederick.e.pinkerton@gm.com [Chemical and Materials Systems Laboratory, General Motors Research and Development Center, Warren, MI 48092 (United States); Balogh, Michael P.; Ellison, Nicole [Chemical and Materials Systems Laboratory, General Motors Research and Development Center, Warren, MI 48092 (United States); Foto, Aldo [Element Materials Technology Wixom, Inc (United States); Sechan, Martin; Tessema, Misle M.; Thompson, Margarita P. [Powertrain Materials/Fluids/AMPPD Engineering and Labs, GFL VE/PT Materials Engineering, General Motors LLC, Pontiac, MI 48340 (United States)

2016-11-01

High energy product neodymium-iron-boron (NdFeB) magnets are the premier candidate for demanding electrified vehicle traction motor applications. Injection molded (IM) or compression molded (CM) magnets made using NdFeB powders are promising routes to improve motor efficiency, cost, and manufacturability. However, IM and CM NdFeB magnets are susceptible to substantial thermal aging losses at motor operating temperatures when exposed to the automatic transmission fluid (ATF) used as a lubricant and cooling medium. The intrinsic coercivity H{sub ci} of NdFeB IM and CM magnets degrades by as much as 18% when aged for 1000 h in ATF at 150 °C, compared to a 3% loss when aged in air. Here we report aging studies of rapidly quenched NdFeB powder in air, ATF, and H{sub 2} gas. Expansion of the NdFeB crystal lattice in both ATF and H{sub 2} identified hydrogen dissociated from the ATF during aging and diffused into the primary NdFeB phase as the probable cause of the coercivity loss of IM and CM magnets. - Highlights: • Injection molded NdFeB magnets age rapidly in automatic transmission fluid (ATF). • Coercivity loss is not due to direct chemical reaction between ATF and the powder. • Chemical reaction with the binder does not play a major role in aging. • Hydrogen dissociates from ATF and diffuses into Nd{sub 2}Fe{sub 14}B, reducing coercivity.

Low pressure powder injection moulding of stainless steel powders

Energy Technology Data Exchange (ETDEWEB)

Zampieron, J.V.; Soares, J.P.; Mathias, F.; Rossi, J.L. [Powder Processing Center CCP, Inst. de Pesquisas Energeticas e Nucleares, Sao Paulo, SP (Brazil); Filho, F.A. [IPEN, Inst. de Pesquisas Energeticas e Nucleares, Cidade Univ., Sao Paulo, SP (Brazil)

2001-07-01

Low-pressure powder injection moulding was used to obtain AISI 316L stainless steel parts. A rheological study was undertaken using gas-atomised powders and binders. The binders used were based on carnauba wax, paraffin, low density polyethylene and microcrystalline wax. The metal powders were characterised in terms of morphology, particle size distribution and specific surface area. These results were correlated to the rheological behaviour. The mixture was injected in the shape of square bar specimens to evaluate the performance of the injection process in the green state, and after sintering. The parameters such as injection pressure, viscosity and temperature were analysed for process optimisation. The binders were thermally removed in low vacuum with the assistance of alumina powders. Debinding and sintering were performed in a single step. This procedure shortened considerably the debinding and sintering time. (orig.)

Set of thermal neutron-scattering experiments for the Weapons Neutron Research Facility

International Nuclear Information System (INIS)

Brugger, R.M.

1975-12-01

Six classes of experiments form the base of a program of thermal neutron scattering at the Weapons Neutron Research (WNR) Facility. Three classes are to determine the average microscopic positions of atoms in materials and three are to determine the microscopic vibrations of these atoms. The first three classes concern (a) powder sample neutron diffraction, (b) small angle scattering, and (c) single crystal Laue diffraction. The second three concern (d) small kappa inelastic scattering, (e) scattering surface phonon measurements, and (f) line widths. An instrument to couple with the WNR pulsed source is briefly outlined for each experiment

Synthesis and characterization of powders calcium phosphate for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Oliveira, D.M.P. de; Prants, W.T.; Camargo, N.H.A.; Gemelli, E., E-mail: daniellapinheiro@gmail.com, E-mail: w_prants@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: dma2ec@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

2009-07-01

Scientists of different areas research the bioceramics as new materials to substitute parts of the human body. The bioceramics of the calcium phosphate have the advantage present similar chemical composition to the structure of the bony apatite of the human skeleton. In this study, calcium phosphate powder was synthesized chemically using the solution of phosphorus pentoxide (P{sub 2}O{sub 5}) and calcium oxide (CaO) necessary for molar Ca/P =1.67. These works aim the study of different thermal treatments, physics and of the microstructure properties. For characterization the bony matrix were used the techniques of: X-ray diffraction (DRX); Scanning Electronic Microscopy (SEM) and Differential Scanning Calorimetry (DSC). (author)

Mechanical and thermal properties of polypropylene (PP) composites filled with modified shell waste

Energy Technology Data Exchange (ETDEWEB)

Yao, Z.T., E-mail: sxyzt@126.com [College of Materials Science and Environmental Engineering, Hangzhou Dianzi University, Hangzhou 310018 (China); Chen, T. [Department of Ocean Science and Engineering, Zhejiang University, Hangzhou 310058 (China); Li, H.Y. [Zhoushan Ocean Research Institute, Zhejiang University, Zhoushan 316021 (China); Xia, M.S., E-mail: msxia@zju.edu.cn [Department of Ocean Science and Engineering, Zhejiang University, Hangzhou 310058 (China); Ye, Y.; Zheng, H. [Department of Ocean Science and Engineering, Zhejiang University, Hangzhou 310058 (China)

2013-11-15

Highlights: • Adding modified shell powder could significantly increase the properties of PP. • The modified shell powder could act as a nucleating agent in PP matrix. • The modified shell powder has a potential to be used as a bio-filler. -- Abstract: Shell waste, with its high content of calcium carbonate (CaCO{sub 3}) plus organic matrix, has a potential to be used as a bio-filler. In this work, shell waste was modified by furfural and then incorporated to reinforce polypropylene (PP). The shell waste and modified powder were characterized by means of X-ray diffraction (XRD), scanning electron microscopy equipped with an energy dispersive spectrometer (SEM-EDS), X-ray photoelectronic spectroscopy (XPS), and Fourier transformed infrared spectroscopy (FTIR). The mechanical and thermal properties of neat PP and PP composites were investigated as well. Thermal gravimetric (TG) analyses confirmed the reinforcing role of modified powder in PP composites. The mechanical properties studied showed that adding modified powder could significantly increase the impact strength, elongation at break point and flexural modulus of composites. The maximum incorporation content could reach 15 wt.% with a good balance between toughness and stiffness of PP composites. Differential scanning calorimetry (DSC) results showed that the modified powder could act as a nucleating agent and thus increase the crystallization temperature of PP. Polarized optical microscopy (POM) observation also indicated that the introduction of modified powder could promote the heterogeneous nucleation of PP matrix.

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

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.

The use of pattern decomposition to study the combined X-ray diffraction effects of crystallite size and stacking faults in ex-oxalate zinc oxide

International Nuclear Information System (INIS)

Langford, J.I.; Boultif, A.; Auffredic, J.P.; Louer, D.

1993-01-01

The microstructure of ZnO powder, obtained from thermal decomposition of the oxalate and studied previously by electron microscopy and adsorption calorimetry, was investigated by means of X-ray powder diffraction pattern decomposition. A Williamson-Hall plot revealed that some lines were broadened solely due to the effects of crystallite size, whereas other breadths included a contribution due to stacking faults. Spherical and cylindrical models are used to describe the form of the crystallites and procedures are presented for separating 'size' effects from 'mistake' broadening. This leads to estimates of the mean dimensions of the crystallites and the stacking-fault probability. The analysis demonstrates that, with good-quality data for a large number of reflections, a considerable amount of detailed information can be obtained about microstructure. On the other hand, it reveals some of the limitations of current procedures for modelling diffraction line profiles. (orig.)

Synthesis and Thermal Characterization of Hydroxyapatite Powders Obtained by Sol-Gel Technique

Science.gov (United States)

Jiménez-Flores, Y.; Camacho, N.; Rojas-Trigos, J. B.; Suárez, M.

The development of bioactive materials presents an interesting and an extremely relevant problem to solve, in the development of customized cranial and maxillofacial prosthesis, bioactive coating, and cements, for example. In such areas, one of the more employed materials is the synthetic hydroxyapatite, due to its proved biocompatibility with the human body; however, there are few studies about the thermal affinity with the biological surroundings, and most of them are centered in the thermal stability of the hydroxyapatite instead of its transient thermal response. In the present paper, the synthesis and physical-chemical characterization of hydroxyapatite samples, obtained by the sol-gel technique employing ultrasonic mixing, are reported. Employing X-ray diffraction patterns, XEDS and FTIR spectra, the crystal symmetry, chemical elements, and the present functional groups of the studied samples were determined and found to correspond to those reported in the literature, with a stoichiometry close to the ideal for biological applications. Additionally, by means of the photoacoustic detection and infrared photothermal radiometry (IPTR) techniques, the thermal response of the samples was obtained. Analyzing the photoacoustic data, the synthetized samples show photoacoustic opaqueness, responding in the thermally thick regime in the measurement range, and their thermal effusivity was also determined, having values of 1.47 folds the thermal effusivity of the mandibular human bone. Finally, from the IPTR measurements, the thermal diffusivity and thermal conductivity of the samples were also determined, having good agreement with the reported values for synthetic hydroxyapatite. The structural and thermophysical properties of the here reported samples show that the synthesized samples have good thermal affinity with the mandibular human bone tissue, and are suitable for biomedical applications.

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)

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

OpenAIRE

Svіtlana HAVENKO; Victoria KOCHUBEI; Marta LABETSKA; Svitlana KHADZHYNOVA; Edmundas KIBIRKŠTIS; Ingrida Venytė

2015-01-01

In order to improve the integration of blind people into society, suitable conditions should be provided for them. The expansion of Braille (BR) use could serve the purpose. Depending on the materials used for Braille, it can be formed or printed in different ways: embossing, screen printing, thermoforming, digital printing. The aim of this research is to determine the effect of thermal properties of screen printing inks and inks with thermo-powder on the qualitative parameters of Braille. Sc...

High Thermal Dissipation of Al Heat Sink When Inserting Ceramic Powders by Ultrasonic Mechanical Coating and Armoring.

Science.gov (United States)

Tsai, Wei-Yu; Huang, Guan-Rong; Wang, Kuang-Kuo; Chen, Chin-Fu; Huang, J C

2017-04-26

Aluminum alloys, which serve as heat sink in light-emitting diode (LED) lighting, are often inherent with a high thermal conductivity, but poor thermal total emissivity. Thus, high emissive coatings on the Al substrate can enhance the thermal dissipation efficiency of radiation. In this study, the ultrasonic mechanical coating and armoring (UMCA) technique was used to insert various ceramic combinations, such as Al₂O₃, SiO₂, or graphite, to enhance thermal dissipation. Analytic models have been established to couple the thermal radiation and convection on the sample surface through heat flow equations. A promising match has been reached between the theoretical predictions and experimental measurements. With the adequate insertion of ceramic powders, the temperature of the Al heat sinks can be lowered by 5-11 °C, which is highly favorable for applications requiring cooling components.

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)

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.

Developments in diffraction databases

International Nuclear Information System (INIS)

Jenkins, R.

1999-01-01

Full text: There are a number of databases available to the diffraction community. Two of the more important of these are the Powder Diffraction File (PDF) maintained by the International Centre for Diffraction Data (ICDD), and the Inorganic Crystal Structure Database (ICSD) maintained by Fachsinformationzentrum (FIZ, Karlsruhe). In application, the PDF has been used as an indispensable tool in phase identification and identification of unknowns. The ICSD database has extensive and explicit reference to the structures of compounds: atomic coordinates, space group and even thermal vibration parameters. A similar database, but for organic compounds, is maintained by the Cambridge Crystallographic Data Centre. These databases are often used as independent sources of information. However, little thought has been given on how to exploit the combined properties of structural database tools. A recently completed agreement between ICDD and FIZ, plus ICDD and Cambridge, provides a first step in complementary use of the PDF and the ICSD databases. The focus of this paper (as indicated below) is to examine ways of exploiting the combined properties of both databases. In 1996, there were approximately 76,000 entries in the PDF and approximately 43,000 entries in the ICSD database. The ICSD database has now been used to calculate entries in the PDF. Thus, to derive d-spacing and peak intensity data requires the synthesis of full diffraction patterns, i.e., we use the structural data in the ICSD database and then add instrumental resolution information. The combined data from PDF and ICSD can be effectively used in many ways. For example, we can calculate PDF data for an ideally random crystal distribution and also in the absence of preferred orientation. Again, we can use systematic studies of intermediate members in solid solutions series to help produce reliable quantitative phase analyses. In some cases, we can study how solid solution properties vary with composition and

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.

Crystal structure and thermal expansion of CsCaI3:Eu and CsSrBr3:Eu scintillators

Science.gov (United States)

Loyd, Matthew; Lindsey, Adam; Patel, Maulik; Koschan, Merry; Melcher, Charles L.; Zhuravleva, Mariya

2018-01-01

The distorted-perovskite scintillator materials CsCaI3:Eu and CsSrBr3:Eu prepared as single crystals have shown promising potential for use in radiation detection applications requiring a high light yield and excellent energy resolution. We present a study using high temperature powder X-ray diffraction experiments to examine a deleterious high temperature phase transition. High temperature phases were identified through sequential diffraction pattern Rietveld refinement in GSAS II. We report the linear coefficients of thermal expansion for both high and low temperature phases of each compound. Thermal expansion for both compositions is greatest in the [0 0 1] direction. As a result, Bridgman growth utilizing a seed oriented with the [0 0 1] along the growth direction should be used to mitigate thermal stress.

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

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

Swelling of radiation-cured polymer precursor powder for silicon carbide by pyrolysis

Directory of Open Access Journals (Sweden)

Akinori Takeyama

2015-12-01

Full Text Available Ceramic yield, density, volume change and pore size distribution were measured for radiation- and thermally cured PCS powder when they were pyrolyzed in the temperature range of 673–973 K. Higher ceramic yield was obtained for radiation-cured powder due to smaller amount of evolved gas. Temperature dependence of volume change and the total pore volume show that the formation and disappearance of pores in the powders were determined by the volume shrinkage and evolution of decomposed gases. Volume shrinkage narrowed the pore size distribution for radiation-cured powder. For thermally cured powder, the narrowing of size distribution was disturbed by aggregated pores. Smaller amount of evolved gas from radiation-cured powder relative to thermally cured powder prevented the aggregation of pores and provided the narrow size distribution.

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...

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

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

International Nuclear Information System (INIS)

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

2010-12-01

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

The thermal behaviour of cuprite: An XRD-EXAFS combined approach

International Nuclear Information System (INIS)

Dapiaggi, M.; Tiano, W.; Artioli, G.; Sanson, A.; Fornasini, P.

2003-01-01

Cuprite (Cu 2 O) is a low thermal expansion material with a negative thermal expansion coefficient below room temperature. Its peculiar thermal behaviour encompasses the increase of the shear modulus with increasing temperature, and the presence of rather intense symmetry-forbidden eeo reflections below room temperature. The thermal expansion of cuprite was studied at low temperature (between 5 and 298 K) by means of high-resolution (10 -5 A) X-ray powder diffraction at European Synchrotron Radiation Facility (Grenoble, BM16) and extended X-ray absorption fine structure (EXAFS) (BM29). Negative thermal expansion is confirmed up to 200 K, by EXAFS as well as by XRD measurements, and no sign of transition was found in XRD data. The comparison between EXAFS and XRD results provides a valuable insight into vibrational behaviour of cuprite at low temperature

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.

Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Vaxelaire, N; Labat, S; Thomas, O [Aix-Marseille University, IM2NP, FST avenue Escadrille Normandie Niemen, F-13397 Marseille Cedex (France); Proudhon, H; Forest, S [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Kirchlechner, C; Keckes, J [Erich Schmid Institute for Material Science, Austrian Academy of Science and Institute of Metal Physics, University of Leoben, Jahnstrasse 12, 8700 Leoben (Austria); Jacques, V; Ravy, S [Synchrotron SOLEIL, L' Orme des merisiers, Saint-Aubin BP 48, 91192 Gif-sur-Yvette Cedex (France)], E-mail: nicolas.vaxelaire@univ-cezanne.fr

2010-03-15

Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

International Nuclear Information System (INIS)

Vaxelaire, N; Labat, S; Thomas, O; Proudhon, H; Forest, S; Kirchlechner, C; Keckes, J; Jacques, V; Ravy, S

2010-01-01

Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

Study of thermal stability of ultrafine-grained copper by means of electron back scattering diffraction

Czech Academy of Sciences Publication Activity Database

Man, O.; Pantělejev, L.; Kunz, Ludvík

2010-01-01

Roč. 51, č. 2 (2010), s. 209-213 ISSN 1345-9678 R&D Projects: GA AV ČR 1QS200410502 Institutional research plan: CEZ:AV0Z20410507 Keywords : ultra-fine grained copper * thermal stability of microstructure * electron back scattering diffraction * grain size * texture Subject RIV: JG - Metallurgy Impact factor: 0.779, year: 2010

Low temperature synthesis of nanocrystalline lanthanum monoaluminate powders by chemical coprecipitation

Energy Technology Data Exchange (ETDEWEB)

Kuo, C.-L. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, C.-L. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Chen, T.-Y. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Chen, G.-J. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Yuan-Tung Road, Chungli, Taoyuan 320, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)]. E-mail: CJShih@kmu.edu.tw; Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China)

2007-08-16

Nanocrystalline lanthanum monoaluminate (LaAlO{sub 3}) powders were prepared by chemical coprecipitation using 25 vol.% of NH{sub 4}OH, 0.05 M La(NO{sub 3}){sub 3}.6H{sub 2}O and 0.05 M Al(NO{sub 3}){sub 3}.9H{sub 2}O aqueous solutions as the starting materials. Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analyses (TGA/DTA), X-ray diffraction (XRD), Raman spectrometry, specific surface area (BET) analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) were utilized to characterize the LaAlO{sub 3} powders prepared by chemical coprecipitation. The crystallization temperature of the LaAlO{sub 3} precursor gels precipitated at pH 9 is estimated as 810 deg. C by TG/DTA. The XRD pattern of the LaAlO{sub 3} precursor gels precipitated at pH 8-12 and calcined at 700 deg. C for 6 h shows a broad arciform continuum exist between 24{sup o} and 32{sup o} and sharp peaks of LaAlO{sub 3} except the precursor gels precipitated at pH 9. For the LaAlO{sub 3} precursor gels precipitated at pH 9 and calcined at 700 deg. C for 6 h, the formation of the perovskite LaAlO{sub 3} phase occurs and the presence of crystalline impurities is not found. The crystallite size of LaAlO{sub 3} slightly increases from 37.8 to 41.5 nm with calcination temperature increasing from 700 to 900 deg. C for 6 h. The LaAlO{sub 3} powders prepared by chemical coprecipitation have a considerably large specific surface of 30 m{sup 2}/g. The relative density greater than 97% is obtained when these nanocrystalline LaAlO{sub 3} powders are sintered at 1550 deg. C for 2 h.

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)

The preparation of UO2 powder: effect of ammonium uranate properties

International Nuclear Information System (INIS)

Woolfrey, J.L.

1978-01-01

Ammonium uranate (AU) powders were precipitated from a uranyl nitrate solution with gaseous ammonia. The decomposition of the powders in hydrogen was studied to determine those properties of AU which affect the decomposition reactions and influence the properties of the final UO 2 powder. The thermal decomposition was affected by the initial composition (ammonia and nitrate content) and the morphology of the AU powders. The amount of self-reduction increased with increasing combined ammonia content and decreased with increasing nitrate content. The specific surface area of the decomposed powder increased with increasing total ammonia content and initial surface area of the precursor AU powder. Thermal treatment of the decomposed powder can be used to modify such effects and, in commercial powder production, is used to control the properties of the final UO 2 powder. (Auth.)

Synthesis of Cu-coated Graphite Powders Using a Chemical Reaction Process

Energy Technology Data Exchange (ETDEWEB)

Jang, Jun-Ho; Park, Hyun-Kuk; Oh, Ik-Hyun [Korea Institute of Industrial Technology (KITECH), Gwangju (Korea, Republic of); Lim, Jae-Won [Chonbuk National University, Jeonju (Korea, Republic of)

2017-05-15

In this paper, Cu-coated graphite powders for a low thermal expansion coefficient and a high thermal conductivity are fabricated using a chemical reaction process. The Cu particles adhere to the irregular graphite powders and they homogeneously disperse in the graphite matrix. Cu-coated graphite powders are coarser at approximately 3-4 μm than the initial graphite powders; furthermore, their XRD patterns exhibit a low intensity in the oxide peak with low Zn powder content. For the passivation powders, the transposition solvent content has low values, and the XRD pattern of the oxide peaks is almost non-existent, but the high transposition solvent content does not exhibit a difference to the non-passivation treated powders.

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.

Heat transfer in large compacts of SYNROC powder

International Nuclear Information System (INIS)

Buykx, W.J.

1984-01-01

The parameters determining the time required to reach temperature uniformity in a shock heated cylindrical compact of SYNROC powder are identified as the dimensions of the compact and the thermal diffusivity of the material. The effect of shape and size of the compact are discussed, and an experimental study of the factors influencing the thermal diffusivity of compacted SYNROC powder is described

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

Thermal and X-ray diffraction analysis studies during the decomposition of ammonium uranyl nitrate

OpenAIRE

Kim, B. H.; Lee, Y. B.; Prelas, M. A.; Ghosh, T. K.

2012-01-01

Two types of ammonium uranyl nitrate (NH4)2UO2(NO3)4?2H2O and NH4UO2(NO3)3, were thermally decomposed and reduced in a TG-DTA unit in nitrogen, air, and hydrogen atmospheres. Various intermediate phases produced by the thermal decomposition and reduction process were investigated by an X-ray diffraction analysis and a TG/DTA analysis. Both (NH4)2UO2(NO3)4?2H2O and NH4UO2(NO3)3 decomposed to amorphous UO3 regardless of the atmosphere used. The amorphous UO3 from (NH4)2UO2(NO3)4?2H2O was crysta...

Pyrolysis characteristics and kinetic parameters determination of biomass fuel powders by differential thermal gravimetric analysis (TGA/DTG)

International Nuclear Information System (INIS)

El-Sayed, Saad A.; Mostafa, M.E.

2014-01-01

Highlights: • The sugarcane bagasse powder has better energy value compared to the cotton stalks. • Bagasse moisture is entrained in its cell walls and its evaporation needs more energy. • The cotton stalks is more reactive and readily combustible than the bagasse powders. • A lower E and A 0 has been found for bagasse compared with cotton stalks powders. • Calculated E of bagasse and cotton stalks by direct and integral methods are different. - Abstract: The kinetics of the thermal decomposition of the two biomass materials (sugarcane bagasse and cotton stalks powders) were evaluated using a differential thermo-gravimetric analyzer under a non-isothermal condition. Two distinct reaction zones were observed for the two biomasses. The direct Arrhenius plot method and the integral method were applied for determination of kinetic parameters: activation energy, pre-exponential factor, and order of reaction. The weight loss curve showed that pyrolysis of sugarcane bagasse and cotton stalks took place mainly in the range of 200–500 °C. The activation energy of the sugarcane bagasse powder obtained by the direct Arrhenius plot method ranged between 43 and 53.5 kJ/mol. On the other side, the integral method shows larger values of activation energy (77–87.7 kJ/mol). The activation energy of the cotton stalks powder obtained by the direct Arrhenius plot method was ranged between 98.5 and 100.2 kJ/mol, but the integral method shows larger values of activation energy (72.5–127.8 kJ/mol)

Preparation and soft magnetic properties of spark plasma sintered compacts based on Fe–Si–B glassy powder

Energy Technology Data Exchange (ETDEWEB)

Neamţu, B.V., E-mail: bogdan.neamtu@stm.utcluj.ro [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Marinca, T.F.; Chicinaş, I. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Isnard, O. [Institut Néel, CNRS/University Joseph Fourier, BP 166, 38042 Grenoble Cédex 9 (France); Popa, F. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Păşcuţă, P. [Physics and Chemistry Department Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania)

2014-07-05

Highlights: • Amorphous powder of Fe{sub 75}Si{sub 20}B{sub 5} (at.%) was prepared by wet mechanical alloying. • Spark plasma sintering was used for compaction of amorphous Fe{sub 75}Si{sub 20}B{sub 5} powder. • Increasing SPS time/temperature leads to improvement of AC/DC compacts properties. - Abstract: Amorphous powder of Fe{sub 75}Si{sub 20}B{sub 5} (at.%) was prepared by wet mechanical alloying route using benzene as surfactant. The amorphous phase is obtained after 60 h of milling. Structural, morphological, and thermal characteristics were investigated. The as-milled powder consists in micrometric particles with a mean diameter of 10.4 μm which are formed by the agglomeration of smaller particles. The amorphous powder is thermally stable up to the temperature of 490 °C. Spark plasma sintered compacts were prepared from the amorphous powders at sintering temperatures of 800, 850 and 900 °C. The phases formation and their evolution was investigated by X-ray diffraction technique showing that Fe{sub 3}Si and Fe{sub 2}B are the main phases formed during the spark plasma sintering process. Fe{sub 75}Si{sub 20}B{sub 5} (at.%) samples in the form of a ring were investigated in DC and AC magnetization regime. It was found that the boride phase formation (during sintering) and the low density of the compacts affect the magnetic properties of the compacts. In addition, a superficial contamination of the compacts with carbon (a layer of 2–3 μm) was evidenced, contributing thus to their soft magnetic deterioration. Increasing of the saturation induction, maximum relative permeability and initial relative permeability was observed by increasing both sintering temperature and time. It was generally observed that the compacts with high density have higher total core losses at high frequency.

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)

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.

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)

Thermally induced diffraction losses for a Gaussian pump beam and optimization of the mode-to-pump ratio in an end-pumped Nd:GdVO4 laser

International Nuclear Information System (INIS)

Wang, Y T; Li, W J; Pan, L L; Yu, J T; Zhang, R H

2013-01-01

The analytical model of thermally induced diffraction losses for a Gaussian pump beam are derived as functions of the mode-to-pump ratio and pump power in end-pumped Nd-doped lasers considering the energy transfer upconversion effects. The mode-to-pump ratio is optimized based on it. The results show that the optimum mode-to-pump ratio with the thermally induced diffraction losses is less than 0.65, and it is less than the results in which the thermally induced diffraction losses are neglected. The theoretical model is applied to a diode-end-pumped Nd:GdVO 4 laser operating at 1342 nm, and the theoretical calculations are in good agreement with the experimental results. (paper)

The pressure bonding ability of uranium dioxide powders in relation to the evolution of their surface properties

International Nuclear Information System (INIS)

Danroc, J.

1982-09-01

The long term storage of sinterable uranium dioxide powders generally improves their pressure bonding ability and the strength of the resulting green pellets. Evidence of the gradual evolution of the surface texture and composition of these powders during storage at room temperature and pressure has been provided by infrared spectroscopy, X-ray diffraction and thermogravimetric and microcalorimetric methods. These techniques demonstrated the existence of a thin adherent surface layer of UO 3 2H 2 0. Such a natural evolutionary process can be reproduced and substantially amplified by subjecting the powder to thermal treatments at temperatures up to 90 0 C in a moist air environment. It was shown that powder treated in this manner could be more readily compacted into strong green pellets than could raw material. The tensile strength, commonly regarded as a quality test for such pellets and measured by the brazilian method, was found to be at least twice that of normal pellets. The high density and geometric integrity of these sintered products ensures the extrapolation of these preparation techniques to the mass production of nuclear reactor fuel pellets [fr

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

Residual stress determination in thermally sprayed metallic deposits by neutron diffraction

International Nuclear Information System (INIS)

Keller, Thomas; Margadant, Nikolaus; Pirling, Thilo; Riegert-Escribano, Maria J.; Wagner, Werner

2004-01-01

Neutron diffraction was used to obtain spatially resolved strain and stress profiles in thermally sprayed metallic 'NiCrAlY' deposits (chemical composition 67 wt.% Ni, 22 wt.% Cr, 10 wt.% Al, 1 wt.% Y) and the underlying steel substrates. Samples of four different spray techniques were analyzed: atmospheric and water stabilized plasma spraying (APS and WSP), flame spraying (FS) and wire arc spraying (WAS). The results are quantitatively compared with the average in-plane residual stress determined by complementary bending tests and the hole drilling technique. While the stress profiles from the surface to the interface in the deposits are similar for all investigated spray techniques, their absolute values and gradients vary strongly. This is attributed to different quenching stresses from the impinging particles, different thermal histories the deposit/substrate systems undergo during the spraying and subsequent cooling, and also to different coating properties. In the water stabilized plasma sprayed and the wire arc sprayed deposits, a gradient in the stress-free lattice parameter was observed. Crack formation is found to be a dominant mechanism for stress relaxation in the surface plane

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.)

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)

Microstructure and thermal diffusivity in hydroxyapatite, dense bone and metals for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Mendez, M.; Diaz G, J.A.I.; Calderon, A. [CICATA-IPN, 11500 Mexico D.F. (Mexico)

2007-07-01

Full text: We report X-Ray diffraction and SEM analysis in hydroxyapatite obtained in powder form, as well as a SEM analysis in titanium, 316l stainless steel and dense bone in longitudinal and transversal cutting. Moreover, we realized a thermal diffusivity measurement in these materials in order to obtain the thermal compatibility between them. We use the photoacoustic technique in heat transmission configuration in order to obtain the thermal diffusivity values in the samples. Our results show a good thermal compatibility (74%) between hydroxyapatite and bone. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications. (Author)

Microstructure and thermal diffusivity in hydroxyapatite, dense bone and metals for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Mendez, M.; Diaz G, J.A.I.; Calderon, A. [CICATA-IPN, Legaria 694, 11500 Mexico D.F. (Mexico)

2006-07-01

We report X-Ray diffraction and SEM analysis in hydroxyapatite obtained in powder form, as well as a SEM analysis in titanium, 316l stainless steel and dense bone in longitudinal and transversal cutting. Moreover, we realized a thermal diffusivity measurement in these materials in order to obtain the thermal compatibility between them. We use the photoacoustic technique in heat transmission configuration in order to obtain the thermal diffusivity values in the samples. Our results show a good thermal compatibility (74%) between hydroxyapatite and bone. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications. (Author)

Microstructure and thermal diffusivity in hydroxyapatite, dense bone and metals for biomedical applications

International Nuclear Information System (INIS)

Mendez, M.; Diaz G, J.A.I.; Calderon, A.

2006-01-01

We report X-Ray diffraction and SEM analysis in hydroxyapatite obtained in powder form, as well as a SEM analysis in titanium, 316l stainless steel and dense bone in longitudinal and transversal cutting. Moreover, we realized a thermal diffusivity measurement in these materials in order to obtain the thermal compatibility between them. We use the photoacoustic technique in heat transmission configuration in order to obtain the thermal diffusivity values in the samples. Our results show a good thermal compatibility (74%) between hydroxyapatite and bone. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications. (Author)

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.

Optically stimulated luminescence of ZnO obtained by thermal treatment of ZnS chemically synthesized

International Nuclear Information System (INIS)

Cruz V, C.; Burruel I, S.E.; Orante B, V.R.; Grijalva M, H.; Perez S, R.; Bernal, R.

2005-01-01

In this work, we report the optically stimulated luminescence (OSL) dosimetry of new nano phosphors of ZnO obtained by thermal annealing of chemically synthesized ZnS powder. The synthesized ZnS nano powder was compressed in order to form pellet shaped pellets, which were afterwards subjected to a thermal annealing at 700 C during 24 h under air atmosphere. X-ray diffraction (XRD) patterns and energy-disperse X-ray Spectrometry (EDS) analyses confirmed the transformation of ZnS to ZnO. Samples were exposed to several doses of beta radiation up to 600 Gy, and the optically stimulated luminescence with 470 nm wavelength light was recorded as a function of dose. The intensity of the OSL signal increases by increasing dose, for what it is concluded that these new phosphor materials are suitable to be used in optically stimulated luminescence dosimetry. (Author)

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

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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.

Sintering of Cu–Al2O3 nano-composite powders produced by a thermochemical route

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MARIJA KORAC

2007-11-01

Full Text Available This paper presents the synthesis of nano-composite Cu–Al2O3 powder by a thermochemical method and sintering, with a comparative analysis of the mechanical and electrical properties of the obtained solid samples. Nano-crystalline Cu–Al2O3 powders were produced by a thermochemical method through the following stages: spray-drying, oxidation of the precursor powder, reduction by hydrogen and homogenization. Characterization of powders included analytical electron microscopy (AEM coupled with energy dispersive spectroscopy (EDS, differenttial thermal and thermogravimetric (DTA–TGA analysis and X-ray diffraction (XRD analysis. The size of the produced powders was 20–50 nm, with a noticeable presence of agglomerates. The composite powders were characterized by a homogenous distribution of Al2O3 in a copper matrix. The powders were cold pressed at a pressure of 500 MPa and sintered in a hydrogen atmosphere under isothermal conditions in the temperature range from 800 to 900 °C for up to 120 min. Characterization of the Cu–Al2O3 sintered system included determination of the density, relative volume change, electrical and mechanical properties, examination of the microstructure by SEM and focused ion beam (FIB analysis, as well as by EDS. The obtained nano-composite, the structure of which was, with certain changes, presserved in the final structure, provided a sintered material with a homogenеous distribution of dispersoid in a copper matrix, with exceptional effects of reinforcement and an excellent combination of mechanical and electrical properties.

X-ray diffraction study of thermal stress relaxation in ZnO films deposited by magnetron sputtering

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Conchon, F. [Institut P' , Universite de Poitiers-Ensma-UPR CNRS 3346, 86962 Futuroscope (France); Renault, P.O., E-mail: pierre.olivier.renault@univ-poitiers.f [Institut P' , Universite de Poitiers-Ensma-UPR CNRS 3346, 86962 Futuroscope (France); Le Bourhis, E.; Krauss, C.; Goudeau, P. [Institut P' , Universite de Poitiers-Ensma-UPR CNRS 3346, 86962 Futuroscope (France); Barthel, E.; Grachev, S. Yu.; Sondergard, E. [Lab. Surface du Verre et Interfaces (SVI), UMR 125, 93303 Aubervilliers (France); Rondeau, V.; Gy, R. [Lab. Recherche de Saint-Gobain (SGR), 93303 Aubervilliers (France); Lazzari, R.; Jupille, J. [Institut des Nanosciences de Paris (INSP), UMR 7588, 75015 Paris (France); Brun, N. [Lab. Physique des Solides (LPS), UMR 8502, 91405 Orsay (France)

2010-12-30

X-ray diffraction stress analyses have been performed on two different thin films deposited onto silicon substrate: ZnO and ZnO encapsulated into Si{sub 3}N{sub 4} layers. We showed that both as-deposited ZnO films are in a high compressive stress state. In situ X-ray diffraction measurements inside a furnace revealed a relaxation of the as-grown stresses at temperatures which vary with the atmosphere in the furnace and change with Si{sub 3}N{sub 4} encapsulation. The observations show that Si{sub 3}N{sub 4} films lying on both sides of the ZnO film play an important role in the mechanisms responsible for the stress relaxation during heat treatment. The different temperatures observed for relaxation in ambient and argon atmospheres suggest that the thermally activated stress relaxation may be attributed to a variation of the stoichiometry of the ZnO films. The present observations pave the way to fine tuning of the residual stresses through thermal treatment parameters.

A combined stretching-tilting mechanism produces negative, zero and positive linear thermal expansion in a semi-flexible Cd(II)-MOF.

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