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Sample records for powder diffraction thermal

  1. Powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Hart, M.

    1995-12-31

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

  2. Powder diffraction

    International Nuclear Information System (INIS)

    Hart, M.

    1995-01-01

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

  3. Diffraction. Powder, amorphous, liquid

    International Nuclear Information System (INIS)

    Sosnowska, I.M.

    1999-01-01

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

  4. Neutron Powder Diffraction in Sweden

    International Nuclear Information System (INIS)

    Tellgren, R.

    1986-01-01

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

  5. 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

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

    Directory of Open Access Journals (Sweden)

    Íris Duarte

    2016-09-01

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

  7. The analysis of powder diffraction data

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  8. 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

  9. 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.

  10. Uniting Electron Crystallography and Powder Diffraction

    CERN Document Server

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

    2012-01-01

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

  11. 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.

  12. 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

  13. Applications of neutron powder diffraction in materials research

    International Nuclear Information System (INIS)

    Kennedy, S.J.

    1996-01-01

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

  14. 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...

  15. 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...

  16. Rietveld analysis, powder diffraction and cement

    International Nuclear Information System (INIS)

    Peterson, V.

    2002-01-01

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

  17. Time-resolved Neutron Powder Diffraction

    International Nuclear Information System (INIS)

    Pannetier, J.

    1986-01-01

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

  18. 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)

  19. 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.

  20. 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

  1. 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

  2. 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.)

  3. 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.

  4. 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.)

  5. 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

  6. Development and directions of powder diffraction on proteins

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-07-01

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

  7. Development and directions of powder diffraction on proteins

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Paszkowicz, W.

    2006-01-01

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

  9. 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

  10. 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 ...

  11. Powder diffraction from a continuous microjet of submicrometer protein crystals.

    Science.gov (United States)

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

    2008-11-01

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

  12. Thermally induced phase transformation of pearl powder

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2015-10-01

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

  14. 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

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

    International Nuclear Information System (INIS)

    Fujii, Kotaro

    2015-01-01

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

  16. 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.)

  17. 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)

  18. Powder diffraction studies using anomalous dispersion

    International Nuclear Information System (INIS)

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

    1993-01-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  20. 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.

  1. 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

  2. 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)

  3. 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)

  4. 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.

  5. Fundamentals of powder x-ray diffraction practice

    International Nuclear Information System (INIS)

    Raftery, T.

    2002-01-01

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

  6. 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.

  7. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  8. 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)

  9. 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.)

  10. 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...

  11. 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.

  12. 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

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. 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

  4. 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....

  5. 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

  6. 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.

  7. 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....

  8. 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.

  9. 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...

  10. 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

  11. 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

  12. 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...

  13. 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...

  14. 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...

  15. 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

  16. 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

  17. 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.

  18. 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.

  19. 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.)

  20. 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)

  1. 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.

  2. 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

  3. 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

  4. Qualitative analysis of powder x-ray diffraction data

    International Nuclear Information System (INIS)

    Raftery, T.

    1999-01-01

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

  5. 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

  6. 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)

  7. 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

  8. 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

  9. 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

  10. 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.

  11. 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

  12. 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...

  13. 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)

  14. 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

  15. 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

  16. 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.

  17. 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.

  18. 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

  19. 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...

  20. 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.

  1. 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.

  2. 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

  3. Thermal Behaviour of Sm0.5 R 0.5FeO3 (R = Pr, Nd) Probed by High-Resolution X-ray Synchrotron Powder Diffraction.

    Science.gov (United States)

    Pavlovska, Olena; Vasylechko, Leonid; Buryy, Oleh

    2016-12-01

    Mixed ferrites Sm0.5Pr0.5FeO3 and Sm0.5Nd0.5FeO3 with orthorhombic perovskite structure isotypic with GdFeO3 were synthesized by solid-state reaction technique in air at 1473 K. Structural parameters obtained at room temperature prove a formation of continuous solid solutions in the SmFeO3-PrFeO3 and SmFeO3-NdFeO3 pseudo-binary systems. Sm0.5Pr0.5FeO3 and Sm0.5Nd0.5FeO3 show strongly anisotropic nonlinear thermal expansion: thermal expansion in the b direction is twice lower than in the a and c directions. The average linear thermal expansion coefficients of Sm0.5Pr0.5FeO3 and Sm0.5Nd0.5FeO3 in the temperature range of 298-1173 K are in the limits of (9.0-11.1) × 10(-6) K(-1), which is close to the values reported for the parent RFeO3 compounds. Subtle anomalies in the lattice expansion of Sm0.5Pr0.5FeO3 and Sm0.5Nd0.5FeO3 detected at 650-750 K reflect magnetoelastic coupling at the magnetic ordering temperature T N.

  4. 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

  5. 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.

  6. 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

  7. 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

  8. 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 ...

  9. 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.

  10. 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.

  11. 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.

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

    International Nuclear Information System (INIS)

    Zhang, Y.

    1988-01-01

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

  13. 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

  14. 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

  15. 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.

  16. 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...

  17. 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

  18. 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.

  19. Fast X-ray powder diffraction on I11 at Diamond.

    Science.gov (United States)

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

    2011-07-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

    Rius, J.; Miravitlles, C.

    1988-01-01

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

  2. 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

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

    International Nuclear Information System (INIS)

    James, M.

    1999-01-01

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

  4. 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.

  5. 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.)

  6. 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

  7. 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)

  8. 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

  9. 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.)

  10. 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 ...

  11. 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...

  12. 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.)

  13. 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

  14. 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)

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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.)

  20. 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)

  1. 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.)

  2. 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.

  3. 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

  4. 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...

  5. 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

  6. 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.

  7. 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...

  8. 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)

  9. 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.

  10. 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

  11. 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)

  12. 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)

  13. 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)

  14. 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

  15. 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.

  16. 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

  17. 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)

  18. 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...

  19. 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)

  20. 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)

  1. 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

  2. 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.

  3. 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.)

  4. 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…

  5. 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

  6. 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...

  7. 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.

  8. 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.

  9. 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.

  10. 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)

  11. 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)

  12. 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.

  13. 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.

  14. 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

  15. 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)>>>>

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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).

  2. 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...

  3. 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

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

    Science.gov (United States)

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

    2014-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-08-07

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

  6. 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.)

  7. 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

  8. 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

  9. 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.

  10. 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.

  11. Titanium and zirconium metal powder spheroidization by thermal plasma processes

    OpenAIRE

    Bissett, H.; van der Walt, I.J.; Havenga, J.L.; Nel, J.T.

    2015-01-01

    New technologies used to manufacture high-quality components, such as direct laser sintering, require spherical powders of a narrow particle size distribution as this affects the packing density and sintering mechanism. The powder also has to be chemically pure as impurities such as H, O, C, N, and S causes brittleness, influence metal properties such as tensile strength, hardness, and ductility, and also increase surface tension during processing. Two new metal powder processes have been dev...

  12. 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.

  13. 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.

  14. 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.

  15. 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...

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

    International Nuclear Information System (INIS)

    Charpin, P.; Hauptman, A.

    1960-01-01

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

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

    Science.gov (United States)

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

    2003-10-01

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

  18. 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.

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

    International Nuclear Information System (INIS)

    Streek, Jacco van de; Neumann, Marcus A.

    2014-01-01

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

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

    International Nuclear Information System (INIS)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-11-01

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

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

    International Nuclear Information System (INIS)

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

    1984-01-01

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    1977-01-01

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

  5. 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.

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

    Science.gov (United States)

    Yamamura, Shigeo; Momose, Yasunori

    2003-06-18

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1976-12-15

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

  8. 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.

  9. 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

  10. 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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  13. 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.

  14. 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.

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    1985-11-01

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

  17. 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.

  18. Quantitative determination of mineral composition by powder X-ray diffraction

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1986-01-01

    A method is described of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where mless than or equal ton, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K/sub j/=(X/sub j//X/sub l/)(I/sub l//I/sub j/) for each mineral (j=2...n) in the group of known minerals (j=2...n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; identifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X/sub j//X/sub l/ for each mineral (j=2...m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I/sub j/ of each mineral in the test sample to the measured highest integrated intensity peak I/sub l/ of the reference mineral in the test sample, and from the previously determined standard coefficients, X/sub j//X/sub l/=K/sub j/(I/sub j//I/sub l/

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  20. 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

  1. 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.

  2. 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

  3. 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.)

  4. 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.

  5. 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.)

  6. 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)

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  8. X-ray powder diffraction camera for high-field experiments

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-09-01

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

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

    International Nuclear Information System (INIS)

    Giacovazzo, C.

    1996-01-01

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

  11. 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.

  12. 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

  13. 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.

  14. 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

  15. New processing for DEB powder for thermal batteries

    Science.gov (United States)

    Szwarc, R.; Walton, R. D.

    1980-06-01

    The electrochemical batteries employed are primary reserve batteries which employ a pelletized cell design. Each cell consists of an electrolyte-depolarizer pellet sandwiched between an anode and a heat pellet. The depolarizer-electrolyte, commonly referred to as DEB, is composed of CaCrO4, LiClKC1 eutectic and SiO2 binder powder, which has been blended and pressed into pellets. The DEB pellet serves as electrolyte and as active cathode when the salt becomes molten upon battery activation. The heat pellet serves the dual purpose of providing the heat necessary to activate the battery and as the cathode current collector. The heat pellet is composed of iron powder and KC104. Since activated life requirements for batteries vary from seconds up to one hour, the battery must be well insulated to conserve the heat produced by the ignition of the heat pellets to maintain the electrolyte in a molten state and to protect sensitive electronic components in contact with the battery case. Because the electrolyte, particularly LiCl, is hygroscopic, the baterries are hermetically sealed in stainless steel cans, and are manufactured in dryrooms maintaned at 3% relative humidity or better.

  16. 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)

  17. 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.

  18. 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

  19. 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

  20. 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)

  1. 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

  2. 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)

  3. 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.

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

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

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

  5. 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.

  6. 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.

  7. 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)

  8. 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.

  9. 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...

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  11. 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

  12. 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

  13. 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

  14. 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...

  15. 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.

  16. 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

  17. 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

  18. 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)

  19. 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)

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

    International Nuclear Information System (INIS)

    Constantinescu, B.

    2003-01-01

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

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

    Science.gov (United States)

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

    2014-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-12-09

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

  3. 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).

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  7. 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.

  8. 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)

  9. 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.

  10. 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.

  11. 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...

  12. 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.

  13. 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

  14. 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

  15. 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...

  16. 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

  17. 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.

  18. 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.

  19. 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.

  20. A study of the thermal behavior of terrestrial tridymite by continuous X-ray diffraction

    Science.gov (United States)

    Smelik, Eugene A.; Reeber, Robert R.

    1990-06-01

    Phase transition behavior of two types of terrestrial tridymite; crystals from Topaz Mountain in the Thomas Range of northwestern Utah and Smith Peak in Plumas County, California; were investigated. The Topaz Mtn. samples were characterized at room temperature using optical, X-ray diffraction (Debye-Scherrer, rotation, and Laue), and transmission electron microscopy (TEM) methods. Least-squares refinement of the powder data yielded an orthorhombic cell with a = 17.072 Å, b = 9.923 Å, and c = 16.291 Å. The tridymite is designated PO-2 (nomenclature of Nukui and Nakazawa 1980). This material is complexly twinned and has severe stacking disorder parallel to [001]. Additional X-ray experiments were performed on one Plumas County crystal and four Topaz Mtn. crystals during heating from room temperature to a minimum of 320° C with one run attaining a maximum temperature of 532° C. Crystal to crystal behavior was somewhat variable suggesting kinetic barriers to transition controlled by the detailed structural state of each crystal. The Laue results indicated that the transition behavior of these multiple twinned tridymites could be conveniently divided into two classes: discontinuous and continuous. The discontinuous diffraction effects were generally associated with major structural transitions. Continuous diffraction effects involved gradual structural distortions of the tridymite framework that occurred over discrete ranges of temperature. Upon cooling, many of the minor effects were not reversible while the major transitions were reversible with some temperature hysteresis. Comparison of initial and final diffraction patterns indicated that the starting and ending structures were very similar but not identical. From the five experiments, three distinct patterns emerged based on the major transitions observed: Type I behavior (Topaz Mtn.) characterized by three major changes at 175 187° C, 283 302° C, and 348 352° C, Type II behavior (Plumas Co.) characterized

  1. 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

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. Thermal diffuse scattering in time-of-flight neutron diffraction studied on SBN single crystals

    International Nuclear Information System (INIS)

    Prokert, F.; Savenko, B.N.; Balagurov, A.M.

    1994-01-01

    At time-of-flight (TOF) diffractometer D N-2, installed at the pulsed reactor IBR-2 in Dubna, Sr x Ba 1-x Nb 2 O 6 mixed single crystals (SBN-x) of different compositions (0.50 < x< 0.75) were investigated between 15 and 773 K. The diffraction patterns were found to be strongly influenced by the thermal diffuse scattering (TDS). The appearance of the TDS from the long wavelength acoustic models of vibration in single crystals is characterized by the ratio of the velocity of sound to the velocity of neutron. Due to the nature of the TOF Laue diffraction technique used on D N-2, the TDS around Bragg peaks has rather a complex profile. An understanding of the TDS close to Bragg peaks is essential in allowing the extraction of the diffuse scattering occurring at the diffuse ferroelectric phase transition in SBN crystals. 11 refs.; 9 figs.; 1 tab. (author)

  8. 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.

  9. 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.

  10. X-ray diffraction, IR spectroscopy and thermal characterization of partially hydrolyzed guar gum.

    Science.gov (United States)

    Mudgil, Deepak; Barak, Sheweta; Khatkar, B S

    2012-05-01

    Guar gum was hydrolyzed using cellulase from Aspergillus niger at 5.6 pH and 50°C temperature. Hydrolyzed guar gum sample was characterized using Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, dilute solution viscometry and rotational viscometry. Viscometry analysis of native guar gum showed a molecular weight of 889742.06, whereas, after enzymatic hydrolysis, the resultant product had a molecular weight of 7936.5. IR spectral analysis suggests that after enzymatic hydrolysis of guar gum there was no major transformation of functional group. Thermal analysis revealed no major change in thermal behavior of hydrolyzed guar gum. It was shown that partial hydrolysis of guar gum could be achieved by inexpensive and food grade cellulase (Aspergillus niger) having commercial importance and utilization as a functional soluble dietary fiber for food industry. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Neutron diffraction and thermal studies of amorphous CS2 realised by low-temperature vapour deposition

    International Nuclear Information System (INIS)

    Yamamuro, O.; Matsuo, T.; Onoda-Yamamuro, N.; Takeda, K.; Munemura, H.; Tanaka, S.; Misawa, M.

    2003-01-01

    We have succeeded in preparing amorphous carbon disulphide (CS 2 ) by depositing its vapour on a cold substrate at 10 K. Complete formation of the amorphous state has been confirmed by neutron diffraction and differential thermal analysis (DTA). The amorphous sample crystallized at ca. 70 K, which is lower than the hypothetical glass transition temperature (92 K) estimated from the DTA data of the (CS 2 ) x (S 2 Cl 2 ) 1-x binary mixture. CS 2 , a symmetric linear tri-atomic molecule, is the simplest of the amorphized molecular substances whose structural and thermal information has been reported so far. Comparison of the static structure factors S(Q) has shown that the orientational correlation of CS 2 molecules may be much stronger in the amorphous state than in the liquid state at higher temperature. (authors)

  12. 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...

  13. 1-(2-furoyl)-3,3-(diphenyl)thiourea: spectroscopic characterization and structural study from X-ray powder diffraction using simulated annealing

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

  14. 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.

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

    Science.gov (United States)

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

    2013-12-01

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

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

    OpenAIRE

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

    2002-01-01

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

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

    DEFF Research Database (Denmark)

    Grube, Elisabeth; Nielsen, Ulla Gro

    2015-01-01

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

  18. 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....

  19. 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.

  20. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Palin, L

    2005-03-15

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

  2. 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.

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    Lee Brooks

    2015-09-01

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

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Differential thermal, Thermogravimetric and X-ray diffraction investigation of hydration phases in cementitious waste form

    International Nuclear Information System (INIS)

    Khalil, M.Y.; Nagy, M.E.; El-Sourougy, M.R.; Zaki, A.A.

    1996-01-01

    Hydration phases of cement determine the final properties of the product. Adding other components to the cement paste may alter the final phases formed and affect properties of the hardened products. In this work ordinary portland cement and/or blast furnace slag cement were hardened with low-or intermediate-level radioactive liquid wastes and different additives. Hydration phases were investigated using differential thermal, thermogravimetric, and X-ray diffraction techniques. Low-and intermediate-level liquid wastes were found not to affect the hydration phases of cement. The addition of inorganic exchangers and latex were found to affect the hydration properties of the cement waste system. This resulted in a reduction of compressive strength. On the contrary, addition of epoxy also affected the hydration causing increase in compressive strength. 10 figs., 2 tabs

  15. Analysis of rocks involving the x-ray diffraction, infrared and thermal gravimetric techniques

    International Nuclear Information System (INIS)

    Ikram, M.; Rauf, M.A.; Munir, N.

    1998-01-01

    Chemical analysis of rocks and minerals are usually obtained by a number of analytical techniques. The purpose of present work is to investigate the chemical composition of the rock samples and also to find that how far the results obtained by different instrumental methods are closely related. Chemical tests wee performed before using the instrumental techniques in order to determined the nature of these rocks. The chemical analysis indicated mainly the presence of carbonate and hence the carbonate nature of these rocks. The x-ray diffraction, infrared spectroscopy and thermal gravimetric analysis techniques were used for the determination of chemical composition of these samples. The results obtained by using these techniques have shown a great deal of similarities. (author)

  16. High pressure sample container for thermal neutron spectroscopy and diffraction on strongly scattering fluids

    International Nuclear Information System (INIS)

    Verkerk, P.; Pruisken, A.M.M.

    1979-01-01

    A description is presented of the construction and performance of a container for thermal neutron scattering on a fluid sample with about 1.5 cm -1 macroscopic cross section (neglecting absorption). The maximum pressure is about 900 bar. The container is made of 5052 aluminium capillary with inner diameter 0.75 mm and wall thickness 0.25 mm; it covers a neutron beam with a cross section of 9 X 2.5 cm 2 . The container has been successfully used in neutron diffraction and time-of-flight experiments on argon-36 at 120 K and several pressures up to 850 bar. It is shown that during these measurements the temperature gradient over the sample as well as the error in the absolute temperature were both less than 0.05 K. Subtraction of the Bragg peaks due to container scattering in diffraction experiments may be dfficult, but seems feasible because of the small amount of aluminium in the neutron beam. Correction for container scattering and multiple scattering in time-of-flight experiments may be difficult only in the case of coherently scattering samples and small scattering angles. (Auth.)

  17. Thermal dehydration of potash alum studied by Raman spectroscopy and X-ray diffraction analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kishimura, Hiroaki, E-mail: kisimura@nda.ac.jp; Imasu, Yuhta; Matsumoto, Hitoshi

    2015-01-15

    The thermal dehydrations of potash alum caused by heating at various temperatures for at least 2 h were investigated by ex situ Raman spectroscopy and X-ray diffraction (XRD) analyses in air. With increasing the heating temperature, all Raman peaks were observed to broaden, while an additional broad peak appeared at approximately 1030 cm{sup −1} and shifted toward higher wavenumbers. In addition, the Raman band assigned to the O–H stretching mode weakened. The orientational disorder (OD) of the sulfate ions, as indicated by the intensity ratio of doublet peaks at 989 and 974 cm{sup −1}, was found to increase with increasing the heating temperature. The XRD patterns demonstrated that a structural phase transition from crystalline KAl(SO{sub 4}){sub 2}⋅12H{sub 2}O to amorphous phases began at around 75 °C, while broadening of the Raman peaks and an increase in OD also suggested the onset of an amorphous phase. Raman peaks corresponding to anhydrous KAl(SO{sub 4}){sub 2} appeared at approximately 180 °C. It was concluded that the elimination of water molecules was responsible for increase in the extent of OD, and this in turn induced the observed phase transitions. The formation of the amorphous phases observed in this work was similar to the pressure-induced amorphization of KAl(SO{sub 4}){sub 2}⋅12H{sub 2}O. - Highlights: • The thermal dehydration of potash alum proceeds through several steps. • Raman spectra and X-ray diffraction reveal the amorphization of the heated samples. • A transition from the amorphous phase to the KAl(SO{sub 4}){sub 2} crystal phase is observed in the sample heated at 180 °C.

  18. 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.

  19. 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.

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

    NARCIS (Netherlands)

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

    2006-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

  2. 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.

  3. Thermal expansion and decomposition of jarosite: a high-temperature neutron diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Hongwu [Los Alamos National Laboratory; Zhao, Yusheng [Los Alamos National Laboratory; Vogel, Sven C [Los Alamos National Laboratory; Hickmott, Donald D [Los Alamos National Laboratory; Daemen, Luke L [Los Alamos National Laboratory; Hartl, Monika A [Los Alamos National Laboratory

    2009-01-01

    The structure of deuterated jarosite, KFe{sub 3}(SO{sub 4}){sub 2}(OD){sub 6}, was investigated using time-of-flight neutron diffraction up to its dehydroxylation temperature. Rietveld analysis reveals that with increasing temperature, its c dimension expands at a rate {approx}10 times greater than that for a. This anisotropy of thermal expansion is due to rapid increase in the thickness of the (001) sheet of [Fe(O,OH){sub 6}] octahedra and [SO{sub 4}] tetrahedra with increasing temperature. Fitting of the measured cell volumes yields a coefficient of thermal expansion, a = a{sub 0} + a{sub 1} T, where a{sub 0} = 1.01 x 10{sup -4} K{sup -1} and a{sub 1} = -1.15 x 10{sup -7} K{sup -2}. On heating, the hydrogen bonds, O1{hor_ellipsis}D-O3, through which the (001) octahedral-tetrahedral sheets are held together, become weakened, as reflected by an increase in the D{hor_ellipsis}O1 distance and a concomitant decrease in the O3-D distance with increasing temperature. On further heating to 575 K, jarosite starts to decompose into nanocrystalline yavapaiite and hematite (as well as water vapor), a direct result of the breaking of the hydrogen bonds that hold the jarosite structure together.

  4. 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

  5. Residual stress determination in thermally sprayed metallic deposits by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-05-25

    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.

  6. TEV—A Program for the Determination of the Thermal Expansion Tensor from Diffraction Data

    Directory of Open Access Journals (Sweden)

    Thomas Langreiter

    2015-02-01

    Full Text Available TEV (Thermal Expansion Visualizing is a user-friendly program for the calculation of the thermal expansion tensor αij from diffraction data. Unit cell parameters determined from temperature dependent data collections can be provided as input. An intuitive graphical user interface enables fitting of the evolution of individual lattice parameters to polynomials up to fifth order. Alternatively, polynomial representations obtained from other fitting programs or from the literature can be entered. The polynomials and their derivatives are employed for the calculation of the tensor components of αij in the infinitesimal limit. The tensor components, eigenvalues, eigenvectors and their angles with the crystallographic axes can be evaluated for individual temperatures or for temperature ranges. Values of the tensor in directions parallel to either [uvw]’s of the crystal lattice or vectors (hkl of reciprocal space can be calculated. Finally, the 3-D representation surface for the second rank tensor and pre- or user-defined 2-D sections can be plotted and saved in a bitmap format. TEV is written in JAVA. The distribution contains an EXE-file for Windows users and a system independent JAR-file for running the software under Linux and Mac OS X. The program can be downloaded from the following link: http://www.uibk.ac.at/mineralogie/downloads/TEV.html (Institute of Mineralogy and Petrography, University of Innsbruck, Innsbruck, Austria

  7. 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.

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

    Directory of Open Access Journals (Sweden)

    Elisa Rodeghero

    2017-02-01

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

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  11. X-ray diffraction and thermal analysis of kaolins particle size fractions

    Directory of Open Access Journals (Sweden)

    Patricia dos Santos

    2013-09-01

    Full Text Available Kaolins are common geological materials and have high concentrations of kaolinite as well as the clay fraction of tropical and subtropical soils of Brazil. The characterization of kaolin is a proxy of assessing the contribution of kaolinite to important soil chemical and mineralogical attributes. This study evaluated four kaolins (commercial kaolin A (CCA, commercial kaolin B (CCB, pink sandy kaolin A (CRA and green sandy kaolin A (CVA in the original form and after particle size separation into: sand (200-53 mm, coarse silt (53-20 m, fine silt (20-2 m, large clay (2-1m, medium clay (1-0.5 m and fine clay (<0.5m fractions. The minerals were identified by X-ray diffraction (XRD and evaluated for crystallinity (kaolinite and halloysite through indexes Hughes and Brown, Amigó, Bramão and the dehydroxylation temperature. The physical fractionation was efficient to concentrate minerals in specific size fractions which were not identified in the original material. In CCA kaolin was concentrated one mineral which remains unidentified in fine fractions, in kaolin CRA, zircon was concentrated in the coarse silt and different silicates in the fine fractions, in kaolin CCB were concentrated kaolinite and a silicate in the medium and coarse clay fractions. The estimate by X-ray diffraction overestimated the amount of kaolinite and halloysite underestimated when compared to quantification by thermal gravimetric analysis The crystallinity index exhibit different behaviors depending on the mineralogy of each material, thus the correlation between the crystallinity of kaolinite and / or halloysite and other variables, may be compromised, especially in materials with distinct geological origins.

  12. 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.

  13. 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...

  14. 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.)

  15. 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

  16. Powder metallurgical nanostructured medium carbon bainitic steel: Kinetics, structure, and in situ thermal stability studies

    Energy Technology Data Exchange (ETDEWEB)

    Lonardelli, I., E-mail: il244@cam.ac.uk [University of Cambridge, Materials Science and Metallurgy, Pembroke Street, Cambridge CB2 3QZ (United Kingdom); University of Trento, Materials Engineering and Industrial Technologies, via Mesiano 77, 38123 Trento (Italy); Bortolotti, M. [Fondazione Bruno Kessler, via Sommarive 18, 38123 Trento (Italy); Beek, W. van [Swiss-Norwegian Beamlines, ESRF, BP 220, 38043 Grenoble Cedex (France); Girardini, L.; Zadra, M. [K4-Sint, via Dante 300, 38057 Pergine Valsugana (Italy); Bhadeshia, H.K.D.H. [University of Cambridge, Materials Science and Metallurgy, Pembroke Street, Cambridge CB2 3QZ (United Kingdom)

    2012-10-15

    It has been possible to produce incredibly fine plates of bainitic ferrite separated by a percolating network of retained austenite in a medium carbon steel produced by mechanical alloying followed by spark plasma sintering and isothermal heat treatment. This is because the sintering process limits the growth of the austenite grains to such an extent that the martensite-start temperature is suppressed in spite of the medium carbon concentration. Furthermore, the fine austenite grain size accelerates the bainite transformation, which can therefore be suppressed to low temperatures to obtain a nanostructure. Microscopy and in situ synchrotron X-ray diffraction were used to investigate the morphology and the thermal stability of the retained austenite during continuous heating. These latter experiments revealed a gradient of carbon concentration in the retained austenite and a reduced thermal stability in high carbon film-austenite. It was also possible to correlate the evolution of defect density and carbon depletion in both retained austenite and bainitic ferrite during tempering.

  17. 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

  18. 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

  19. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-07-01

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

  1. Rapid thermal processing chamber for in-situ x-ray diffraction

    International Nuclear Information System (INIS)

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F.; Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S.

    2015-01-01

    Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs −1 , and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi 2 O 3 -SiO 2 glass frit obtained during heating with ramp rates 5 °C s −1 and 100 °C s −1 , revealing numerous phase changes

  2. Rapid thermal processing chamber for in-situ x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F., E-mail: mftoney@slac.stanford.edu [SSRL, SLAC National Accelerator Laboratory, 2575, Sand Hill Road, Menlo Park, California 94025 (United States); Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S. [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States)

    2015-01-15

    Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs{sup −1}, and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi{sub 2}O{sub 3}-SiO{sub 2} glass frit obtained during heating with ramp rates 5 °C s{sup −1} and 100 °C s{sup −1}, revealing numerous phase changes.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-01

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

  4. 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.

  5. Thermal stability and creep behaviour of MgNiYCe-rich mischmetal alloys processed by a powder metallurgy route

    Czech Academy of Sciences Publication Activity Database

    Peréz, P.; Milička, Karel; Badia, J. M.; Garcés, G.; Antoranz, J. M.; Gonzáles, S.; Dobeš, Ferdinand; Adeva, P.

    289-292, - (2009), s. 127-136 ISSN 1012-0386. [DIMAT 2008, International Conference on Diffusion in Materials /7./. Lanzarote, Canary Islands, 28.10.2008-31.10.2008] Grant - others:Ministerio de Ciencia y Tecnologia (ES) MAT2006-11731-C02 Institutional research plan: CEZ:AV0Z20410507 Keywords : magnesium alloys * powder metallurgy * microstructure * thermal stability * creep Subject RIV: JG - Metallurgy

  6. 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

  7. 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

  8. 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)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-01

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

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

    Science.gov (United States)

    Fix, I; Steffens, K J

    2004-05-01

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

  14. 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)

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-26

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

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

    Science.gov (United States)

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

    1990-12-01

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

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

    Science.gov (United States)

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

    1991-02-01

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

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

    Science.gov (United States)

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

    2016-12-19

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

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

    Science.gov (United States)

    Vogt, Frederick G; Williams, Glenn R

    2012-07-01

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

  1. Multiphysics simulation of thermal phenomena in direct laser metal powder deposition

    CSIR Research Space (South Africa)

    Pityana, SL

    2016-11-01

    Full Text Available presents on two dimensional multi-physics models to describe the physical mechanism of heat transfer, melting and solidification that take place during and post laser-powder interaction. The simulated transient temperature profile, the geometrical features...

  2. Plasma spheroidization of iron powders in a non-transferred DC thermal plasma jet

    International Nuclear Information System (INIS)

    Kumar, S.; Selvarajan, V.

    2008-01-01

    In this paper, the results of plasma spheroidization of iron powders using a DC non-transferred plasma spray torch are presented. The morphology of the processed powders was characterized through scanning electron microscopy (SEM) and optical microscopy (OM). The percentages of spheroidized powders were calculated by the shape factors such as the Irregularity Parameter (IP) and Roundness (RN). A maximum of 83% of spheroidization can be achieved. The spheroidization results are compared with the theoretical estimation and they are found to be in good agreement. The phase composition of the spheroidized powder was analyzed by XRD. The effect of plasma jet temperature and plasma gas flow rate on spheroidization is discussed. At low plasma gas flow rates and at high plasma jet temperatures, the percentage of spheroidization is high

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

    Science.gov (United States)

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

    Two types of ammonium uranyl nitrate (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O and NH 4 UO 2 (NO 3 ) 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 (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O and NH 4 UO 2 (NO 3 ) 3 decomposed to amorphous UO 3 regardless of the atmosphere used. The amorphous UO 3 from (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O was crystallized to γ-UO 3 regardless of the atmosphere used without a change in weight. The amorphous UO 3 obtained from decomposition of NH 4 UO 2 (NO 3 ) 3 was crystallized to α-UO 3 under a nitrogen and air atmosphere, and to β-UO 3 under a hydrogen atmosphere without a change in weight. Under each atmosphere, the reaction paths of (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O and NH 4 UO 2 (NO 3 ) 3 were as follows: under a nitrogen atmosphere: (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4 ·H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4  → NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → γ-UO 3  → U 3 O 8 , NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → α-UO 3  → U 3 O 8 ; under an air atmosphere: (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4 ·H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4  → NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → γ-UO 3  → U 3 O 8 , NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → α-UO 3  → U 3 O 8 ; and under a hydrogen atmosphere: (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4 ·H 2 O → (NH 4 ) 2 UO 2 (NO 3 ) 4  → NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → γ-UO 3  → α-U 3 O 8  → UO 2 , NH 4 UO 2 (NO 3 ) 3  → A-UO 3  → β-UO 3  → α-U 3 O 8  → UO 2 .

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

    African Journals Online (AJOL)

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

  5. Effect of Young's modulus evolution on residual stress measurement of thermal barrier coatings by X-ray diffraction

    International Nuclear Information System (INIS)

    Chen, Q.; Mao, W.G.; Zhou, Y.C.; Lu, C.

    2010-01-01

    Subjected to thermal cycling, the apparent Young's modulus of air plasma-sprayed (APS) 8 wt.% Y 2 O 3 -stabilized ZrO 2 (8YSZ) thermal barrier coatings (TBCs) was measured by nanoindentation. Owing to the effects of sintering and porous microstructure, the apparent Young's modulus follows a Weibull distribution and changes from 50 to 93 GPa with an increase of thermal cycling. The evolution of residual stresses in the top coating of an 8YSZ TBC system was determined by X-ray diffraction (XRD). The residual stresses derived from the XRD data are well consistent with that obtained by the Vickers indention. It is shown that the evolution of Young's modulus plays an important role in improving the measurement precision of residual stresses in TBCs by XRD.

  6. Assessment of properties thermal sprayed coatings realised using cermet blend powder

    Directory of Open Access Journals (Sweden)

    J. Brezinová

    2014-10-01

    Full Text Available The article deals with the assessment of selected properties of plasma sprayed coatings based on ZrSiO4 doped with different volume fractions of metal dopant (Ni. Mixed powders are cermet blends. Aim of the work consists of verificating the possibility to replace the application of Ni interlayer by adding Ni directly to the ceramic powder and apply them together in a single technological operation. The coatings were studied from point of view of their structure, porosity, adhesion of the coatings in relation to the volume of dopant added and wear resistance. The best properties reached composite coating doped with 12 % Ni.

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

    International Nuclear Information System (INIS)

    Wertz, D.L.; Bissell, M.

    1994-01-01

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

  8. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

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

    2015-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Tatiana Minkina

    2017-04-01

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

  10. Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction--a benchmark structure-property study.

    Science.gov (United States)

    Lock, Nina; Jensen, Ellen M L; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B

    2013-07-14

    Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0-2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water-isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5-7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300-1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

  11. Mixed-linker UiO-66: structure-property relationships revealed by a combination of high-resolution powder X-ray diffraction and density functional theory calculations.

    Science.gov (United States)

    Taddei, Marco; Tiana, Davide; Casati, Nicola; van Bokhoven, Jeroen A; Smit, Berend; Ranocchiari, Marco

    2017-01-04

    The use of mixed-linker metal-organic frameworks (MIXMOFs) is one of the most effective strategies to modulate the physical-chemical properties of MOFs without affecting the overall crystal structure. In many instances, MIXMOFs have been recognized as solid solutions, with random distribution of ligands, in agreement with the empirical rule known as Vegard's law. In this work, we have undertaken a study combining high-resolution powder X-ray diffraction (HR-PXRD) and density functional theory (DFT) calculations with the aim of understanding the reasons why UiO-66-based amino- and bromo-functionalized MIXMOFs (MIXUiO-66) undergo cell expansion obeying Vegard's law and how this behaviour is related to their physical-chemical properties. DFT calculations predict that the unit cell in amino-functionalized UiO-66 experiences only minor expansion as a result of steric effects, whereas major modification to the electronic features of the framework leads to weaker metal-linker interaction and consequently to the loss of stability at higher degrees of functionalization. For bromo-functionalized UiO-66, steric repulsion due to the size of bromine yields a large cell expansion, but the electronic features remain very similar to pristine UiO-66, preserving the stability of the framework upon functionalization. MIXUiO-66 obtained by either direct synthesis or by post-synthetic exchange shows Vegard-like behaviour, suggesting that both preparation methods yield solid solutions, but the thermal stability and the textural properties of the post-synthetic exchanged materials do not display a clear dependence on the chemical composition, as observed for the MOFs obtained by direct synthesis.

  12. Neutron diffraction and thermal studies of amorphous CS{sub 2} realised by low-temperature vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Yamamuro, O.; Matsuo, T. [Osaka Univ., Dept. of Chemistry, Graduate School of Sciences (Japan); Onoda-Yamamuro, N. [Tokyo Denki Univ., College of Sciences and Technology (Japan); Takeda, K. [Naruto Univ., Dept. of Chemistry, Tokushima (Japan); Munemura, H.; Tanaka, S.; Misawa, M. [Niigata Univ. (Japan). Faculty of Science

    2003-08-01

    We have succeeded in preparing amorphous carbon disulphide (CS{sub 2}) by depositing its vapour on a cold substrate at 10 K. Complete formation of the amorphous state has been confirmed by neutron diffraction and differential thermal analysis (DTA). The amorphous sample crystallized at ca. 70 K, which is lower than the hypothetical glass transition temperature (92 K) estimated from the DTA data of the (CS{sub 2}){sub x}(S{sub 2}Cl{sub 2}){sub 1-x} binary mixture. CS{sub 2}, a symmetric linear tri-atomic molecule, is the simplest of the amorphized molecular substances whose structural and thermal information has been reported so far. Comparison of the static structure factors S(Q) has shown that the orientational correlation of CS{sub 2} molecules may be much stronger in the amorphous state than in the liquid state at higher temperature. (authors)

  13. Effect of particle- and specimen-level transport on product state in compacted-powder combustion synthesis and thermal debinding of polymers from molded powders

    Science.gov (United States)

    Oliveira, Amir Antonio Martins

    The existence of large gradients within particles and fast temporal variations in the temperature and species concentration prevents the use of asymptotic approximations for the closure of the volume-averaged, specimen-level formulations. In this case a solution of the particle-level transport problem is needed to complement the specimen-level volume-averaged equations. Here, the use of combined specimen-level and particle-level models for transport in reactive porous media is demonstrated with two examples. For the gasless compacted-powder combustion synthesis, a three-scale model is developed. The specimen-level model is based on the volume-averaged equations for species and temperature. Local thermal equilibrium is assumed and the macroscopic mass diffusion and convection fluxes are neglected. The particle-level model accounts for the interparticle diffusion (i.e., the liquid migration from liquid-rich to liquid-lean regions) and the intraparticle diffusion (i.e., the species mass diffusion within the product layer formed at the surface of the high melting temperature component). It is found that the interparticle diffusion controls the extent of conversion to the final product, the maximum temperature, and to a smaller degree the propagation velocity. The intraparticle diffusion controls the propagation velocity and to a smaller degree the maximum temperature. The initial stages of thermal degradation of EVA from molded specimens is modeled using volume-averaged equations for the species and empirical models for the kinetics of the thermal degradation, the vapor-liquid equilibrium, and the diffusion coefficient of acetic acid in the molten polymer. It is assumed that a bubble forms when the partial pressure of acetic acid exceeds the external ambient pressure. It is found that the removal of acetic acid is characterized by two regimes, a pre-charge dominated regime and a generation dominated regime. For the development of an optimum debinding schedule, the

  14. Inhomogeneous thermal expansion of metallic glasses in atomic-scale studied by in-situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Taghvaei, Amir Hossein, E-mail: amirtaghvaei@gmail.com [Department of Materials Science and Engineering, Shiraz University of Technology, Shiraz (Iran, Islamic Republic of); Shakur Shahabi, Hamed [IFW Dresden, Institute for Complex Materials, Helmholtzstr. 20, 01069 Dresden (Germany); Bednarčik, Jozef [Photon Science DESY, Notkestraße 85, 22603 Hamburg (Germany); Eckert, Jürgen [IFW Dresden, Institute for Complex Materials, Helmholtzstr. 20, 01069 Dresden (Germany); TU Dresden, Institute of Materials Science, 01062 Dresden (Germany)

    2015-01-28

    Numerous investigations have demonstrated that the elastic strain in metallic glasses subjected to mechanical loading could be inhomogeneous in the atomic-scale and it increases with distance from an average atom and eventually reaches the macroscopic strain at larger inter-atomic distances. We have observed a similar behavior for the thermal strain imposed by heating of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} glassy particles below the glass transition temperature by analysis of the scattering data obtained by in-situ high-energy synchrotron X-ray diffraction (XRD). The results imply that the volumetric thermal strains calculated from the shift in position of the principal diffraction maximum and reduced pair correlation function (PDF) peaks are in good agreement for the length scales beyond 0.6 nm, corresponding to the atoms located over the third near-neighbor shell. However, smaller and even negative volumetric thermal strains have been calculated based on the shifts in the positions of the second and first PDF peaks, respectively. The structural changes of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} glassy particles are accompanied by decreasing the average coordination number of the first near-neighbor shell, which manifests the occurrence of local changes in the short-range order upon heating. It is believed that the detected length-scale dependence of the volumetric thermal strain is correlated with the local atomic rearrangements taking place in the topologically unstable regions of the glass governed by variations in the atomic-level stresses.

  15. Preparation of nuclear oxide powders via thermal decomposition. Ex: ThO2

    International Nuclear Information System (INIS)

    Bayoglu, A. S.; Yayli, A.; Tarhan, M.; Bayram, Y.; Aybers, M. T.; Kopuz, B.

    1986-01-01

    In this paper, the influence of thorium oxalate precipitation variable (temperature, digertion time, agitation and addition rate of oxalic acid, etc.) and calcination parameters (temperature and time) upon the properties of derived powder characteristics (specific surface area, cryctallite size, morphology, etc.) was investigated. The results obtained indicate that the temperature has an important effect upon the particle morphology among the thorium oxalate precipitation variables. The low precipitation temperature gives the smaller particles. The ThO 2 powder has the same shape and the size of the parent oxalate. The precipitations variables don't exhibit an appreciable change on the specific surface area and crystallite size. The calcination temperature and time has an important influence on the specific surface area which is an exponentielly decreasing function of the temperature due to the introparticle sintering. The calcination temperature has not a noticeable effect between 700 C o -900 C o on the particle sizes and morphology. (author)

  16. Ghost imaging and ghost diffraction with pseudo-thermal light generated by means of a programmable SLM

    International Nuclear Information System (INIS)

    Capeluto, M G; Schmiegelow, C T; Francisco, D; Ledesma, S; Iemmi, C; Duisterwinkel, H

    2011-01-01

    Ghost imaging and ghost diffraction are techniques in which information about the object or about its diffraction pattern is extracted by measuring the correlation between a reference beam and a beam that passes through the object. Although first experiments were carried on by using entangled photons, it was demonstrated that this technique can be performed by splitting incoherent pseudo-thermal radiation such as that obtained with a laser passing through a moving diffuser. In this work we implemented the use of a programmable phase spatial light modulator (SLM) in order to replace the rotating ground glass. In this way the random phase distributions obtained from the moving diffuser can be emulated by displaying onto the SLM different realizations of a random function with uniform distribution. Based on the programmability of the modulator we have studied the influence of diverse parameters such as speckle size or phase distributions in the final image quality. We carry on the experiment for two different cases ghost imaging and far field ghost diffraction.

  17. 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.

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

    Science.gov (United States)

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

    2003-01-01

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

  19. Improved 3-omega measurement of thermal conductivity in liquid, gases, and powders using a metal-coated optical fiber.

    Science.gov (United States)

    Schiffres, Scott N; Malen, Jonathan A

    2011-06-01

    A novel 3ω thermal conductivity measurement technique called metal-coated 3ω is introduced for use with liquids, gases, powders, and aerogels. This technique employs a micron-scale metal-coated glass fiber as a heater/thermometer that is suspended within the sample. Metal-coated 3ω exceeds alternate 3ω based fluid sensing techniques in a number of key metrics enabling rapid measurements of small samples of materials with very low thermal effusivity (gases), using smaller temperature oscillations with lower parasitic conduction losses. Its advantages relative to existing fluid measurement techniques, including transient hot-wire, steady-state methods, and solid-wire 3ω are discussed. A generalized n-layer concentric cylindrical periodic heating solution that accounts for thermal boundary resistance is presented. Improved sensitivity to boundary conductance is recognized through this model. Metal-coated 3ω was successfully validated through a benchmark study of gases and liquids spanning two-orders of magnitude in thermal conductivity. © 2011 American Institute of Physics

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2018-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-15

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

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

    International Nuclear Information System (INIS)

    Johnsen, Rune E.; Krumeich, Frank; Norby, Poul

    2010-01-01

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

  4. 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)

  5. 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

  6. Comparative evaluation of thermal decomposition behavior and thermal stability of powdered ammonium nitrate under different atmosphere conditions.

    Science.gov (United States)

    Yang, Man; Chen, Xianfeng; Wang, Yujie; Yuan, Bihe; Niu, Yi; Zhang, Ying; Liao, Ruoyu; Zhang, Zumin

    2017-09-05

    In order to analyze the thermal decomposition characteristics of ammonium nitrate (AN), its thermal behavior and stability under different conditions are studied, including different atmospheres, heating rates and gas flow rates. The evolved decomposition gases of AN in air and nitrogen are analyzed with a quadrupole mass spectrometer. Thermal stability of AN at different heating rates and gas flow rates are studied by differential scanning calorimetry, thermogravimetric analysis, paired comparison method and safety parameter evaluation. Experimental results show that the major evolved decomposition gases in air are H 2 O, NH 3 , N 2 O, NO, NO 2 and HNO 3 , while in nitrogen, H 2 O, NH 3 , NO and HNO 3 are major components. Compared with nitrogen atmosphere, lower initial and end temperatures, higher heat flux and broader reaction temperature range are obtained in air. Meanwhile, higher air gas flow rate tends to achieve lower reaction temperature and to reduce thermal stability of AN. Self-accelerating decomposition temperature of AN in air is much lower than that in nitrogen. It is considered that thermostability of AN is influenced by atmosphere, heating rate and gas flow rate, thus changes of boundary conditions will influence its thermostability, which is helpful to its safe production, storage, transportation and utilization. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0{<=}x{<=}0.5): X-ray diffraction, energy dispersive spectrometry and differential thermal analysis

    Energy Technology Data Exchange (ETDEWEB)

    Grima Gallardo, P.; Munoz, M.; Ruiz, J. [Centro de Estudios en Semiconductores (C.E.S.), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela); Delgado, G.E. [Laboratorio de Cristalografia, Dpto. Quimica, Fac. Ciencias, Universidad de Los Andes, Merida 5101 (Venezuela); Briceno, J.M. [Laboratorio de Analisis Quimico y Estructural (LAQUEM), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela)

    2004-07-01

    The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0powder diffraction, energy dispersion spectrometry and differential thermal analysis. The solubility of MgSe in CuGaSe{sub 2} was found to be nearly complete for all the compositions studied, although traces of MgSe appear as a secondary phase at x{>=}0.15. All the alloys showed the chalcopyrite structure and the lattice parameters of the unit cell do not follow a linear behavior but showed a soft local maximum at x {proportional_to} 0.15. In the single-phase field, the increasing behavior of the lattice parameters can be reproduced using an extension for quaternary alloys of Jaffe and Zunger's model for chalcopyrites. (copyright 2004 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  8. High resolution electron back-scatter diffraction analysis of thermally and mechanically induced strains near carbide inclusions in a superalloy

    Energy Technology Data Exchange (ETDEWEB)

    Karamched, Phani S., E-mail: phani.karamched@materials.ox.ac.uk [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Wilkinson, Angus J. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom)

    2011-01-15

    Cross-correlation-based analysis of electron back-scatter diffraction (EBSD) patterns has been used to obtain high angular resolution maps of lattice rotations and elastic strains near carbides in a directionally solidified superalloy MAR-M-002. Lattice curvatures were determined from the EBSD measurements and used to estimate the distribution of geometrically necessary dislocations (GNDs) induced by the deformation. Significant strains were induced by thermal treatment due to the lower thermal expansion coefficient of the carbide inclusions compared to that of the matrix. In addition to elastic strains the mismatch was sufficient to have induced localized plastic deformation in the matrix leading to a GND density of 3 x 10{sup 13} m{sup -2} in regions around the carbide. Three-point bending was then used to impose strain levels within the range {+-}12% across the height of the bend bar. EBSD lattice curvature measurements were then made at both carbide-containing and carbide-free regions at different heights across the bar. The average GND density increases with the magnitude of the imposed strain (both in tension and compression), and is markedly higher near the carbides particles. The higher GND densities near the carbides (order of 10{sup 14} m{sup -2}) are generated by the large strain gradients produced around the plastically rigid inclusion during mechanical deformation with some minor contribution from the pre-existing residual deformation caused by the thermal mismatch between carbide and nickel matrix.

  9. Diffraction phase microscopy imaging and multi-physics modeling of the nanoscale thermal expansion of a suspended resistor.

    Science.gov (United States)

    Wang, Xiaozhen; Lu, Tianjian; Yu, Xin; Jin, Jian-Ming; Goddard, Lynford L

    2017-07-04

    We studied the nanoscale thermal expansion of a suspended resistor both theoretically and experimentally and obtained consistent results. In the theoretical analysis, we used a three-dimensional coupled electrical-thermal-mechanical simulation and obtained the temperature and displacement field of the suspended resistor under a direct current (DC) input voltage. In the experiment, we recorded a sequence of images of the axial thermal expansion of the central bridge region of the suspended resistor at a rate of 1.8 frames/s by using epi-illumination diffraction phase microscopy (epi-DPM). This method accurately measured nanometer level relative height changes of the resistor in a temporally and spatially resolved manner. Upon application of a 2 V step in voltage, the resistor exhibited a steady-state increase in resistance of 1.14 Ω and in relative height of 3.5 nm, which agreed reasonably well with the predicted values of 1.08 Ω and 4.4 nm, respectively.

  10. Thermal decomposition and X-ray diffraction of sulphate efflorescent minerals from El Jaroso Ravine, Sierra Almagrera, Spain

    International Nuclear Information System (INIS)

    Frost, Ray L.; Wain, Daria; Martens, Wayde N.; Locke, Ashley C.; Martinez-Frias, Jesus; Rull, Fernando

    2007-01-01

    Two evaporite minerals from the El Jaroso Ravine, Spain have been analysed by thermogravimetry coupled with an evolved gas mass spectrometer. X-ray diffraction results proved the evaporite minerals were a mixture of sulphates including the minerals magnesiocopiapite, coquimbite and possibly alunogen. Thermal decomposition of the unoxidised samples showed steps at 52, 99 and 143 deg. C confirmed by mass spectrometric results and attributed to adsorbed water, interstitial water and chemically bonded water. This evaporite mineral rock showed two higher temperature decomposition steps at 555 and 599 deg. C with mass losses of 19.6 and 7.8%. Slightly different temperatures for the thermal decomposition of the oxadada sample were observed at 52, 64.5 and 100 deg. C. Two higher temperature mass loss steps at 560.5 and 651 deg. C were observed for the oxidised sample. By comparison of the thermal analysis patterns of halotrichite and jarosite it can be shown that the El Jaroso samples are mineral sulphates and not halotrichite or jarosite

  11. Thermal decomposition and X-ray diffraction of sulphate efflorescent minerals from El Jaroso Ravine, Sierra Almagrera, Spain

    Energy Technology Data Exchange (ETDEWEB)

    Frost, Ray L. [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia)]. E-mail: r.frost@qut.edu.au; Wain, Daria [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Martens, Wayde N. [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Locke, Ashley C. [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Martinez-Frias, Jesus [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Cristalografia y Mineralogia, Unidad Asociada al Centro de Astrobiologia INTA-CSIC, Universidad de Valladolid, 47006 Valladolid (Spain); Rull, Fernando [Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Cristalografia y Mineralogia, Unidad Asociada al Centro de Astrobiologia INTA-CSIC, Universidad de Valladolid, 47006 Valladolid (Spain)

    2007-08-25

    Two evaporite minerals from the El Jaroso Ravine, Spain have been analysed by thermogravimetry coupled with an evolved gas mass spectrometer. X-ray diffraction results proved the evaporite minerals were a mixture of sulphates including the minerals magnesiocopiapite, coquimbite and possibly alunogen. Thermal decomposition of the unoxidised samples showed steps at 52, 99 and 143 deg. C confirmed by mass spectrometric results and attributed to adsorbed water, interstitial water and chemically bonded water. This evaporite mineral rock showed two higher temperature decomposition steps at 555 and 599 deg. C with mass losses of 19.6 and 7.8%. Slightly different temperatures for the thermal decomposition of the oxadada sample were observed at 52, 64.5 and 100 deg. C. Two higher temperature mass loss steps at 560.5 and 651 deg. C were observed for the oxidised sample. By comparison of the thermal analysis patterns of halotrichite and jarosite it can be shown that the El Jaroso samples are mineral sulphates and not halotrichite or jarosite.

  12. 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)

  13. Quantitative X-ray Diffraction (QXRD) analysis for revealing thermal transformations of red mud.

    Science.gov (United States)

    Liao, Chang-Zhong; Zeng, Lingmin; Shih, Kaimin

    2015-07-01

    Red mud is a worldwide environmental problem, and many authorities are trying to find an economic solution for its beneficial application or/and safe disposal. Ceramic production is one of the potential waste-to-resource strategies for using red mud as a raw material. Before implementing such a strategy, an unambiguous understanding of the reaction behavior of red mud under thermal conditions is essential. In this study, the phase compositions and transformation processes were revealed for the Pingguo red mud (PRM) heat-treated at different sintering temperatures. Hematite, perovskite, andradite, cancrinite, kaolinite, diaspore, gibbsite and calcite phases were observed in the samples. However, unlike those red mud samples from the other regions, no TiO2 (rutile or anatase) or quartz were observed. Titanium was found to exist mainly in perovskite and andradite while the iron mainly existed in hematite and andradite. A new silico-ferrite of calcium and aluminum (SFCA) phase was found in samples treated at temperatures above 1100°C, and two possible formation pathways for SFCA were suggested. This is the first SFCA phase to be reported in thermally treated red mud, and this finding may turn PRM waste into a material resource for the iron-making industry. Titanium was found to be enriched in the perovskite phase after 1200°C thermal treatment, and this observation indicated a potential strategy for the recovery of titanium from PRM. In addition to noting these various resource recovery opportunities, this is also the first study to quantitatively summarize the reaction details of PRM phase transformations at various temperatures. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Coherent phonon excitation and linear thermal expansion in structural dynamics and ultrafast electron diffraction of laser-heated metals.

    Science.gov (United States)

    Tang, Jau

    2008-04-28

    In this study, we examine the ultrafast structural dynamics of metals induced by a femtosecond laser-heating pulse as probed by time-resolved electron diffraction. Using the two-temperature model and the Grüneisen relationship we calculate the electron temperature, phonon temperature, and impulsive force at each atomic site in the slab. Together with the Fermi-Pasta-Ulam anharmonic chain model we calculate changes of bond distance and the peak shift of Bragg spots or Laue rings. A laser-heated thin slab is shown to exhibit "breathing" standing-wave behavior, with a period equal to the round-trip time for sound wave and a wavelength twice the slab thickness. The peak delay time first increases linearly with the thickness (linear thermal expansion due to lattice temperature jump are shown to contribute to the overall structural changes. Differences between these two mechanisms and their dependence on film thickness and other factors are discussed.

  15. Diffraction grating strain gauge method: error analysis and its application for the residual stress measurement in thermal barrier coatings

    Science.gov (United States)

    Yin, Yuanjie; Fan, Bozhao; He, Wei; Dai, Xianglu; Guo, Baoqiao; Xie, Huimin

    2018-03-01

    Diffraction grating strain gauge (DGSG) is an optical strain measurement method. Based on this method, a six-spot diffraction grating strain gauge (S-DGSG) system has been developed with the advantages of high and adjustable sensitivity, compact structure, and non-contact measurement. In this study, this system is applied for the residual stress measurement in thermal barrier coatings (TBCs) combining the hole-drilling method. During the experiment, the specimen’s location is supposed to be reset accurately before and after the hole-drilling, however, it is found that the rigid body displacements from the resetting process could seriously influence the measurement accuracy. In order to understand and eliminate the effects from the rigid body displacements, such as the three-dimensional (3D) rotations and the out-of-plane displacement of the grating, the measurement error of this system is systematically analyzed, and an optimized method is proposed. Moreover, a numerical experiment and a verified tensile test are conducted, and the results verify the applicability of this optimized method successfully. Finally, combining this optimized method, a residual stress measurement experiment is conducted, and the results show that this method can be applied to measure the residual stress in TBCs.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  17. Emanation thermal analysis study of the preparation of ruthenia-titania-based finely dispersed powders

    Czech Academy of Sciences Publication Activity Database

    Balek, V.; Mitsuhashi, T.; Zeleňák, V.; Večerníková, Eva; Šubrt, Jan; Haneda, H.; Bezdička, Petr

    2002-01-01

    Roč. 248, č. 1 (2002), s. 47-53 ISSN 0021-9797 Institutional research plan: CEZ:AV0Z4032918 Keywords : emanation thermal analysis * TiO2 * RuO2 Subject RIV: CA - Inorganic Chemistry Impact factor: 1.466, year: 2002

  18. Infrared absorption study of ammonium uranates and uranium oxide powders formed during their thermal decomposition

    International Nuclear Information System (INIS)

    Rofail, N.H.; ELfekey, S.A.

    1992-01-01

    Ammonium uranates (AU) were precipitated from a nuclear-pure uranyl nitrate solution using different precipitating agents. IR spectra of the obtained uranates and oxides formed during their thermal decomposition have been studied. The results indicated that the precipitating agent, mode of stirring, washing and calcining temperature are important factors for a specific oxide formation.4 FIG., 3 TAB

  19. Photopyroelectric assessment of the thermal effusivity of fresh hen egg and of rehydrated egg powders

    NARCIS (Netherlands)

    Szafner, G.; Nemeth, C.; Bicanic, D.D.; Doka, O.

    2015-01-01

    The availability of thermo-physical data of foods and their constituents is of general importance to food industry. The thermal effusivity e is one among the relevant thermodynamical quantities. The latter is normally calculated from the relationship e = (¿¿c)½, where c is specific heat, ¿ is the

  20. 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

  1. High-Resolution Powder Diffractometer HRPT for Thermal Neutrons at SINQ

    International Nuclear Information System (INIS)

    Fischer, P.; Koch, M.; Koennecke, M.; Pomjakushin, V.; Schefer, J.; Schlumpf, N.

    1999-01-01

    The new neutron powder diffractometer at the Swiss continuous spallation neutron source SINQ is designed as a flexible instrument for high resolution [best values δd/d: ( -3 with d = lattice spacing in the high resolution or high intensity modes, respectively]. It uses large scattering angles 2Θ M = 120 deg or 90 deg of the monochromator, a 28 cm high, vertically focusing wafer type Ge(hkk) monochromator and a position-sensitive 3 He detector(3.6 bar) produced by Cerca at Romans, France. It has 1600 (25x64) detectors with an angular separation of 0.1 deg and includes modern electronics developed by E. Berruyer, Cerca and PSI. The SICS software of PSI controls the instrument with a server running on an unix workstation and clients written in Java through the TCP/IP network. The design principles and first experiences are presented. The interdisciplinary applications of HRPT will permit high-resolution refinement of chemical and magnetic structures as well as phase analysis including the detection of defects and internal microstrain. In particular real-time investigations of chemical or structural changes and of magnetic phase transitions in crystalline, quasicrystalline, amorphous and liquid samples including technically interesting new materials are possible. (author)

  2. 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.

  3. Study by X-ray diffraction and mechanical analysis of the residual stress generation during thermal spraying

    International Nuclear Information System (INIS)

    Pina, J.; Dias, A.; Lebrun, J.L.

    2003-01-01

    Thermally sprayed coatings are formed by the deposition of molten or partially molten particles, propelled onto a substrate where they impact, spread and solidify rapidly. Residual stresses are expected within the sprayed deposit as a consequence of the release of thermal and kinetic energies. A wide range of materials and two spraying techniques are considered in this study, namely atmospheric plasma spraying (APS) and high-velocity oxygen fuel. Stresses were determined by the X-ray diffraction (XRD) method. The results were compared with those calculated by mechanical analysis of stress relief in coatings detached from the substrate. Comparison of the results for adherent and free-standing coatings shows that the residual stress state can be resolved in terms of the components suggested by models that propose two stages of stress generation: quenching stresses and secondary-cooling stresses. The in-depth distribution of residual stresses, through the coating thickness, is discussed in terms of the nature of the coating system

  4. Synthetic hydroxyapatites doped with Zn(II) studied by X-ray diffraction, infrared, Raman and thermal analysis

    Science.gov (United States)

    Guerra-López, José R.; Echeverría, Gustavo A.; Güida, Jorge A.; Viña, Raúl; Punte, Graciela

    2015-06-01

    Calcium hydroxyapatite (CaHap) formation when different amounts of Zn(II) are present in the mother solution has been investigated by atomic absorption, infrared and Raman spectroscopies, X-ray diffraction and thermal analysis (DTA and TG). The studied samples have been synthesized at T=95 °C and pH 9 in air. The analysis of the results have shown that the pure CaHap sample crystallizes in the monoclinic form P21/b. Concentrations up to 20% of Zn(II) in the mother solution, equivalent to smaller concentrations in solid (up to 9.1% in wt), favor the formation of the hexagonal apatite, P63/m, while Zn(II) concentrations higher than 20% in solution help an amorphous phase development where vibrational spectra indicated coexistence of two phases: an apatite and ZnNH4PO4·H2O. Infrared data of thermal treated samples endorse that HPO42- ion had not been incorporated in Zn(II) doped samples during the synthesis process. Present results also allow to conclude that Zn(II) cation exhibits a preference to occupy the Ca2 site of the apatite structure and induces water adsorption and a small quantity of CO32- cation incorporation, leading to formation of a less crystalline Ca deficient apatite.

  5. 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.

  6. About properties of ZrO2 thermal protective coatings obtained from spherical powder mixtures

    Science.gov (United States)

    Berdnik, O. B.; Tsareva, I. N.; Tarasenko, Yu P.

    2017-05-01

    It is developed the technology of high-energy plasma spraying of the zirconium dioxide (ZrO2) thermal protective coating on the basis of ZrO2 tetragonal and cubic phases with the spheroidal grain shape and the columnar substructure, with the total porosity P = 4 %, the hardness HV = 12 GPa, the roughness parameter R a ˜ 6 μm, the thickness 0.3-3 mm. As a sublayer it is used the heat-resistant coating of “Ni-Co-Cr-Al-Y” system with an intermetallic phase composition and the layered microstructure of the grains.

  7. 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.

  8. 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.

  9. 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

  10. 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)

  11. Effect of thermally induced porosity on an as-HIP powder metallurgy superalloy

    Science.gov (United States)

    Dreshfield, R. L.; Miner, R. V., Jr.

    1979-01-01

    The impact of thermally induced porosity on the mechanical properties of an as-hot-isostatically-pressed and heat treated pressing made from low carbon Astroloy was determined. Porosity in the disk-shape pressing studied ranged from 2.6 percent at the bore to 1.4 percent at the rim. Tensile, yield strength, ductility, and rupture life of the rim of the porous pressing was only slightly inferior to the rim of sound pressings. The strength, ductility, and rupture life of the bore of the porous pressing was severely degraded compared to sound pressings. At strain ranges typical of commercial jet engine designs, the rim of the porous pressing had slightly inferior fatigue life to sound pressings.

  12. Effects of thermally induced porosity on an as-HIP powder metallurgy superalloy

    Science.gov (United States)

    Dreshfield, R. L.; Miner, R. V., Jr.

    1980-01-01

    The effect of thermally induced porosity on the mechanical properties of an as-hot-isostatically pressed and heat-treated pressing made from low carbon Astroloy is examined. Tensile, stress-rupture, creep, and low cycle fatigue tests were performed and the results were compared with industrial acceptance criteria. It is shown that the porous pressing has a porosity gradient from the rim to the bore with the bore having 1-1/2% greater porosity. Mechanical properties of the test ring below acceptance level are tensile reduction in area at room temperature and 538 C and time for 0.1% creep at 704 C. It is also found that the strength, ductility, and rupture life of the rim are slightly inferior to those of the rim of the sound pressings, while those of the bore are generally below the acceptable level. At strain ranges typical of commercial aircraft engines, the low cycle fatigue life of the rim of the porous pressings is slightly lower than that of the sound pressings.

  13. Plasma Treatment of Agave Fiber Powder and Its Effect on the Mechanical and Thermal Properties of Composites Based on Polyethylene

    Directory of Open Access Journals (Sweden)

    Florentino Soriano Corral

    2016-01-01

    Full Text Available Composites based on low-density polyethylene (LDPE were prepared with Agave fiber powder (AFP that was coated by plasma polymerization process using ethylene gas. Treated and pristine AFP were analyzed by infrared spectroscopy, scanning electron microscopy, and contact water angle for the assessment of surface properties. The polymer composites were prepared by melt mixing using 0, 5, 10, and 20 wt% of AFP and their mechanical and thermal properties were measured. Dispersion evaluation in water confirmed that the AFP treated changed from hydrophilic to hydrophobic behavior and it was also corroborated with water contact angle tests. The addition of treated and untreated AFP (200 mesh at 20 wt% promotes an increase of Young’s modulus of the composites of up to 60% and 32%, respectively, in relation to the neat matrix. Also, an increase of crystallinity of LDPE was observed by the addition of treated and untreated AFP; however no significant effect on the crystallization temperature was observed in LDPE containing AFP.

  14. X-Ray diffraction analysis of thermally evaporated copper tin selenide thin films at different annealing temperature

    International Nuclear Information System (INIS)

    Mohd Amirul Syafiq Mohd Yunos; Zainal Abidin Talib; Wan Mahmood Mat Yunus; Josephine Liew Ying Chyi; Wilfred Sylvester Paulus

    2010-01-01

    Semiconductor thin films Copper Tin Selenide, Cu 2 SnSe 3 , a potential compound for semiconductor radiation detector or solar cell applications were prepared by thermal evaporation method onto well-cleaned glass substrates. The as-deposited films were annealed in flowing purified nitrogen, N 2 , for 2 hours in the temperature range from 100 to 500 degree Celsius. The structure of as-deposited and annealed films has been studied by X-ray diffraction technique. The semi-quantitative analysis indicated from the Reitveld refinement show that the samples composed of Cu 2 SnSe 3 and SnSe. These studies revealed that the films were structured in mixed phase between cubic space group F-43 m (no. 216) and orthorhombic space group P n m a (no. 62). The crystallite size and lattice strain were determined from Scherrer calculation method. The results show that increasing in annealing temperature resulted in direct increase in crystallite size and decrease in lattice strain. (author)

  15. 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.

  16. 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...

  17. 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

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

    Czech Academy of Sciences Publication Activity Database

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

    2014-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-12-15

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

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

    Science.gov (United States)

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

    1990-12-01

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

  2. 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 ...

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

    Energy Technology Data Exchange (ETDEWEB)

    Ogborne, D.M.; Weller, M.T.; Lanchester, P.C. (Dept. of Chemistry and Physics, Univ. of Southampton (United Kingdom))

    1992-09-15

    Samples of Tl[sub 2]Ba[sub 2]Ca[sub 2]Cu[sub 3]O[sub 10-y] have been prepared with three different oxygen stoichiometries by reaction under various oxygen gas partial pressures. Powder neutron diffraction studies on these materials show that for y > 0 oxygen vacancies exist in the thallium-oxygen layer; filling this site results in a contraction of the lattice with concomitant reduction in the apical Cu-O bond length but with an expansion of the copper-oxygen interlayer distance. These structural changes which occur as a function of oxygen content are discussed in terms of the superconducting properties of these materials. (orig.).

  4. Neutron powder diffraction investigation on the crystal and magnetic structure of (Ho{sub 0.50+x}Ca{sub 0.50-x})(Mn{sub 1-x}Cr{sub x})O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-10-19

    The crystal and magnetic structure of (Ho{sub 0.50+x}Ca{sub 0.50-x})(Mn{sub 1-x}Cr{sub x})O{sub 3} (x = 0.00, 0.01, 0.02, 0.03) has been investigated between 5 and 300 K by means of neutron powder diffraction followed by Rietveld refinement and dc magnetic measurements. During cooling an orthorhombic to monoclinic phase transition occurs on account of the charge and orbital ordering taking place in the Mn sub-lattice; at low temperature phase separation takes place and the main monoclinic phase coexists with a secondary orthorhombic phase, whose amount slightly increases with the increase of Cr content. Cr{sup 3+} is not involved in orbital ordering or superexchange interactions. The charge and magnetic ordering are decoupled: the Mn moments order according to a CE-type structure in all samples. (paper)

  5. Magnetic ordering in the monoclinic structure of Nd5Si1.45Ge2.55 and Pr5Si1.5Ge2.5 studied by means of neutron powder diffraction

    International Nuclear Information System (INIS)

    Magen, C; Ritter, C; Morellon, L; Algarabel, P A; Ibarra, M R

    2004-01-01

    The compounds Nd 5 Si 1.45 Ge 2.55 and Pr 5 Si 1.5 Ge 2.5 have been investigated by means of magnetization measurements and neutron powder diffraction techniques. These alloys present a room-temperature monoclinic Gd 5 Si 2 Ge 2 -type crystallographic structure and, on cooling, both systems order ferromagnetically, at T C = 56 and 32 K, respectively, from a high-temperature paramagnetic to a low-temperature complex canted ferromagnetic state. The monoclinic crystallographic structure remains unchanged upon cooling down to 4 K, demonstrating the existence of a monoclinic ferromagnetic phase, and the possibility of a full decoupling of magnetic and crystallographic degrees of freedom in the 5:4 lanthanide intermetallic compounds

  6. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    International Nuclear Information System (INIS)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N; Sowa, H; Ahsbahs, H; Chernyshev, V V; Dmitriev, V P

    2008-01-01

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, β-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions

  7. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Boldyreva, E V; Goryainov, S V; Seryotkin, Y V; Kolesnik, E N; Shakhtshneider, T P; Ivashevskaya, S N; Drebushchak, T N [Research and Education Center ' Molecular Design and Ecologically Safe Technologies' , REC-008, Novosibirsk State University (Russian Federation); Sowa, H [Goettingen University (Germany); Ahsbahs, H; Chernyshev, V V [Marburg University (Germany); Dmitriev, V P [Swiss-Norwegian Beamline ESRF, Grenoble (France)], E-mail: boldyrev@nsu.ru

    2008-07-15

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, {beta}-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-04-15

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

    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...

  10. Dehydrogenation kinetics for pure and nickel-doped magnesium hydride investigated by in-situ, time-resolved powder diffraction (poster)

    DEFF Research Database (Denmark)

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

    2004-01-01

    temperatures. Apparent activation energies were calculated from Arrhenius plots revealing values of ca. 300 and 250 kJ/mol for the dehydrogenationof pure and nickel-doped magnesium hydride, respectively, in accord with EA= 270 kJ/mol measured by thermal desorption spectroscopy for these non-activated materials...

  11. A novel approach to determine the thermal transition of gum powder/hydro-gels using dynamic mechanical analysis

    Science.gov (United States)

    Nagamadhu, M.; Jeyaraj, P.; Kumar, G. C. Mohan

    2018-04-01

    The dynamic characterization of materials plays a major role in the present area. The many researchers are worked on solid materials and its characterization, it can be tested using dynamic mechanical analyzer (DMA), however, no such work on powder a semiliquid samples. The powder and liquid samples can also easily characterization as like solid samples using DMA. These powder samples are analyzed with a material pocket method which can be used to accurately determine very low levels of variation in powder properties, due to the high sensitivity of DMA to glass transitions. No such DMA studies on hydrogel and Gum powders. The gum powders are used in various applications start from food industries, pharmacy, natural gums paste, biomedical applications etc. among all this applications gum Ghatti is one of the powders using for varies applications. Around 50 milligrams of Ghatti powders are placed inside material pocket and analyzed storage modulus (G'), loss modulus (G″) and tan delta (δ). Also, understand the curing and glass transition effect using water, glycerin and superplastic from room temperature to 200°C. The result shows that storage modulus decreases with increase in temperature in pure Ghatti powder. The surprising improvement in storage modulus was found with an increase in temperature with addition of water, glycerin, and superplastic. However, loss modulus and tan delta are also having very significant influence and also shows a clear peak of the tan delta. The loss modulus results were found to be improved by adding solidifying agents, along with this water and superplastic better influence. But glycerine found to be hydrogel in nature and thermodynamic properties are much influenced by frequency.

  12. Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

    Science.gov (United States)

    Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

    2008-10-01

    In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

  13. Detection of fatigue damage of high and medium pressure rotor by X-ray diffraction method. Survey and research of nondestructive examination of thermal power generation facilities

    Energy Technology Data Exchange (ETDEWEB)

    Yamamoto, Tatsuo; Suesada, Yasuhiko; Nishioka, Noriaki; Goto, Toru; Ito, Hitomi; Kadoya, Yoshikuni

    1987-03-25

    In recent years, the existing thermal power generation facilities have been required to be operated in securing dependability from the standpoints of the operating conditions which have been getting severer and the demands to use them for longer periods, accordingly it is hoped to establish the diagnostic technology of aged deterioration by the non-destructive examination method for the facilities. In the beginning of 1959 the Kansai Electric Power Co. surveyed the current situation of this technology at various thermal power generation turbine facilities and discovered that concerning the diagnostic technology of aged deterioration by the non-destructive examination method, there remained many matters untouched in the basic research field. The company consequently started a survey and research jointly with Mitsubishi Heavy Industries in the first half of 1959. This report summarizes the research on the detection of aged deterioration due to thermal fatigue of Cr-Mo-V rotor material by the X-ray diffraction method which was conducted during the full fiscal year of 1984 and the first half of FY 1985 as a part of the above joint research. With respect to the conditions for the detection method of thermal fatigue damages of dummy grooves of the high and medium pressure rotor by the application of the X-ray diffraction method, it is preferred to measure a diffraction strength curve of the diffraction surface by using a Co tube as X-ray tube and it is also desirable to use a position sensitive proportional counter tube for X-ray detector. (5 figs, 6 refs)

  14. Thermal Stability of Zone Melting p-Type (Bi, Sb)2Te3 Ingots and Comparison with the Corresponding Powder Metallurgy Samples

    Science.gov (United States)

    Jiang, Chengpeng; Fan, Xi'an; Hu, Jie; Feng, Bo; Xiang, Qiusheng; Li, Guangqiang; Li, Yawei; He, Zhu

    2018-04-01

    During the past few decades, Bi2Te3-based alloys have been investigated extensively because of their promising application in the area of low temperature waste heat thermoelectric power generation. However, their thermal stability must be evaluated to explore the appropriate service temperature. In this work, the thermal stability of zone melting p-type (Bi, Sb)2Te3-based ingots was investigated under different annealing treatment conditions. The effect of service temperature on the thermoelectric properties and hardness of the samples was also discussed in detail. The results showed that the grain size, density, dimension size and mass remained nearly unchanged when the service temperature was below 523 K, which suggested that the geometry size of zone melting p-type (Bi, Sb)2Te3-based materials was stable below 523 K. The power factor and Vickers hardness of the ingots also changed little and maintained good thermal stability. Unfortunately, the thermal conductivity increased with increasing annealing temperature, which resulted in an obvious decrease of the zT value. In addition, the thermal stabilities of the zone melting p-type (Bi, Sb)2Te3-based materials and the corresponding powder metallurgy samples were also compared. All evidence implied that the thermal stabilities of the zone-melted (ZMed) p-type (Bi, Sb)2Te3 ingots in terms of crystal structure, geometry size, power factor (PF) and hardness were better than those of the corresponding powder metallurgy samples. However, their thermal stabilities in terms of zT values were similar under different annealing temperatures.

  15. Elucidating the breathing of the metal-organic framework MIL-53(Sc) with ab initio molecular dynamics simulations and in situ X-ray powder diffraction experiments.

    Science.gov (United States)

    Chen, Linjiang; Mowat, John P S; Fairen-Jimenez, David; Morrison, Carole A; Thompson, Stephen P; Wright, Paul A; Düren, Tina

    2013-10-23

    Ab initio molecular dynamics (AIMD) simulations have been used to predict structural transitions of the breathing metal-organic framework (MOF) MIL-53(Sc) in response to changes in temperature over the range 100-623 K and adsorption of CO2 at 0-0.9 bar at 196 K. The method has for the first time been shown to predict successfully both temperature-dependent structural changes and the structural response to variable sorbate uptake of a flexible MOF. AIMD employing dispersion-corrected density functional theory accurately simulated the experimentally observed closure of MIL-53(Sc) upon solvent removal and the transition of the empty MOF from the closed-pore phase to the very-narrow-pore phase (symmetry change from P2(1)/c to C2/c) with increasing temperature, indicating that it can directly take into account entropic as well as enthalpic effects. We also used AIMD simulations to mimic the CO2 adsorption of MIL-53(Sc) in silico by allowing the MIL-53(Sc) framework to evolve freely in response to CO2 loadings corresponding to the two steps in the experimental adsorption isotherm. The resulting structures enabled the structure determination of the two CO2-containing intermediate and large-pore phases observed by experimental synchrotron X-ray diffraction studies with increasing CO2 pressure; this would not have been possible for the intermediate structure via conventional methods because of diffraction peak broadening. Furthermore, the strong and anisotropic peak broadening observed for the intermediate structure could be explained in terms of fluctuations of the framework predicted by the AIMD simulations. Fundamental insights from the molecular-level interactions further revealed the origin of the breathing of MIL-53(Sc) upon temperature variation and CO2 adsorption. These simulations illustrate the power of the AIMD method for the prediction and understanding of the behavior of flexible microporous solids.

  16. High-temperature X-ray powder diffraction as a tool for characterization of smectites, layered double hydroxides, and their intercalates with porphyrins

    Czech Academy of Sciences Publication Activity Database

    Píšková, A.; Bezdička, Petr; Hradil, David; Káfuňková, E.; Lang, Kamil; Večerníková, Eva; Kovanda, F.; Grygar, Tomáš

    2010-01-01

    Roč. 49, č. 4 (2010), s. 363-371 ISSN 0169-1317 R&D Projects: GA ČR(CZ) GA203/06/1244; GA AV ČR KAN100500651; GA AV ČR IAA3032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : smectite * Layered double hydroxides * thermal decomposition Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.303, year: 2010

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

    Directory of Open Access Journals (Sweden)

    Ira V. Rozhdestvenskaya

    2017-05-01

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

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  20. Influence of Ba/Fe mole ratios on magnetic properties, crystallite size and shifting of X-ray diffraction peaks of nanocrystalline BaFe12O19 powder, prepared by sol gel auto combu

    Science.gov (United States)

    Suastiyanti, Dwita; Sudarmaji, Arif; Soegijono, Bambang

    2012-06-01

    Barium hexaferrite BaFe12O19 (BFO) is of great importance as permanent magnets, particularly for magnetic recording as well as in microwave devices. Nano-crystalline BFO powders were prepared by sol gel auto combustion method in citric acid - metal nitrates system. Hence the mole ratios of Ba/Fe were variated at 1:12; 1:11.5 and 1:11. Ratio of cation to fuel was fixed at 1:1. An appropriate amount of amonia solution was added dropwise to this solution with constant stirring until the PH reached 7 in all cases. Heating at 850oC for 10 hours for each sample to get final formation of BFO nanocrystalline. The data from XRD showing the lattice parameters a,c and the unit-cell volume V, confirm that BFO with ratio 1:12 has same crystall parameters with ratio 1:11. Ratio of Ba/Fe 1:12 and 1:11 have diffraction pattern similarly at almost each 2 θ for each samples. Ratio of Ba/Fe 1: 11.5 has the finest crystallite size 22 nm. Almost diffraction pattern peaks of Ba/Fe 1:11.5 move to the left from of Ba/Fe 1:12 then return to diffraction pattern of Ba/Fe 1:12 for Ba/Fe 1:11. SEM observations show the particle size less than 100 nm and the same shape for each sample. Ratio of Ba/Fe 1: 12 gives the highest intrinsic coercive Hc = 427.3 kA/m. The highest remanent magnetization is at ratio 1:11 with Mr = 0.170 T. BFO with mole ratio 1:11.5 has the finest grain 22 nm, good magnetic properties and the highest value of best FoM 89%.

  1. Fabrication of dendritic silver-coated copper powders by galvanic displacement reaction and their thermal stability against oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Park, Yu-Seon [School of Chemical Engineering, Sungkyunkwan University, Suwon 16419 (Korea, Republic of); Farad Materials Co., Ltd., Suwon 16419 (Korea, Republic of); An, Chang Yong; Kannan, Padmanathan Karthick; Seo, Nary [School of Chemical Engineering, Sungkyunkwan University, Suwon 16419 (Korea, Republic of); Zhuo, Kai [School of Chemical Engineering, Sungkyunkwan University, Suwon 16419 (Korea, Republic of); Farad Materials Co., Ltd., Suwon 16419 (Korea, Republic of); Yoo, Tae Kyong [School of Chemical Engineering, Sungkyunkwan University, Suwon 16419 (Korea, Republic of); Chung, Chan-Hwa, E-mail: chchung@skku.edu [School of Chemical Engineering, Sungkyunkwan University, Suwon 16419 (Korea, Republic of); Farad Materials Co., Ltd., Suwon 16419 (Korea, Republic of)

    2016-12-15

    Highlights: • The dendritic silver-coated copper powders with high specific surface area have been prepared using a simple wet chemical reduction process at room temperature. • It is found that the Cu starts to be oxidized into Cu{sub 2}O followed by CuO at elevated temperatures. • The more amount of Ag-coating provides the less oxidation, which confirms that the Ag-shell prevents the Cu-core from oxidation. • The resistivity of dendritic 33.27 wt.% Ag-coated Cu powders was measured to 25.67 μΩ cm after the annealing at 150 °C for 30 min. - Abstract: Two steps of wet chemical processes have been developed for the preparation of core-shell nanostructures of copper and silver, which is a facile and low cost method for the production of large quantity of dendritic powders. First step involves a galvanic displacement reaction with hydrogen evolution which is the motive force of spontaneous electrochemical reaction. To achieve the core-shell structure, silver has been coated on the dendritic copper using the galvanic displacement reaction. The dendritic silver-coated copper powders exhibit high surface-area, excellent conductivity, and good oxidation resistance. It has been found that silver-coated copper powders maintain the electrical conductivity even after annealing at 150 °C for several to tens of minutes, thus it is a promising material and an alternative to pure silver powders in printed electronics application.

  2. Fabrication of dendritic silver-coated copper powders by galvanic displacement reaction and their thermal stability against oxidation

    International Nuclear Information System (INIS)

    Park, Yu-Seon; An, Chang Yong; Kannan, Padmanathan Karthick; Seo, Nary; Zhuo, Kai; Yoo, Tae Kyong; Chung, Chan-Hwa

    2016-01-01

    Highlights: • The dendritic silver-coated copper powders with high specific surface area have been prepared using a simple wet chemical reduction process at room temperature. • It is found that the Cu starts to be oxidized into Cu_2O followed by CuO at elevated temperatures. • The more amount of Ag-coating provides the less oxidation, which confirms that the Ag-shell prevents the Cu-core from oxidation. • The resistivity of dendritic 33.27 wt.% Ag-coated Cu powders was measured to 25.67 μΩ cm after the annealing at 150 °C for 30 min. - Abstract: Two steps of wet chemical processes have been developed for the preparation of core-shell nanostructures of copper and silver, which is a facile and low cost method for the production of large quantity of dendritic powders. First step involves a galvanic displacement reaction with hydrogen evolution which is the motive force of spontaneous electrochemical reaction. To achieve the core-shell structure, silver has been coated on the dendritic copper using the galvanic displacement reaction. The dendritic silver-coated copper powders exhibit high surface-area, excellent conductivity, and good oxidation resistance. It has been found that silver-coated copper powders maintain the electrical conductivity even after annealing at 150 °C for several to tens of minutes, thus it is a promising material and an alternative to pure silver powders in printed electronics application.

  3. 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.

  4. Characterization of silica polymorphs in kaolins by X-ray diffraction before and after phosphoric acid digestion and thermal treatment

    International Nuclear Information System (INIS)

    Kahraman, Sibel; Oenal, Mueserref; Sarikaya, Yueksel; Bozdogan, Ihsan

    2005-01-01

    To characterize silica polymorphs (silicas) in some kaolins, orthophosphoric acid digestion (240 deg. C, 15 min), and thermal treatment (1050 deg. C, 24 h) were applied to eight samples. The original, digested, and heated samples were examined by X-ray diffraction (XRD). Crystalline silica quartz (SiO 2 ) was identified from the standard XRD patterns of the original kaolins; all contained quartz. On the other hand, hydrated partially crystalline silicas (SiO 2 .nH 2 O), such as well-ordered opal-C and opal-CT, were not readily distinguished from high-temperature crystalline silica, α-cristobalite, using standard XRD patterns of the original kaolins because, sharp and intense characteristic XRD peaks (h k l = 1 0 1) centered near 0.4 nm for opal-C, opal-CT, and α-cristobalite coincided. In order to distinguish these silicas the XRD patterns of the digested and heated samples were evaluated. It was observed that the 1 0 1 peaks disappear and sharpen in the course of digestion and heating, respectively. Because, the crystallinity of α-cristobalite does not change by these treatments, it was concluded that the kaolins contain opal-C and opal-CT or their mixtures in amorphous opal-A (SiO 2 .nH 2 O), but not α-cristobalite, which is probably human carcinogen. Because, the crystallinity increases in order opal-CT and opal-C, the narrowing in width at half-maximum peak height (FWHM) 1 0 1 must be more for opal-CT than opal-C by heating. Therefore, to distinguish opal-CT and opal-C from each other, the FWHM values before and after the heating process, were examined. Based on the results, it was estimated that six kaolins contain opal-CT in opal-A matrix, one kaolin contains only opal-A in a trace amount, and one kaolin contains non-opals

  5. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Viani, Alberto, E-mail: viani@itam.cas.cz [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Sotiriadis, Konstantinos [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Len, Adél [Wigner Research Centre for Physics HAS, Konkoly-Thege 29-33, 1121 Budapest (Hungary); Šašek, Petr; Ševčík, Radek [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic)

    2016-06-15

    Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

  7. 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

  8. X-ray diffraction measurement of the linear thermal expansion coefficients of WCoB in the range 300 to 973 K

    International Nuclear Information System (INIS)

    Petrov, K.; Will, G.

    1981-01-01

    High-temperature treatment of tungsten carbide-cobalt hard alloys in TiB 2 media leads to the formation of a surface diffusion coating which contains orthorhombic WCoB. The function of this compound in enhancing wear resistance of cutting tools, is discussed. The thermal expansion of WCoB is of primary interest, since the wear resistance of the coating reflects the degree of matching of the thermal expansion coefficients of the different phases. Preparation of the samples is described and experimental details of the X-ray diffraction measurements are given. The temperature dependence of the lattice parameters for the range 300 to 973 K, and the corresponding linear thermal expansion coefficients along the three principal crystallographic directions, are given. The results are discussed in terms of the bonding features of the solid. (U.K.)

  9. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    International Nuclear Information System (INIS)

    Bindi, Luca

    2009-01-01

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: α a = 1.5 x 10 -5 K -1 , α b = 3.0 x 10 -5 K -1 , α c = 2.2 x 10 -5 K -1 , and the bulk thermal expansion coefficient α V is 5.4 x 10 -5 K -1 for the temperature range 298-463 K

  10. Synthesis of CaCrO{sub 4} powders for the cathode material of the thermal battery by GNP and electrochemical characteristics of Ca/LiCl-KCl/CaCrO{sub 4} thermal battery system

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Whung Whoe

    2000-04-01

    Thermal batteries are one of the devices employing solid electrolyte that are not nonconductive at ambient temperature, and activated by electrochemical reaction when the sufficient heat is supplied to electrolyte to melt. The demand of thermal batteries would be increased because it is cost effective and highly reliable in that no maintenance is necessary, electric power can be generated as necessary and no self discharge unlike the other primary batteries. These thermal batteries are used to the military purposes and satellite communication systems and as an emergency power sources, applied to the important places where power supply should not be interrupted, such as hospital, powder plants, ships and portable communication devices. Therefore, the purpose of this study was focused to obtain the manufacturing technologies of thermal battery on our own, after manufacturing the CaCrO{sub 4} produced by GNP and investigating the electrochemical characteristics of Ca/LiCl-KCl+CaCrO{sub 4}/Ni.

  11. 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

  12. 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.

  13. X-ray diffraction analysis of thermally-induced stress relaxation in ZnO films deposited by magnetron sputtering on (100) Si substrates

    Energy Technology Data Exchange (ETDEWEB)

    Conchon, F., E-mail: florineconchon@gmail.co [Laboratoire de Physique des Materiaux (PHYMAT) UMR 6630, Universite de Poitiers, 86962 Futuroscope-Chasseneuil (France); Renault, P.O.; Goudeau, P.; Le Bourhis, E. [Laboratoire de Physique des Materiaux (PHYMAT) UMR 6630, Universite de Poitiers, 86962 Futuroscope-Chasseneuil (France); Sondergard, E.; Barthel, E.; Grachev, S. [Laboratoire de Surface du Verre et Interfaces (SVI), UMR 125, 93303 Aubervilliers (France); Gouardes, E.; Rondeau, V.; Gy, R. [Laboratoire de 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. [Laboratoire de Physique des Solides (LPS), UMR 8502, 91405 Orsay (France)

    2010-07-01

    Residual stresses in sputtered ZnO films on Si are determined and discussed. By means of X-ray diffraction, we show that as-deposited ZnO films are highly compressively stressed. Moreover, a transition of stress is observed as a function of the post-deposition annealing temperature. After an 800 {sup o}C annealing, ZnO films are tensily stressed while ZnO films encapsulated by Si{sub 3}N{sub 4} are stress-free. With the aid of in-situ X-ray diffraction under ambient and argon atmosphere, we argue that this thermally activated stress relaxation may be attributed to a variation of the stoichiometry of the ZnO films.

  14. High temperature x-ray diffraction of zr-2.5nb during thermal cycling in vacuum

    Directory of Open Access Journals (Sweden)

    Tumanov Mikhail

    2017-01-01

    Full Text Available The cyclic thermal tests in vacuum of zirconium alloy Zr-2.5Nb in the temperature range 250-350°C is established the presence of anomalies of thermal deformation of the crystal lattice, reducing the efficiency of the fuel rods.

  15. Proton diffraction

    International Nuclear Information System (INIS)

    Den Besten, J.L.; Jamieson, D.N.; Allen, L.J.

    1998-01-01

    The Lindhard theory on ion channeling in crystals has been widely accepted throughout ion beam analysis for use in simulating such experiments. The simulations use a Monte Carlo method developed by Barret, which utilises the classical 'billiard ball' theory of ions 'bouncing' between planes or tubes of atoms in the crystal. This theory is not valid for 'thin' crystals where the planes or strings of atoms can no longer be assumed to be of infinite proportions. We propose that a theory similar to that used for high energy electron diffraction can be applied to MeV ions, especially protons, in thin crystals to simulate the intensities of transmission channeling and of RBS spectra. The diffraction theory is based on a Bloch wave solution of the Schroedinger equation for an ion passing through the periodic crystal potential. The widely used universal potential for proton-nucleus scattering is used to construct the crystal potential. Absorption due to thermal diffuse scattering is included. Experimental parameters such as convergence angle, beam tilt and scanning directions are considered in our calculations. Comparison between theory and experiment is encouraging and suggests that further work is justified. (authors)

  16. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-15

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

  18. Stabilization of high-temperature antimony oxide with molybdenum incorporation. Structure of Mo-doped Sb2O4 by powder neutron diffraction and extended X-ray absorption fine structure spectroscopy

    International Nuclear Information System (INIS)

    Teller, R.G.; Antonio, M.R.; Brazdil, J.F.; Mehicic, M.; Grasselli, R.K.

    1985-01-01

    It has been discovered that the presence of MoO 3 lowers the α-β transition in Sb 2 O 4 from 935 to 850 0 C with concurrent dissolution of Mo in the high-temperature (β) form. The structure of Mo-doped β-Sb 2 O 4 has been investigated by powder neutron diffraction, extended X-ray absorption fine structure (EXAFS) and Raman spectroscopies, and scanning-electron microscopy (SEM). Cell parameters: a = 12.0571 (12) A, b = 4.8335 (1) A, c = 5.3838 (6) A, β = 105.579 (5) 0 , monoclinic, space group C2/c, Z = 4. Combining the results of these techniques leads to the hypothesis that Mo is located interstitially within channels of electron density in the Sb 2 O 4 structure with concurrent vacancy of two Sb/sup III/ atoms. There is no apparent oxygen deficiency in the resulting structure. 25 references, 6 figures, 3 tables

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

  1. Thermal behaviour of molecular sieves (SAPO-11/AIPO-11 type) investigated by synchrotron radiation X-ray diffraction (SRXD)

    International Nuclear Information System (INIS)

    Neissendorfer, F.; Jahn, E.; Gusenko, S.N.; Sheromov, M.A.

    1991-01-01

    The structure of molecular sieves is important for a successful application as a catalyzer. The final structure of the synthetic product depends on the technological steps. This process was investigated by in-situ Synchrotron radiation X-ray diffraction. Structural changes in the molecular sieves exist not only during the heating process but also during the following cooling process. (author) 3 figs., 2 refs

  2. Low-Pressure H2, NH3 Microwave Plasma Treatment of Polytetrafluoroethylene (PTFE) Powders: Chemical, Thermal and Wettability Analysis

    Science.gov (United States)

    Hunke, Harald; Soin, Navneet; Shah, Tahir H.; Kramer, Erich; Pascual, Alfons; Karuna, Mallampalli Sri Lakshmi; Siores, Elias

    2015-01-01

    Functionalization of Polytetrafluoroethylene (PTFE) powders of ~6 μm particle size is carried out using low-pressure 2.45 GHz H2, NH3 microwave plasmas for various durations (2.5, 10 h) to chemically modify their surface and alter their surface energy. The X-ray Photoelectron Spectroscopy (XPS) analyses reveal that plasma treatment leads to significant defluorination (F/C atomic ratio of 1.13 and 1.30 for 10 h NH3 and H2 plasma treatments, respectively vs. 1.86 for pristine PTFE), along with the incorporation of functional polar moieties on the surface, resulting in enhanced wettability. Analysis of temperature dependent XPS revealed a loss of surface moieties above 200 °C, however, the functional groups are not completely removable even at higher temperatures (>300 °C), thus enabling the use of plasma treated PTFE powders as potential tribological fillers in high temperature engineering polymers. Ageing studies carried over a period of 12 months revealed that while the surface changes degenerate over time, again, they are not completely reversible. These functionalised PTFE powders can be further used for applications into smart, high performance materials such as tribological fillers for engineering polymers and bio-medical, bio-material applications.

  3. 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.

  4. Thermoelectrical and thermal analyses of copper(II) acetate monohydrate ZnO-matrix composite powder obtained by freeze-drying

    International Nuclear Information System (INIS)

    Bellini, Jusmar Valentin; Pineda, Edgardo Alfonso Gomez; Rocha, Raquel de Almeida; Ponzoni, Andre Luis de Lima; Paesano, Andrea

    2006-01-01

    The thermal history of freeze-dried mixtures of composite powders containing ZnO-matrix and (CH 3 COO) 2 Cu.H 2 O (copper(II) acetate monohydrate) was undertaken by thermal analysis (TA) coupled to thermoelectrical analysis (TEA). Experiments were carried out on compacted samples, under non-isothermal conditions, in air, up to 350 deg. C, by measuring the electrical resistance during heating, called thermoelectrical resistometry (TER), and by differential scanning calorimetry (DSC). Activation energy (E a ) for exothermal events related to the decomposition of (CH 3 COO) 2 Cu (copper(II) acetate, CuAc 2 ), observed within the range 225-325 deg. C, was estimated according to ASTM E 698 method. Values of E a equal to 154 and 155 kJ/mol were obtained by TER and DSC, respectively. TER showed that the thermal decomposition of CuAc 2 involves the liberation of electrons. Results also indicated that TER may be used as an alternative or complementary method for the study of the thermal decomposition mechanisms of transition metal(II) acetates

  5. 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....

  6. Characterization of thermal reaction of aluminum/copper (II) oxide/poly(tetrafluoroethene) nanocomposite by thermogravimetric analysis, differential scanning calorimetry, mass spectrometry and X-ray diffraction

    International Nuclear Information System (INIS)

    Li, Xiangyu; Yang, Hongtao; Li, Yan-chun

    2015-01-01

    Highlights: • The thermal reaction properties of the Al/CuO/PTFE nanocomposite were investigated. • The Al/PTFE and CuO/PTFE nanocomposites were prepared and tested for comparison. • TG/DSC–MS and XRD analysis were performed. • PTFE is oxidizing Al and reducing CuO during the thermal decomposition. - Abstract: The application of fluoropolymers as reactive agent in energetic materials have attracted significant interest recently. In this study, the thermal reaction properties of the aluminum nanoparticles/copper (II) oxide nanoparticles/poly(tetrafluoroethene) (Al-NPs/CuO-NPs/PTFE) nanocomposite (mass ratio of Al-NPs/CuO-NPs/PTFE = 20/60/20) were investigated by means of thermogravimetry/differential scanning calorimetry–mass spectrometry (TG/DSC–MS) and X-ray diffraction (XRD) analyses. The Al-NPs/PTFE (mass ratio of Al-NPs/PTFE = 50/50) and CuO-NPs/PTFE (mass ratio of CuO-NPs/PTFE = 75/25) nanocomposites were also prepared and tested for comparison. It is observed that PTFE is acting as both oxidizer and reducer during the thermal decomposition process of Al-NPs/CuO-NPs/PTFE nanocomposites. Before 615 °C, PTFE is oxidized by CuO-NPs and oxidizing Al-NPs, resulting mass reduction. After 615 °C, the excessive aluminum and copper (I)/copper (II) oxide will proceed the exothermic condensed phase reaction.

  7. Lead recovery and high silica glass powder synthesis from waste CRT funnel glasses through carbon thermal reduction enhanced glass phase separation process

    Energy Technology Data Exchange (ETDEWEB)

    Xing, Mingfei [Henan Key Laboratory Cultivation Base of Mine Environmental Protection and Ecological Remediation, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Fu, Zegang [Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Wang, Yaping, E-mail: wangyp326@163.com [School of Surveying and Land Information Engineering, Henan Polytechnic University, Jiaozuo 454000, Henan China (China); Wang, Jingyu [Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Zhang, Zhiyuan [Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China)

    2017-01-15

    Highlights: • CRT funnel glass was remelted with B{sub 2}O{sub 3} in reducing atmosphere. • A part of PbO was reduced into Pb and detached from the glass phase. • The rest of PbO and other metal oxides were mainly concentrated in the B{sub 2}O{sub 3} phase. • PbO enriched in the interconnected B{sub 2}O{sub 3} phase can be completely leached out by HNO{sub 3}. • High silica glass powder(SiO{sub 2} purity >95%) was obtained after the leaching process. - Abstract: In this study, a novel process for the removal of toxic lead from the CRT funnel glass and synchronous preparation of high silica glass powder was developed by a carbon-thermal reduction enhanced glass phase separation process. CRT funnel glass was remelted with B{sub 2}O{sub 3} in reducing atmosphere. In the thermal process, a part of PbO contained in the funnel glass was reduced into metallic Pb and detached from the glass phase. The rest of PbO and other metal oxides (including Na{sub 2}O, K{sub 2}O, Al{sub 2}O{sub 3,} BaO and CaO) were mainly concentrated in the boric oxide phase. The metallic Pb phase and boric oxide phase were completely leached out by 5 mol/L HNO{sub 3}. The lead removal rate was 99.80% and high silica glass powder (SiO{sub 2} purity >95 wt%) was obtained by setting the temperature, B{sub 2}O{sub 3} added amount and holding time at 1000 °C, 20% and 30 mins, respectively. The prepared high silicate glass powders can be used as catalyst carrier, semipermeable membranes, adsorbents or be remelted into high silicate glass as an ideal substitute for quartz glass. Thus this study proposed an eco-friendly and economical process for recycling Pb-rich electronic glass waste.

  8. 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

  9. Powder diffraction in structural characterization of ...

    Indian Academy of Sciences (India)

    Administrator

    scientists for studying the structure and microstruc- ture of crystalline solids. .... No specific colour brown habit, brown habit, dark red habit, brown habit, dark red ..... polymorphic modifications of this compound, where atom N14 will play a role ...

  10. 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

  11. Impact of the long chain omega-acylceramides on the stratum corneum lipid nanostructure. Part 1: Thermotropic phase behaviour of CER[EOS] and CER[EOP] studied using X-ray powder diffraction and FT-Raman spectroscopy.

    Science.gov (United States)

    Kessner, Doreen; Brezesinski, Gerald; Funari, Sergio S; Dobner, Bodo; Neubert, Reinhard H H

    2010-01-01

    The stratum corneum (SC), the outermost layer of the mammalian skin, is the main skin barrier. Ceramides (CERs) as the major constituent of the SC lipid matrix are of particular interest. At the moment, 11 classes of CERs are identified, but the effect of each single ceramide species is still not known. Therefore in this article, the thermotropic behaviour of the long chain omega-acylceramides CER[EOS] and CER[EOP] was studied using X-ray powder diffraction and FT-Raman spectroscopy. It was found that the omega-acylceramides CER[EOS] and CER[EOP] do not show a pronounced polymorphism which is observed for shorter chain ceramides as a significant feature. The phase behaviour of both ceramides is strongly influenced by the extremely long acyl-chain residue. The latter has a much stronger influence compared with the structure of the polar head group, which is discussed as extremely important for the appearance of a rich polymorphism. Despite the strong influence of the long chain, the additional OH-group of the phyto-sphingosine type CER[EOP] influences the lamellar repeat distance and the chain packing. The less polar sphingosine type CER[EOS] is stronger influenced by the long acyl-chain residue. Hydration is necessary for the formation of an extended hydrogen-bonding network between the polar head groups leading to the appearance of a long-periodicity phase (LPP). In contrast, the more polar CER[EOP] forms the LPP with densely packed alkyl chains already in the dry state.

  12. Non-linear thermal evolution of the crystal structure and phase transitions of LaFeO3 investigated by high temperature X-ray diffraction

    International Nuclear Information System (INIS)

    Selbach, Sverre M.; Tolchard, Julian R.; Fossdal, Anita; Grande, Tor

    2012-01-01

    The crystal structure, anisotropic thermal expansion and structural phase transition of the perovskite LaFeO 3 has been studied by high-temperature X-ray diffraction from room temperature to 1533 K. The structural evolution of the orthorhombic phase with space group Pbnm and the rhombohedral phase with R3 ¯ c structure of LaFeO 3 is reported in terms of lattice parameters, thermal expansion coefficients, atomic positions, octahedral rotations and polyhedral volumes. Non-linear lattice expansion across the antiferromagnetic to paramagnetic transition of LaFeO 3 at T N =735 K was compared to the corresponding behavior of the ferroelectric antiferromagnet BiFeO 3 to gain insight to the magnetoelectric coupling in BiFeO 3 , which is also multiferroic. The first order phase transition of LaFeO 3 from Pbnm to R3 ¯ c was observed at 1228±9 K, and a subsequent transition to Pm3 ¯ m was extrapolated to occur at 2140±30 K. The stability of the Pbnm and R3 ¯ c polymorphs of LaFeO 3 is discussed in terms of the competing enthalpy and entropy of the two crystal polymorphs and the thermal evolution of the polyhedral volume ratio V A /V B . - Graphical abstract: Aniostropic thermal evolution of the lattice parameters and phase transition of LaFeO 3 . Highlights: ► The crystal structure of LaFeO 3 is studied by HTXRD from RT to 1533 K. ► A non-linear expansion across the Néel temperature is observed for LaFeO 3 . ► The ratio V A /V B is used to rationalize the thermal evolution of the structure.

  13. Diffractive interactions

    International Nuclear Information System (INIS)

    Del Duca, V.; Marage, P.

    1996-08-01

    The general framework of diffractive deep inelastic scattering is introduced and reports given in the session on diffractive interactions at the international workshop on deep-inelastic scattering and related phenomena, Rome, April 1996, are presented. (orig.)

  14. X-ray diffraction study of thermally and stress-induced phase transformations in single crystalline Ni-Mn-Ga alloys

    International Nuclear Information System (INIS)

    Martynov, V.V.

    1995-01-01

    Using in-situ single crystal X-ray diffraction methods, thermally- and stress-induced crystal structure evolution was investigated in two Ni-Mn-Ga Heusler-type alloys. For the 51at.%Ni-24at.%Mn-25at.%Ga alloy it was found that application of external stress in a temperature range ∼20 C above the M s at first causes intensity changes of X-ray diffuse scattering peaks in β-phase. Further stressing results in stress-induced phase transformations and under the appropriate conditions three successive martensitic transformations (one is parent-to-martensite and two are martensite-to-martensite transformations) can be stress induced. Of these only the parent-to-martensite transformation can be thermally-induced. Two successive structural transformations (thermally-induced parent-to-martensite and stress-induced martensite-to-martensite transformations) were found in 52at.%Ni-25at.%Mn-23at.%Ga alloy. Crystal structure, lattice parameters, type of modulation, and the length of modulation period for all martensites were identified. (orig.)

  15. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Bindi, Luca [Museo di Storia Naturale, sez. di Mineralogia, Universita di Firenze, Via La Pira 4, I-50121 Firenze (Italy)], E-mail: luca.bindi@unifi.it

    2009-04-03

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: {alpha}{sub a} = 1.5 x 10{sup -5} K{sup -1}, {alpha}{sub b} = 3.0 x 10{sup -5} K{sup -1}, {alpha}{sub c} = 2.2 x 10{sup -5} K{sup -1}, and the bulk thermal expansion coefficient {alpha}{sub V} is 5.4 x 10{sup -5} K{sup -1} for the temperature range 298-463 K.

  16. Probing the thermal stability and the decomposition mechanism of a magnesium-fullerene polymer via X-ray Raman spectroscopy, X-ray diffraction and molecular dynamics simulations.

    Science.gov (United States)

    Aramini, Matteo; Niskanen, Johannes; Cavallari, Chiara; Pontiroli, Daniele; Musazay, Abdurrahman; Krisch, Michael; Hakala, Mikko; Huotari, Simo

    2016-02-21

    We report the microscopic view of the thermal structural stability of the magnesium intercalated fullerene polymer Mg2C60. With the application of X-ray Raman spectroscopy and X-ray diffraction, we study in detail the decomposition pathways of the polymer system upon annealing at temperatures between 300 and 700 °C. We show that there are at least two energy scales involved in the decomposition reaction. Intermolecular carbon bonds, which are responsible for the formation of a 2D fullerene polymer, are broken with a relatively modest thermal energy, while the long-range order of the original polymer remains intact. With an increased thermal energy, the crystal structure in turn is found to undergo a transition to a novel intercalated cubic phase that is stable up to the highest temperature studied here. The local structure surrounding magnesium ions gets severely modified close to, possibly at, the phase transition. We used density functional theory based calculations to study the thermodynamic and kinetic aspects of the collapse of the fullerene network, and to explain the intermediate steps as well as the reaction pathways in the break-up of this peculiar C60 intermolecular bonding architecture.

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

    Czech Academy of Sciences Publication Activity Database

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

    2014-01-01

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

  18. Diffraction theory

    NARCIS (Netherlands)

    Bouwkamp, C.J.

    1954-01-01

    A critical review is presented of recent progress in classical diffraction theory. Both scalar and electromagnetic problems are discussed. The report may serve as an introduction to general diffraction theory although the main emphasis is on diffraction by plane obstacles. Various modifications of

  19. Dynamic study of the thermal stability of impure Ti3SiC2 in argon and air by neutron diffraction

    International Nuclear Information System (INIS)

    Oo, Z.; Low, I.M; O'Connor, B.H.

    2006-01-01

    The dynamic thermal stability and topotactic phase transition of impure Ti 3 SiC 2 in air and argon have been investigated by neutron diffraction (ND). In the presence of a low oxygen partial pressure as in argon, Ti 3 SiC 2 underwent a surface dissociation and TiC and/or Ti 5 Si 3 C were detected at 1200 deg. C. In contrast, oxide layers of rutile (TiO 2 ), TiO and cristobalite (SiO 2 ) were detected at ∼1000, 1250 and 1300 deg. C respectively when exposed to an oxygen-rich environment. Near-surface depth profiling of Ti 3 SiC 2 oxidized in air at 1200 deg. C by secondary ion mass spectroscopy (SIMS) has revealed a distinct gradation in phase composition at the interface of homogeneous rutile and heterogeneous cristobalite-rutile layers

  20. Dynamic study of the thermal stability of impure Ti 3SiC 2 in argon and air by neutron diffraction

    Science.gov (United States)

    Oo, Z.; Low, I. M.; O'Connor, B. H.

    2006-11-01

    The dynamic thermal stability and topotactic phase transition of impure Ti 3SiC 2 in air and argon have been investigated by neutron diffraction (ND). In the presence of a low oxygen partial pressure as in argon, Ti 3SiC 2 underwent a surface dissociation and TiC and/or Ti 5Si 3C were detected at 1200 °C. In contrast, oxide layers of rutile (TiO 2), TiO and cristobalite (SiO 2) were detected at ∼1000, 1250 and 1300 °C respectively when exposed to an oxygen-rich environment. Near-surface depth profiling of Ti 3SiC 2 oxidized in air at 1200 °C by secondary ion mass spectroscopy (SIMS) has revealed a distinct gradation in phase composition at the interface of homogeneous rutile and heterogeneous cristobalite-rutile layers.

  1. A synchrotron X-ray diffraction deconvolution method for the measurement of residual stress in thermal barrier coatings as a function of depth.

    Science.gov (United States)

    Li, C; Jacques, S D M; Chen, Y; Daisenberger, D; Xiao, P; Markocsan, N; Nylen, P; Cernik, R J

    2016-12-01

    The average residual stress distribution as a function of depth in an air plasma-sprayed yttria stabilized zirconia top coat used in thermal barrier coating (TBC) systems was measured using synchrotron radiation X-ray diffraction in reflection geometry on station I15 at Diamond Light Source, UK, employing a series of incidence angles. The stress values were calculated from data deconvoluted from diffraction patterns collected at increasing depths. The stress was found to be compressive through the thickness of the TBC and a fluctuation in the trend of the stress profile was indicated in some samples. Typically this fluctuation was observed to increase from the surface to the middle of the coating, decrease a little and then increase again towards the interface. The stress at the interface region was observed to be around 300 MPa, which agrees well with the reported values. The trend of the observed residual stress was found to be related to the crack distribution in the samples, in particular a large crack propagating from the middle of the coating. The method shows promise for the development of a nondestructive test for as-manufactured samples.

  2. In Situ Study of Microstructure Evolution in Solidification of Hypereutectic Al-Si Alloys with Application of Thermal Analysis and Neutron Diffraction

    Science.gov (United States)

    Sediako, Dimitry G.; Kasprzak, Wojciech

    2015-09-01

    Understanding of the kinetics of solid-phase evolution in solidification of hypereutectic aluminum alloys is a key to control their as-cast microstructure and resultant mechanical properties, and in turn, to enhance the service characteristics of actual components. This study was performed to evaluate the solidification kinetics for three P-modified hypereutectic Al-19 pct Si alloys: namely, Al-Si binary alloy and with the subsequent addition of 2.8 pct Cu and 2.8 pct Cu + 0.7 pct Mg. Metallurgical evaluation included thermodynamic calculations of the solidification process using the FactSage™ 6.2 software package, as well as experimental thermal analysis, and in situ neutron diffraction. The study revealed kinetics of solid α-Al, solid Si, Al2Cu, and Mg2Si evolution, as well as the individual effects of Cu and Mg alloying additions on the solidification path of the Al-Si system. Various techniques applied in this study resulted in some discrepancies in the results. For example, the FactSage computations, in general, resulted in 281 K to 286 K (8 °C to 13 °C) higher Al-Si eutectic temperatures than the ones recorded in the thermal analysis, which are also ~278 K (~5 °C) higher than those observed in the in situ neutron diffraction. None of the techniques can provide a definite value for the solidus temperature, as this is affected by the chosen calculation path [283 K to 303 K (10 °C to 30 °C) higher for equilibrium solidification vs non-equilibrium] for the FactSage analysis; and further complicated by evolution of secondary Al-Cu and Mg-Si phases that commenced at the end of solidification. An explanation of the discrepancies observed and complications associated with every technique applied is offered in the paper.

  3. Mullite and Mullite/ZrO2-7wt.%Y2O3 Powders for Thermal Spraying of Environmental Barrier Coatings

    Science.gov (United States)

    Garcia, E.; Mesquita-Guimarães, J.; Miranzo, P.; Osendi, M. I.; Wang, Y.; Lima, R. S.; Moreau, C.

    2010-01-01

    Mullite and mullite/ZrO2-7wt.%Y2O3 coatings could be thought among the main protective layers for environment barrier coatings (EBCs) to protect Si-based substrates in future gas turbine engines. Considering that feedstock of the compound powder is not commercially available, two powder processing routes Spray Drying (SD) and Flame Spheroidization (FS) were implemented for both types of powders. For each method the particle size, the morphology, and microstructure of the powder particles was determined. In addition, the effect of the heat treatment on the powder crystallinity and microstructure of FS powders was also investigated. To evaluate their suitability as feedstock materials, the powders were plasma sprayed and their in-flight particle characteristics monitored for coatings production. The powder morphology was correlated to the in-flight particle characteristics and splat morphology to gain insight about into the influence of powder characteristics on the coating formation.

  4. 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)

  5. 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)

  6. 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

  7. 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...

  8. Structure and properties of ZnSxSe1-x thin films deposited by thermal evaporation of ZnS and ZnSe powder mixtures

    Science.gov (United States)

    Valeev, R. G.; Romanov, E. A.; Vorobiev, V. L.; Mukhgalin, V. V.; Kriventsov, V. V.; Chukavin, A. I.; Robouch, B. V.

    2015-02-01

    Interest to ZnSxSe1-x alloys is due to their band-gap tunability varying S and Se content. Films of ZnSxSe1-x were grown evaporating ZnS and ZnSe powder mixtures onto SiO2, NaCl, Si and ITO substrates using an original low-cost method. X-ray diffraction patterns and Raman spectroscopy, show that the lattice structure of these films is cubic ZnSe-like, as S atoms replace Se and film compositions have their initial S/Se ratio. Optical absorption spectra show that band gap values increase from 2.25 to 3 eV as x increases, in agreement with the literature. Because S atomic radii are smaller than Se, EXAFS spectra confirm that bond distances and Se coordination numbers decrease as the Se content decreases. The strong deviation from linearity of ZnSe coordination numbers in the ZnSxSe1-x indicate that within this ordered crystal structure strong site occupation preferences occur in the distribution of Se and S ions. The behavior is quantitatively confirmed by the strong deviation from the random Bernoulli distribution of the three sight occupation preference coefficients of the strained tetrahedron model. Actually, the ternary ZnSxSe1-x system is a bi-binary (ZnS+ZnSe) alloy with evanescent formation of ternary configurations throughout the x-range.

  9. 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

  10. S tudies on the phase transitions and properties of tungsten (VI oxide nanoparticles by X - Ray diffraction (XRD and thermal analysis

    Directory of Open Access Journals (Sweden)

    S.F. Abdullah

    2017-11-01

    Full Text Available Tungsten (VI oxide, WO3nanoparticles were synthesized by colloidal gas aphrons(CGAs technique.The resultant WO3nanoparticleswere characterized by thermogravimetric-differential thermal analysis (TG-DTA and X-Ray diffraction (XRD measurements in order to determine the phase transitions, the crystallinity and the size of theWO3nanoparticles. As a comparison, transmission electron microscope (TEM was used to investigate the size of the WO3nanoparticles. The result from XRD and DTA show that the formation of polymorphsWO3nanoparticles have the following sequence: orthorhombic (b-WO3®monoclinic (g-WO3 ®triclinic (d-WO3 ®monoclinic (e-WO3 with respect to the calcination temperature of 400, 500, 600 and 700°C. No diffraction peaks were found in the X-Ray diffraction measurements for the sample heat treated at 300°C (as-prepared, suggesting that an amorphous structure was obtained at this temperature whereas the crystallinity had been obtained by the other samples of theWO3nanoparticles at the calcination temperatures of 400, 500, 600 and 700°C. It is also found that the X-Ray diffraction measurements produced an average diameter of (30 ±5, (50 ±5, (150 ±10 and (200 ±10 nm at calcination temperatures of 400, 500, 600 and 700°C respectively by using Debye-Scherrer formula. The TG curve revealed that the WO3nanoparticles is purely anhydrous since the weight loss is insignificant (0.3 –1.4 % from 30 until 600°C for the WO3nanoparticles calcined at 400°C. Finally, the composition and the purity of the WO3nanoparticleshave been examined by X-Ray photoelectron spectroscopy (XPS. Theresults indicate no significant changes to the composition and the purity of the WO3nanoparticle produced due to the temperature variations

  11. 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)

  12. 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.

  13. The High Performance Shape Memory Effect (HP-SME in Ni Rich NiTi Wires: In Situ X-Ray Diffraction on Thermal Cycling

    Directory of Open Access Journals (Sweden)

    Coduri Mauro

    2015-01-01

    Full Text Available A novel approach for using Shape Memory Alloys (SMA was recently proposed and named highperformance shape memory effect (HP-SME. The HP-SME exploits the thermal cycling of stress-induced martensite for producing extremely high mechanical work with a very stable functional fatigue behaviour in Ni rich NiTi alloy. The latter was found to differ significantly from the functional fatigue behaviour observed for conventional SMA. This study was undertaken in order to elucidate the microstructural modifications at the basis of this particular feature. To this purpose, the functional fatigue was coupled to in situ Synchrotron Radiation X-Ray Diffraction, by recording patterns on wires thermally cycled by Joule effect under a constant applied stress (800 MPa. The accurate analysis the line profile XRD data suggests the accumulation of defects upon functional cycling, while the fibre texture was not observed to change. The functional fatigue exhibits a very similar behaviour as the line broadening of XRD peaks, thus suggesting the accumulation of dislocations as the origin of the mechanism of the permanent deformation.

  14. A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

    Science.gov (United States)

    Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

    2017-01-01

    Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.

  15. CSER 01-008 Canning of Thermally Stabilized Plutonium Oxide Powder in PFP Glovebox HC-21A

    International Nuclear Information System (INIS)

    ERICKSON, D.G.

    2001-01-01

    This document presents the analysis performed to support the canning operation in HC-21A. Most of the actual analysis was performed for the operation in HC-18M and HA-20MB, and is documented in HNF-2707 Rev I a (Erickson 2001a). This document will reference Erickson (2001a) as necessary to support the operation in HC-21A. The plutonium stabilization program at the Plutonium Finishing Plant (PFP) uses heat to convert plutonium-bearing materials into dry powder that is chemically stable for long term storage. The stabilized plutonium is transferred into one of several gloveboxes for the canning process, Gloveboxes HC-18M in Room 228'2, HA-20MB in Room 235B, and HC-21A in Room 230B are to be used for this process. This document presents the analysis performed to support the canning operation in HC-21A. Most of the actual analysis was performed for the operation in HC-I8M and HA-20MB, and is documented in HNF-2707 Rev l a (Erickson 2001a). This document will reference Erickson (2001a) as necessary to support the operation in HC-21A. Evaluation of this operation included normal, base cases, and contingencies. The base cases took the normal operations for each type of feed material and added the likely off-normal events. Each contingency is evaluated assuming the unlikely event happens to the conservative base case. Each contingency was shown to meet the double contingency requirement. That is, at least two unlikely, independent, and concurrent changes in process conditions are required before a criticality is possible

  16. 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.

  17. 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

  18. 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.)

  19. 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...

  20. 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)