WorldWideScience

Sample records for situ high-pressure synchrotron

  1. In-situ Diffraction Study of Magnetite at Simultaneous High Pressure and High Temperature Using Synchrotron Radiation

    Science.gov (United States)

    Wang, L.; Zhang, J.; Wang, S.; Chen, H.; Zhao, Y.

    2014-12-01

    Magnetite intertwined with the evolution of human civilizations, and remains so today. It is technologically and scientifically important by virtue of its unique magnetic and electrical properties. Magnetite is a common mineral found in a variety of geologic environments, and plays an important role in deciphering the oxygen evolution in the Earth's atmosphere and its deep interiors. The latter application asks for the knowledge of the thermal and elastic properties of magnetite at high pressures and temperatures, which is currently not available in literature. We have carried out a few in-situ diffraction experiments on magnetite using white synchrotron radiation at beamline X17B2 of National Synchrotron Light Source (NSLS). A DIA module in an 1100-ton press and WC anvils were employed for compression, and diffraction spectra were collected at simultaneous high pressures (P) and temperatures (T) (up to 9 GPa and 900 oC). Mixture of amorphous boron and epoxy resin was used as pressure medium, and NaCl as pressure marker. Temperature was recorded by W-Re thermocouples. Commercially purchased magnetite powder and a mixture of the said powder and NaCl (1:1) were used as starting material in separate experiments. Preliminary data analyses have yielded following observations: (1) Charge disordering seen at ambient pressure remains active in current experiments, especially at lower pressures (reversibility and degree of cation disordering depend on the starting material and/or experimental P-T path; and (4) cation disordering notably reduces the apparent bulk moduli of magnetite.

  2. Development of in situ Brillouin spectroscopy at high pressure and high temperature with synchrotron radiation and infrared laser heating system: Application to the Earth's deep interior

    Science.gov (United States)

    Murakami, Motohiko; Asahara, Yuki; Ohishi, Yasuo; Hirao, Naohisa; Hirose, Kei

    2009-05-01

    Seismic wave velocity profiles in the Earth provide one of the strongest constraints on structure, mineralogy and elastic properties of the Earth's deep interior. Accurate sound velocity data of deep Earth materials under relevant high-pressure and high-temperature conditions, therefore, are essential for interpretation of seismic data. Such information can be directly obtained from Brillouin scattering measurement. Here we describe an in situ Brillouin scattering system for measurements at high pressure and high temperature using a laser heated diamond anvil cell and synchrotron radiation for sample characterization. The system has been used with single-crystal and polycrystalline materials, and with glass and fluid phase. It provided high quality sound velocity and elastic data with X-ray diffraction data at high pressure and/or high temperature. Those combined techniques can potentially offer the essential information for resolving many remaining issues in mineral physics.

  3. High pressure and synchrotron radiation satellite workshop

    Energy Technology Data Exchange (ETDEWEB)

    Bass, J.; Guignot, N.; Morard, G.; Mezouar, M.; Andrault, D.; Bolfan-Casanova, N.; Sturhahn, W.; Daniel, I.; Reynard, B.; Simionovici, A.; Sanchez Valle, C.; Martinez, I.; Kantor, I.; Dubrovinsky, I.; Mccammon, C.; Dubrovinskaia, N.; Kurnosiv, A.; Kuznetsov, A.; Goncharenko, I.; Loubeyre, P.; Desgreniers, S.; Weck, G.; Yoo, C.S.; Iota, V.; Park, J.; Cynn, H.; Gorelli, F.; Toulemonde, P.; Machon, D.; Merlen, A.; San Miguel, A.; Amboage, M.; Aquilanti, G.; Mathon, O.; Pascarelli, S.; Itie, J.P.; Mcmillan, P.F.; Trapananti, A.; Di Cicco, A.; Panfilis, S. de; Filipponi, A.; Kreisel, J.; Bouvier, P.; Dkhil, B.; Chaabane, B.; Rosner, H.; Koudela, D.; Schwarz, U.; Handestein, A.; Hanfland, M.; Opahle, I.; Koepernik, K.; Kuzmin, M.; Mueller, K.H.; Mydosh, J.; Richter, M.; Hejny, C.; Falconi, S.; Lundegaard, L.F.; Mcmahon, M.I; Loa, I.; Syassen, K.; Wang, X.; Roth, H.; Lorenz, T.; Farber Daniel, I.; Antonangeli Daniele, I.; Krisch, M.; Badro, J.; Fiquet, G.; Occelli, F.; Mao, W.L.; Mao, H.K.; Eng, P.; Kao, C.C.; Shu, J.F.; Hemley, R.J.; Tse, J.S.; Yao, Y.; Deen, P.P.; Paolasini, I.; Braithwaite, D.; Kernavanois, N.; Lapertot, G.; Rupprecht, K.; Leupold, O.; Ponkratz, U.; Wortmann, G.; Beraud, A.; Krisch, M.; Farber, D.; Antonangeli, D.; Aracne, C.; Zarestky, J.L.; Mcqueeney, R.; Mathon, O.; Baudelet, F.; Decremps, F.; Itie, J.P.; Nataf, I.; Pascarelli, S.; Polian, A

    2006-07-01

    The workshop is dedicated to recent advances on science at high pressure at third generation synchrotron sources. A variety of experiments using synchrotron radiation techniques including X-ray diffraction, EXAFS (extended X-ray absorption fine structure), inelastic X-ray scattering, Compton scattering and Moessbauer spectroscopy of crystalline, liquid or amorphous samples, are reported. This document gathers the abstracts of the presentations.

  4. High pressure and synchrotron radiation satellite workshop

    International Nuclear Information System (INIS)

    Bass, J.; Guignot, N.; Morard, G.; Mezouar, M.; Andrault, D.; Bolfan-Casanova, N.; Sturhahn, W.; Daniel, I.; Reynard, B.; Simionovici, A.; Sanchez Valle, C.; Martinez, I.; Kantor, I.; Dubrovinsky, I.; Mccammon, C.; Dubrovinskaia, N.; Kurnosiv, A.; Kuznetsov, A.; Goncharenko, I.; Loubeyre, P.; Desgreniers, S.; Weck, G.; Yoo, C.S.; Iota, V.; Park, J.; Cynn, H.; Gorelli, F.; Toulemonde, P.; Machon, D.; Merlen, A.; San Miguel, A.; Amboage, M.; Aquilanti, G.; Mathon, O.; Pascarelli, S.; Itie, J.P.; Mcmillan, P.F.; Trapananti, A.; Di Cicco, A.; Panfilis, S. de; Filipponi, A.; Kreisel, J.; Bouvier, P.; Dkhil, B.; Chaabane, B.; Rosner, H.; Koudela, D.; Schwarz, U.; Handestein, A.; Hanfland, M.; Opahle, I.; Koepernik, K.; Kuzmin, M.; Mueller, K.H.; Mydosh, J.; Richter, M.; Hejny, C.; Falconi, S.; Lundegaard, L.F.; Mcmahon, M.I; Loa, I.; Syassen, K.; Wang, X.; Roth, H.; Lorenz, T.; Farber Daniel, I.; Antonangeli Daniele, I.; Krisch, M.; Badro, J.; Fiquet, G.; Occelli, F.; Mao, W.L.; Mao, H.K.; Eng, P.; Kao, C.C.; Shu, J.F.; Hemley, R.J.; Tse, J.S.; Yao, Y.; Deen, P.P.; Paolasini, I.; Braithwaite, D.; Kernavanois, N.; Lapertot, G.; Rupprecht, K.; Leupold, O.; Ponkratz, U.; Wortmann, G.; Beraud, A.; Krisch, M.; Farber, D.; Antonangeli, D.; Aracne, C.; Zarestky, J.L.; Mcqueeney, R.; Mathon, O.; Baudelet, F.; Decremps, F.; Itie, J.P.; Nataf, I.; Pascarelli, S.; Polian, A.

    2006-01-01

    The workshop is dedicated to recent advances on science at high pressure at third generation synchrotron sources. A variety of experiments using synchrotron radiation techniques including X-ray diffraction, EXAFS (extended X-ray absorption fine structure), inelastic X-ray scattering, Compton scattering and Moessbauer spectroscopy of crystalline, liquid or amorphous samples, are reported. This document gathers the abstracts of the presentations

  5. High-pressure behavior of synthetic mordenite-Na. An in situ single-crystal synchrotron X-ray diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Lotti, Paolo; Merlini, Marco [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; Gatta, G. Diego [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; CNR, Bari (Italy). Int. di Cristallografia; Liermann, Hanns-Peter [DESY, Hamburg (Germany). Photon Sciences

    2015-05-01

    The high-pressure behavior of a synthetic mordenite-Na (space group: Cmcm or Cmc2{sub 1}) was studied by in situ single-crystal synchrotron X-ray diffraction with a diamond anvil cell up to 9.22(7) GPa. A phase transition, likely displacive in character, occurred between 1.68(7) and 2.70(8) GPa, from a C-centered to a primitive space group: possibly Pbnm, Pbnn or Pbn2{sub 1}. Fitting of the experimental data with III-BM equations of state allowed to describe the elastic behavior of the high-pressure polymorph with a primitive lattice. A very high volume compressibility [K{sub V0} = 25(2) GPa, β{sub V0} = 1/K{sub V0} = 0.040(3) GPa{sup -1}; K{sub V}' = (∂K{sub V}/∂P){sub T} = 2.0(3)], coupled with a remarkable elastic anisotropy (β{sub b}>>β{sub c}>β{sub a}), was found. Interestingly, the low-P and high-P polymorphs show the same anisotropic compressional scheme. A structure collapse was not observed up to 9.22(7) GPa, even though a strong decrease of the number of observed reflections at the highest pressures suggests an impending amorphization. The structure refinements performed at room-P, 0.98(2) and 1.68(7) GPa allowed to describe, at a first approximation, the mechanisms that govern the framework deformation in the low-P regime: the bulk compression is strongly accommodated by the increase of the ellipticity of the large 12-membered ring channels running along [001].

  6. Experimental issues in in-situ synchrotron x-ray diffraction at high pressure and temperature by using a laser-heated diamond-anvil cell

    International Nuclear Information System (INIS)

    Yoo, C.S.

    1997-01-01

    An integrated technique of diamond-anvil cell, laser-heating and synchrotron x-ray diffraction technologies is capable of structural investigation of condensed matter in an extended region of high pressures and temperatures above 100 GPa and 3000 K. The feasibility of this technique to obtain reliable data, however, strongly depends on several experimental issues, including optical and x-ray setups, thermal gradients, pressure homogeneity, preferred orientation, and chemical reaction. In this paper, we discuss about these experimental issues together with future perspectives of this technique for obtaining accurate data

  7. Advances and synergy of high pressure sciences at synchrotron sources

    International Nuclear Information System (INIS)

    Liu, H.; Ehm, L.; Duffy, T.; Crichton, W.; Aoki, K.

    2009-01-01

    Introductory overview to the special issue papers on high-pressure sciences and synchrotron radiation. High-pressure research in geosciences, materials science and condensed matter physics at synchrotron sources is experiencing growth and development through synergistic efforts around the world. A series of high-pressure science workshops were organized in 2008 to highlight these developments. One of these workshops, on 'Advances in high-pressure science using synchrotron X-rays', was held at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, USA, on 4 October 2008. This workshop was organized in honour of Drs Jingzhu Hu and Quanzhong Guo in celebration of their retirement after up to 18 years of dedicated service to the high-pressure community as beamline scientists at X17 of NSLS. Following this celebration of the often unheralded role of the beamline scientist, a special issue of the Journal of Synchrotron Radiation on Advances and Synergy of High-Pressure Sciences at Synchrotron Sources was proposed, and we were pleased to invite contributions from colleagues who participated in the workshop as well as others who are making similar efforts at synchrotron sources worldwide.

  8. High-pressure synchrotron infrared spectroscopy at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Hemley, R.J.; Goncharov, A.F.; Lu, R.; Struzhkin, V.V.; Li, M.; Mao, H.K.

    1998-01-01

    The paper describes a synchrotron infrared facility for high-pressure spectroscopy and microspectroscopy at the National Synchrotron Light-Source (NSLS). Located at beamline U2B on the VUV ring of the NSLS, the facility utilizes a commercial FT-IR together with custom-built microscope optics designed for a variety of diamond anvil cell experiments, including low- and high- temperature studies. The system contains an integrated laser optical/grating spectrometer for concurrent optical experiments. The facility has been used to characterize a growing number of materials to ultrahigh pressure and has been instrumental of new high-pressure phenomena. Experiments on dense hydrogen to >200 GPa have led to the discovery of numerous unexpected properties of this fundamental system. The theoretically predicted molecular-atomic transition of H 2 O ice to the symmetric hydrogen-bonded structure has been identified, and new classes of high-density clathrates and molecular compounds have been characterized. Experiments on natural and synthetic mineral samples have been performed to study hydrogen speciation, phase transformations, and microscopic inclusions in multiphase assemblages. Detailed information on the behavior of new materials, including novel high-pressure glasses and ceramics, has also been obtained

  9. In Situ Raman Study of Liquid Water at High Pressure.

    Science.gov (United States)

    Romanenko, Alexandr V; Rashchenko, Sergey V; Goryainov, Sergey V; Likhacheva, Anna Yu; Korsakov, Andrey V

    2018-06-01

    A pressure shift of Raman band of liquid water (H 2 O) may be an important tool for measuring residual pressures in mineral inclusions, in situ barometry in high-pressure cells, and as an indicator of pressure-induced structural transitions in H 2 O. However, there was no consensus as to how the broad and asymmetric water Raman band should be quantitatively described, which has led to fundamental inconsistencies between reported data. In order to overcome this issue, we measured Raman spectra of H 2 O in situ up to 1.2 GPa using a diamond anvil cell, and use them to test different approaches proposed for the description of the water Raman band. We found that the most physically meaningful description of water Raman band is the decomposition into a linear background and three Gaussian components, associated with differently H-bonded H 2 O molecules. Two of these components demonstrate a pronounced anomaly in pressure shift near 0.4 GPa, supporting ideas of structural transition in H 2 O at this pressure. The most convenient approach for pressure calibration is the use of "a linear background + one Gaussian" decomposition (the pressure can be measured using the formula P (GPa) = -0.0317(3)·Δν G (cm -1 ), where Δν G represents the difference between the position of water Raman band, fitted as a single Gaussian, in measured spectrum and spectrum at ambient pressure).

  10. HPCAT: an integrated high-pressure synchrotron facility at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Shen, Guoyin; Chow, Paul; Xiao, Yuming; Sinogeikin, Stanislav; Meng, Yue; Yang, Wenge; Liermann, Hans-Peter; Shebanova, Olga; Rod, Eric; Bommannavar, Arunkumar; Mao, Ho-Kwang

    2008-01-01

    The high pressure collaborative access team (HPCAT) was established to advance cutting edge, multidisciplinary, high-pressure (HP) science and technology using synchrotron radiation at sector 16 of the Advanced Photon Source of Argonne National Laboratory. The integrated HPCAT facility has established four operating beamlines in nine hutches. Two beamlines are split in energy space from the insertion device (16ID) line, whereas the other two are spatially divided into two fans from the bending magnet (16BM) line. An array of novel X-ray diffraction and spectroscopic techniques has been integrated with HP and extreme temperature instrumentation at HPCAT. With a multidisciplinary approach and multi-institution collaborations, the HP program at the HPCAT has been enabling myriad scientific breakthroughs in HP physics, chemistry, materials, and Earth and planetary sciences.

  11. High-pressure X-ray diffraction experiments on US using synchrotron radiation

    International Nuclear Information System (INIS)

    Olsen, J.S.; Steenstrup, S.

    1983-12-01

    High-pressure X-ray diffraction studies have been performed on US up to 40 GPa using synchrotron radiation and a diamond anvil cell. The measured value of the bulk modulus B 0 = 92 GPa is in reasonable agreement with calculations. The high-pressure behaviour indicates a phase transformation to US III at about 15 GPa. The transformation is a smooth deformation process, which starts with a tetragonal structure asub(tetr) = asub(cub)/√2, csub(tetr) = 2asub(cub) and continues with an orthorhombic structure with a = 375(3)pm, b = 345(3)pm, c = 1069 (24)pm at 35 GPa; it is of second order nature within experimental errors and it should involve some contributions from uranium f electrons. (orig.)

  12. High-pressure x-ray diffraction study on lithium borohydride using a synchrotron radiation

    Science.gov (United States)

    Nakano, S.; Nakayama, A.; Kikegawa, T.

    2008-07-01

    Lithium borohydride (LiBH4) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P42/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH4.

  13. High-pressure x-ray diffraction study on lithium borohydride using a synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Nakano, S [National Institute for Materials Science, Tsukuba, Ibaraki 305-0044 (Japan); Nakayama, A [Department of Materials Science and Engineering, Meijo University, Nagoya 468-8502 (Japan); Kikegawa, T [Photon Factory (PF), Institute of Materials Structure Science, High Energy Accelerator Research Organization (KEK), Ibaraki 305-0801 (Japan)], E-mail: NAKANO.Satoshi@nims.go.jp

    2008-07-15

    Lithium borohydride (LiBH{sub 4}) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P4{sub 2}/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH{sub 4}.

  14. Apparatus development for high-pressure X-ray diffraction using synchrotron radiation

    International Nuclear Information System (INIS)

    Martinez, L.G.; Orlando, M.T.D.; Rossi, J.L.; Passamai Junior, J.L.; Melo, F.C.L.; Ferreira, F.F.

    2006-01-01

    Some phenomena in the field of condensed matter physics can be studied when the matter is submitted to extreme conditions of pressure, magnetic fields or temperatures. Once submitted to these conditions it is generally necessary to measure the properties of the matter in situ. The existence of a synchrotron light laboratory in Brazil opens up the chance of studying materials in extreme conditions by techniques like X-ray diffraction and absorption. However, when compared to high-energy synchrotrons accelerators, the Brazilian source offers a narrower energy range and lower flux. These facts impose limitation to perform diffraction experiments by energy dispersion and, consequently, the use of pressure cells with denser anvils like diamond. However, for a lower-pressure range, preliminary studies showed the viability of measurements in an angular dispersion configuration. This allows the use of silicon carbide anvils B 4C . In this work it is described the development of a hydrostatic pressure cell suitable for X-rays diffraction measurements in the Brazilian Synchrotron Light Laboratory using materials and technologies developed by the institutions and researchers involved in this project (IPEN, UFES, CTA and LNLS). This development can provide the scientific community with the possibility of performing X-ray diffraction measurements under hydrostatic pressure, initially up to 2 GPa, with possibilities of increasing the maximum pressure to higher values, with or without application of magnetic fields and high or low temperatures. (author)

  15. High-pressure X-ray diffraction studies on ThS up to 40 GPa using synchrotron radiation

    International Nuclear Information System (INIS)

    Benedict, U.; Spirlet, J.C.; Gerward, L.; Olsen, J.S.

    1983-12-01

    High-pressure X-ray diffraction studies have been performed on ThS up to 40 GPa using synchrotron radiation and a diamond anvil cell. The measured value of the bulk modulus B 0 =145 GPa is in disagreement with a previous measurement. The high-pressure behaviour indicates a phase transformation to ThS II starting at 15 to 20 GPa. The transformation is of second order nature, the resulting structure can be described as distorted fcc. (orig.)

  16. High pressure X-ray diffraction studies on ThS up to 40 GPa using synchrotron radiation

    International Nuclear Information System (INIS)

    Benedict, U.; Spirlet, J.C.; Gerward, L.; Olsen, J.S.

    1984-01-01

    High pressure X-ray diffraction studies (up to 40 GPa) were performed on ThS using synchrotron radiation and a diamond anvil cell. The measured value of 145 GPa for the bulk modulus B 0 disagrees with a previous measurement. The high pressure behaviour indicates a phase transformation to ThS II starting at 15 - 20 GPa. The transformation is of the second-order type, and the resulting structure can be described as distorted f.c.c. (Auth.)

  17. Experimental in situ investigations of turbulence under high pressure.

    Science.gov (United States)

    Song, Kwonyul; Al-Salaymeh, Ahmed; Jovanovic, Jovan; Rauh, Cornelia; Delgado, Antonio

    2010-02-01

    In tube injection systems applied in high-pressure processing of packed biomaterials and foods, the pressure-transmitting medium is injected into the vessel to increase the pressure up to 1000 MPa, generating a submerged liquid-free jet. The presence of a turbulent-free jet during the pressurization phase and its positive influence on the homogeneity of the product treatment has already been examined by computational fluid dynamics investigations. However, no experimental data have supported the existence and properties of turbulent flow under high-pressure (HP) conditions up to 400 MPa. This contribution presents the development of two experimental setups: HP-laser Doppler anemometry and HP-hot wire anemometry. For the first time the time-averaged velocity profiles of a free jet during pressurization up to 300 MPa at different Reynolds numbers (Re) have been obtained. In this article, the dependence of the velocity profiles on the Re is discussed in detail. Moreover, the relaminarization phenomenon of the turbulent pipe flow most likely caused by the compressibility effects and viscosity changes of the pressure-transmitting medium is examined.

  18. 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

  19. In situ high-pressure measurement of crystal solubility by using neutron diffraction

    Science.gov (United States)

    Chen, Ji; Hu, Qiwei; Fang, Leiming; He, Duanwei; Chen, Xiping; Xie, Lei; Chen, Bo; Li, Xin; Ni, Xiaolin; Fan, Cong; Liang, Akun

    2018-05-01

    Crystal solubility is one of the most important thermo-physical properties and plays a key role in industrial applications, fundamental science, and geoscientific research. However, high-pressure in situ measurements of crystal solubility remain very challenging. Here, we present a method involving high-pressure neutron diffraction for making high-precision in situ measurements of crystal solubility as a function of pressure over a wide range of pressures. For these experiments, we designed a piston-cylinder cell with a large chamber volume for high-pressure neutron diffraction. The solution pressures are continuously monitored in situ based on the equation of state of the sample crystal. The solubility at a high pressure can be obtained by applying a Rietveld quantitative multiphase analysis. To evaluate the proposed method, we measured the high-pressure solubility of NaCl in water up to 610 MPa. At a low pressure, the results are consistent with the previous results measured ex situ. At a higher pressure, more reliable data could be provided by using an in situ high-pressure neutron diffraction method.

  20. A Synchrotron Mössbauer Spectroscopy Study of a Hydrated Iron-Sulfate at High Pressures

    Science.gov (United States)

    Perez, T. M.; Finkelstein, G. J.; Solomatova, N. V.; Jackson, J. M.

    2017-12-01

    Szomolnokite is a monohydrated ferrous iron sulfate mineral, FeSO4*H2O, where the ferrous iron atoms are in octahedral coordination with four corners shared with SO4 and two with H2O. While somewhat rare on Earth, szomolnokite has been detected on the surface of Mars along with several other hydrated sulfates and suggested to occur near the surface of Venus [1,2]. It is not clear if these sulfates are a result of reactions occurring at depth driven by changes in the behavior of iron in the sulfate. To date, only a few high-pressure studies have been conducted on hydrated iron sulfates using Mössbauer spectroscopy. Our study represents a first step towards understanding of the electronic environment of iron in a monohydrated sulfate at pressure. Using a hydrostatic helium pressure-transmitting medium, the pressure dependence of iron's site-specific behavior in a synthetic szomolnokite powdered sample was explored up to about 100 GPa with time-resolved synchrotron Mössbauer spectroscopy at the Advanced Photon Source of Argonne National Laboratory. At 1 bar, the Mössbauer spectrum is well described by three Fe2+-like sites, consistent with conventional Mössbauer spectra reported in Dyar et al. [3]. At pressures up to 20 GPa, changes in the hyperfine parameters are most likely due to a structural phase transition. Above this pressure, a fourth site is required to explain the time-spectra. Changes in the electronic configuration of iron, such as those due to a phase transition and/or a spin crossover, will affect the material's compressibility and transport properties. We will compare our high-pressure trends with those of other iron-bearing phases and discuss the relative influence on the dynamics of terrestrial planetary interiors. 1. Bishop et al. (2014) What Lurks in the Martian Rocks and Soil? Investigations of Sulfates, Phosphates, and Perchlorates. Spectral and thermal properties of perchlorate salts and implications for Mars. Am. Min. 99(8-9), 1580

  1. Time-resolved x-ray diffraction measurement of C60 under high pressure and temperature using synchrotron radiation

    International Nuclear Information System (INIS)

    Horikawa, T; Suito, K; Kobayashi, M; Onodera, A

    2002-01-01

    C 60 has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C 60 structure are presented and the relevance to the hardness of materials derived from C 60 is discussed

  2. EXAFS measurements under high pressure conditions using a combination of a diamond anvil cell and synchrotron radiation

    International Nuclear Information System (INIS)

    Sueno, Shigeho; Nakai, Izumi; Imafuku, Masayuki; Morikawa, Hideki; Kimata, Mitsuyoshi; Ohsumi, Kazumasa; Nomura, Masaharu; Shimomura, Osamu.

    1986-01-01

    EXAFS spectra for Fe, Co, Ni K-edges were successfully measured under high pressure conditions using a combination of a set of normal 1/8 carat diamond anvils, synchrotron radiation and a scintillation counter. A newly developed motor controlled goniometer stage was used for adjusting the position of a miniature diamond anvil cell. On the measurement of Cr and Mn spectra, specially designed thinner diamond anvil was necessary. EXAFS analysis of bis(dimethylglyoximato)nickel(II) at pressures from 1 atm to 5.6 GPa was made. (author)

  3. High-pressure phases of uranium monophosphide studied by synchrotron x-ray diffraction

    DEFF Research Database (Denmark)

    Olsen, J. Staun; Gerward, Leif; Benedict, U.

    1988-01-01

    X-ray diffraction studies have been performed on UP powder for pressures up to 51 GPa using synchrotron radiation and a diamond-anvil cell. At ambient pressure UP has the rocksalt structure. The bulk modulus has been determined to B0=102(4) GPa and its pressure derivative to B0’=4.0(8). The cubic...

  4. High pressure Moessbauer spectroscopy with nuclear resonant forward scattering of synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Nasu, Saburo [Osaka Univ., Toyonaka (Japan). Faculty of Engineering Science

    1996-04-01

    The first observation of the pressure-induced transition from the antiferromagnetic to the ferromagnetic SrFeO{sub 3} was succeeded by measuring Moessbauer spectroscopy under high pressure produced by the diamond anvil cell (DAC). Sample is a polycrystal powder of antiferromagnetic SrFe0{sub 3} with the Neel temperature T{sub N}=140 K, the cubic system and perovskite type crystal. The average pressures used were 44 GPa and 74 GPa (300 K). SrFeO{sub 3} is paramagnetic material at 300 K, but the Neel temperature increases more than 300 K under high pressure and the quantized axis turns to the external magnetic field, so that we take it as it means the system displaying the phase transition to the ferromagnet. By the method, we can practice the measurement at low and high temperature under the external magnetic field by using the polarized light source. (S.Y.)

  5. High pressure in-situ X-ray diffraction study on Zn-doped magnetite nanoparticles

    Science.gov (United States)

    Ferrari, S.; Bilovol, V.; Pampillo, L. G.; Grinblat, F.; Errandonea, D.

    2018-03-01

    We have performed high pressure synchrotron X-ray powder diffraction experiments on two different samples of Zn-doped magnetite nanoparticles (formula Fe(3-x)ZnxO4; x = 0.2, 0.5). The structural behavior of then a noparticles was studied up to 13.5 GPa for x = 0.2, and up to 17.4 GPa for x = 0.5. We have found that both systems remain in the cubic spinel structure as expected for this range of applied pressures. The analysis of the unit cell volume vs. pressure results in bulk modulus values lower than in both end-members, magnetite (Fe3O4) and zinc ferrite (ZnFe2O4), suggesting that chemical disorder may favor compressibility, which is expected to improve the increase of the Neel temperature under compression.

  6. High-pressure synchrotron x-ray diffraction and infrared microspectroscopy: applications to dense hydrous phases

    CERN Document Server

    Liu, Z; Yang, H; Mao Ho Kwang; Hemley, R J

    2002-01-01

    Synchrotron x-ray diffraction (XRD) and infrared (IR) absorption spectra of hydrous and 'anhydrous' forms of phase X were measured to 30 GPa at room temperature. Three OH stretching modes were found in the hydrous phase, and surprisingly one sharp OH mode was observed in the previously characterized anhydrous phase. All OH stretching modes soften and broaden with increasing pressure and become very weak above approx 20 GPa. XRD indicates that the crystal structure remains stable up to 30 GPa. Combining IR absorption and XRD results, the behaviour is attributed to pressure-induced distortion of the Si sub 2 O sub 7 groups and disorder of the hydrogen atoms. The bulk moduli of the hydrous and 'anhydrous' phases are in the region of 74 GPa.

  7. High pressure phases of uranium monophosphide studied by synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Staun Olson, J.; Gerward, L.; Benedict, U.; Dabos, S.; Vogt, O.

    1988-01-01

    X-ray diffraction studies have been performed on UP powder for pressures up to 51 GPa using synchrotron radiation and a diamond anvil cell. At ambient pressure UP has the rocksalt structure. The bulk modulus has been determined to B 0 = 102(4) GPa and its pressure derivative to B 0 ' = 4.0(8). The cubic phase has been found to transform to a new phase, UP II, at about 10 GPa. UP II can be characterized by a rhombohedral Bravais lattice. UP II transforms to an orthorhombic phase, UP III, at 28 GPa. No volume change has been observed at the two transitions. The influence of the 5f electrons on the transformations is discussed. (orig.)

  8. Experimental determination of bulk modulus of 14Å tobermorite using high pressure synchrotron X-ray diffraction

    KAUST Repository

    Oh, Jae Eun; Clark, Simon M.; Wenk, Hans-Rudolf; Monteiro, Paulo J.M.

    2012-01-01

    Using a diamond anvil cell, 14 Å tobermorite, a structural analogue of calcium silicate hydrates (C-S-H), was examined by high-pressure synchrotron X-ray diffraction up to 4.8 GPa under hydrostatic conditions. The bulk modulus of 14 Å tobermorite was calculated, K o = 47 GPa. Comparison of the current results with previous high pressure studies on C-S-H(I) indicates that: (1) the compression behavior of the lattice parameters a and b of 14 Å tobermorite and C-S-H(I) are very similar, implying that both materials may have very similar Ca-O layers, and also implying that an introduction of structural defects into the Ca-O layers may not substantially change in-plane incompressibility of the ab plane of 14 Å tobermorite; and (2) the bulk modulus values of 14 Å tobermorite and C-S-H(I) are dominated by the incompressibility of the lattice parameter c, which is directly related to the interlayer spacing composed of dreierketten silicate chains, interlayer Ca, and water molecules. © 2011 Elsevier Ltd. All rights reserved.

  9. Experimental determination of bulk modulus of 14Å tobermorite using high pressure synchrotron X-ray diffraction

    KAUST Repository

    Oh, Jae Eun

    2012-02-01

    Using a diamond anvil cell, 14 Å tobermorite, a structural analogue of calcium silicate hydrates (C-S-H), was examined by high-pressure synchrotron X-ray diffraction up to 4.8 GPa under hydrostatic conditions. The bulk modulus of 14 Å tobermorite was calculated, K o = 47 GPa. Comparison of the current results with previous high pressure studies on C-S-H(I) indicates that: (1) the compression behavior of the lattice parameters a and b of 14 Å tobermorite and C-S-H(I) are very similar, implying that both materials may have very similar Ca-O layers, and also implying that an introduction of structural defects into the Ca-O layers may not substantially change in-plane incompressibility of the ab plane of 14 Å tobermorite; and (2) the bulk modulus values of 14 Å tobermorite and C-S-H(I) are dominated by the incompressibility of the lattice parameter c, which is directly related to the interlayer spacing composed of dreierketten silicate chains, interlayer Ca, and water molecules. © 2011 Elsevier Ltd. All rights reserved.

  10. High Pressure In Situ X-ray Diffraction Study of MnO to 120 GPa and Comparison with Shock Compression Experiment

    Science.gov (United States)

    Yagi, Takehiko; Kondo, Tadashi; Syono, Yasuhiko

    1997-07-01

    In order to clarify the nature of the phase transformation in MnO observed at around 90 GPa by shock compression experiment (Syono et al., this symposium), high pressure in situ x-ray experiments were carried out up to 120 GPa. Powdered sample was directly compressed in Mao-Bell type diamond anvil and x-ray experiments were carried out using angle dispersive technique by combining synchrotron radiation and imaging plate detector. Distortion of the B1 structured phase into hexagonal unit cell was observed from 25-40 GPa, which continues to increase up to 90 GPa. At around 90 GPa, discontinuous change of the diffraction was observed. This new phase cannot be explained by a simple B2 structure and the analysis of this phase is in progress. This high pressure phase has metallic appearance, which reverses to transparent MnO on release of pressure.

  11. In Situ Observation of Gypsum-Anhydrite Transition at High Pressure and High Temperature

    Institute of Scientific and Technical Information of China (English)

    LIU Chuan-Jiang; ZHENG Hai-Fei

    2012-01-01

    An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC).The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 MPa.With increasing temperature,the anhydrite (CaSO4) phase precipitates at 250 320℃ in the pressure range of 1.0 1.5 GPa,indicating that under a saturated water condition,both stable conditions of pressure and temperature and high levels of Ca and SO4 ion concentrations in aqueous solution are essential for the formation of anhydrite.A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(GPa) =0.0068T - 0.7126 (250℃≤T≤320℃).Anhydrite remained stable during rapid cooling of the sample chamber,showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is irreversible at high pressure and high temperature.%An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC). The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 Mpa. With increasing temperature, the anhydrite (CaSO4) phase precipitates at 250-320℃ in the pressure range of 1.0-1.5 Gpa, indicating that under a saturated water condition, both stable conditions of pressure and temperature and high levels of Ca and SO4 ion concentrations in aqueous solution are essential for the formation of anhydrite. A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(Gpa) = 0.0068T - 0.7126 (250℃≤T≤320℃). Anhydrite remained stable during rapid cooling of the sample chamber, showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is

  12. In situ structural analysis of calcium aluminosilicate glasses under high pressure.

    Science.gov (United States)

    Muniz, R F; de Ligny, D; Martinet, C; Sandrini, M; Medina, A N; Rohling, J H; Baesso, M L; Lima, S M; Andrade, L H C; Guyot, Y

    2016-08-10

    In situ micro-Raman spectroscopy was used to investigate the structural evolution of OH(-)-free calcium aluminosilicate glasses, under high pressure and at room temperature. Evaluation was made of the role of the SiO2 concentration in percalcic join systems, for Al/(Al  +  Si) in the approximate range from 0.9 to 0.2. Under high pressure, the intensity of the main band related to the bending mode of bridging oxygen ([Formula: see text][T-O-T], where T  =  Si or Al) decreased gradually, suggesting that the bonds were severely altered or even destroyed. In Si-rich glasses, compression induced a transformation of Q (n) species to Q (n-1). In the case of Al-rich glass, the Al in the smallest Q (n) units evolved from tetrahedral to higher-coordinated Al (([5])Al and ([6])Al). Permanent structural changes were observed in samples recovered from the highest pressure of around 15 GPa and, particularly for Si-rich samples, the recovered structure showed an increase of three-membered rings in the Si/Al tetrahedral network.

  13. In Situ Observation of Gypsum-Anhydrite Transition at High Pressure and High Temperature

    International Nuclear Information System (INIS)

    Liu Chuan-Jiang; Zheng Hai-Fei

    2012-01-01

    An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC). The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 MPa. With increasing temperature, the anhydrite (CaSO 4 ) phase precipitates at 250–320°C in the pressure range of 1.0–1.5GPa, indicating that under a saturated water condition, both stable conditions of pressure and temperature and high levels of Ca and SO 4 ion concentrations in aqueous solution are essential for the formation of anhydrite. A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(GPa) = 0.0068T−0.7126 (250°C≤T≤320°C). Anhydrite remained stable during rapid cooling of the sample chamber, showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is irreversible at high pressure and high temperature. (geophysics, astronomy, and astrophysics)

  14. In situ detection of two-stage crystallization in ZrTiCuNiBe under high pressure and high temperature

    CERN Document Server

    Sun, L L; Wu, Q; Zhan, Z J; Cao, L M; Wang, L M; Shao, G J; Zhang, J; Wang, W K

    2002-01-01

    Structural changes in bulk metallic Zr sub 4 sub 1 sub . sub 2 Ti sub 1 sub 3 sub . sub 8 Cu sub 1 sub 2 sub . sub 5 Ni sub 1 sub 0 Be sub 2 sub 2 sub . sub 5 glass subjected to heat treatments under high pressure were investigated by means of synchrotron radiation x-ray diffraction (SRXRD). In situ SRXRD measurements showed that the crystallization process of this material is comprised of two stages. Subsequent heating at 10 GPa converts the sample from the amorphous (Am) phase into a metastable fcc phase and then leads to the fcc phase changing back to the Am phase, indicating that there is a kind of 'reversible' phase transition phenomenon occurring in the alloy. Such phenomenon is explained on the basis of free energy considerations.

  15. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    International Nuclear Information System (INIS)

    Prilliman, Gerald Stephen

    2003-01-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe 2 O 3 ) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the γ to the α structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the α structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced α phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the α phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition that must be overridden with pressure

  16. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Prilliman, Stephen Gerald [Univ. of California, Berkeley, CA (United States)

    2003-01-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe2O3) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the γ to the α structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the α structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced α phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the α phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition

  17. High pressure in situ X-ray diffraction study of MnO to 137 GPa and comparison with shock compression experiment

    Science.gov (United States)

    Yagi, T.; Kondo, T.; Syono, Y.

    1998-07-01

    In order to clarify the nature of the phase transformation in MnO observed at around 90 GPa by shock compression experiment, high pressure in situ X-ray observations were carried out up to 137 GPa. Powdered sample was directly compressed in Mao-Bell type diamond anvil cell and X-ray experiments were carried out using angle dispersive technique by combining synchrotron radiation and imaging plate detector. Distortion of the B1 structured phase was observed above about 40 GPa, which continues to increase up to 90 GPa. Two discontinuous changes of the diffraction profiles were observed at around 90 GPa and 120 GPa. The nature of the intermediate phase between 90 GPa and 120 GPa is not clear yet. It is neither cesium chloride (B2) nor nickel arsenide (B8) structure. On the other hand, the diffraction profile above 120 GPa can be reasonably well explained by the B8 structure. High pressure phases above 90 GPa have metallic luster and all the transformations are reversible on release of pressure.

  18. Time-resolved x-ray diffraction measurement of C{sub 60} under high pressure and temperature using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Horikawa, T [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Suito, K [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Kobayashi, M [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Onodera, A [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan)

    2002-11-11

    C{sub 60} has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C{sub 60} structure are presented and the relevance to the hardness of materials derived from C{sub 60} is discussed.

  19. In situ visualization of thermal distortions of synchrotron radiation optics

    International Nuclear Information System (INIS)

    Revesz, P.; Kazimirov, A.; Bazarov, I.

    2007-01-01

    We have developed a new in situ method to measure heating-induced distortions of the surface of the first monochromator crystal exposed to high-power white synchrotron radiation beam. The method is based on recording the image of a stationary grid of dots captured by a CCD camera as reflected from the surface of a crystal with and without a heat load. The three-dimensional surface profile (heat bump) is then reconstructed from the distortions of the original pattern. In experiments performed at the CHESS A2 wiggler beam line we measured the heat bumps with the heights of up to 600 nm produced by a wiggler beam with total power in the range of 15-60 W incident on the (1 1 1) Si crystal at various angles between 3 deg. and 15 deg

  20. X-ray diffraction at high pressure and high/low temperatures using synchrotron radiation. Applications in the study of spinel structures

    International Nuclear Information System (INIS)

    Gerward, L.; Jiang, J.Z.; Olsen, J.S.; Recio, J.M.; Wakowska, A.

    2004-01-01

    High-pressure x-ray diffraction made a quantum leap in the 1960's with the advent of the diamond-anvil cell. This ingenious device, where two opposing diamond faces apply pressure to a tiny sample, made it possible to replicate the pressure near the core of the Earth by turning a thumbscrew. Multianvil cells, such as the Japanese MAX80 press, were developed for combined high-pressure and high-temperature studies. The availability n at about the same time n of dedicated synchrotron radiation sources of hard x-rays was another big step forward. Since then, the white-beam energy-dispersive method has been the workhorse for high pressure, high-temperature x-ray diffraction, although it is now gradually being replaced by high-resolution monochromatic methods based on the image plate, the CCD camera or other electronic area detectors. The first part of the paper is a review of high-pressure x-ray diffraction (HPXRD), covering roughly the last three decades. Physical parameters, such as the bulk modulus, the compressibility and the equation of state, are defined. The diamond-anvil cell, the multianvil press and other high-pressure devices are described, as well as synchrotron radiation sources and recording techniques. Examples are drawn from current experimental and theoretical research on crystal structures of the spinel type. Accurate structural parameters have been determined at ambient conditions and at low temperatures using single-crystal diffraction and four-circle diffractometers. The uniform high-pressure behavior of the oxide spinels has been investigated in detail and compared with the corresponding behavior of selenium-based spinels. The synthesis of advanced novel materials is exemplified in the case of the cubic spinel Si 3 N 4 . This and other nitrogen spinels, which have a bulk modulus of about 300 GPa modulated by the actual cation, are opening a road towards superhard materials. The paper finishes off with an outlook into the future, where new

  1. In Situ Observations of Thermoreversible Gelation and Phase Separation of Agarose and Methylcellulose Solutions under High Pressure.

    Science.gov (United States)

    Kometani, Noritsugu; Tanabe, Masahiro; Su, Lei; Yang, Kun; Nishinari, Katsuyoshi

    2015-06-04

    Thermoreversible sol-gel transitions of agarose and methylcellulose (MC) aqueous solutions on isobaric cooling or heating under high pressure up to 400 MPa have been investigated by in situ observations of optical transmittance and falling-ball experiments. For agarose, which undergoes the gelation on cooling, the application of pressure caused a gradual rise in the cloud-point temperature over the whole pressure range examined, which is almost consistent with the pressure dependence of gelling temperature estimated by falling-ball experiments, suggesting that agarose gel is stabilized by compression and that the gelation occurs nearly in parallel with phase separation under ambient and high-pressure conditions. For MC, which undergoes the gelation on heating, the cloud-point temperature showed a slight rise with an initial elevation of pressure up to ∼150 MPa, whereas it showed a marked depression above 200 MPa. In contrast, the gelling temperature of MC, which is nearly identical to the cloud-point temperature at ambient pressure, showed a monotonous rise with increasing pressure up to 350 MPa, which means that MC undergoes phase separation prior to gelation on heating under high pressure above 200 MPa. Similar results were obtained for the melting process of MC gel on cooling. The unique behavior of the sol-gel transition of MC under high pressure has been interpreted in terms of the destruction of hydrophobic hydration by compression.

  2. Automated high-pressure titration system with in situ infrared spectroscopic detection

    International Nuclear Information System (INIS)

    Thompson, Christopher J.; Martin, Paul F.; Chen, Jeffrey; Schaef, Herbert T.; Rosso, Kevin M.; Felmy, Andrew R.; Loring, John S.; Benezeth, Pascale

    2014-01-01

    A fully automated titration system with infrared detection was developed for investigating interfacial chemistry at high pressures. The apparatus consists of a high-pressure fluid generation and delivery system coupled to a high-pressure cell with infrared optics. A manifold of electronically actuated valves is used to direct pressurized fluids into the cell. Precise reagent additions to the pressurized cell are made with calibrated tubing loops that are filled with reagent and placed in-line with the cell and a syringe pump. The cell's infrared optics facilitate both transmission and attenuated total reflection (ATR) measurements to monitor bulk-fluid composition and solid-surface phenomena such as adsorption, desorption, complexation, dissolution, and precipitation. Switching between the two measurement modes is accomplished with moveable mirrors that direct the light path of a Fourier transform infrared spectrometer into the cell along transmission or ATR light paths. The versatility of the high-pressure IR titration system was demonstrated with three case studies. First, we titrated water into supercritical CO 2 (scCO 2 ) to generate an infrared calibration curve and determine the solubility of water in CO 2 at 50 °C and 90 bar. Next, we characterized the partitioning of water between a montmorillonite clay and scCO 2 at 50 °C and 90 bar. Transmission-mode spectra were used to quantify changes in the clay's sorbed water concentration as a function of scCO 2 hydration, and ATR measurements provided insights into competitive residency of water and CO 2 on the clay surface and in the interlayer. Finally, we demonstrated how time-dependent studies can be conducted with the system by monitoring the carbonation reaction of forsterite (Mg 2 SiO 4 ) in water-bearing scCO 2 at 50 °C and 90 bar. Immediately after water dissolved in the scCO 2 , a thin film of adsorbed water formed on the mineral surface, and the film thickness increased with time as the

  3. Automated high-pressure titration system with in situ infrared spectroscopic detection

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Christopher J., E-mail: chris.thompson@pnnl.gov; Martin, Paul F.; Chen, Jeffrey; Schaef, Herbert T.; Rosso, Kevin M.; Felmy, Andrew R.; Loring, John S. [Pacific Northwest National Laboratory, Richland, Washington 99352 (United States); Benezeth, Pascale [Géosciences Environnement Toulouse (GET), CNRS-Université de Toulouse, 31400 Toulouse (France)

    2014-04-15

    A fully automated titration system with infrared detection was developed for investigating interfacial chemistry at high pressures. The apparatus consists of a high-pressure fluid generation and delivery system coupled to a high-pressure cell with infrared optics. A manifold of electronically actuated valves is used to direct pressurized fluids into the cell. Precise reagent additions to the pressurized cell are made with calibrated tubing loops that are filled with reagent and placed in-line with the cell and a syringe pump. The cell's infrared optics facilitate both transmission and attenuated total reflection (ATR) measurements to monitor bulk-fluid composition and solid-surface phenomena such as adsorption, desorption, complexation, dissolution, and precipitation. Switching between the two measurement modes is accomplished with moveable mirrors that direct the light path of a Fourier transform infrared spectrometer into the cell along transmission or ATR light paths. The versatility of the high-pressure IR titration system was demonstrated with three case studies. First, we titrated water into supercritical CO{sub 2} (scCO{sub 2}) to generate an infrared calibration curve and determine the solubility of water in CO{sub 2} at 50 °C and 90 bar. Next, we characterized the partitioning of water between a montmorillonite clay and scCO{sub 2} at 50 °C and 90 bar. Transmission-mode spectra were used to quantify changes in the clay's sorbed water concentration as a function of scCO{sub 2} hydration, and ATR measurements provided insights into competitive residency of water and CO{sub 2} on the clay surface and in the interlayer. Finally, we demonstrated how time-dependent studies can be conducted with the system by monitoring the carbonation reaction of forsterite (Mg{sub 2}SiO{sub 4}) in water-bearing scCO{sub 2} at 50 °C and 90 bar. Immediately after water dissolved in the scCO{sub 2}, a thin film of adsorbed water formed on the mineral surface

  4. In-situ study of the thermal properties of hydrate slurry by high pressure DSC

    Energy Technology Data Exchange (ETDEWEB)

    Sari, O.; Hu, J.; Brun, F.; Erbeau, N. [Institute of Thermal Engineering, University of Applied Sciences of Western Switzerland, Yverdon-les-Bains (Switzerland); Homsy, P. [Nestec, Vevey (Switzerland); Logel, J.-C. [Axima Refrigeration, Bischheim (France)

    2008-07-01

    Knowing the enthalpy of hydrate slurry is very essential for energy balance and industrial applications. No direct measurement processes had been developed in this field in the past time. A new experimental method with special device has been developed to carry out on-line measurement of the thermal properties for hydrate slurry under dynamic conditions. With this special device, it is possible to deliver the hydrate slurry to the high pressure DSC (Differential Scanning Calorimetry) directly from the production tank or pipes. Thermal data acquisition will be performed afterwards by DSC. The investigated conditions were at pressure of 30 bar and temperature of {approx}+7 {sup o}C. The dissociation enthalpy of CO{sub 2} hydrate slurry was about 54 kJ/kg, corresponding 10.8% of solid fraction. The on-line measurement results for CO{sub 2} hydrate slurry give a good tendency to apply this phase change slurry to the industrial refrigeration process. (author)

  5. Hydraulic High Pressure Valve Controller Using the In-Situ Pressure Difference

    Science.gov (United States)

    Bao, Xiaoqi (Inventor); Sherrit, Stewart (Inventor); Badescu, Mircea (Inventor); Bar-Cohen, Yoseph (Inventor); Hall, Jeffery L. (Inventor)

    2016-01-01

    A hydraulic valve controller that uses an existing pressure differential as some or all of the power source for valve operation. In a high pressure environment, such as downhole in an oil or gas well, the pressure differential between the inside of a pipe and the outside of the pipe may be adequately large to drive a linear slide valve. The valve is operated hydraulically by a piston in a bore. When a higher pressure is applied to one end of the bore and a lower pressure to the other end, the piston moves in response to the pressure differential and drives a valve attached to it. If the pressure differential is too small to drive the piston at a sufficiently high speed, a pump is provided to generate a larger pressure differential to be applied. The apparatus is conveniently constructed using multiport valves, which can be rotary valves.

  6. The thermal equation of state of FeTiO3 ilmenite based on in situ X-ray diffraction at high pressures and temperatures

    International Nuclear Information System (INIS)

    Tronche, E.J.; Van Kan Parker, M.; De Vries, J.; Wang, Y.; Sanehire, T.; Li, J.; Chen, B.; Gao, L.; Klemme, S.; McCammon, C.A.; Van Westerenen, W.

    2010-01-01

    We present in situ measurements of the unit-cell volume of a natural terrestrial ilmenite (Jagersfontein mine, South Africa) and a synthetic reduced ilmenite (FeTiO 3 ) at simultaneous high pressure and high temperature up to 16 GPa and 1273 K. Unit-cell volumes were determined using energy-dispersive synchrotron X-ray diffraction in a multi-anvil press. Moessbauer analyses show that the synthetic sample contained insignificant amounts of Fe 3+ both before and after the experiment. Results were fit to Birch-Murnaghan thermal equations of state, which reproduce the experimental data to within 0.5 and 0.7 GPa for the synthetic and natural samples, respectively. At ambient conditions, the unit-cell volume of the natural sample (V 0 = 314.75 ± 0.23 (1σ) (angstrom) 3 ) is significantly smaller than that of the synthetic sample (V 0 = 319.12 ± 0.26 (angstrom) 3 ). The difference can be attributed to the presence of impurities and Fe 3+ in the natural sample. The 1 bar isothermal bulk moduli K T0 for the reduced ilmenite is slightly larger than for the natural ilmenite (181 ± 7 and 165 ± 6 GPa, respectively), with pressure derivatives K(prime) 0 = 3 ± 1. Our results, combined with literature data, suggest that the unit-cell volume of reduced ilmenite is significantly larger than that of oxidized ilmenite, whereas their thermoelastic parameters are similar. Our data provide more appropriate input parameters for thermo-chemical models of lunar interior evolution, in which reduced ilmenite plays a critical role.

  7. Determination of the bulk modulus of hydroxycancrinite, a possible zeolitic precursor in geopolymers, by high-pressure synchrotron X-ray diffraction

    KAUST Repository

    Oh, Jae Eun

    2011-11-01

    Crystalline zeolitic materials, such as hydroxycancrinite, hydroxysodalite, herschelite and nepheline, are often synthesized from geopolymerization using fly-ash and solutions of NaOH at high temperatures. Comprised mainly of 6-membered aluminosilicate rings that act as basic building units, their crystal structures may provide insight into the reaction products formed in NaOH-activated fly ash-based geopolymers. Recent research indicates that the hydroxycancrinite and hydroxysodalite may play an important role as possible analogues of zeolitic precursor in geopolymers. Herein is reported a high pressure synchrotron study of the behavior of hydroxycancrinite exposed to pressures up to 6.1 GPa in order to obtain its bulk modulus. A refined equation of state for hydroxycancrinite yielded a bulk modulus of Ko = 46 ± 5 GPa (assuming Ko′ = 4.0) for a broad range of applied pressure. When low pressure values are excluded from the fit and only the range of 2.5 and 6.1 GPa is considered, the bulk modulus of hydroxycancrinite was found to be Ko = 46.9 ± 0.9 GPa (Ko′ = 4.0 ± 0.4, calculated). Comparison with the literature shows that all zeolitic materials possessing single 6-membered rings (i.e., hydroxycancrinite, sodalite and nepheline) have similar bulk moduli. © 2011 Elsevier Ltd. All rights reserved.

  8. In situ study starch gelatinization under ultra-high hydrostatic pressure using synchrotron SAXS

    KAUST Repository

    Yang, Zhi; Gu, Qinfen; Lam, Elisa; Tian, Feng; Chaieb, Saharoui; Hemar, Yacine

    2015-01-01

    The gelatinization of waxy (very low amylose) corn and potato starches by high hydrostatic pressure (HHP) (up to ∼1 GPa) was investigated in situ using synchrotron small-angle X-ray scattering (SAXS) on samples held in a diamond anvil cell (DAC

  9. Effects of high pressure on internally self-assembled lipid nanoparticles: a synchrotron small-angle X-ray scattering (SAXS) study

    Czech Academy of Sciences Publication Activity Database

    Kulkarni, C. V.; Yaghmur, A.; Steinhart, Miloš; Kriechbaum, M.; Rappolt, M.

    2016-01-01

    Roč. 32, č. 45 (2016), s. 11907-11917 ISSN 0743-7463 Institutional support: RVO:61389013 Keywords : self-assebled lipid nanoparticles * synchrotron * SAXS Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.833, year: 2016

  10. Ductile crack initiation and propagation assessed via in situ synchrotron radiation-computed laminography

    International Nuclear Information System (INIS)

    Morgeneyer, T.F.; Helfen, L.; Sinclair, I.; Proudhon, H.; Xu, F.; Baumbach, T.

    2011-01-01

    Ductile crack initiation and propagation within a naturally aged aluminium alloy sheet has been observed in situ via synchrotron radiation-computed laminography, a technique specifically adapted to three-dimensional imaging of thin objects that are laterally extended. Voids and intermetallic particles, and their subsequent evolution during ductile crack extension at different associated levels of stress triaxiality, were clearly observed within fracture coupons of a reasonable engineering length-scale, overcoming the conventional sample size limitation of computed tomography at high resolutions.

  11. High-Pressure and High-Temperature in situ X-Ray Diffraction Study of FeP2 up to 70 GPa

    International Nuclear Information System (INIS)

    Gu Ting-Ting; Wu Xiang; Qin Shan; Liu Jing; Li Yan-Chun; Zhang Yu-Feng

    2012-01-01

    The high-pressure and high-temperature structural behavior of FeP 2 is investigated by means of synchrotron x-ray powder diffraction combined with a laser heating technique up to 70 GPa and at least 1800 K. No phase transition of FeP 2 occurs up to 68 GPa at room temperature. While a new phase of FeP 2 assigned to the CuAl 2 -type structure (I4/mcm, Z = 4) is observed at 70 GPa after laser-heating. This new phase presents a quenchable property on decompression to ambient conditions. Our results update previous experimental data and are consistent with theoretical studies. (condensed matter: structure, mechanical and thermal properties)

  12. Synchrotron in-situ deformation experiments of perovskite + (Mg,Fe)O aggregates under shallow lower mantle conditions (Invited)

    Science.gov (United States)

    Girard, J.; Amulele, G.; Farla, R. J.; Liu, Z.; Mohiuddin, A.; Karato, S.

    2013-12-01

    Experimental studies on rheological properties of mantle's minerals are crucial to understand the dynamics of Earth's interior, but direct experimental studies under the relevant lower mantle conditions are challenging. Most of the earlier studies were performed at lower mantle pressures but low temperatures using DAC (diamond anvil cell) (e.g., Merkel et al., 2003)), and in DAC experiments strain-rate and stress are unknown. Some previous studies were carried out under high pressures and high temperatures (e.g, Cordier et al., 2004) , but quantitative results on rheological behaviour of said minerals were not obtained. Here we present the results of the first in-situ deformation experiments of perovskite + (Mg,Fe)O (Pv + fp) aggregates using RDA (rotational Drickamer apparatus). The RDA has a better support for the anvils at high pressure than the more commonly used D-DIA apparatus and hence we can reach higher pressures and temperatures than the D-DIA. We have recently made new modifications to the cell assembly to reach the lower mantle conditions with less interference in X-ray diffraction patterns by the surrounding materials. The starting material was ringwoodite synthesized using a multi-anvil. In-situ deformation experiments were then carried at pressure up to 28 GPa (calculated from thermal EOS of Pt) and estimated temperatures up to 2200 K using RDA. Under these conditions, ringwoodite transformed to Pv + fp. We subsequently deformed the sample between strain rates of 10-4 to 10-5 s-1. Stress and strain were measured in-situ using X-ray synchrotron beam. The recovered sample analyses show evidence of perovskite+(Mg,Fe)O microstructure (Fig. 1). The radial X-ray diffraction data are being analysed to determine the stress levels of two minerals. Also microstructures of deformed specimens are studied to understand the deformation mechanisms and strain partitioning. The results will contribute towards our understanding of the rheological properties of the

  13. Ultrafine grain formation in Mg–Zn alloy by in situ precipitation during high-pressure torsion

    International Nuclear Information System (INIS)

    Meng, Fanqiang; Rosalie, Julian M.; Singh, Alok; Somekawa, Hidetoshi; Tsuchiya, Koichi

    2014-01-01

    A ultrafine-grained structure was produced in a Mg–3.4Zn (at.%) alloy subjected to high-pressure torsion (HPT) at ambient temperature. Hardness and X-ray diffraction measurements indicated the microstructure reached a steady state after three revolutions. Transmission electron microscopy observations showed equiaxed, dynamically recrystallized grains with an average diameter of 140 nm after 20 revolutions, substantially less than the steady-state grain size in pure Mg deformed by HPT. This is attributed to the formation of precipitates during processing, which impedes the growth of recrystallized grains

  14. 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...

  15. In situ measurement of magnesium carbonate formation from CO2 using static high-pressure and -temperature 13C NMR.

    Science.gov (United States)

    Surface, J Andrew; Skemer, Philip; Hayes, Sophia E; Conradi, Mark S

    2013-01-02

    We explore a new in situ NMR spectroscopy method that possesses the ability to monitor the chemical evolution of supercritical CO(2) in relevant conditions for geological CO(2) sequestration. As a model, we use the fast reaction of the mineral brucite, Mg(OH)(2), with supercritical CO(2) (88 bar) in aqueous conditions at 80 °C. The in situ conversion of CO(2) into metastable and stable carbonates is observed throughout the reaction. After more than 58 h of reaction, the sample was depressurized and analyzed using in situ Raman spectroscopy, where the laser was focused on the undisturbed products through the glass reaction tube. Postreaction, ex situ analysis was performed on the extracted and dried products using Raman spectroscopy, powder X-ray diffraction, and magic-angle spinning (1)H-decoupled (13)C NMR. These separate methods of analysis confirmed a spatial dependence of products, possibly caused by a gradient of reactant availability, pH, and/or a reaction mechanism that involves first forming hydroxy-hydrated (basic, hydrated) carbonates that convert to the end-product, anhydrous magnesite. This carbonation reaction illustrates the importance of static (unmixed) reaction systems at sequestration-like conditions.

  16. In situ SAXS study on cationic and non-ionic surfactant liquid crystals using synchrotron radiation.

    Science.gov (United States)

    Fritscher, C; Hüsing, N; Bernstorff, S; Brandhuber, D; Koch, T; Seidler, S; Lichtenegger, H C

    2005-11-01

    In situ synchrotron small-angle X-ray scattering was used to investigate various surfactant/water systems with hexagonal and lamellar structures regarding their structural behaviour upon heating and cooling. Measurements of the non-ionic surfactant Triton X-45 (polyethylene glycol 4-tert-octylphenyl ether) at different surfactant concentrations show an alignment of the lamellar liquid-crystalline structure close to the wall of the glass capillaries and also a decrease in d-spacing following subsequent heating/cooling cycles. Additionally, samples were subjected to a weak magnetic field (0.3-0.7 T) during heating and cooling, but no influence of the magnetic field was observed.

  17. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  18. In-situ high-pressure measurements and detailed numerical predictions of the catalytic reactivity of methane over platinum

    Energy Technology Data Exchange (ETDEWEB)

    Reinke, M.; Mantzaras, I.; Schaeren, R.; Bombach, R.; Inauen, A.; Schenker, S.

    2003-03-01

    The catalytic reactivity of methane over platinum at pressures of up to 14 bar was evaluated with in-situ Raman measurements and detailed numerical predictions from two different heterogeneous chemical reaction schemes. The best agreement to the measurements was achieved with Deutschmann's reaction scheme that yielded the correct trend for the pressure dependence of the catalytic reactivity, although in absolute terms the reactivity was overpredicted. The catalytic reactivity was consistently underpredicted at all pressures with the reaction scheme of Vlachos. (author)

  19. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  20. Laser-induced incandescence (LII) diagnostic for in situ monitoring of nanoparticle synthesis in a high-pressure arc discharge

    Science.gov (United States)

    Yatom, Shurik; Vekselman, Vladislav; Mitrani, James; Stratton, Brentley; Raitses, Yevgeny; LaboratoryPlasma Nanosynthesis Team

    2016-10-01

    A DC arc discharge is commonly used for synthesis of carbon nanoparticles, including buckyballs, carbon nanotubes, and graphene flakes. In this work we show the first results of nanoparticles monitored during the arc discharge. The graphite electrode is vaporized by high current (60 A) in a buffer Helium gas leading to nanoparticle synthesis in a low temperature plasma. The arc was shown to oscillate, which can possibly influence the nano-synthesis. To visualize the nanoparticles in-situ we employ the LII technique. The nanoparticles with radii >50 nm, emerging from the arc area are heated with a short laser pulse and incandesce. The resulting radiation is captured with an ICCD camera, showing the location of the generated nanoparticles. The images of incandescence are studied together with temporally synchronized fast-framing imaging of C2 emission, to connect the dynamics of arc instabilities, C2 molecules concentration and nanoparticles. The time-resolved incandescence signal is analyzed with combination of ex-situ measurements of the synthesized nanoparticles and LII modeling, to provide the size distribution of produced nanoparticles. This work was supported by US Department of Energy, Office of Science, Basic Energy Sciences, Materials Sciences and Engineering Division.

  1. Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature

    Energy Technology Data Exchange (ETDEWEB)

    Miyagi, Lowell [Department of Geology and Geophysics, University of Utah, Salt Lake City, Utah 84112 (United States); Department of Earth Sciences, Montana State University, Bozeman, Montana 59717 (United States); Kanitpanyacharoen, Waruntorn; Kaercher, Pamela; Wenk, Hans-Rudolf; Alarcon, Eloisa Zepeda [Department of Earth and Planetary Science, University of California, Berkeley, California 94720 (United States); Raju, Selva Vennila [Advanced Light Source, Lawrence Berkeley Laboratory, Berkeley, California 94720 (United States); HiPSEC, Department of Physics, University of Nevada, Las Vegas, Nevada 89154 (United States); Knight, Jason; MacDowell, Alastair [Advanced Light Source, Lawrence Berkeley Laboratory, Berkeley, California 94720 (United States); Williams, Quentin [Department of Earth and Planetary Science, University of California, Santa Cruz, California 95064 (United States)

    2013-02-15

    To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate and optimize conditions for combined resistive and laser heating. For example, in Run1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg{sub 0.9}Fe{sub 0.1})O in Run3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.

  2. High pressure flow reactor for in situ X-ray absorption spectroscopy of catalysts in gas-liquid mixtures—A case study on gas and liquid phase activation of a Co-Mo/Al2O3 hydrodesulfurization catalyst

    NARCIS (Netherlands)

    van Haandel, L.; Hensen, E.J.M.; Weber, Th.

    2017-01-01

    An in situ characterization of heterogeneous catalysts under industrial operating conditions may involve high pressure and reactants in both the gas and the liquid phase. In this paper, we describe an in situ XAS flow reactor, which is suitable to operate under such conditions (pmax 20 bar, Tmax 350

  3. Evaluation of load case ''switch-off of the high pressure pump of the emergency core cooling system'', measures of verification and in situ-test

    International Nuclear Information System (INIS)

    Trobitz, M.; Mattheis, A.; Kerkhof, K.; Hippelein, K.; Hofstoetter, P.

    1998-01-01

    Within the framework of periodic safety inspection of the Gundremmingen power station (RWE-Bayernwerk - KRB II), the load collectives used for the design of safety-relevant systems and components were checked for their consistency with latest updates of the design basis. It was found that there was no analytical information or study available describing a particular process and its effects, namely switch-off of the high-pressure feedwater pump of the emergency core cooling system. The paper reports the work performed for closing the gap, including preparatory analyses, accompanying measures such as vibration measurements during plant shut-down, as well as the preparation and performance of the in-situ test. The experimental results and the comparative evaluation of calculated and experimental data are presented. (orig./CB) [de

  4. Platinum Iron Intermetallic Nanoparticles Supported on Carbon Formed In Situ by High-Pressure Pyrolysis for Efficient Oxygen Reduction

    DEFF Research Database (Denmark)

    Hu, Yang; Jensen, Jens Oluf; Zhang, Wei

    2016-01-01

    Carbon-supported PtFe alloy catalysts are synthesized by the one-step, high-temperature pyrolysis of Pt, Fe, and C precursors. As a result of the high temperature, the formed PtFe nanoparticles possess highly ordered, face-centered tetragonal, intermetallic structures with a mean size of ≈11.8 nm....... At 0.9 V versus the reversible hydrogen electrode, the PtFe nanoparticles show a 6.8 times higher specific activity than the reference Pt/C catalyst towards the oxygen reduction reaction (ORR) as well as excellent stability, most likely because of the durable intermetallic structure and the preleaching...... treatment of the catalyst. During these preliminary syntheses, we found that a portion of the PtFe nanoparticles is buried in the in situ formed carbon phase, which limits Pt utilization in the catalyst and results in a mass-specific activity equivalent to the commercial Pt/C catalyst. Moreover...

  5. Small-angle x-ray scattering and density measurements of liquid Se50-Te50 mixture at high temperatures and high pressures using synchrotron radiation

    International Nuclear Information System (INIS)

    Kajihara, Y; Inui, M; Matsuda, K; Tomioka, Y

    2010-01-01

    We have carried out small-angle x-ray scattering and x-ray transmission measurements of liquid Se 50 -Te 50 mixture at SPring-8 in Japan and obtained the structure factor S(Q) at small-Q region (0.6 -1 ) and the density at high temperatures and high pressures up to 1000 0 C and 180 MPa. We report preliminary results in this paper. With increasing temperature, the density shows a minimum at around 500 0 C and a maximum at around 700 0 C. On the other hand, S(0) becomes maximum and S(Q) strongly depends on Q at around 600 0 C, which is about the middle temperature where the density shows the minimum and maximum. The temperatures shift to lower side when the pressure increases. These results prove that, with increasing temperature, the sample exhibits gradual transition from low-density structure to high-density structure, which causes mesoscopic density fluctuations in the intermediate temperature region.

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

    DEFF Research Database (Denmark)

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

    2015-01-01

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

  7. In situ observations of solidification processes in γ-TiAl alloys by synchrotron radiation

    International Nuclear Information System (INIS)

    Shuleshova, Olga; Holland-Moritz, Dirk; Loeser, Wolfgang; Voss, Andrea; Hartmann, Helena; Hecht, Ulrike; Witusiewicz, Victor T.; Herlach, Dieter M.; Buechner, Bernd

    2010-01-01

    In situ observations of phase transformations involving melts are performed using energy-dispersive diffraction of synchrotron X-rays on electromagnetically levitated γ-TiAl alloys containing Nb. The determined primary solidification modes, confirmed by microstructure analysis, delivered new reliable data about the boundary of the α(Ti) solidification domain, which differs in the various Ti-Al-Nb phase diagram descriptions. These data have been used for a reassessment of the thermodynamic database of the ternary Ti-Al-Nb system. The new description realistically reflects the experimental findings. Liquidus and solidus temperatures determined by the pyrometric method agree fairly well with the calculated values. Direct experimental information on the nature of the reactions along the univariant lines is provided.

  8. In-situ shearing interferometry of National Synchrotron Light Source mirrors

    International Nuclear Information System (INIS)

    Qian, S.N.; Rarback, H.; Shu, D.; Takacs, P.Z.

    1987-01-01

    In situ mirror distortion measurements were made with a lateral shearing interferometer on three mirrors in beam line X17T at the National Syn203hrotron Light Source. Lateral shearing interference is insensitive to vibrational motion in five of the six degrees of freedom, so it is well-suited for investigations in the synchrotron radiation (SR) environment. No distortion was seen in an uncooled silicon carbide mirror and in a colled copper alloy mirror on X17TB, but a change in the radius of an uncooled electroless nickel-plated aluminium cylinder mirror of about 6.2% was observed on X17TA. Angular vibrations in the 2 to 3 arc second range were easily observed on one of the beam lines, as was an overall mirror rotation in the arc second range

  9. Methodology for in situ synchrotron X-ray studies in the laser-heated diamond anvil cell

    DEFF Research Database (Denmark)

    Mezouar, M.; Giampaoli, R.; Garbarino, G.

    2017-01-01

    A review of some important technical challenges related to in situ diamond anvil cell laser heating experimentation at synchrotron X-ray sources is presented. The problem of potential chemical reactions between the sample and the pressure medium or the carbon from the diamond anvils is illustrated...

  10. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chakraborty, R., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu [Department of Mechanical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); West, B.; Stuckelberger, M.; Bertoni, M. I. [School of Electrical, Computer and Energy Engineering, Arizona State University, Tempe, Arizona 85287 (United States); Lai, B.; Maser, J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2015-11-15

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H{sub 2}Se and H{sub 2}S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn{sub x}Ga{sub 1−x}Se{sub 2} (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25–400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  11. High pressure and high temperature EXAFS and diffraction study of AgI

    International Nuclear Information System (INIS)

    Yoshiasa, Akira; Arima, Hiroshi; Fukui, Hiroshi; Okube, Maki; Katayama, Yoshinori; Ohtaka, Osamu

    2009-01-01

    We have determined the precise P-T phase diagram of AgI by in-situ high-pressure high-temperature synchrotron experiments. X-ray diffraction and XAFS measurements were performed up to 6.0 GPa and 1100 K using a multi-anvil high-pressure device and synchrotron radiation from SPring-8. In the disordered rock-salt phase, Ag ions occupy both octahedral and tetrahedral sites and twenty percent of Ag ions occupy the tetrahedral site as a maximum value at 2 GPa. From the viewpoint of the local structure analyses, some sudden changes are recognized near broad phase transition point. Analysis of EXAFS Debye-Waller factor is useful because the force constant can be decided directly even at high pressure and high temperature. Pressure influences greatly the effective potential and anharmonicity decreases with increasing pressure. (author)

  12. Dynamics of barite growth in porous media quantified by in situ synchrotron X-ray tomography

    Science.gov (United States)

    Godinho, jose; Gerke, kirill

    2016-04-01

    Current models used to formulate mineral sequestration strategies of dissolved contaminants in the bedrock often neglect the effect of confinement and the variation of reactive surface area with time. In this work, in situ synchrotron X-ray micro-tomography is used to quantify barite growth rates in a micro-porous structure as a function of time during 13.5 hours with a resolution of 1 μm. Additionally, the 3D porous network at different time frames are used to simulate the flow velocities and calculate the permeability evolution during the experiment. The kinetics of barite growth under porous confinement is compared with the kinetics of barite growth on free surfaces in the same fluid composition. Results are discussed in terms of surface area normalization and the evolution of flow velocities as crystals fill the porous structure. During the initial hours the growth rate measured in porous media is similar to the growth rate on free surfaces. However, as the thinner flow paths clog the growth rate progressively decreases, which is correlated to a decrease of local flow velocity. The largest pores remain open, enabling growth to continue throughout the structure. Quantifying the dynamics of mineral precipitation kinetics in situ in 4D, has revealed the importance of using a time dependent reactive surface area and accounting for the local properties of the porous network, when formulating predictive models of mineral precipitation in porous media.

  13. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

    Energy Technology Data Exchange (ETDEWEB)

    Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik (Hull)

    2014-12-11

    Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

  14. In situ study starch gelatinization under ultra-high hydrostatic pressure using synchrotron SAXS

    KAUST Repository

    Yang, Zhi

    2015-12-13

    The gelatinization of waxy (very low amylose) corn and potato starches by high hydrostatic pressure (HHP) (up to ∼1 GPa) was investigated in situ using synchrotron small-angle X-ray scattering (SAXS) on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio (by weight), were pressurized and measured at room temperature. During HHP, both SAXS peak areas (corresponding to the lamellar phase) of waxy corn and potato starches decreased suggesting the starch gelatinization increases with increasing pressure. As pressure increased, lamellar peak broadened and the power law exponent increased in low q region. 1D linear correlation function was further employed to analyse SAXS data. For both waxy potato and waxy corn starches, the long period length and the average thickness of amorphous layers decreased when the pressure increased. While for both of waxy starches, the thickness of the crystalline layer first increased, then decreased when the pressure increased. The former is probably due to the out-phasing of starch molecules, and the latter is due to the water penetrating into the crystalline region during gelatinization and to pressure induced compression.

  15. In situ synchrotron XRD analysis of the kinetics of spodumene phase transitions.

    Science.gov (United States)

    L Moore, Radhika; Mann, Jason P; Montoya, Alejandro; Haynes, Brian S

    2018-04-25

    The phase transition by thermal activation of natural α-spodumene was followed by in situ synchrotron XRD in the temperature range 896 to 940 °C. We observed both β- and γ-spodumene as primary products in approximately equal proportions. The rate of the α-spodumene inversion is first order and highly sensitive to temperature (apparent activation energy ∼800 kJ mol-1). The γ-spodumene product is itself metastable, forming β-spodumene, with the total product mass fraction ratio fγ/fβ decreasing as the conversion of α-spodumene continues. We found the relationship between the product yields and the degree of conversion of α-spodumene to be the same at all temperatures in the range studied. A model incorporating first order kinetics of the α- and γ-phase inversions with invariant rate constant ratio describes the results accurately. Theoretical phonon analysis of the three phases indicates that the γ phase contains crystallographic instabilities, whilst the α and β phases do not.

  16. In situ observation of rolling contact fatigue cracks by laminography using ultrabright synchrotron radiation

    Directory of Open Access Journals (Sweden)

    Y. Nakai

    2015-10-01

    Full Text Available In rolling contact fatigue (RCF, cracks usually initiate from inclusions beneath the surface and propagate to the contact surface. In the present study, synchrotron radiation computed laminography (SRCL imaging was performed to observe flaking defects during the RCF of a high-strength steel. Specially fabricated inclusion-rich steel plate specimens were employed in the experiments. For the in situ observation of crack propagation, a compact RCF testing machine was developed, and a 4D analysis scheme was applied to the data obtained by SRCL. RCF tests were carried out near the measurement hatch of the beam line used SRCL to enable the successive observation of crack initiation and growth behaviors. Specimens before and after the occurrence of flaking were observed by SRCL, and flaking defects and cracks under the surface were successfully detected. As a result, details of the crack initiation and flaking process in RCF could be discussed. Shear-type horizontal cracks were found to initiate after the initiation and propagation of tensile-type vertical cracks along inclusions, where the face of the vertical cracks was perpendicular to the rolling direction and rolling surface. Therefore, the formation of vertical cracks is considered to affect shear-type crack formation and flaking, where the shape and length of inclusions also affect the initiation and propagation of vertical cracks.

  17. Synchrotron radiation microbeam X-ray fluorescence analysis of zinc concentration in remineralized enamel in situ.

    Science.gov (United States)

    Matsunaga, Tsunenori; Ishizaki, Hidetaka; Tanabe, Shuji; Hayashi, Yoshihiko

    2009-05-01

    Remineralization is an indispensable phenomenon during the natural healing process of enamel decay. The incorporation of zinc (Zn) into enamel crystal could accelerate this remineralization. The present study was designed to investigate the concentration and distribution of Zn in remineralized enamel after gum chewing. The experiment was performed at the Photon Factory. Synchrotron radiation was monochromatized and X-rays were focused into a small beam spot. The X-ray fluorescence (XRF) from the sample was detected with a silicon (Si) (lithium (Li)) detector. X-ray beam energy was tuned to detect Zn. The examined samples were small enamel fragments remineralized after chewing calcium phosphate-containing gum in situ. The incorporation of Zn atom into hydroxyapatite (OHAP), the main component of enamel, was measured using Zn K-edge extended X-ray absorption fine structure (EXAFS) with fluorescence mode at the SPring-8. A high concentration of Zn was detected in a superficial area 10-microm deep of the sectioned enamel after gum chewing. This concentration increased over that in the intact enamel. The atomic distance between Zn and O in the enamel was calculated using the EXAFS data. The analyzed atomic distances between Zn and O in two sections were 0.237 and 0.240 nm. The present experiments suggest that Zn is effectively incorporated into remineralized enamel through the physiological processes of mineral deposition in the oral cavity through gum-chewing and that Zn substitution probably occurred at the calcium position in enamel hydroxyapatite.

  18. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    Energy Technology Data Exchange (ETDEWEB)

    Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

    2017-04-15

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

  19. In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy

    Data.gov (United States)

    U.S. Environmental Protection Agency — In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy showing spectral fitting and linear...

  20. In Situ XRD Studies of ZnO/GaN Mixtures at High Pressure and High Temperature: Synthesis of Zn-Rich (Ga1-xZnx)(N1-xOx) Photocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, J.A.; Chen, H.; Wang, L.; Bai, J.; Hanson, J.C.; Warren, J.B.; Muckerman, J.T.; Fujita, E.

    2010-02-04

    The high-pressure, high-temperature conditions for the synthesis of Zn-rich (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions from mixtures of ZnO/GaN were explored using synchrotron-based in situ time-resolved X-ray diffraction (XRD). Following a new synthetic path, (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a Zn content up to 75% were prepared for the first time. The structures of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions were characterized by XRD and X-ray absorption fine structure (XAFS) analyses and were in excellent agreement with the predictions of density functional calculations. These materials adopt a wurtzite crystal structure with metal-N or metal-O bond distances in the range of 1.95-1.98 {angstrom}. Although the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions seem to be stable over the full range of compositions, no ideal solid solution formation was observed. In all cases, the lattice parameters were larger than those of ideal solid solutions. The variation of the lattice parameter c showed an upward double bowing curve, as was predicted by theoretical calculations. Also, no ideal behavior was observed in the electronic properties of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions. X-ray absorption spectra at the Zn and Ga K-edges of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) systems showed significant electronic perturbations with respect to ZnO and GaN. The synthesized (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solution with a Zn content of 50% displayed the ability to absorb visible light well above 500 nm. This material has a great potential for splitting water under visible light irradiation. The availability of (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a high Zn content opens the door to fully explore the application of these materials in photocatalysis.

  1. In Situ XRD Studies of ZnO/GaN Mixtures at High Pressure and High Temperature: Synthesis of Zn-Rich (Ga1-xZnx)(N1-xOx) Photocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Chen, H.; Wang, L; Bai, J; Hanson, J; Warren, J; Muckerman, J; Fujita, E; Rodriguez, J

    2010-01-01

    The high-pressure, high-temperature conditions for the synthesis of Zn-rich (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions from mixtures of ZnO/GaN were explored using synchrotron-based in situ time-resolved X-ray diffraction (XRD). Following a new synthetic path, (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a Zn content up to {approx}75% were prepared for the first time. The structures of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions were characterized by XRD and X-ray absorption fine structure (XAFS) analyses and were in excellent agreement with the predictions of density functional calculations. These materials adopt a wurtzite crystal structure with metal-N or metal-O bond distances in the range of 1.95-1.98 {angstrom}. Although the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions seem to be stable over the full range of compositions, no ideal solid solution formation was observed. In all cases, the lattice parameters were larger than those of ideal solid solutions. The variation of the lattice parameter c showed an upward double bowing curve, as was predicted by theoretical calculations. Also, no ideal behavior was observed in the electronic properties of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions. X-ray absorption spectra at the Zn and Ga K-edges of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) systems showed significant electronic perturbations with respect to ZnO and GaN. The synthesized (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solution with a Zn content of 50% displayed the ability to absorb visible light well above 500 nm. This material has a great potential for splitting water under visible light irradiation. The availability of (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a high Zn content opens the door to fully explore the application of these materials in photocatalysis.

  2. An in situ synchrotron X-ray diffraction study of precipitation kinetics in a severely deformed Cu–Ni–Si alloy

    Energy Technology Data Exchange (ETDEWEB)

    Azzeddine, H.; Mehdi, B. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Hennet, L. [Conditions Extrêmes et Matériaux: Haute Température et Irradiation, CNRS-CEMHTI, 1D Ave de la Recherche Scientifique, 45071 Orléans Cedex 2 (France); Thiaudière, D. [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, 91192 Gif-sur-Yvette Cedex (France); Alili, B. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Kawasaki, M., E-mail: megumi@hanyang.ac.kr [Division of Materials Science and Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Departments of Aerospace and Mechanical Engineering and Materials Science, University of Southern California, Los Angeles, CA 90089-1453 (United States); Bradai, D. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Langdon, T.G. [Departments of Aerospace and Mechanical Engineering and Materials Science, University of Southern California, Los Angeles, CA 90089-1453 (United States); Materials Research Group, Faculty of Engineering and the Environment, University of Southampton, Southampton SO17 1BJ (United Kingdom)

    2014-03-01

    In situ synchrotron X-ray diffraction was used to study the decomposition kinetics of a metastable Cu–2.5Ni–0.6Si (wt%) alloy after severe plastic deformation by equal-channel angular pressing (ECAP) and high-pressure torsion (HPT). The measurements were performed at room temperature and also at high temperatures of 723, 823 and 973 K in order to determine the ageing effect after processing. Two forms of precipitates, namely δ-Ni{sub 2}Si and γ-Ni{sub 5}Si{sub 2}, were identified and the sequence of their appearance was well established for ECAP processing and ageing. There was no detection of either a modulated structure resulting from spinodal decomposition or an ordered structure nucleated from the modulated structure. An X-ray hybrid pixel array detector (XPAD-S140 detector) permitted the detection of the nucleation stages of the δ-Ni{sub 2}Si phase that began soon after 24 s of ageing at 723 K. There was also no trace of any amorphization of the matrix phase.

  3. Sample environment for in situ synchrotron XRD measurements for CO2 interaction with subsurface materials

    Science.gov (United States)

    Elbakhshwan, M.; Gill, S.; Weidner, R.; Ecker, L.

    2017-12-01

    Sequestration of CO2 in geological formations requires a deep understanding of its interaction with the cement-casing components in the depleted oil and gas wells. Portland cement is used to seal the wellbores; however it tends to interact with the CO2. Therefore it is critical to investigate the wellbore integrity over long term exposure to CO2. Studies showed that, CO2 leakage is due to the flow through the casing-cement microannulus, cement-cement fractures, or the cement-caprock interface. The objective of this work is to gain a better understanding of the dissolution process of the cement-casing in the CO2 flow channels alongside with the carbonation reactions at the interfaces using XRF, XANES and X-ray tomography techniques. In this study, a synthetic wellbore system, consisting of cement with an embedded rectangular length of steel casing that had grooves to accommodate fluid flow, was used to investigate the casing-cement microannulus through core-flood experiments. The objective of this work is to gain a better understanding of the dissolution process of the cement-casing in the CO2 flow channels alongside with the carbonation reactions at the interfaces using a sample environment designed and built for in situ X-ray diffraction in the National Synchrotron Light Source II (NSLS II). The formation of carbonate phases at cement -fluid and cement-steel/fluid interfaces will be monitored in real time. Samples may be exposed to super critical CO2 at pressures above 1100 psi and temperatures around 50°C. The reaction cell is built from hastealloy to provide corrosion resistance, while the experimental temperature and pressure are controlled with thermocouples and pressure vessel.

  4. Investigation of CaO-CO₂ reaction kinetics by in-situ XRD using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Biasin, A.; Segre, C. U.; Salviulo, G.; Zorzi, F.; Strumendo, M. [Padova; (IIT)

    2015-02-05

    In this work, in-situ synchrotron radiation x-ray powder diffraction (SR-XRPD), performed at the Advanced Photon Source (APS) facilities of the Argonne National Laboratory, was applied to investigate the CaO–CO2 reaction. A set of CO2 absorption experiments were conducted in a high temperature reaction capillary with a controlled atmosphere (CO2 partial pressure of 1 bar), in the temperature range between 450 °C and 750 °C using CaO based sorbents obtained by calcination of commercial calcium carbonate. The evolution of the crystalline phases during CO2 uptake by the CaO solid sorbents was monitored for a carbonation time of 20 min as a function of the carbonation temperature and of the calcination conditions. The Rietveld refinement method was applied to estimate the calcium oxide conversion during the reaction progress and the average size of the initial (at the beginning of carbonation) calcium oxide crystallites. The measured average initial carbonation rate (in terms of conversion time derivative) of 0.280 s-1 (±13.2% standard deviation) is significantly higher than the values obtained by thermo-gravimetric analysis and reported thus far in the literature. Additionally, a dependence of the conversion versus time curves on the initial calcium oxide crystallite size was observed and a linear relationship between the initial CaO crystallite size and the calcium oxide final conversion was identified.

  5. In situ synchrotron diffraction of lead-zirconate-titanate at its morphotropic phase boundary

    International Nuclear Information System (INIS)

    Schoenau, K.A.

    2008-01-01

    Ferroelectric lead zirconate titanate ceramics (PZT,Pb(Zr x Ti 1-x )O 3 ) find in industry intensifiedly applications as piezoactors. Their largest macroscopic strain under electric field they show in the region of the morphotropic phase boundary (MPB), the transition region between the Ti rich tetragonal and the Zr rich structure. The structure of PZT at the MPB was controversially discussed since the detection of a monoclinic intermediate phase by Noheda et al. [Appl. Phys. Lett.,74(14), 2059(1999)], whereby into the considerations the domain structure of the material not entered, which however is essentially responsible for the reaction under electric field. In order to understand the domain structure of PZT under electric field and to study possible causes for the fatigue behaviour of the material under bipolar cycling a bridge must be built between macroscopic and local structure. For this at the measuring place B2 of the Hasylab, Hamburg, synchrotron X-ray powder diffractometry was in situ performed under different sample environments in transmission geometry, which was correlated with transmission-electron-microscopical studies and electron spin resonance. Samples with compositions over the whole MPB were beside temperature-dependent measurements measured at room temperature in high resolution and under applied electric field. Furthermore for studies under electric field at elevated temperatures a special E-field furnace was constructed. It could be shown the large piezoelectric reaction of PZT at its MPB is strongly correlated with a diminishment of the domain structure, which simulates in X-ray diffraction a lower symmetric phase. The stability range of the nanodomains with temperature and electric field reflects in the switching behaviour of the matter and by the detection of a relaxor behavior of the nanodomain structure for the first time a direct comparison with relaxoceramics is possible. The varying stress conditions within the sample influence

  6. Visualizing and measuring flow in shale matrix using in situ synchrotron X-ray microtomography

    Science.gov (United States)

    Kohli, A. H.; Kiss, A. M.; Kovscek, A. R.; Bargar, J.

    2017-12-01

    Natural gas production via hydraulic fracturing of shale has proliferated on a global scale, yet recovery factors remain low because production strategies are not based on the physics of flow in shale reservoirs. In particular, the physical mechanisms and time scales of depletion from the matrix into the simulated fracture network are not well understood, limiting the potential to optimize operations and reduce environmental impacts. Studying matrix flow is challenging because shale is heterogeneous and has porosity from the μm- to nm-scale. Characterizing nm-scale flow paths requires electron microscopy but the limited field of view does not capture the connectivity and heterogeneity observed at the mm-scale. Therefore, pore-scale models must link to larger volumes to simulate flow on the reservoir-scale. Upscaled models must honor the physics of flow, but at present there is a gap between cm-scale experiments and μm-scale simulations based on ex situ image data. To address this gap, we developed a synchrotron X-ray microscope with an in situ cell to simultaneously visualize and measure flow. We perform coupled flow and microtomography experiments on mm-scale samples from the Barnett, Eagle Ford and Marcellus reservoirs. We measure permeability at various pressures via the pulse-decay method to quantify effective stress dependence and the relative contributions of advective and diffusive mechanisms. Images at each pressure step document how microfractures, interparticle pores, and organic matter change with effective stress. Linking changes in the pore network to flow measurements motivates a physical model for depletion. To directly visualize flow, we measure imbibition rates using inert, high atomic number gases and image periodically with monochromatic beam. By imaging above/below X-ray adsorption edges, we magnify the signal of gas saturation in μm-scale porosity and nm-scale, sub-voxel features. Comparing vacuumed and saturated states yields image

  7. 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...

  8. Solids, liquids, and gases under high pressure

    Science.gov (United States)

    Mao, Ho-Kwang; Chen, Xiao-Jia; Ding, Yang; Li, Bing; Wang, Lin

    2018-01-01

    Pressure has long been recognized as a fundamental thermodynamic variable but its application was previously limited by the available pressure vessels and probes. The development of megabar diamond anvil cells and a battery of associated in-laboratory and synchrotron techniques at the turn of the century have opened a vast new window of opportunities. With the addition of the pressure dimension, we are facing a new world with an order of magnitude more materials to be discovered than all that have been explored at ambient pressure. Pressure drastically and categorically alters all elastic, electronic, magnetic, structural, and chemical properties, and pushes materials across conventional barriers between insulators and superconductors, amorphous and crystalline solids, ionic and covalent compounds, vigorously reactive and inert chemicals, etc. In the process, it reveals surprising high-pressure physics and chemistry and creates novel materials. This review describes the principles and methodology used to reach ultrahigh static pressure: the in situ probes, the physical phenomena to be investigated, the long-pursued goals, the surprising discoveries, and the vast potential opportunities. Exciting examples include the quest for metallic hydrogen, the record-breaking superconducting temperature of 203 K in HnS , the complication of "free-electron gas" alkali metals, the magnetic collapse in 3 d transition elements, the pressure-induced superconductivity from topological insulators, the novel stoichiometry in simple compounds, the interaction of nanoscience, the accomplishment of 750 GPa pressure, etc. These highlights are the integral results of technological achievements, specific measurements, and theoretical advancement; therefore, the same highlights will appear in different sections corresponding to these different aspects. Overall, this review demonstrates that high-pressure research is a new dimension in condensed-matter physics.

  9. High pressure phase transitions and compressibilities of Er2Zr2O7 and Ho2Zr2O7

    Science.gov (United States)

    Zhang, F. X.; Lang, M.; Becker, U.; Ewing, R. C.; Lian, J.

    2008-01-01

    Phase stability and compressibility of rare earth zirconates with the defect-fluorite structure were investigated by in situ synchrotron x-ray diffraction. A sluggish defect-fluorite to a cotunnitelike phase transformation occurred at pressures of ˜22 and ˜30GPa for Er2Zr2O7 and Ho2Zr2O7, respectively. Enhanced compressibility was found for the high pressure phase as a result of increasing cation coordination number and cation-anion bond length.

  10. High Pressure Phase Transitions and Compressibilities of Er2Zr2O7 and Ho2Zr2O7

    Energy Technology Data Exchange (ETDEWEB)

    Zhang,F.; Lang, M.; Becker, U.; Ewing, R.; Lian, J.

    2008-01-01

    Phase stability and compressibility of rare earth zirconates with the defect-fluorite structure were investigated by in situ synchrotron x-ray diffraction. A sluggish defect-fluorite to a cotunnitelike phase transformation occurred at pressures of {approx} 22 and {approx} 30 GPa for Er2Zr2O7 and Ho2Zr2O7, respectively. Enhanced compressibility was found for the high pressure phase as a result of increasing cation coordination number and cation-anion bond length.

  11. Structural phase transition of BaZrO3 under high pressure

    International Nuclear Information System (INIS)

    Yang, Xue; Li, Quanjun; Liu, Ran; Liu, Bo; Zhang, Huafang; Jiang, Shuqing; Zou, Bo; Cui, Tian; Liu, Bingbing; Liu, Jing

    2014-01-01

    We studied the phase transition behavior of cubic BaZrO 3 perovskite by in situ high pressure synchrotron X-ray diffraction experiments up to 46.4 GPa at room temperature. The phase transition from cubic phase to tetragonal phase was observed in BaZrO 3 for the first time, which takes place at 17.2 GPa. A bulk modulus 189 (26) GPa for cubic BaZrO 3 is derived from the pressure–volume data. Upon decompression, the high pressure phase transforms into the initial cubic phase. It is suggested that the unstable phonon mode caused by the rotation of oxygen octahedra plays a crucial role in the high pressure phase transition behavior of BaZrO 3

  12. In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

    Science.gov (United States)

    Takahasi, Masamitu

    2018-05-01

    The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

  13. Probing Stress States in Silicon Nanowires During Electrochemical Lithiation Using In Situ Synchrotron X-Ray Microdiffraction

    Directory of Open Access Journals (Sweden)

    Imran Ali

    2018-04-01

    Full Text Available Silicon is considered as a promising anode material for the next-generation lithium-ion battery (LIB due to its high capacity at nanoscale. However, silicon expands up to 300% during lithiation, which induces high stresses and leads to fractures. To design silicon nanostructures that could minimize fracture, it is important to understand and characterize stress states in the silicon nanostructures during lithiation. Synchrotron X-ray microdiffraction has proven to be effective in revealing insights of mechanical stress and other mechanics considerations in small-scale crystalline structures used in many important technological applications, such as microelectronics, nanotechnology, and energy systems. In the present study, an in situ synchrotron X-ray microdiffraction experiment was conducted to elucidate the mechanical stress states during the first electrochemical cycle of lithiation in single-crystalline silicon nanowires (SiNWs in an LIB test cell. Morphological changes in the SiNWs at different levels of lithiation were also studied using scanning electron microscope (SEM. It was found from SEM observation that lithiation commenced predominantly at the top surface of SiNWs followed by further progression toward the bottom of the SiNWs gradually. The hydrostatic stress of the crystalline core of the SiNWs at different levels of electrochemical lithiation was determined using the in situ synchrotron X-ray microdiffraction technique. We found that the crystalline core of the SiNWs became highly compressive (up to -325.5 MPa once lithiation started. This finding helps unravel insights about mechanical stress states in the SiNWs during the electrochemical lithiation, which could potentially pave the path toward the fracture-free design of silicon nanostructure anode materials in the next-generation LIB.

  14. High pressure synthesis of amorphous TiO2 nanotubes

    Directory of Open Access Journals (Sweden)

    Quanjun Li

    2015-09-01

    Full Text Available Amorphous TiO2 nanotubes with diameters of 8-10 nm and length of several nanometers were synthesized by high pressure treatment of anatase TiO2 nanotubes. The structural phase transitions of anatase TiO2 nanotubes were investigated by using in-situ high-pressure synchrotron X-ray diffraction (XRD method. The starting anatase structure is stable up to ∼20GPa, and transforms into a high-density amorphous (HDA form at higher pressure. Pressure-modified high- to low-density transition was observed in the amorphous form upon decompression. The pressure-induced amorphization and polyamorphism are in good agreement with the previous results in ultrafine TiO2 nanoparticles and nanoribbons. The relationship between the LDA form and α-PbO2 phase was revealed by high-resolution transmission electron microscopy (HRTEM study. In addition, the bulk modulus (B0 = 158 GPa of the anatase TiO2 nanotubes is smaller than those of the corresponding bulks and nanoparticles (180-240 GPa. We suggest that the unique open-ended nanotube morphology and nanosize play important roles in the high pressure phase transition of TiO2 nanotubes.

  15. High-pressure apparatus

    NARCIS (Netherlands)

    Schepdael, van L.J.M.; Bartels, P.V.; Berg, van den R.W.

    1999-01-01

    The invention relates to a high-pressure device (1) having a cylindrical high-pressure vessel (3) and prestressing means in order to exert an axial pressure on the vessel. The vessel (3) can have been formed from a number of layers of composite material, such as glass, carbon or aramide fibers which

  16. High-pressure crystallography

    Science.gov (United States)

    Katrusiak, A.

    2008-01-01

    The history and development of high-pressure crystallography are briefly described and examples of structural transformations in compressed compounds are given. The review is focused on the diamond-anvil cell, celebrating its 50th anniversary this year, the principles of its operation and the impact it has had on high-pressure X-ray diffraction.

  17. In-situ Raman spectroscopic study of aluminate speciation in H2O-KOH solutions at high pressures and temperatures

    Science.gov (United States)

    Mookherjee, M.; Keppler, H.; Manning, C. E.

    2009-12-01

    The solubility of corundum in H2O is low even at high pressure and temperatures. Therefore, it is commonly assumed that alumina remains essentially immobile during fluid-rock interaction. However, field and experimental evidence suggests that alumina solubility is strongly enhanced in the presence of silica as well as in alkaline solutions. In order to understand what controls the alumina solubility and how it is enhanced as a function of fluid composition, we conducted Raman-spectroscopic study of Al speciation in aqueous fluids at high pressure and temperature. Experiments were carried out in an externally heated hydrothermal diamond-anvil cell equipped with low-fluorescence diamonds and iridium gaskets. Raman spectra were collected with a Horiba Jobin-Yvon Labram HR spectrometer using the 514 nm line of an argon laser for excitation. In a first series of experiments, the speciation of alumina was studied in a 1 M KOH solution in equilibrium with corundum up to 700 oC and ~1 GPa. The Raman spectra show a prominent band at 618 cm-1 interpreted to arise from Al-O stretching vibrations associated with the tetrahedral [Al(OH)4]1- species. At higher pressure and temperature, an additional vibrational mode appears in the spectra at 374 cm-1 (full width at half maximum ~ 20 cm-1). This feature is tentatively attributed to [(OH)3Al-O-Al(OH)3]2- (Moolenaar et al. 1970, Jour. Phys. Chem., 74, 3629-3636). No evidence for KAl(OH)4 was observed, consistent with piston cylinder experiments at 700 oC and 1 GPa (Wohlers & Manning, 2009, Chem. Geol., 262, 310). Upon cooling from high-pressure and high temperature, slow kinetics of corundum regrowth lead to oversaturation in the solutions, as evidenced by sharp peaks at 930 and 1066 cm-1 observed upon cooling. These features are probably due to colloidal aluminum hydroxide. The results provide the first evidence for aluminate polymerization at high pressure and temperature, and offer insights into the causes for enhancement of

  18. Shining a light on Jarosite: formation, alteration and stability studies using in situ experimental synchrotron and neutron techniques.

    Science.gov (United States)

    Brand, H. E. A.; Scarlett, N. V. Y.; Wilson, S. A.; Frierdich, A. J.; Grey, I. E.

    2016-12-01

    Jarosites and related minerals are critical to a range of mineral processing and research applications. They are used in the removal of iron species from smelting processes; they occur in metal bioleaching systems, and they are present in acid mine drainage environments. There has been a recent resurgence in interest in jarosites since their detection on Mars. In this context, the presence of jarosite has been recognised as a likely indicator of liquid water at the surface of Mars in the past & it is thought that their study will provide insight into the environmental history of Mars. Acid sulfate soils cover large areas of the Australian coastline and are likely to be a major constituent of the Martian environment. The oxidation of acid sulfate soils, coupled with potential release of heavy metals and acidic groundwaters, can have serious consequences for fragile ecosystems. Understanding these sediments will provide insight into the biogeochemical processes that affect the lifetimes of transient mineral species on Earth, and may be used to better understand soil acidification, contaminant mobility at sites affected by acid and metalliferous drainage, and even constrain past weathering and putative biosignatures on Mars. Knowledge of the behaviour of jarosite minerals under the actual conditions that they are found in is crucial to understanding their potential environmental impacts on both Earth and Mars. To this end, we are engaged in a program to study the formation, stability and alteration of natural and synthetic jarosite minerals using a complementary suite of in situ synchrotron and neutron techniques. There are 3 sections to this work that will introduce the experimental techniques and sample environments that make these measurements possible: Studying the nucleation and growth of jarosites under laboratory conditions. The experimentation consisted of time-resolved synchrotron small angle X-ray scattering and X-ray diffraction. Studying the stability of

  19. Applications of synchrotron microradiography in materials science-in situ visualization of the growth of metallic alloy crystals

    International Nuclear Information System (INIS)

    Wang Tongmin; Zhu Jing; Cao Fei; Wang Kun; Bao Yongming; Xie Honglan; Huang Wanxia

    2012-01-01

    Metals and their alloys are an important type of structural and functional material and have been widely used in the aerospace, automobile, shipbuilding and other industries. The macro-properties of metallic alloys actually depend on their microstructures. The evolution of their microstructures generally involves a dynamic process of crystal growth on the scale of micrometers. The crystal growth of these alloys is still a puzzle to us due to their opacity. Conventional metallography techniques are limited by the high temperature of the phase changes so it is not possible to perform in situ observation of the evolving crystal morphology. The in situ visualization of the crystal growth has now become possible with the application of synchrotron radiation imaging techniques, which are just the right key to unravel the mystery mentioned above. In this paper, the development and current state-of-the-art of in situ crystal growth visualization are reviewed. Some typical application examples are presented, and promising applications in materials science are further expected. (authors)

  20. In situ synchrotron x-ray characterization of microstructure formation in solidification processing of Al-based metallic alloys

    International Nuclear Information System (INIS)

    Billia, Bernard; Nguyen-Thi, Henri; Mangelinck-Noel, Nathalie

    2010-01-01

    The microstructure formed during the solidification step has a major influence on the properties of materials processed by major techniques (casting, welding ...). In situ and real-time characterization by synchrotron X-ray imaging is the method of choice to unveil the dynamical formation of the solidification microstructure in metallic alloys, and thus provide precise data for the critical validation of the theoretical predictions that is needed for sound advancement of modeling and numerical simulation. After a description of the experimental procedure used at the European Synchrotron Radiation Facility (ESRF), dynamical phenomena in the formation of the grain structure and dendritic or equiaxed solidification microstructure in Al-based alloys are presented. Beyond fluid flow interaction, earth gravity induces stresses, deformation and fragmentation in the dendritic mush. Settling of dendrite arms and equiaxed grains thus occurs, in particular in the columnar to equiaxed transition. Other types of stresses and strains are caused by the mere formation of the solidification microstructure itself. In white-beam X-ray topography, stresses and strains are manifested by specific contrasts and breaking of the Laue images into several pieces. Finally, quantitative analysis of the grey level in radiographs enables the analysis of solute segregation, which noticeably results in solutal poisoning of growth when equiaxed grains are interacting. (author)

  1. Transformation Heat Treatment of Rapidly Quenched Nb3A1 Precursor Monitored in situ by High Energy Synchrotron Diffraction

    CERN Document Server

    Scheuerlein, C; Di Michiel, M; Jin, X; Takeuchi, T; Kikuchi, A; Tsuchiya, K; Nakagawa, K; Nakamoto, T

    2013-01-01

    Nb3Al superconductors are studied for use in high field magnets. Fine grained Nb3Al with nearly stoichiometric Al content is obtained by a Rapid Heating Quenching and Transformation (RHQT) process. We describe a non destructive in situ study of the transformation process step of a RHQ Nb3Al precursor wire with ramp rates of either 120 °C/h or 800 °C/h. High energy synchrotron x-ray diffraction measurements show the transformation from a Nb(Al)SS supersaturated solid solution into Nb3Al. When heating with a ramp rate of 120 °C/h a strong reduction of the Nb(Al)SS (110) diffraction peak component is observed when the temperature exceeds 660 °C. Additional diffraction peaks are detectable in the approximate temperature interval 610 °C - 750 °C and significant Nb3Al growth is observed above 730 °C.

  2. Mechanically activated SHS reaction in the Fe-Al system: in-situ time resolved diffraction using synchrotron radiation

    International Nuclear Information System (INIS)

    Gaffet, E.; Charlot, F.; Klein, D.; Bernard, F.; Niepce, J.C.

    1998-01-01

    The mechanical activation self propagating high temperature synthesis (M.A.S.H.S.) processing is a new way to produce nanocrystalline iron aluminide intermetallic compounds. This process is maily the combination of two steps; in the one hand, a mechanical activation where the Fe - Al powder mixture was milled during a short time at given energy and frequency of shocks and in the other hand, a self propagating high temperature synthesis (S.H.S.) reaction, for which the exothermicity of the Fe + Al reaction is used. This fast propagated MASHS reaction has been in-situ investigated using the time resolved X-ray diffraction (TRXRD) using a X-ray synchrotron beam and an infrared thermography camera, allowing the coupling of the materials structure and the temperature field. The effects of the initial mean compositions, of the milling conditions as well as of the compaction parameters on the MASHS reaction are reported. (orig.)

  3. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    International Nuclear Information System (INIS)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-01-01

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed

  4. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-10-31

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed.

  5. High-pressure tritium

    International Nuclear Information System (INIS)

    Coffin, D.O.

    1976-01-01

    Some solutions to problems of compressing and containing tritium gas to 200 MPa at 700 0 K are discussed. The principal emphasis is on commercial compressors and high-pressure equipment that can be easily modified by the researcher for safe use with tritium. Experience with metal bellows and diaphragm compressors has been favorable. Selection of materials, fittings, and gauges for high-pressure tritium work is also reviewed briefly

  6. High pressure synthesis of zeolite/polymer nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Haines, Julien; Thibaud, Jean-Marc; Rouquette, Jerome; Cambon, Olivier; Di Renzo, Francesco, E-mail: julien.haines@univ-montp2.fr [Institut Charles Gerhardt Montpellier (France); Lee, Arie van der [Institut Europeen des Membranes, Montpellier (France); Scelta, Demetrio; Ceppatelli, Matteo; Dziubek, Kamil; Gorelli, Federico; Bini, Roberto; Santoro, Mario [European Laboratory for Non Linear Spectroscopy, Firenze (Italy)

    2016-07-01

    Full text: Polymerization of simple organic molecules under high pressure in the subnanometric pores of pure SiO{sub 2} zeolites can be used to produce novel nanocomposite materials, which can be recovered at ambient P and have remarkable mechanical, electrical or optical properties. Polymerization of ethylene in silicalite was studied in situ at high pressure by IR and results in a nanocomposite with isolated chains of non-conducting polyethylene strongly confined in the pores based on single crystal x-ray diffraction data. The nanocomposite is much less compressible than silicalite and has a positive rather than a negative thermal expansion coefficient. In order to target novel electrical and optical properties, isolated chains of conducting polymers can also be prepared in the pores of zeolite hosts at high pressure, such as polyacetylene, which was polymerized under pressure in the pores of the 1-D zeolite TON. The structure of this nanocomposite was determined by synchrotron x-ray powder diffraction data with complete pore filling corresponding to one planar polymer chain confined in each pore with a zig-zag configuration in the yz plane. This very strong confinement can be expected to strongly modify the electrical properties of polyacetylene. In this nanocomposite, our theoretical calculations indicate that the electronic density of states of polyacetylene exhibit van Hove singularities related to quantum 1D confinement, which could lead to future technological applications. This new material is susceptible to have applications in nanoelectronics, nanophotonics and energy and light harvesting. Completely novel nanocomposites were prepared by the polymerization of carbon monoxide CO in silicalite and TON. In these materials, isolated, ideal polycarbonyl chains are obtained in contrast to the non-stoichiometric, branched bulk polymers obtained by high pressure polymerization of this simple system. These poly CO/zeolite composites could be interesting energetic

  7. In Situ Synchrotron XRD on a Capillary Li-O2 Battery Cell

    DEFF Research Database (Denmark)

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

    2014-01-01

    of a electrolyte filled capillary with anode and cathode in each end suspended on stainless steel wires, the oxygen in-let is placed on the cathode side of the capillary with a flushing system for oxygen in-let. In this study we present a flexible design of a capillary based Li-O2 battery with discharge and charge...... a stainless steel wire where the cathode is attached. The in situ XRD measurements show how the Li2O2 growth depend on current discharge rate and how the FWHM changes dependent on reflection and charge/discharge.Several cells were tested both ex situ and in situ, and in situ XRD for 1st discharge/charge and 2...

  8. Characteristic densities of low- and high-pressure liquid SnI4

    International Nuclear Information System (INIS)

    Fuchizaki, Kazuhiro; Hamaya, Nozomu; Katayama, Yoshinori

    2013-01-01

    An in situ synchrotron x-ray absorption measurement was carried out to estimate the density of liquid SnI 4 . The characteristic densities of the low- and high-pressure liquids were found to be 4.6-4.7 and 4.9-5.0 g/cm 3 , respectively, and their region is separated at around 1.7 GPa. The difference in density, although a slight amount of 0.3-0.4 g/cm 3 , strongly suggests the existence of a weak but discontinuous phase transition at that pressure between the two liquid regions. (author)

  9. Formation of nanocrystalline MgB sub 2 under high pressure

    CERN Document Server

    Sun, L; Kikegawa, T; Cao, L; Zhan, Z; Wu, Q; Wu, X; Wang, W

    2002-01-01

    The microstructural features of MgB sub 2 at ambient pressure and high pressure have been investigated by means of in situ synchrotron radiation x-ray diffraction and transmission electron microscopy (TEM). The x-ray diffraction measurements indicated that nanocrystalline MgB sub 2 formed in the pressure range of 26.3-30.2 GPa. TEM investigations reveal complex structure domains with evident lattice distortion in the relevant samples. The superconductivity of nanocrystalline MgB sub 2 was measured and compared with that of the starting sample of MgB sub 2.

  10. In-situ synchrotron PXRD study of spinel LiMn2O4 nanocrystal formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    Many solvothermal reactions have a great potential for environmentally friendly and easily scalable way for producing nanocrystalline materials on an industrial scale. Here we study hydrothermal formation of spinel LiMn2O4 which is a well-known cathode material for Li-ion batteries. The LiMn2O4...... nanoparticles are formed by reducing KMnO4 in an aqueous solution containing Li-ions. The reducing agent is an alcohol (here ethanol) and the reaction takes place under high pressure and temperature. The LiMn2O4 nanocrystals are unstable towards further reduction to Mn3O4 nanocrystals. Possible reaction route...

  11. In-situ synchrotron PXRD study of spinel LiMn2O4 formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    structural properties for the reaction being studied. Normally the reactions are started by heating and a constant temperature is kept throughout the experiment. In this study the hydrothermal reaction previously shown to produce spinel LiMn2O4 nanoparticles is studied in-situ to learn more about the phase......O4, depending on the initial concentration if Li-ions. An impurity phase, identified as Mn3O4, is also detected in different concentrations depending on reaction time and temperature. We have developed an experimental technique for in-situ measurements of solvothermal reactions under sub...... in the in-situ measurements it gives a unique opportunity to study reaction kinetics and thermodynamic quantities of the reactions. A temperature study of the reaction has been conducted to see how the formation rate and particle growth is affected by temperature while the precursor concentration is kept...

  12. Fascination at high pressures

    International Nuclear Information System (INIS)

    Chidambaram, R.

    1992-01-01

    Research at high pressures has developed into an interdisciplinary area which has important implications for and applications in the areas of physics, chemistry, materials sciences, planetary sciences, biology, engineering sciences and technology. The state of-the-art in this field is reviewed and future directions are indicated. (M.G.B.)

  13. High Pressure Biomass Gasification

    Energy Technology Data Exchange (ETDEWEB)

    Agrawal, Pradeep K [Georgia Tech Research Corporation, Atlanta, GA (United States)

    2016-07-29

    According to the Billion Ton Report, the U.S. has a large supply of biomass available that can supplement fossil fuels for producing chemicals and transportation fuels. Agricultural waste, forest residue, and energy crops offer potential benefits: renewable feedstock, zero to low CO2 emissions depending on the specific source, and domestic supply availability. Biomass can be converted into chemicals and fuels using one of several approaches: (i) biological platform converts corn into ethanol by using depolymerization of cellulose to form sugars followed by fermentation, (ii) low-temperature pyrolysis to obtain bio-oils which must be treated to reduce oxygen content via HDO hydrodeoxygenation), and (iii) high temperature pyrolysis to produce syngas (CO + H2). This last approach consists of producing syngas using the thermal platform which can be used to produce a variety of chemicals and fuels. The goal of this project was to develop an improved understanding of the gasification of biomass at high pressure conditions and how various gasification parameters might affect the gasification behavior. Since most downstream applications of synags conversion (e.g., alcohol synthesis, Fischer-Tropsch synthesis etc) involve utilizing high pressure catalytic processes, there is an interest in carrying out the biomass gasification at high pressure which can potentially reduce the gasifier size and subsequent downstream cleaning processes. It is traditionally accepted that high pressure should increase the gasification rates (kinetic effect). There is also precedence from coal gasification literature from the 1970s that high pressure gasification would be a beneficial route to consider. Traditional approach of using thermogravimetric analyzer (TGA) or high-pressure themogravimetric analyzer (PTGA) worked well in understanding the gasification kinetics of coal gasification which was useful in designing high pressure coal gasification processes. However

  14. Phase transition and water incorporation into Eu2Sn2O7 pyrochlore at high pressure

    Science.gov (United States)

    Zhang, F. X.; Lang, M.; Ewing, R. C.

    2016-04-01

    Structural changes of europium stannate pyrochlore, Eu2Sn2O7, have been investigated at high pressures with in situ Raman spectroscopy, photoluminescence (PL), and synchrotron X-ray diffraction (XRD) techniques. The XRD measurements suggest that a pressure-induced phase transition starts at 34.4 GPa. The PL spectrum from Eu3+ cations also suggests a phase transition above 36 GPa. XRD analysis shows that the unit cell of the cubic phase deviates from the equation of state at pressures above 23.8 GPa. This is due to the incorporation of water from the pressure medium in the structure at high pressures, which is confirmed by optical spectroscopy measurements.

  15. Manipulation of Samples at Extreme Temperatures for Fast in-situ Synchrotron Measurements

    Energy Technology Data Exchange (ETDEWEB)

    Weber, Richard [Materials Development, Inc., Arlington Heights, IL (United States)

    2016-04-22

    An aerodynamic sample levitation system with laser beam heating was integrated with the APS beamlines 6 ID-D, 11 ID-C and 20 BM-B. The new capability enables in-situ measurements of structure and XANES at extreme temperatures (300-3500 °C) and in conditions that completely avoid contact with container surfaces. In addition to maintaining a high degree of sample purity, the use of aerodynamic levitation enables deep supercooling and greatly enhanced glass formation from a wide variety of melts and liquids. Development and integration of controlled extreme sample environments and new measurement techniques is an important aspect of beamline operations and user support. Processing and solidifying liquids is a critical value-adding step in manufacturing semiconductors, optical materials, metals and in the operation of many energy conversion devices. Understanding structural evolution is of fundamental importance in condensed materials, geology, and biology. The new capability provides unique possibilities for materials research and helps to develop and maintain a competitive materials manufacturing and energy utilization industry. Test samples were used to demonstrate key features of the capability including experiments on hot crystalline materials, liquids at temperatures from about 500 to 3500 °C. The use of controlled atmospheres using redox gas mixtures enabled in-situ changes in the oxidation states of cations in melts. Significant innovations in this work were: (i) Use of redox gas mixtures to adjust the oxidation state of cations in-situ (ii) Operation with a fully enclosed system suitable for work with nuclear fuel materials (iii) Making high quality high energy in-situ x-ray diffraction measurements (iv) Making high quality in-situ XANES measurements (v) Publishing high impact results (vi) Developing independent funding for the research on nuclear materials This SBIR project work led to a commercial instrument product for the niche market of processing and

  16. In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

    International Nuclear Information System (INIS)

    Chen, Xian; Tamura, Nobumichi; MacDowell, Alastair; James, Richard D.

    2016-01-01

    The alloy Cu_2_5Au_3_0Zn_4_5 undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

  17. Structural stability at high pressure, electronic, and magnetic properties of BaFZnAs: A new candidate of host material of diluted magnetic semiconductors

    International Nuclear Information System (INIS)

    Chen Bi-Juan; Deng Zheng; Wang Xian-Cheng; Feng Shao-Min; Yuan Zhen; Zhang Si-Jia; Liu Qing-Qing; Jin Chang-Qing

    2016-01-01

    The layered semiconductor BaFZnAs with the tetragonal ZrCuSiAs-type structure has been successfully synthesized. Both the in-situ high-pressure synchrotron x-ray diffraction and the high-pressure Raman scattering measurements demonstrate that the structure of BaFZnAs is stable under pressure up to 17.5 GPa at room temperature. The resistivity and the magnetic susceptibility data show that BaFZnAs is a non-magnetic semiconductor. BaFZnAs is recommended as a candidate of the host material of diluted magnetic semiconductor. (special topic)

  18. In situ study at high pressure and temperature of the environment of water in hydrous Na and Ca aluminosilicate melts and coexisting aqueous fluids

    Science.gov (United States)

    Le Losq, Charles; Dalou, Célia; Mysen, Bjorn O.

    2017-07-01

    The bonding and speciation of water dissolved in Na silicate and Na and Ca aluminosilicate melts were inferred from in situ Raman spectroscopy of the samples, in hydrothermal diamond anvil cells, while at crustal temperature and pressure conditions. Raman data were also acquired on Na silicate and Na and Ca aluminosilicate glasses, quenched from hydrous melts equilibrated at high temperature and pressure in a piston cylinder apparatus. In the hydrous melts, temperature strongly influences O-H stretching ν(O-H) signals, reflecting its control on the bonding of protons between different molecular complexes. Pressure and melt composition effects are much smaller and difficult to discriminate with the present data. However, the chemical composition of the melt + fluid system influences the differences between the ν(O-H) signals from the melts and the fluids and, hence, between their hydrogen partition functions. Quenching modifies the O-H stretching signals: strong hydrogen bonds form in the glasses below the glass transition temperature Tg, and this phenomenon depends on glass composition. Therefore, glasses do not necessarily record the O-H stretching signal shape in melts near Tg. The melt hydrogen partition function thus cannot be assessed with certainty using O-H stretching vibration data from glasses. From the present results, the ratio of the hydrogen partition functions of hydrous silicate melts and aqueous fluids mostly depends on temperature and the bulk melt + fluid system chemical composition. This implies that the fractionation of hydrogen isotopes between magmas and aqueous fluids in water-saturated magmatic systems with differences in temperature and bulk chemical composition will be different.

  19. Deuterium high pressure target

    International Nuclear Information System (INIS)

    Perevozchikov, V.V.; Yukhimchuk, A.A.; Vinogradov, Yu.I.

    2001-01-01

    The design of the deuterium high-pressure target is presented. The target having volume of 76 cm 3 serves to provide the experimental research of muon catalyzed fusion reactions in ultra-pure deuterium in the temperature range 80-800 K under pressures of up to 150 MPa. The operation of the main systems of the target is described: generation and purification of deuterium gas, refrigeration, heating, evacuation, automated control system and data collection system

  20. In situ synchrotron X-ray studies during metal-organic chemical vapor deposition of semiconductors

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Carol [Northern Illinois Univ., DeKalb, IL (United States); Argonne National Lab., Argonne, IL (United States); Highland, Matthew J.; Perret, Edith; Fuoss, Paul H.; Streiffer, Stephen K.; Stephenson, G. Brian [Argonne National Lab., Argonne, IL (United States); Richard, Marie-Ingrid [Universite Paul Cezanne Aix-Marseille, Marseille (France)

    2012-07-01

    In-situ, time-resolved techniques provide valuable insight into the complex interplay of surface structural and chemical evolution occurring during materials synthesis and processing of semiconductors. Our approach is to observe the evolution of surface structure and morphology at the atomic scale in real-time during metal organic vapor phase deposition (MOCVD) by using grazing incidence x-ray scattering and X-ray fluorescence, coupled with visible light scattering. Our vertical-flow MOCVD chamber is mounted on a 'z-axis' surface diffractometer designed specifically for these studies of the film growth, surface evolution and the interactions within a controlled growth environment. These techniques combine the ability of X-rays to penetrate a complex environment for measurements during growth and processing, with the sensitivity of surface scattering techniques to atomic and nanoscale structure. In this talk, we outline our program and discuss examples from our in-situ and real-time X-ray diffraction and fluorescence studies of InN, GaN, and InGaN growth on GaN(0001).

  1. Development of a laser-based heating system for in situ synchrotron-based X-ray tomographic microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fife, Julie L., E-mail: julie.fife@psi.ch [Laboratory for Synchrotron Radiation, Swiss Light Source, Paul Scherrer Institut, Villigen (Switzerland); Computational Materials Laboratory, Ecole Polytechnique Federale de Lausanne, Lausanne (Switzerland); Rappaz, Michel [Computational Materials Laboratory, Ecole Polytechnique Federale de Lausanne, Lausanne (Switzerland); Pistone, Mattia [Institute for Geochemistry and Petrology, Swiss Federal Institute of Technology of Zurich, Zurich (Switzerland); Celcer, Tine [Laboratory for Synchrotron Radiation, Swiss Light Source, Paul Scherrer Institut, Villigen (Switzerland); The Centre of Excellence for Biosensors, Instrumentation and Process Control, Solkan (Slovenia); Mikuljan, Gordan [Laboratory for Synchrotron Radiation, Swiss Light Source, Paul Scherrer Institut, Villigen (Switzerland); Stampanoni, Marco [Laboratory for Synchrotron Radiation, Swiss Light Source, Paul Scherrer Institut, Villigen (Switzerland); Institute for Biomedical Engineering, Swiss Federal Institute of Technology and University of Zurich, Zurich (Switzerland)

    2012-05-01

    A laser-based heating system has been developed at the TOMCAT beamline of the Swiss Light Source for in situ observations of moderate-to-high-temperature applications of materials. Understanding the formation of materials at elevated temperatures is critical for determining their final properties. Synchrotron-based X-ray tomographic microscopy is an ideal technique for studying such processes because high spatial and temporal resolutions are easily achieved and the technique is non-destructive, meaning additional analyses can take place after data collection. To exploit the state-of-the-art capabilities at the tomographic microscopy and coherent radiology experiments (TOMCAT) beamline of the Swiss Light Source, a general-use moderate-to-high-temperature furnace has been developed. Powered by two diode lasers, it provides controlled localized heating, from 673 to 1973 K, to examine many materials systems and their dynamics in real time. The system can also be operated in various thermal modalities. For example, near-isothermal conditions at a given sample location can be achieved with a prescribed time-dependent temperature. This mode is typically used to study isothermal phase transformations; for example, the formation of equiaxed grains in metallic systems or to nucleate and grow bubble foams in silicate melts under conditions that simulate volcanic processes. In another mode, the power of the laser can be fixed and the specimen moved at a constant speed in a user-defined thermal gradient. This is similar to Bridgman solidification, where the thermal gradient and cooling rate control the microstructure formation. This paper details the experimental set-up and provides multiple proofs-of-concept that illustrate the versatility of using this laser-based heating system to explore, in situ, many elevated-temperature phenomena in a variety of materials.

  2. Structure property relationship of biological nano composites studies by combination of in-situ synchrotron scattering and mechanical tests

    International Nuclear Information System (INIS)

    Martinschitz, K.

    2005-06-01

    Biological materials represent hierarchical nano fibre composites with complicated morphology and architecture varying on the nm level. The mechanical response of those materials is influenced by many parameters like chemical composition and crystal structure of constituents, preferred orientation, internal morphology with specific sizes of features etc. In-situ wide-angle x-ray scattering (WAXS) combined with mechanical tests provide a unique means to evaluate structural changes in biological materials at specific stages of tensile experiments. In this way it is possible to identify distinct architectural/compositional elements responsible for specific mechanical characteristics of the biological materials. In this thesis, structure-property relationship is analyzed using in-situ WAXS in the tissues of Picea abies, coir fibre, bacterial cellulose and cellulose II based composites. The experiments were performed at the beamline ID01 of European synchrotron radiation facility in Grenoble, France. The tissues were strained in a tensile stage, while the structural changes were monitored using WAXS. Complex straining procedures were applied including cyclic straining. One of the main goals was to understand the stiffness recovery and strain hardening effects in the tissues. The results demonstrate that, in all cellulosics, the orientation of the cellulose crystallites is only the function of the external strain while the stiffness depends on the specific stage of the tensile experiment. Whenever the strain is increased, the tissues exhibit stiffness equal or larger than the initial one. The recovery of the mechanical function is attributed to the molecular mechanistic effects operating between the crystalline domains of the cellulose. (author)

  3. In-situ, high pressure and temperature experimental determination of hydrogen isotope fractionation between coexisting hydrous melt and silicate-saturated aqueous fluid

    Science.gov (United States)

    Mysen, B. O.

    2012-12-01

    Hydrogen isotope fractionation between water-saturated silicate melt and silicate-saturated aqueous fluid has been determined experimentally, in-situ with the samples in the 450-800C and 101-1567 MPa temperature and pressure range, respectively. The temperatures are, therefore higher than those where hydrogen bonding in fluids and melts is important [1]. The experiments were conducted with a hydrothermal diamond anvil cell (HDAC) as the high-temperature/-pressure tool and vibrational spectroscopy to determine D/H fractionation. Compositions were along the haploandesite join, Na2Si4O9 - Na2(NaAl)4O9 [Al/(Al+Si)=0-0.1], and a 50:50 (by volume) H2O:D2O fluid mixture as starting material. Platinum metal was used to enhance equilibration rate. Isotopic equilibrium was ascertained by using variable experimental duration at given temperature and pressure. In the Al-free Na-silicate system, the enthalpy change of the (D/H) equilibrium of fluid is 3.1±0.7 kJ/mol, whereas for coexisting melt, ΔH=0 kJ/mol within error. With Al/(Al+Si)=0.1, ΔH=5.2±0.9 kJ/mol for fluid and near 0 within error for coexisting melt melt. For the exchange equilibrium between melt and fluid, H2O(melt)+D2O(fluid)=H2O(fluid)+D2O(melt), the ΔH=4.6±0.7 and 6.5±0.7 kJ/mol for the two Al-free and Al-bearing compositions, respectively, respectively. The D/H equilibration within fluids and melts and, therefore, D/H partitioning between coexisting fluid and melt reflect the influence of dissolved H2O(D2O) in melts and dissolved silicate components in H2O(D2O) fluid on their structure. The positive temperature- and pressure-dependence of silicate solubility and on silicate structure in silicate-saturated aqueous fluid governs the D/H fractionation in the fluid because increasing silicate solute concentration in fluid results in silicate polymerization [2]. These structural effects may be analogous to observed solute-dependent oxygen isotope fractionation between brine and CO2 [3]. In the temperature

  4. High pressure research at CHESS

    International Nuclear Information System (INIS)

    Brister, K.

    1992-01-01

    Since February 1990 there has been a dedicated high pressure line at the Cornell High Energy Synchrotron Source (CHESS). This facility provides X-ray instrumentation for energy dispersive X-ray diffraction and Laue diffraction using diamond anvil cells. Both hard-bend magnet and wiggler radiation are available as well as focused monochromatic radiation. In addition, support instrumentation is also available; a ruby system, laser heating, sample loading, and data analysis software. Experienced users need only to bring their diamond anvil cells and samples and can leave with the initial data analysis finished. Research using diamond anvil cells will be introduced and the facility will be described. Some of the diamond anvil cell research done at CHESS will be reviewed, including crystalline to amorphous transitions (R.R. Winters et al., Chem. Phys, in press), properties of C 6 0 under stress (S.J. Duclos et al., Nature 351 (1991) 380), deep earthquakes (T.C. Wu et al., submitted to J. Geophys. Res.)l, and reaching pressures of the center of Earth (A.L. Ruoff et al., Rev. Sci. Instr. 61 (1990) 3830). (orig.)

  5. Processing of Bi-2212 and Nb$_3$Sn studied in situ by high energy synchrotron diffraction and micro-tomography

    CERN Document Server

    Kadar, Julian

    Next generation superconducting wires have been studied to obtain more information on the evolution of phase growth, crystallite size and strain state during wire processing. The high energy scattering beam line ID15 at the European Synchrotron Radiation Facility provides a very high flux of high energy photons for very fast in situ X-ray diffraction and micro-tomography studies of Bi-2212/Ag and Nb$_3$S/Cu wire samples. The typical wire processing conditions could be imitated in the X-ray transparent furnace at ID15 for diffraction and tomography studies. Efficient data analysis is mandatory in order to handle the very fast data acquisition rate. For this purpose an Excel-VBA based program was developed that allows a semi-automated fitting and tracking of peaks with pre-set constraints. With this method, more than one thousand diffraction patterns have been analysed to extract d-spacing, peak intensity and peak width values. X ray absorption micro tomograms were recorded simultaneously with the X-ray diffrac...

  6. Stress-dependent crystal structure of lanthanum strontium cobalt ferrite by in situ synchrotron X-ray diffraction

    Science.gov (United States)

    Geiger, Philipp T.; Khansur, Neamul H.; Riess, Kevin; Martin, Alexander; Hinterstein, Manuel; Webber, Kyle G.

    2018-02-01

    Lanthanum strontium cobalt ferrite La1-xSrxCo1-yFeyO3-δ (LSCF) is one of the most studied mixed ionic-electronic conductor materials due to electrical and transport properties, which are attractive for intermediate temperature solid oxide fuel cells (SOFCs), oxygen permeation membranes, and catalysis. The integration of such materials, however, depends on the thermal as well as mechanical behavior. LSCF exhibits nonlinear hysteresis during compressive stress-strain measurements, marked by a remanent strain and coercive stress, i.e., ferroelasticity. However, the origin of ferroelastic behavior has not been investigated under high compressive stress. This study, therefore, investigates the microscopic origin of stress-induced mechanical behavior in polycrystalline (La0.6Sr0.4)0.95Co0.2Fe0.8O3-δ using in situ synchrotron x-ray diffraction. The data presented here reveals that the strain response originates from the intrinsic lattice strain as well as the extrinsic domain switching strain without any apparent change in crystallographic symmetry. A comparison of the calculated microscopic strain contribution with that of a macroscopic measurement indicates a significant change in the relative contributions of intrinsic and extrinsic strain depending on the applied stress state, i.e., under maximum stress and after unloading. Direct evidence of the microscopic origin of stress-strain response outlined in this paper may assist in guiding materials design with the improved mechanical reliability of SOFCs.

  7. In situ 3D characterization of high temperature fatigue damage mechanisms in a cast aluminum alloy using synchrotron X-ray tomography

    International Nuclear Information System (INIS)

    Dezecot, Sebastien; Buffiere, Jean-Yves; Koster, Alain; Maurel, Vincent; Szmytka, Fabien; Charkaluk, Eric; Dahdah, Nora; El Bartali, Ahmed; Limodin, Nathalie; Witz, Jean-Francois

    2016-01-01

    Fatigue tests were performed at 250 °C on a cast AlSi7Cu3Mg aluminum alloy and monitored with Synchrotron in situ X-ray tomography in order to understand the micro-mechanisms of crack initiation and propagation. The analysis of the 3D images reveals that internal shrinkage pores are responsible for the main crack initiation. Crack propagation is mainly due to the complex and highly interconnected network of hard particles of the eutectic regions.

  8. en (Be_3Al_2Si_6O_1_8) by using a diamond anvil cell and in situ synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Fan, Dawei; Xu, Jingui; Kuang, Yunqian; Li, Xiaodong; Li, Yanchun; Xie, Hongsen

    2015-01-01

    High-pressure single-crystal synchrotron X-ray diffraction was carried out on a single crystal of natural beryl compressed in a diamond anvil cell. The pressure-volume (P-V) data from room pressure to 9.51 GPa were fitted by a third-order Birch-Murnaghan equation of state (BM-EoS) and resulted in unit-cell volume V_0 = 675.5 ± 0.1 Aa"3, isothermal bulk modulus K_0 = 180 ± 2 GPa, and its pressure derivative K_0"' = 4.2 ± 0.5. We also calculated V_0 = 675.5 ± 0.1 Aa"3 and K_0 = 181 ± 1GPa with fixed K_0"' at 4.0 and then obtained the axial moduli for a (K_a_0)-axis and c (K_c_0)-axis of 209 ± 1 and 141 ± 2 GPa by ''linearized'' BM-EoS approach. The axial compressibilities of a-axis and c-axis are β_a = 1.59 x 10"-"3 GPa"-"1 and β_c = 2.36 x 10"-"3 GPa"-"1 with an anisotropic ratio of β_a:β_c = 0.67:1.00. On the other hand, the pressure-volume-temperature (P-V-T) EoS of the natural beryl has also been measured at temperatures up to 750 K and at pressures up to 16.81 GPa, using diamond anvil cell in conjunction with in situ synchrotron angle-dispersive powder X-ray diffraction. The P-V data at room temperature and at a pressure range of 0.0001-15.84 GPa were then analyzed by third-order BM-EoS and yielded V_0 = 675.3 ± 0.1 Aa"3, K_0 = 180 ± 2 GPa, K_0"' = 4.2 ± 0.3. With K_0"' fixed to 4.0, we also obtained V_0 = 675.2 ± 0.1 Aa"3 and K_0 = 182 ± 1 GPa. Consequently, we fitted the P-V-T data with high-temperature BM-EoS approach using the resultant K_0"' (4.2) from room-temperature BM-EoS and then obtained the thermoelastic parameters of V_0 = 675.3 ± 0.2 Aa"3, K_0 = 180 ± 1 GPa, temperature derivative of the bulk modulus (∂K/∂T)_P = -0.017 ± 0.004 GPa K"-"1, and thermal expansion coefficient at ambient conditions α_0 = (2.82 ± 0.74) x 10"-"6 K"-"1. Present results were also compared with previous studies for beryl. From the comparison of these fittings, we propose to constrain K_0 = 180 GPa and K_0"' = 4.2 for beryl. And we also observed that

  9. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weekes, H.E. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Jones, N.G. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); Lindley, T.C. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Dye, D., E-mail: david.dye@imperial.ac.uk [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom)

    2016-09-15

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample’s transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSS{sub D,H}) and precipitation (TSS{sub P,H}).

  10. In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

    Energy Technology Data Exchange (ETDEWEB)

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  11. Assessment of In Situ Time Resolved Shock Experiments at Synchrotron Light Sources*

    Science.gov (United States)

    Belak, J.; Ilavsky, J.; Hessler, J. P.

    2005-07-01

    Prior to fielding in situ time resolved experiments of shock wave loading at the Advanced Photon Source, we have performed feasibility experiments assessing a single photon bunch. Using single and poly-crystal Al, Ti, V and Cu shock to incipient spallation on the gas gun, samples were prepared from slices normal to the spall plane of thickness 100-500 microns. In addition, single crystal Al of thickness 500 microns was shocked to incipient spallation and soft recovered using the LLNL e-gun mini-flyer system. The e-gun mini-flyer impacts the sample target producing a 10's ns flat-top shock transient. Here, we present results for imaging, small-angle scattering (SAS), and diffraction. In particular, there is little SAS away from the spall plane and significant SAS at the spall plane, demonstrating the presence of sub-micron voids. * Use of the Advanced Photon Source was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. W-31-109-Eng-38 and work performed under the auspices of the U.S. Department of Energy by University of California, Lawrence Livermore National Laboratory under Contract W-7405-Eng-48.

  12. 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.

  13. High pressure mechanical seal

    Science.gov (United States)

    Babel, Henry W. (Inventor); Anderson, Raymond H. (Inventor)

    1996-01-01

    A relatively impervious mechanical seal is formed between the outer surface of a tube and the inside surface of a mechanical fitting of a high pressure fluid or hydraulic system by applying a very thin soft metal layer onto the outer surface of the hard metal tube and/or inner surface of the hard metal fitting. The thickness of such thin metal layer is independent of the size of the tube and/or fittings. Many metals and alloys of those metals exhibit the requisite softness, including silver, gold, tin, platinum, indium, rhodium and cadmium. Suitably, the coating is about 0.0025 millimeters (0.10 mils) in thickness. After compression, the tube and fitting combination exhibits very low leak rates on the order or 10.sup.-8 cubic centimeters per second or less as measured using the Helium leak test.

  14. Prospects of using synchrotron radiation facilities with diamond-anvil cells

    International Nuclear Information System (INIS)

    Manghani, M.H.; Ming, L.C.; Jamieson, J.C.

    1980-01-01

    Diamond-anvil pressure cells have proven versatile and useful for conducting high pressure research in the submegabar range. The interfacing of diamond-anvil cell technology with synchrotron facilities seems a logical new step for carrying out in situ X-ray diffraction studies of materials under extreme conditions of combined high pressure and temperature. The conventional film method of X-ray diffraction has definite limitations which call for the energy dispersive analysis techniques. Various potential high pressure-temperature studies in geophysis and related fields involving the use of diamond-anvil cell, synchrotron facilities and energy dispersive techniques are exemplified. For geophysical studies the conditions prevailing in 86% of the Earth's volume are capable of being simulated completely in pressure, and partially in pressure and temperature, simultaneously. (orig.)

  15. High-pressure system for Compton scattering experiments

    International Nuclear Information System (INIS)

    Oomi, G.; Honda, F.; Kagayama, T.; Itoh, F.; Sakurai, H.; Kawata, H.; Shimomura, O.

    1998-01-01

    High-pressure apparatus for Compton scattering experiments has been developed to study the momentum distribution of conduction electrons in metals and alloys at high pressure. This apparatus was applied to observe the Compton profile of metallic Li under pressure. It was found that the Compton profile at high pressure could be obtained within several hours by using this apparatus and synchrotron radiation. The result on the pressure dependence of the Fermi momentum of Li obtained here is in good agreement with that predicted from the free-electron model

  16. High pressure phases of terbium: Possibility of a thcp phase

    International Nuclear Information System (INIS)

    Staun Olsen, J.; Steenstrup, S.; Gerward, L.

    1985-01-01

    High pressure phases of trivalent Tb studied by energy dispersive X-ray diffraction with synchrotron radiation exhibits the closed packed sequence (hcp -> Sm -> dhcp -> fcc) typical of the trivalent rare earth metals. Furthermore, a phase consistent with a triple hexagonal closed packed (thcp) structure was observed in a narrow pressure range around 30 GPa. (orig.)

  17. In-situ and operando characterization of batteries with energy-dispersive synchrotron x-ray diffraction

    Science.gov (United States)

    Paxton, William Arthur

    Batteries play a pivotal role in the low-carbon society that is required to thwart the effects of climate change. Alternative low-carbon energy sources, such as wind and solar, are often intermittent and unreliable. Batteries are able capture their energy and deliver it later when it is needed. The implementation of battery systems in grid-level and transportation sectors is essential for efficient use of alternative energy sources. Scientists and engineers need better tools to analyze and measure the performance characteristics of batteries. One of the main hindrances in the progress of battery research is that the constituent electrode materials are inaccessible once an electrochemical cell is constructed. This leaves the researcher with a limited number of available feedback mechanisms to assess the cell's performance, e.g., current, voltage, and impedance. These data are limited in their ability to reveal the more-localized smaller-scale structural mechanisms on which the batteries' performance is so dependent. Energy-dispersive x-ray diffraction (EDXRD) is one of the few techniques that can internally probe a sealed battery. By analyzing the structural behavior of battery electrodes, one is able to gain insight to the physical properties on which the battery's performance is dependent. In this dissertation, EDXRD with ultrahigh energy synchrotron radiation is used to probe the electrodes of manufactured primary and secondary lithium batteries under in-situ and operando conditions. The technique is then applied to solve specific challenges facing lithium ion batteries. Diffraction spectra are collected from within a battery at 40 micrometer resolution. Peak-fitting is used to quantitatively estimate the abundance of lithiated and non-lithiated phases. Through mapping the distribution of phases within, structural changes are linked to the battery's galvanic response. A three-dimensional spatial analysis of lithium iron phosphate batteries suggests that evolution

  18. Advances in martensitic transformations in Cu-based shape memory alloys achieved by in situ neutron and synchrotron X-ray diffraction methods

    Czech Academy of Sciences Publication Activity Database

    Malard, B.; Šittner, Petr; Berveiller, S.; Patoor, E.

    2012-01-01

    Roč. 13, č. 3 (2012), s. 280-292 ISSN 1631-0705 R&D Projects: GA ČR GAP108/10/1296; GA ČR GAP107/12/0800 EU Projects: European Commission(XE) 262806 - SmartNets Institutional research plan: CEZ:AV0Z10100520 Keywords : stress induced martensitic transformation * Cu-based shape memory alloys * neutron diffraction * X-ray * synchrotron * in situ * multiscale analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.818, year: 2012

  19. In situ synchrotron X-ray diffraction study of surface scale formation during CO2 corrosion of carbon steel at temperatures up to 90 oC

    International Nuclear Information System (INIS)

    Ingham, B.; Ko, M.; Kear, G.; Kappen, P.; Laycock, N.; Kimpton, J.A.; Williams, D.E.

    2010-01-01

    In situ synchrotron X-ray diffraction was used to follow the formation of corrosion product scales on carbon steel in CO 2 saturated brine at temperatures from 40 to 90 o C. The corrosion process was accelerated by applying a small anodic current, and in selected tests a scale inhibitor, amino trimethylene phosphonic acid (ATMPA), was added. Siderite was identified as the major phase in the scale formed in all conditions. With increasing temperature, the scale formation rate increased, while the scale thickness and crystallite size decreased. Above 60 o C, the scale became increasingly protective. The scale thickness and crystallite size decreased with increasing ATMPA concentration.

  20. Measurement of Localized Corrosion Rates at Inclusion Particles in AA7075 by In Situ Three Dimensional (3D) X-ray Synchrotron Tomography

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Sudhanshu S.; Williams, Jason J.; Stannard, Tyler J.; Xiao, Xianghui; De Carlo, Francesco; Chawla, Nikhilesh

    2016-03-01

    In situ X-ray synchrotron tomography was used to measure the localized corrosion rate of Mg2Si particles present in 7075 aluminum alloys in deionized ultra-filtered (DIUF) water. The evolution of hydrogen bubbles was captured as a function of time and the measured volume was used to calculate the local corrosion rate of Mg2Si particles. It was shown that in the absence of chloride ions, stress was needed to create fresh particle surfaces, either by fracture or debonding, to initiate corrosion at the particles.

  1. X-ray Diffraction Study of Arsenopyrite at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    D Fan; M Ma; W Zhou; S Wei; Z Chen; H Xie

    2011-12-31

    The high-pressure X-ray diffraction study of a natural arsenopyrite was investigated up to 28.2 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at National Synchrotron Light Source, Brookhaven National Laboratory. The 16:3:1 methanol-ethanol-water mixture was used as a pressure-transmitting medium. Pressures were measured using the ruby-fluorescence method. No phase change has been observed up to 28.2 GPa. The isothermal equation of state (EOS) was determined. The values of K{sub 0}, and K'{sub 0} refined with a third-order Birch-Murnaghan EOS are K{sub 0} = 123(9) GPa, and K'{sub 0} = 5.2(8). Furthermore, we confirm that the linear compressibilities ({beta}) along a, b and c directions of arsenopyrite is elastically isotropic ({beta}{sub a} = 6.82 x 10{sup -4}, {beta}{sub b} = 6.17 x 10{sup -4} and {beta}{sub c} = 6.57 x 10{sup -4} GPa{sup -1}).

  2. In-Situ Synchrotron Radiation Study of Formation and Growth of Crystalline CexZr1-xO2 Nanoparticles Synthesized in Supercritical Water

    DEFF Research Database (Denmark)

    Tyrsted, Christoffer; Becker-Christensen, Jacob; Hald, Peter

    2010-01-01

    -zirconia system, the growth of ceria and zirconia nanoparticles is fundamentally different under supercritical water conditions. For comparison, ex situ synthesis has also been performed using an in-house supercritical flow reactor. The resulting samples were analyzed using PXRD, small-angle X-ray scattering......In situ synchrotron powder X-ray diffraction (PXRD) measurements have been conducted to follow the nucleation and growth of crystalline CexZr1-xO2 nanoparticles synthesized in supercritical water with a full substitution variation (x = 0, 0.2, 0.5, 0.8, and 1.0). Direction-dependent growth curves...... are determined and described using reaction kinetic models. A distinct change in growth kinetics is observed with increasing cerium content. For x = 0.8 and 1.0 (high cerium content), the growth is initially limited by the surface reaction kinetics; however, at a size of ∼6 nm, the growth changes and becomes...

  3. High pressure synthesis of amorphous TiO{sub 2} nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Quanjun; Liu, Ran; Wang, Tianyi; Xu, Ke; Dong, Qing; Liu, Bo; Liu, Bingbing, E-mail: liubb@jlu.edu.cn [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Liu, Jing [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)

    2015-09-15

    Amorphous TiO{sub 2} nanotubes with diameters of 8-10 nm and length of several nanometers were synthesized by high pressure treatment of anatase TiO{sub 2} nanotubes. The structural phase transitions of anatase TiO{sub 2} nanotubes were investigated by using in-situ high-pressure synchrotron X-ray diffraction (XRD) method. The starting anatase structure is stable up to ∼20GPa, and transforms into a high-density amorphous (HDA) form at higher pressure. Pressure-modified high- to low-density transition was observed in the amorphous form upon decompression. The pressure-induced amorphization and polyamorphism are in good agreement with the previous results in ultrafine TiO{sub 2} nanoparticles and nanoribbons. The relationship between the LDA form and α-PbO{sub 2} phase was revealed by high-resolution transmission electron microscopy (HRTEM) study. In addition, the bulk modulus (B{sub 0} = 158 GPa) of the anatase TiO{sub 2} nanotubes is smaller than those of the corresponding bulks and nanoparticles (180-240 GPa). We suggest that the unique open-ended nanotube morphology and nanosize play important roles in the high pressure phase transition of TiO{sub 2} nanotubes.

  4. Unravelling the High-Pressure Behaviour of Dye-Zeolite L Hybrid Materials

    Directory of Open Access Journals (Sweden)

    Lara Gigli

    2018-02-01

    Full Text Available Self-assembly of chromophores nanoconfined in porous materials such as zeolite L has led to technologically relevant host-guest systems exploited in solar energy harvesting, photonics, nanodiagnostics and information technology. The response of these hybrid materials to compression, which would be crucial to enhance their application range, has never been explored to date. By a joint high-pressure in situ synchrotron X-ray powder diffraction and ab initio molecular dynamics approach, herein we unravel the high-pressure behaviour of hybrid composites of zeolite L with fluorenone dye. High-pressure experiments were performed up to 6 GPa using non-penetrating pressure transmitting media to study the effect of dye loading on the structural properties of the materials under compression. Computational modelling provided molecular-level insight on the response to compression of the confined dye assemblies, evidencing a pressure-induced strengthening of the interaction between the fluorenone carbonyl group and zeolite L potassium cations. Our results reveal an impressive stability of the fluorenone-zeolite L composites at GPa pressures. The remarkable resilience of the supramolecular organization of dye molecules hyperconfined in zeolite L channels may open the way to the realization of optical devices able to maintain their functionality under extreme conditions.

  5. 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.

  6. Fundamentals of high pressure adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Y.P.; Zhou, L. [Tianjin University, Tianjin (China). High Pressure Adsorption Laboratory

    2009-12-15

    High-pressure adsorption attracts research interests following the world's attention to alternative fuels, and it exerts essential effect on the study of hydrogen/methane storage and the development of novel materials addressing to the storage. However, theoretical puzzles in high-pressure adsorption hindered the progress of application studies. Therefore, the present paper addresses the major theoretical problems that challenged researchers: i.e., how to model the isotherms with maximum observed in high-pressure adsorption; what is the adsorption mechanism at high pressures; how do we determine the quantity of absolute adsorption based on experimental data. Ideology and methods to tackle these problems are elucidated, which lead to new insights into the nature of high-pressure adsorption and progress in application studies, for example, in modeling multicomponent adsorption, hydrogen storage, natural gas storage, and coalbed methane enrichment, was achieved.

  7. Anomalous phase transition of InN nanowires under high pressure

    International Nuclear Information System (INIS)

    Tang Shun-Xi; Zhu Hong-Yang; Jiang Jun-Ru; Wu Xiao-Xin; Dong Yun-Xuan; Zhang Jian; Cui Qi-Liang; Yang Da-Peng

    2015-01-01

    Uniform InN nanowires were studied under pressures up to 35.5 GPa by using in situ synchrotron radiation x-ray diffraction technique at room temperature. An anomalous phase transition behavior has been discovered. Contrary to the results in the literature, which indicated that InN undergoes a fully reversible phase transition from the wurtzite structure to the rocksalt type structure, the InN nanowires in this study unusually showed a partially irreversible phase transition. The released sample contained the metastable rocksalt phase as well as the starting wurtzite one. The experimental findings of this study also reveal the potentiality of high pressure techniques to synthesize InN nanomaterials with the metastable rocksalt type structure, in addition to the generally obtained zincblende type one. (paper)

  8. High-pressure x-ray diffraction of icosahedral Zr-Al-Ni-Cu-Ag quasicrystals

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Saksl, Karel; Rasmussen, Helge Kildahl

    2001-01-01

    temperature using synchrotron radiation. The icosahedral quasicrystal structure is retained up to the highest hydrostatic pressure used (approximately 28 GPa) and is reversible after decompression. The bulk modulus at zero pressure and its pressure derivative of the icosahedral Zr-Al-Ni-Cu-Ag quasicrystal......The effect of pressure on the structural stability of icosahedral Zr-Al-Ni-Cu-Ag quasicrystals forming from a Zr65Al7.5Ni10Cu7.5Ag10 metallic glass with a supercooled liquid region of 44 K has been investigated by in situ high-pressure angle-dispersive x-ray powder diffraction at ambient......-Al-Ni-Cu-Ag quasicrystals induced by pressure....

  9. The high-pressure behavior of bloedite

    DEFF Research Database (Denmark)

    Comodi, Paola; Nazzareni, Sabrina; Balic Zunic, Tonci

    2014-01-01

    High-pressure single-crystal synchrotron X‑ray diffraction was carried out on a single crystal of bloedite [Na2Mg(SO4)24H2O] compressed in a diamond-anvil cell. The volume-pressure data, collected up to 11.2 GPa, were fitted by a second- and a third-order Birch-Murnaghan equation of state (EOS....... Pressure decreases significantly the distortion of Na coordination. Up to 10 GPa, the donor-acceptor oxygen distances decrease significantly and the difference between the two water molecules decreases with an increase in the strengths of hydrogen bonds. At the same time, the bond lengths from Na and Mg...... to O atoms of the water molecules decrease faster than other bonds to these cations suggesting that there is a coupling between the Na-Ow and Mg-Ow bond strengths and the “hydrogen transfer” to acceptor O atoms....

  10. SrWO4 at high pressures

    International Nuclear Information System (INIS)

    Grzechnik, A.; Crichton, W.A.; Hanfland, M.

    2005-01-01

    Room-temperature high-pressure behaviour of SrWO 4 scheelite (I4 1 /a, Z=4) has been studied to 20.7 GPa in a diamond anvil cell using synchrotron angle-dispersive X-ray powder diffraction. Above 10 GPa, it transforms to the fergusonite structure (I2/a, Z=4). Both scheelite and fergusonite types are ordered superstructures of fluorite (Fm anti 3m, Z=4). There is no significant volume collapse at the scheelite-fergusonite phase transition. However, the compression data including both phases of strontium tungstate cannot be fitted by a common Birch-Murnaghan equation of state. An onset of decomposition into component oxides occurs at about 15 GPa. The pressure-induced transformations are irreversible. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  11. High pressure studies on uranium and thorium silicide compounds: Experiment and theory

    DEFF Research Database (Denmark)

    Yagoubi, S.; Heathman, S.; Svane, A.

    2013-01-01

    The actinide silicides ThSi, USi and USi2 have been studied under high pressure using both theory and experiment. High pressure synchrotron X-ray diffraction experiments were performed on polycrystalline samples in diamond anvil cells at room temperature and for pressures up to 54, 52 and 26 GPa...

  12. In situ room temperature tensile deformation of a 1% CrMoV bainitic steel using synchrotron and neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weisser, M.A. [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Ecole Polytechnique Federale de Lausanne (EPFL), Institute of Materials (IMX), CH-1012 Lausanne (Switzerland); Evans, A.D.; Van Petegem, S. [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Holdsworth, S.R. [EMPA Materials Science and Technology, CH-8600 Duebendorf (Switzerland); Van Swygenhoven, H., E-mail: helena.vs@psi.ch [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Ecole Polytechnique Federale de Lausanne (EPFL), Institute of Materials (IMX), CH-1012 Lausanne (Switzerland)

    2011-06-15

    Neutron and synchrotron X-ray diffraction spectra have been acquired during room temperature tensile deformation of a creep-resistant bainitic 1% CrMoV steel, in order to study the evolution of internal microstresses and load-sharing mechanisms between the ferrite matrix and the various carbides. Cementite takes load from the plastifying matrix at the onset of macroscopic plasticity resulting in residual interphase stresses. Single peak fitting indicates an elastic anisotropic behaviour of cementite.

  13. High Pressure Industrial Water Facility

    Science.gov (United States)

    1992-01-01

    In conjunction with Space Shuttle Main Engine testing at Stennis, the Nordberg Water Pumps at the High Pressure Industrial Water Facility provide water for cooling the flame deflectors at the test stands during test firings.

  14. High Pressure Research on Materials

    Indian Academy of Sciences (India)

    example, represents the stress on the x plane in the y direction. There are three .... optical studies and studying compressibility of fluids. 3.2 Opposed ..... [4] G N Peggs, High Pressure Measurement Techniques, Applied Science. Publishers ...

  15. An in situ synchrotron energy-dispersive diffraction study of the hydration of oilwell cement systems under high temperature/autoclave conditions up to 130 deg. C

    International Nuclear Information System (INIS)

    Colston, Sally L.; Barnes, Paul; Jupe, Andrew C.; Jacques, Simon D.M.; Hall, Christopher; Livesey, Paul; Dransfield, John; Meller, Nicola; Maitland, Geoffrey C.

    2005-01-01

    The technique of synchrotron energy dispersive diffraction has been developed for in situ studies of cement hydration under autoclave conditions. This has been applied to oilwell cements hydrating at typical oilwell temperatures up to 130 deg. C. The results show clearly the detailed interplay between 11 detectable phases, from which a phase transformation scheme has been derived; this illustrates the progression of hydration up to 130 deg. C for two extreme cases, with and without conservation of water content and autoclave pressure. The monosulphate hydrate phases are found to exhibit different stability bounds, with a surprising sequence of the 14-water, 10-water then 12-water monosulphate as temperature/time increases; the latter form is particularly associated with conditions of water/pressure loss. The effect of retarders on C 3 S dissolution and CH formation is negligible above 70 deg. C, whereas the effect on the calcium sulphoaluminate hydrates is more complex, and possible reasons for this are discussed

  16. 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.

  17. In situ measurement of electromigration-induced transient stress in Pb-free Sn-Cu solder joints by synchrotron radiation based X-ray polychromatic microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Kunz, Martin; Tu, King-Ning; Lai, Yi-Shao

    2009-12-01

    Electromigration-induced hydrostatic elastic stress in Pb-free SnCu solder joints was studied by in situ synchrotron X-ray white beam microdiffraction. The elastic stresses in two different grains with similar crystallographic orientation, one located at the anode end and the other at the cathode end, were analyzed based on the elastic anisotropy of the Beta-Sn crystal structure. The stress in the grain at the cathode end remained constant except for temperature fluctuations, while the compressive stress in the grain at the anode end was built-up as a function of time during electromigration until a steady state was reached. The measured compressive stress gradient between the cathode and the anode is much larger than what is needed to initiate Sn whisker growth. The effective charge number of Beta-Sn derived from the electromigration data is in good agreement with the calculated value.

  18. In situ measurement of electromigration-induced transient stress in Pb-free Sn-Cu solder joints by synchrotron radiation based X-ray polychromatic microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Kunz, Martin; Tu, King-Ning; Lai, Yi-Shao

    2009-05-15

    Electromigration-induced hydrostatic elastic stress in Pb-free SnCu solder joints was studied by in situ synchrotron X-ray white beam microdiffraction. The elastic stresses in two different grains with similar crystallographic orientation, one located at the anode end and the other at the cathode end, were analyzed based on the elastic anisotropy of the {beta}-Sn crystal structure. The stress in the grain at the cathode end remained constant except for temperature fluctuations, while the compressive stress in the grain at the anode end was built-up as a function of time during electromigration until a steady state was reached. The measured compressive stress gradient between the cathode and the anode is much larger than what is needed to initiate Sn whisker growth. The effective charge number of {beta}-Sn derived from the electromigration data is in good agreement with the calculated value.

  19. High-Pressure Oxygen Generation for Outpost EVA Study

    Science.gov (United States)

    Jeng, Frank F.; Conger, Bruce; Ewert, Michael K.; Anderson, Molly S.

    2009-01-01

    The amount of oxygen consumption for crew extravehicular activity (EVA) in future lunar exploration missions will be significant. Eight technologies to provide high pressure EVA O2 were investigated. They are: high pressure O2 storage, liquid oxygen (LOX) storage followed by vaporization, scavenging LOX from Lander followed by vaporization, LOX delivery followed by sorption compression, water electrolysis followed by compression, stand-alone high pressure water electrolyzer, Environmental Control and Life Support System (ECLSS) and Power Elements sharing a high pressure water electrolyzer, and ECLSS and In-Situ Resource Utilization (ISRU) Elements sharing a high pressure electrolyzer. A trade analysis was conducted comparing launch mass and equivalent system mass (ESM) of the eight technologies in open and closed ECLSS architectures. Technologies considered appropriate for the two architectures were selected and suggested for development.

  20. High Pressure Reduction of Selenite by Shewanella oneidensis MR-1

    Science.gov (United States)

    Picard, A.; Daniel, I.; Testemale, D.; Letard, I.; Bleuet, P.; Cardon, H.; Oger, P.

    2007-12-01

    High-pressure biotopes comprise cold deep-sea environments, hydrothermal vents, and deep subsurface or deep-sea sediments. The latter are less studied, due to the technical difficulties to sample at great depths without contamination. Nevertheless, microbial sulfate reduction and methanogenesis have been found to be spatially distributed in deep deep-sea sediments (1), and sulfate reduction has been shown to be actually more efficient under high hydrostatic pressure (HHP) in some sediments (2). Sulfate-reducing bacteria obtained from the Japan Sea are characterized by an increased sulfide production under pressure (3,4). Unfortunately, investigations of microbial metabolic activity as a function of pressure are extremely scarce due to the experimental difficulty of such measurements at high hydrostatic pressure. We were able to measure the reduction of selenite Se(IV) by Shewanella oneidensis MR-1 as a function of pressure, to 150 MPa using two different high-pressure reactors that allow in situ X-ray spectroscopy measurements on a synchrotron source. A first series of measurements was carried out in a low-pressure Diamond Anvil Cell (DAC) of our own design (5) at ID22 beamline at ESRF (European Synchrotron Radiation Facility); a second one was performed in an autoclave (6) at the BM30B beamline at ESRF. Selenite reduction by strain MR-17 was monitored from ambient pressure to 150 MPa over 25 hours at 30 deg C by XANES spectroscopy (X-ray Analysis of Near Edge Structure). Spectra were recorded hourly in order to quantify the evolution of the oxidation state of selenium with time. Stationary-phase bacteria were inoculated at a high concentration into fresh growth medium containing 5 or 10 M of sodium selenite and 20 mM sodium lactate. Kinetic parameters of the Se (IV) reduction by Shewanella oneidensis strain MR-1 could be extracted from the data, as a function of pressure. They show 1) that the rate constant k of the reaction is decreased by a half at high pressure

  1. Path Dependency of High Pressure Phase Transformations

    Science.gov (United States)

    Cerreta, Ellen

    2017-06-01

    At high pressures titanium and zirconium are known to undergo a phase transformation from the hexagonal close packed (HCP), alpha-phase to the simple-hexagonal, omega-phase. Under conditions of shock loading, the high-pressure omega-phase can be retained upon release. It has been shown that temperature, peak shock stress, and texture can influence the transformation. Moreover, under these same loading conditions, plastic processes of slip and twinning are also affected by similar differences in the loading path. To understand this path dependency, in-situ velocimetry measurements along with post-mortem metallographic and neutron diffraction characterization of soft recovered specimens have been utilized to qualitatively understand the kinetics of transformation, quantify volume fraction of retained omega-phase and characterize the shocked alpha and omega-phases. Together the work described here can be utilized to map the non-equilibrium phase diagram for these metals and lend insight into the partitioning of plastic processes between phases during high pressure transformation. In collaboration with: Frank Addesssio, Curt Bronkhorst, Donald Brown, David Jones, Turab Lookman, Benjamin Morrow, Carl Trujillo, Los Alamos National Lab.; Juan Pablo Escobedo-Diaz, University of New South Wales; Paulo Rigg, Washington State University.

  2. IN-SITU SYNCHROTRON PXRD STUDY OF SPINEL TYPE LiMn2O4 NANOCRYSTAL FORMATION

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    Many solvothermal reactions have a great potential for environmentally friendly and easily scalable way for producing nanocrystalline materials on an industrial scale. Here we study hydrothermal formation of spinel LiMn2O4 which is a well-known cathode material for Li-ion batteries. The LiMn2O4...... nanoparticles are formed by reducing KMnO4 in an aqueous solution containing Li-ions. The reducing agent is an alcohol (here ethanol) and the reaction takes place under high pressure and temperature. The LiMn2O4 nanocrystals are unstable towards further reduction to Mn3O4 nanocrystals. Proposed reaction route...

  3. Static tensile deformation behavior of a lean duplex stainless steel studied by in situ neutron diffraction and synchrotron radiation white x-rays

    International Nuclear Information System (INIS)

    Tsuchida, Noriyuki; Kawahata, Taiji; Ishimaru, Eiichiro; Takahashi, Akihiko; Suzuki, Hiroshi; Shobu, Takahisa

    2013-01-01

    To investigate the tensile deformation behavior of a lean duplex stainless steel (S32101) from the viewpoints of plastic deformability among phases or grains, we performed static tensile tests, in situ neutron diffraction, and white x-ray diffraction experiments at room temperature. In the static tensile tests, the S32101 steel displayed a larger uniform elongation and a better tensile strength-uniform elongation balance than a commercial SUS329J4L duplex stainless steel. A larger uniform elongation of S32101 is associated with the macroscopic work hardening behavior that a work hardening rate higher than the flow stress can maintain up until high true strains. From the experimental results of synchrotron radiation white x-ray diffraction experiments, the hard phase of S32101 was changed from the ferrite (α) phase to austenite (γ) one during tensile deformation. This led to a larger stress partitioning between the phases at the latter stage of deformation. From the experimental results of in situ neutron diffraction, it was found that the stress partitioning of the γ phase in the S32101 was the largest among the present results. Therefore, the larger work hardening rate of S32101 can be explained by the large stress partitioning of the γ phase, that between γ and α phases and γ volume fraction. (author)

  4. In-situ study of electromigration-induced grain rotation in Pb-free solder joint by synchrotron microdiffraction

    International Nuclear Information System (INIS)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2008-01-01

    The rotation of Sn grains in Pb-free flip chip solder joints hasn't been reported in literature so far although it has been observed in Sn strips. In this letter, we report the detailed study of the grain orientation evolution induced by electromigration by synchrotron based white beam X-ray microdiffraction. It is found that the grains in solder joint rotate more slowly than in Sn strip even under higher current density. On the other hand, based on our estimation, the reorientation of the grains in solder joints also results in the reduction of electric resistivity, similar to the case of Sn strip. We will also discuss the reason why the electric resistance decreases much more in strips than in the Sn-based solders, and the different driving force for the grain growth in solder joint and in thin film interconnect lines

  5. In-situ study of electromigration-induced grain rotation in Pb-free solder joint by synchrotron microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2008-10-31

    The rotation of Sn grains in Pb-free flip chip solder joints hasn't been reported in literature so far although it has been observed in Sn strips. In this letter, we report the detailed study of the grain orientation evolution induced by electromigration by synchrotron based white beam X-ray microdiffraction. It is found that the grains in solder joint rotate more slowly than in Sn strip even under higher current density. On the other hand, based on our estimation, the reorientation of the grains in solder joints also results in the reduction of electric resistivity, similar to the case of Sn strip. We will also discuss the reason why the electric resistance decreases much more in strips than in the Sn-based solders, and the different driving force for the grain growth in solder joint and in thin film interconnect lines.

  6. High-pressure sodium lamp

    NARCIS (Netherlands)

    1996-01-01

    A high pressure sodium lamp of the invention is provided with a discharge vessel (20) which is enclosed with intervening space (1) by an outer bulb (10), which space contains a gas-fill with at least 70 mol. % nitrogen gas. Electrodes (30a, 30b) are positioned in the discharge vessel (20) and are

  7. Intermolecular Interactions at high pressure

    DEFF Research Database (Denmark)

    Eikeland, Espen Zink

    2016-01-01

    In this project high-pressure single crystal X-ray diffraction has been combined with quantitative energy calculations to probe the energy landscape of three hydroquinone clathrates enclosing different guest molecules. The simplicity of the hydroquinone clathrate structures together with their st...

  8. High-pressure water facility

    Science.gov (United States)

    2006-01-01

    NASA Test Operations Group employees, from left, Todd Pearson, Tim Delcuze and Rodney Wilkinson maintain a water pump in Stennis Space Center's high-pressure water facility. The three were part of a group of employees who rode out Hurricane Katrina at the facility and helped protect NASA's rocket engine test complex.

  9. Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation.

    Science.gov (United States)

    Schroeder, J L; Thomson, W; Howard, B; Schell, N; Näslund, L-Å; Rogström, L; Johansson-Jõesaar, M P; Ghafoor, N; Odén, M; Nothnagel, E; Shepard, A; Greer, J; Birch, J

    2015-09-01

    We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (>50 keV), high photon flux (>10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (film formation processes. The high-energy synchrotron-radiation based x-rays result in small scattering angles (industry-relevant processes. We openly encourage the materials research community to contact us for collaborative opportunities using this unique and versatile scientific instrument.

  10. Stability of Hydrogen-Bonded Supramolecular Architecture under High Pressure Conditions: Pressure-Induced Amorphization in Melamine-Boric Acid Adduct

    International Nuclear Information System (INIS)

    Wang, K.; Duan, D.; Wang, R.; Lin, A.; Cui, Q.; Liu, B.; Cui, T.; Zou, B.; Zhang, X.

    2009-01-01

    The effects of high pressure on the structural stability of the melamine-boric acid adduct (C3N6H6 2H3BO3, M 2B), a three-dimensional hydrogen-bonded supramolecular architecture, were studied by in situ synchrotron X-ray diffraction (XRD) and Raman spectroscopy. M 2B exhibited a high compressibility and a strong anisotropic compression, which can be explained by the layerlike crystal packing. Furthermore, evolution of XRD patterns and Raman spectra indicated that the M 2B crystal undergoes a reversible pressure-induced amorphization (PIA) at 18 GPa. The mechanism for the PIA was attributed to the competition between close packing and long-range order. Ab initio calculations were also performed to account for the behavior of hydrogen bonding under high pressure.

  11. High pressure phase transformations revisited.

    Science.gov (United States)

    Levitas, Valery I

    2018-04-25

    High pressure phase transformations play an important role in the search for new materials and material synthesis, as well as in geophysics. However, they are poorly characterized, and phase transformation pressure and pressure hysteresis vary drastically in experiments of different researchers, with different pressure transmitting media, and with different material suppliers. Here we review the current state, challenges in studying phase transformations under high pressure, and the possible ways in overcoming the challenges. This field is critically compared with fields of phase transformations under normal pressure in steels and shape memory alloys, as well as plastic deformation of materials. The main reason for the above mentioned discrepancy is the lack of understanding that there is a fundamental difference between pressure-induced transformations under hydrostatic conditions, stress-induced transformations under nonhydrostatic conditions below yield, and strain-induced transformations during plastic flow. Each of these types of transformations has different mechanisms and requires a completely different thermodynamic and kinetic description and experimental characterization. In comparison with other fields the following challenges are indicated for high pressure phase transformation: (a) initial and evolving microstructure is not included in characterization of transformations; (b) continuum theory is poorly developed; (c) heterogeneous stress and strain fields in experiments are not determined, which leads to confusing material transformational properties with a system behavior. Some ways to advance the field of high pressure phase transformations are suggested. The key points are: (a) to take into account plastic deformations and microstructure evolution during transformations; (b) to formulate phase transformation criteria and kinetic equations in terms of stress and plastic strain tensors (instead of pressure alone); (c) to develop multiscale continuum

  12. High pressure phase transformations revisited

    Science.gov (United States)

    Levitas, Valery I.

    2018-04-01

    High pressure phase transformations play an important role in the search for new materials and material synthesis, as well as in geophysics. However, they are poorly characterized, and phase transformation pressure and pressure hysteresis vary drastically in experiments of different researchers, with different pressure transmitting media, and with different material suppliers. Here we review the current state, challenges in studying phase transformations under high pressure, and the possible ways in overcoming the challenges. This field is critically compared with fields of phase transformations under normal pressure in steels and shape memory alloys, as well as plastic deformation of materials. The main reason for the above mentioned discrepancy is the lack of understanding that there is a fundamental difference between pressure-induced transformations under hydrostatic conditions, stress-induced transformations under nonhydrostatic conditions below yield, and strain-induced transformations during plastic flow. Each of these types of transformations has different mechanisms and requires a completely different thermodynamic and kinetic description and experimental characterization. In comparison with other fields the following challenges are indicated for high pressure phase transformation: (a) initial and evolving microstructure is not included in characterization of transformations; (b) continuum theory is poorly developed; (c) heterogeneous stress and strain fields in experiments are not determined, which leads to confusing material transformational properties with a system behavior. Some ways to advance the field of high pressure phase transformations are suggested. The key points are: (a) to take into account plastic deformations and microstructure evolution during transformations; (b) to formulate phase transformation criteria and kinetic equations in terms of stress and plastic strain tensors (instead of pressure alone); (c) to develop multiscale continuum

  13. In situ biological dose mapping estimates the radiation burden delivered to 'spared' tissue between synchrotron X-ray microbeam radiotherapy tracks.

    Directory of Open Access Journals (Sweden)

    Kai Rothkamm

    Full Text Available Microbeam radiation therapy (MRT using high doses of synchrotron X-rays can destroy tumours in animal models whilst causing little damage to normal tissues. Determining the spatial distribution of radiation doses delivered during MRT at a microscopic scale is a major challenge. Film and semiconductor dosimetry as well as Monte Carlo methods struggle to provide accurate estimates of dose profiles and peak-to-valley dose ratios at the position of the targeted and traversed tissues whose biological responses determine treatment outcome. The purpose of this study was to utilise γ-H2AX immunostaining as a biodosimetric tool that enables in situ biological dose mapping within an irradiated tissue to provide direct biological evidence for the scale of the radiation burden to 'spared' tissue regions between MRT tracks. Γ-H2AX analysis allowed microbeams to be traced and DNA damage foci to be quantified in valleys between beams following MRT treatment of fibroblast cultures and murine skin where foci yields per unit dose were approximately five-fold lower than in fibroblast cultures. Foci levels in cells located in valleys were compared with calibration curves using known broadbeam synchrotron X-ray doses to generate spatial dose profiles and calculate peak-to-valley dose ratios of 30-40 for cell cultures and approximately 60 for murine skin, consistent with the range obtained with conventional dosimetry methods. This biological dose mapping approach could find several applications both in optimising MRT or other radiotherapeutic treatments and in estimating localised doses following accidental radiation exposure using skin punch biopsies.

  14. Structure and bulk modulus of Ln-doped UO{sub 2} (Ln = La, Nd) at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Rittman, Dylan R., E-mail: drittman@stanford.edu [Department of Geological Sciences, Stanford University, Stanford, CA 94305 (United States); Park, Sulgiye; Tracy, Cameron L. [Department of Geological Sciences, Stanford University, Stanford, CA 94305 (United States); Zhang, Lei [Peter A. Rock Thermochemistry Laboratory and NEAT ORU, University of California Davis, Davis, CA 95616 (United States); Department of Chemical Engineering and Materials Science, University of California Davis, Davis, CA 95616 (United States); Palomares, Raul I.; Lang, Maik [Department of Nuclear Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Navrotsky, Alexandra [Peter A. Rock Thermochemistry Laboratory and NEAT ORU, University of California Davis, Davis, CA 95616 (United States); Department of Chemical Engineering and Materials Science, University of California Davis, Davis, CA 95616 (United States); Mao, Wendy L. [Department of Geological Sciences, Stanford University, Stanford, CA 94305 (United States); Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, CA 94025 (United States); Ewing, Rodney C. [Department of Geological Sciences, Stanford University, Stanford, CA 94305 (United States)

    2017-07-15

    The structure of lanthanide-doped uranium dioxide, Ln{sub x}U{sub 1-x}O{sub 2-0.5x+y} (Ln = La, Nd), was investigated at pressures up to ∼50–55 GPa. Samples were synthesized with different lanthanides at different concentrations (x ∼ 0.2 and 0.5), and all were slightly hyperstoichiometric (y ∼ 0.25–0.4). In situ high-pressure synchrotron X-ray diffraction was used to investigate their high-pressure phase behavior and determine their bulk moduli. All samples underwent a fluorite-to-cotunnite phase transformation with increasing pressure. The pressure of the phase transformation increased with increasing hyperstoichiometry, which is consistent with results from previous computational simulations. Bulk moduli are inversely proportional to both the ionic radius of the lanthanide and its concentration, as quantified using a weighted cationic radius ratio. This trend was found to be consistent with the behavior of other elastic properties measured for Ln-doped UO{sub 2}, such as Young's modulus. - Highlights: •Ln-doped UO{sub 2} transforms from fluorite to cotunnite at high pressure. •Transition pressure increases with increasing hyperstoichiometry. •Bulk modulus decreases with increasing Ln-dopant radius and concentration.

  15. In-situ observation of oxidation of Ti(0001) surface by real-time photoelectron spectroscopy using synchrotron radiation

    CERN Document Server

    Takakuwa, Y; Yoshigoe, A; Teraoka, Y; Mizuno, Y; Tonda, H; Homma, T

    2003-01-01

    Temperature dependence of the initial oxidation kinetics of Ti(0001) surface was investigated by low energy electron diffraction (LEED) and real-time photoelectron spectroscopy using synchrotron radiation of surface- and bulk-sensitive photon energies. LEED observation revealed that oxide layers grow epitaxially with different surface structures depending on temperature: 1x1 at 200degC and sq root 3 x sq root 3 at 400degC. From the oxygen uptake curve measured by O 1s photo-electron intensity, it was clarified that oxygen diffusion through the epitaxially grown oxide layer is significantly enhanced with raising temperature, making the oxide layer thicker than 70A at 400degC. The chemical shift components observed for Ti 2p showed that TiO sub 2 becomes predominant at the subsurface with O sub 2 dose, while the stoichiometry of oxide near the interface is maintained as TiO and Ti sub 2 O sub 3 , for both cases at 200degC and 400degC. Thus it is concluded that the epitaxial growth of a very thin oxide on the Ti...

  16. Dynamics of mineral crystallization from precipitated slab-derived fluid phase: first in situ synchrotron X-ray measurements

    Science.gov (United States)

    Malaspina, Nadia; Alvaro, Matteo; Campione, Marcello; Wilhelm, Heribert; Nestola, Fabrizio

    2015-03-01

    Remnants of the fluid phase at ultrahigh pressure (UHP) in subduction environments may be preserved as primary multiphase inclusions in UHP minerals. The mode of crystallization of daughter minerals during precipitation within the inclusion and/or the mechanism of interaction between the fluid at supercritical conditions and the host mineral are still poorly understood from a crystallographic point of view. A case study is represented by garnet-orthopyroxenites from the Maowu Ultramafic Complex (China) deriving from harzburgite precursors metasomatized at ~4 GPa, 750 °C by a silica- and incompatible trace element-rich fluid phase. This metasomatism produced poikilitic orthopyroxene and inclusion-rich garnet porphyroblasts. Solid multiphase primary inclusions in garnet display a size within a few tens of micrometres and negative crystal shapes. Infilling minerals (spinel: 10-20 vol%; amphibole, chlorite, talc, mica: 80-90 vol%) occur with constant volume proportions and derive from trapped solute-rich aqueous fluids. To constrain the possible mode of precipitation of daughter minerals, we performed for the first time a single-crystal X-ray diffraction experiment by synchrotron radiation at Diamond Light Source. In combination with electron probe microanalyses, this measurement allowed the unique identification of each mineral phase and reciprocal orientations. We demonstrated the epitaxial relationship between spinel and garnet and between some hydrous minerals. Such information is discussed in relation to the physico-chemical aspects of nucleation and growth, shedding light on the mode of mineral crystallization from a fluid phase trapped at supercritical conditions.

  17. Methodology for Analyzing Strain States During In-Situ Thermomechanical Cycling in Individual Lead Free Solder Joints Using Synchrotron Radiation

    International Nuclear Information System (INIS)

    Zhou, Bite; Bieler, Thomas R.; Lee, Tae-Kyu; Liu, Kuo-Chuan

    2009-01-01

    To examine how a lead-free solder joint deforms in a thermal cycling environment, both the elastic and plastic stress and strain behavior must be understood. Methods to identify evolution of the internal strain (stress) state during thermal cycling are described. A slice of a package containing a single row of solder joints was thermally cycled from 0 C to 100 C with a period of about 1 h with concurrent acquisition of transmission Laue patterns using synchrotron radiation. These results indicated that most joints are single crystals, with some being multicrystals with no more than a few Sn grain orientations. Laue patterns were analyzed to estimate local strains in different crystal directions at different temperatures during a thermal cycle. While the strains perpendicular to various crystal planes all vary in a similar way, the magnitude of strain varies. The specimens were subsequently given several hundred additional thermal cycles and measured again to assess changes in the crystal orientations. These results show that modest changes in crystal orientations occur during thermal cycling.

  18. High-Pressure Design of Advanced BN-Based Materials

    Directory of Open Access Journals (Sweden)

    Oleksandr O. Kurakevych

    2016-10-01

    Full Text Available The aim of the present review is to highlight the state of the art in high-pressure design of new advanced materials based on boron nitride. Recent experimental achievements on the governing phase transformation, nanostructuring and chemical synthesis in the systems containing boron nitride at high pressures and high temperatures are presented. All these developments allowed discovering new materials, e.g., ultrahard nanocrystalline cubic boron nitride (nano-cBN with hardness comparable to diamond, and superhard boron subnitride B13N2. Thermodynamic and kinetic aspects of high-pressure synthesis are described based on the data obtained by in situ and ex situ methods. Mechanical and thermal properties (hardness, thermoelastic equations of state, etc. are discussed. New synthetic perspectives, combining both soft chemistry and extreme pressure–temperature conditions are considered.

  19. Computer simulation at high pressure

    International Nuclear Information System (INIS)

    Alder, B.J.

    1977-11-01

    The use of either the Monte Carlo or molecular dynamics method to generate equations-of-state data for various materials at high pressure is discussed. Particular emphasis is given to phase diagrams, such as the generation of various types of critical lines for mixtures, melting, structural and electronic transitions in solids, two-phase ionic fluid systems of astrophysical interest, as well as a brief aside of possible eutectic behavior in the interior of the earth. Then the application of the molecular dynamics method to predict transport coefficients and the neutron scattering function is discussed with a view as to what special features high pressure brings out. Lastly, an analysis by these computational methods of the measured intensity and frequency spectrum of depolarized light and also of the deviation of the dielectric measurements from the constancy of the Clausius--Mosotti function is given that leads to predictions of how the electronic structure of an atom distorts with pressure

  20. Terbium oxide at high pressures

    International Nuclear Information System (INIS)

    Dogra, Sugandha; Sharma, Nita Dilawar; Singh, Jasveer; Bandhyopadhyay, A.K.

    2011-01-01

    In this work we report the behaviour of terbium oxide at high pressures. The as received sample was characterized at ambient by X-ray diffraction and Raman spectroscopy. The X-ray diffraction showed the sample to be predominantly cubic Tb 4 O 7 , although a few peaks also match closely with Tb 2 O 3 . In fact in a recent study done on the same sample, the sample has been shown to be a mixture of Tb 4 O 7 and Tb 2 O 3 . The sample was subjected to high pressures using a Mao-Bell type diamond anvil cell upto a pressure of about 42 GPa with ruby as pressure monitor

  1. Cryogenic, Absolute, High Pressure Sensor

    Science.gov (United States)

    Chapman, John J. (Inventor); Shams. Qamar A. (Inventor); Powers, William T. (Inventor)

    2001-01-01

    A pressure sensor is provided for cryogenic, high pressure applications. A highly doped silicon piezoresistive pressure sensor is bonded to a silicon substrate in an absolute pressure sensing configuration. The absolute pressure sensor is bonded to an aluminum nitride substrate. Aluminum nitride has appropriate coefficient of thermal expansion for use with highly doped silicon at cryogenic temperatures. A group of sensors, either two sensors on two substrates or four sensors on a single substrate are packaged in a pressure vessel.

  2. Cryogenic High Pressure Sensor Module

    Science.gov (United States)

    Chapman, John J. (Inventor); Shams, Qamar A. (Inventor); Powers, William T. (Inventor)

    1999-01-01

    A pressure sensor is provided for cryogenic, high pressure applications. A highly doped silicon piezoresistive pressure sensor is bonded to a silicon substrate in an absolute pressure sensing configuration. The absolute pressure sensor is bonded to an aluminum nitride substrate. Aluminum nitride has appropriate coefficient of thermal expansion for use with highly doped silicon at cryogenic temperatures. A group of sensors, either two sensors on two substrates or four sensors on a single substrate are packaged in a pressure vessel.

  3. Brillouin scattering at high pressures

    International Nuclear Information System (INIS)

    Grimsditch, M.; Polian, A.

    1988-02-01

    Technical advances which have made Brillouin scattering a useful tool in high pressure diamond anvil cell (DAC) studies, viz. multipassing and tandem operation of Fabry-Perot interferometers, are reviewed. Experimental aspects, such as allowed scattering geometries, are outlined and the data analysis required to transform Brillouin spectra into sound velocities and elastic constants is presented. Experimental results on H 2 , N 2 , Ar, and He are presented, and the close relationship between the Brillouin scattering results and equations of state is highlighted

  4. High Pressure X-Ray Diffraction Studies on Nanocrystalline Materials

    Science.gov (United States)

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

    2003-01-01

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

  5. Strain engineered pyrochlore at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Rittman, Dylan R.; Turner, Katlyn M.; Park, Sulgiye; Fuentes, Antonio F.; Park, Changyong; Ewing, Rodney C.; Mao, Wendy L.

    2017-05-22

    Strain engineering is a promising method for next-generation materials processing techniques. Here, we use mechanical milling and annealing followed by compression in diamond anvil cell to tailor the intrinsic and extrinsic strain in pyrochlore, Dy2Ti2O7 and Dy2Zr2O7. Raman spectroscopy, X-ray pair distribution function analysis, and X-ray diffraction were used to characterize atomic order over short-, medium-, and long-range spatial scales, respectively, under ambient conditions. Raman spectroscopy and X-ray diffraction were further employed to interrogate the material in situ at high pressure. High-pressure behavior is found to depend on the species and concentration of defects in the sample at ambient conditions. Overall, we show that defects can be engineered to lower the phase transformation onset pressure by ~50% in the ordered pyrochlore Dy2Zr2O7, and lower the phase transformation completion pressure by ~20% in the disordered pyrochlore Dy2Zr2O7. These improvements are achieved without significantly sacrificing mechanical integrity, as characterized by bulk modulus.

  6. In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

    International Nuclear Information System (INIS)

    Yun, Di; Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M.

    2015-01-01

    U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

  7. In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

    Energy Technology Data Exchange (ETDEWEB)

    Yun, Di, E-mail: diyun1979@xjtu.edu.cn [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Xi' an Jiao Tong University, 28 Xian Ning West Road, Xi' an 710049 (China); Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M. [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

    2015-12-15

    U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

  8. High-pressure structures of methane hydrate

    International Nuclear Information System (INIS)

    Hirai, H; Uchihara, Y; Fujihisa, H; Sakashita, M; Katoh, E; Aoki, K; Yamamoto, Y; Nagashima, K; Yagi, T

    2002-01-01

    Three high-pressure structures of methane hydrate, a hexagonal structure (str. A) and two orthorhombic structures (str. B and str. C), were found by in situ x-ray diffractometry and Raman spectroscopy. The well-known structure I (str. I) decomposed into str. A and fluid at 0.8 GPa. Str. A transformed into str. B at 1.6 GPa, and str. B further transformed into str. C at 2.1 GPa which survived above 7.8 GPa. The fluid solidified as ice VI at 1.4 GPa, and the ice VI transformed to ice VII at 2.1 GPa. The bulk moduli, K 0 , for str. I, str. A, and str. C were calculated to be 7.4, 9.8, and 25.0 GPa, respectively

  9. Following the electroreduction of uranium dioxide to uranium in LiCl–KCl eutectic in situ using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Brown, L.D.; Abdulaziz, R.; Jervis, R.; Bharath, V.J. [Electrochemical Innovation Lab, Dept. Chemical Engineering, UCL, London WC1E 7JE (United Kingdom); Atwood, R.C.; Reinhard, C.; Connor, L.D. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Simons, S.J.R.; Inman, D.; Brett, D.J.L. [Electrochemical Innovation Lab, Dept. Chemical Engineering, UCL, London WC1E 7JE (United Kingdom); Shearing, P.R., E-mail: p.shearing@ucl.ac.uk [Electrochemical Innovation Lab, Dept. Chemical Engineering, UCL, London WC1E 7JE (United Kingdom)

    2015-09-15

    Highlights: • We investigated the electroreduction of UO{sub 2} to U in LiCl/KCL eutectic molten salt. • Combined electrochemical measurement and in situ XRD is utilised. • The electroreduction appears to occur in a single, 4-electron-step, process. • No intermediate compounds were observed. - Abstract: The electrochemical reduction of uranium dioxide to metallic uranium has been investigated in lithium chloride–potassium chloride eutectic molten salt. Laboratory based electrochemical studies have been coupled with in situ energy dispersive X-ray diffraction, for the first time, to deduce the reduction pathway. No intermediate phases were identified using the X-ray diffraction before, during or after electroreduction to form α-uranium. This suggests that the electrochemical reduction occurs via a single, 4-electron-step, process. The rate of formation of α-uranium is seen to decrease during electrolysis and could be a result of a build-up of oxygen anions in the molten salt. Slow transport of O{sup 2−} ions away from the UO{sub 2} working electrode could impede the electrochemical reduction.

  10. Micromechanics of deformation of metallic-glass-matrix composites from in situ synchrotron strain measurements and finite element modeling

    International Nuclear Information System (INIS)

    Ott, R.T.; Sansoz, F.; Molinari, J.F.; Almer, J.; Ramesh, K.T.; Hufunagel, T.C.

    2005-01-01

    In situ X-ray scattering and finite element modeling (FEM) were used to examine the micromechanics of deformation of in situ formed metallic-glass-matrix composites consisting of Ta-rich particles dispersed in an amorphous matrix. The strain measurements show that under uniaxial compression the second-phase particles yield at an applied stress of approx. 325 MPa. After yielding, the particles do not strain harden significantly; we show that this is due to an increasingly hydrostatic stress state arising from the lateral constraint on deformation of the particles imposed by the elastic matrix. Shear band initiation in the matrix is not due to the difference in elastic properties between the matrix and the particles. Rather, the development of a plastic misfit strain causes stress concentrations around the particles, resulting in localized yielding of the matrix by shear band formation at an applied stress of approx. 1450 MPa, considerably lower than the macroscopic yield stress of the composite (approx. 1725 MPa). Shear bands do not propagate at the lower stress because the yield criterion of the matrix is only satisfied in the region immediately around the particles. At the higher stresses, the yield criterion is satisfied in large regions of the matrix, allowing extensive shear band propagation and significant macroscopic plastic deformation. However, the presence of the particles makes the stress state highly inhomogeneous, which may partially explain why fracture is suppressed in the composite, allowing the development of large plastic strains

  11. In-situ synchrotron x-ray study of the crystallization behavior of Ce0.9La0.1O2−x thin films deposited on NiW alloy substrates by chemical solution method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; Abrahamsen, Asger Bech

    2011-01-01

    The phase and texture formation of La doped CeO2 (CLO) films deposited by the chemical solution method are studied by in situ synchrotron x-ray diffraction. It is found that the CLO crystallites forms excellent in-plane texture as soon as the phase appears at 860°C, indicating that interfacial nu...... by diffusion. The success of this work demonstrates the possibility of studying crystallization behaviors of solution derived films using a non-destructive method, which has the potential of being applicable to most types of thin film samples.......The phase and texture formation of La doped CeO2 (CLO) films deposited by the chemical solution method are studied by in situ synchrotron x-ray diffraction. It is found that the CLO crystallites forms excellent in-plane texture as soon as the phase appears at 860°C, indicating that interfacial...

  12. 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.

  13. In situ synchrotron X-ray diffraction of ferroelastic La0.8Ca0.2CoO3 ceramics during uniaxial compression

    International Nuclear Information System (INIS)

    Vullum, Per Erik; Mastin, Johann; Wright, Jonathan; Einarsrud, Mari-Ann; Holmestad, Randi; Grande, Tor

    2006-01-01

    Uniaxial compression of rhombohedral La 0.8 Ca 0.2 CoO 3 ceramics has been studied in situ using synchrotron X-ray diffraction. The intensities of Bragg reflections parallel and perpendicular to the stress field were simultaneously detected as a function of the stress. Reorientation of ferroelastic domains due to the uniaxial stress was demonstrated. With increasing stress the volume fraction of domains with the hexagonal c-axis parallel to the stress axis increased at the expense of domains with the c-axis perpendicular to the stress axis. The strain in the polycrystalline materials evolved unevenly with increasing stress due to crystallographic anisotropy. In energetically favourable domains with the c-axis parallel to the stress axis, the rhombohedral distortion from cubic symmetry increased, while the crystal structure became closer to cubic in domains with the c-axis perpendicular to the stress. Successive compression/decompression cycles to higher maximum stress resulted in a higher volume fraction of reoriented domains both at maximum stress and after decompression

  14. In situ synchrotron X-ray powder diffraction study of the early hydration of α-tricalcium phosphate/tricalcium silicate composite bone cement

    Energy Technology Data Exchange (ETDEWEB)

    Morejon-Alonso, Loreley; Correa, Jose Raul, E-mail: lmorejon@fq.uh.cu [Departamento de Quimica General, Facultad de Quimica, Universidad de La Habana, UH (Cuba); Motisuke, Mariana [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil); Carrodeguas, Raul Garcia [Universidade Federal de Campina Grande (UFCG), Campina Grande, PB (Brazil). Laboratorio de Avaliacao e Desenvolvimento de Biomateriais do Nordeste; Santos, Luis Alberto dos [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Escola de Engenharia. Departamento de Materiais

    2015-01-15

    Bioactivity, osteogenicity and mechanical properties of α-tricalcium phosphate (α-TCP) based phosphates cements can be improved by adding tricalcium silicate (C{sub 3}S); however, the addition of C{sub 3}S delays the precipitation and growth of calcium deficient hydroxyapatite (CDHA). Thus, the aim of this work was the study of in situ setting reaction of α-TCP/C{sub 3}S composite bone cement under high energy X-ray generated by a synchrotron source within the first 72h. The results showed that the addition of C{sub 3}S induces the precipitation of nanosized CDHA at early times depending on the added content. Calculated crystallite sizes showed that the higher the content of C{sub 3}S, the smaller the crystal size at the beginning of the precipitation. These results are different from those obtained by conventional XRD method, suggesting that the proposed technique is a powerful tool in determining the composition and extent of reaction of CPCs surfaces in real time. (author)

  15. Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

    International Nuclear Information System (INIS)

    Haboub, Abdel; Nasiatka, James R.; MacDowell, Alastair A.; Bale, Hrishikesh A.; Cox, Brian N.; Marshall, David B.; Ritchie, Robert O.

    2014-01-01

    A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C

  16. In situ synchrotron analysis of lattice rotations in individual grains during stress-induced martensitic transformations in a polycrystalline CuAlBe shape memory alloy

    International Nuclear Information System (INIS)

    Berveiller, S.; Malard, B.; Wright, J.; Patoor, E.; Geandier, G.

    2011-01-01

    Highlights: → 3DXRD, Laue microdiffraction measurements of grain rotation in a shape memory alloy. → During stress-induced martensitic transformation, the austenite grains rotate. → This rotation reverses with the reverse transformation. → The austenite grains splits into various orientations with martensite formation. - Abstract: Two synchrotron diffraction techniques, three-dimensional X-ray diffraction and Laue microdiffraction, are applied to studying the deformation behaviour of individual grains embedded in a Cu 74 Al 23 Be 3 superelastic shape memory alloy. The average lattice rotation and the intragranular heterogeneity of orientations are measured during in situ tensile tests at room temperature for four grains of mean size ∼1 mm. During mechanical loading, all four grains rotate and the mean rotation angle increases with austenite deformation. As the martensitic transformation occurs, the rotation becomes more pronounced, and the grain orientation splits into several sub-domains: the austenite orientation varies on both sides of the martensite variant. The mean disorientation is ∼1 o . Upon unloading, the sub-domains collapse and reverse rotation is observed.

  17. In situ synchrotron X-ray diffraction study of scale formation during CO{sub 2} corrosion of carbon steel in sodium and magnesium chloride solutions

    Energy Technology Data Exchange (ETDEWEB)

    Ingham, B. [Industrial Research Limited, P.O. Box 31-310, Lower Hutt 5045 (New Zealand); MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, P.O. Box 600, Wellington 6140 (New Zealand); Ko, M., E-mail: m.ko@questintegrity.com [MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, P.O. Box 600, Wellington 6140 (New Zealand); Quest Integrity Group, P.O. Box 38-096, Lower Hutt 5045 (New Zealand); School of Chemical Sciences, University of Auckland, Private Bag 92019, Auckland 1022 (New Zealand); Laycock, N. [Quest Integrity Group, P.O. Box 38-096, Lower Hutt 5045 (New Zealand); Burnell, J. [Industrial Research Limited, P.O. Box 31-310, Lower Hutt 5045 (New Zealand); Kappen, P. [Centre for Materials and Surface Science, Department of Physics, La Trobe University, Bundoora, VIC 3086 (Australia); Kimpton, J.A. [Australian Synchrotron, 800 Blackburn Road, Clayton, VIC 3168 (Australia); Williams, D.E. [MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, P.O. Box 600, Wellington 6140 (New Zealand); School of Chemical Sciences, University of Auckland, Private Bag 92019, Auckland 1022 (New Zealand)

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer We studied the scale formation processes of carbon steel in CO{sub 2} saturated brine at 80 Degree-Sign C. Black-Right-Pointing-Pointer Protective scales were formed in all tests. Black-Right-Pointing-Pointer Only FeCO{sub 3} formed in saturated brine while Fe(OH){sub 2}CO{sub 3} detected with presence of MgCl{sub 2}. Black-Right-Pointing-Pointer MgCl{sub 2} accelerates the onset of siderite precipitation. - Abstract: In situ synchrotron X-ray diffraction was used to follow the formation of corrosion products on carbon steel in CO{sub 2} saturated NaCl solution and mixed NaCl/magnesium chloride (MgCl{sub 2}) at 80 Degree-Sign C. Siderite (FeCO{sub 3}) was the only phase formed in NaCl solution, while Fe(OH){sub 2}CO{sub 3} was also detected when MgCl{sub 2} was present. The proposed model is that siderite precipitation, occurring once the critical supersaturation was exceeded within a defined boundary layer, caused local acidification which accelerated the anodic dissolution of iron. The current fell once a complete surface scale was formed. It is suggested that MgCl{sub 2} addition decreased the required critical supersaturation for precipitation.

  18. In-Situ Observations of Longitudinal Compression Damage in Carbon-Epoxy Cross Ply Laminates Using Fast Synchrotron Radiation Computed Tomography

    Science.gov (United States)

    Bergan, Andrew C.; Garcea, Serafina C.

    2017-01-01

    The role of longitudinal compressive failure mechanisms in notched cross-ply laminates is studied experimentally with in-situ synchrotron radiation based computed tomography. Carbon/epoxy specimens loaded monotonically in uniaxial compression exhibited a quasi-stable failure process, which was captured with computed tomography scans recorded continuously with a temporal resolutions of 2.4 seconds and a spatial resolution of 1.1 microns per voxel. A detailed chronology of the initiation and propagation of longitudinal matrix splitting cracks, in-plane and out-of-plane kink bands, shear-driven fiber failure, delamination, and transverse matrix cracks is provided with a focus on kink bands as the dominant failure mechanism. An automatic segmentation procedure is developed to identify the boundary surfaces of a kink band. The segmentation procedure enables 3-dimensional visualization of the kink band and conveys the orientation, inclination, and spatial variation of the kink band. The kink band inclination and length are examined using the segmented data revealing tunneling and spatial variations not apparent from studying the 2-dimensional section data.

  19. In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

    International Nuclear Information System (INIS)

    Mainz, R.; Klenk, R.

    2011-01-01

    In this work we present a method for the in situ analysis of elemental depth distributions in thin films using a combined evaluation of synchrotron x-ray fluorescence and energy-dispersive x-ray diffraction signals. We recorded diffraction and fluorescence signals simultaneously during the reactive annealing of thin films. By means of the observed diffraction signals, the time evolution of phases in the thin films during the annealing processes can be determined. We utilized this phase information to parameterize the depth distributions of the elements in the films. The time-dependent fluorescence signals were then taken to determine the parameters representing the parameterized depth distributions. For this latter step, we numerically calculated the fluorescence intensities for a given set of depth distributions. These calculations handle polychromatic excitation and arbitrary functions of depth distributions and take into account primary and secondary fluorescence. Influences of lateral non-uniformities of the films, as well as the accuracy limits of the method, are investigated. We apply the introduced method to analyze the evolution of elemental depth distributions and to quantify the kinetic parameters during a synthesis process of CuInS 2 thin films via the reactive annealing of Cu-In precursors in a sulfur atmosphere.

  20. In situ synchrotron X-ray diffraction study of scale formation during CO2 corrosion of carbon steel in sodium and magnesium chloride solutions

    International Nuclear Information System (INIS)

    Ingham, B.; Ko, M.; Laycock, N.; Burnell, J.; Kappen, P.; Kimpton, J.A.; Williams, D.E.

    2012-01-01

    Highlights: ► We studied the scale formation processes of carbon steel in CO 2 saturated brine at 80 °C. ► Protective scales were formed in all tests. ► Only FeCO 3 formed in saturated brine while Fe(OH) 2 CO 3 detected with presence of MgCl 2 . ► MgCl 2 accelerates the onset of siderite precipitation. - Abstract: In situ synchrotron X-ray diffraction was used to follow the formation of corrosion products on carbon steel in CO 2 saturated NaCl solution and mixed NaCl/magnesium chloride (MgCl 2 ) at 80 °C. Siderite (FeCO 3 ) was the only phase formed in NaCl solution, while Fe(OH) 2 CO 3 was also detected when MgCl 2 was present. The proposed model is that siderite precipitation, occurring once the critical supersaturation was exceeded within a defined boundary layer, caused local acidification which accelerated the anodic dissolution of iron. The current fell once a complete surface scale was formed. It is suggested that MgCl 2 addition decreased the required critical supersaturation for precipitation.

  1. In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction-A powerful new technique for the characterization of electrochemical surfaces and interfaces

    Energy Technology Data Exchange (ETDEWEB)

    De Marco, Roland [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)]. E-mail: r.demarco@exchange.curtin.edu.au; Jiang, Z.-T. [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Martizano, Jay [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Lowe, Alex [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Pejcic, Bobby [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Riessen, Arie van [Materials Research Group, Department of Applied Physics, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)

    2006-08-15

    A marriage of electrochemical impedance spectroscopy (EIS) and in situ synchrotron radiation grazing incidence X-ray diffraction (SR-GIXRD) has provided a powerful new technique for the elucidation of the mechanistic chemistry of electrochemical systems. In this study, EIS/SR-GIXRD has been used to investigate the influence of metal ion buffer calibration ligands, along with natural organic ligands in seawater, on the behaviour of the iron chalcogenide glass ion-selective electrode (ISE). The SR-GIXRD data demonstrated that citrate - a previously reported poor iron calibration ligand for the analysis of seawater - induced an instantaneous and total dissolution of crystalline GeSe and Sb{sub 2}Se{sub 3} in the modified surface layer (MSL) of the ISE, while natural organic ligands in seawater and a mixture of ligands in a mimetic seawater ligand system protected the MSL's crystalline inclusions of GeSe and Sb{sub 2}Se{sub 3} from oxidative attack. Expectedly, the EIS data showed that citrate induced a loss in the medium frequency time constant for the MSL of the ISE, while seawater's natural organic ligands and the mimetic ligand system preserved the medium frequency EIS response characteristics of the ISE's MSL. The new EIS/SR-GIXRD technique has provided insights into the suitability of iron calibration ligands for the analysis of iron in seawater.

  2. In Situ Synchrotron X-Ray Diffraction Characterization of the Synthesis of Graphene Oxide and Reduced Graphene Oxide

    DEFF Research Database (Denmark)

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

    2015-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) synthesised from GO, has a promising future in fields ranging from electronics to energy technologies[1]. GO may be synthesized by the modified Hummer’s method[2], where a mixture of potassium permanganate and concentrated sulfuric acid forms...... by placing a mixture of permanganate and sulphuric acid in a capillary next to graphite. The synthesis was then initiated by gently pushing the fluid mixture into the powder with N2 gas. The in situ XRD of the GO synthesis showed how the oxidation reaction proceeds in three separate stages, as seen in Figure...... 1. The first stage was the dissolution of potassium permanganate, followed by an intercalation stage and subsequent formation of crystalline material. The GO 001 diffraction peak was observed early during the synthesis, in the second stage, and the intensity of the 001 diffraction increased during...

  3. High pressure experimental water loop

    International Nuclear Information System (INIS)

    Grenon, M.

    1958-01-01

    A high pressure experimental water loop has been made for studying the detection and evolution of cladding failure in a pressurized reactor. The loop has been designed for a maximum temperature of 360 deg. C, a maximum of 160 kg/cm 2 and flow rates up to 5 m 3 /h. The entire loop consists of several parts: a main circuit with a canned rotor circulation pump, steam pressurizer, heating tubes, two hydro-cyclones (one de-gasser and one decanter) and one tubular heat exchanger; a continuous purification loop, connected in parallel, comprising pressure reducing valves and resin pots which also allow studies of the stability of resins under pressure, temperature and radiation; following the gas separator is a gas loop for studying the recombination of the radiolytic gases in the steam phase. The preceding circuits, as well as others, return to a low pressure storage circuit. The cold water of the low pressure storage flask is continuously reintroduced into the high pressure main circuit by means of a return pump at a maximum head of 160 kg /cm 2 , and adjusted to the pressurizer level. This loop is also a testing bench for the tight high pressure apparatus. The circulating pump and the connecting flanges (Oak Ridge type) are water-tight. The feed pump and the pressure reducing valves are not; the un-tight ones have a system of leak recovery. To permanently check the tightness the circuit has been fitted with a leak detection system (similar to the HRT one). (author) [fr

  4. Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation

    OpenAIRE

    Schroeder, Jeremy; Thomson, W.; Howard, B.; Schell, N.; Näslund, Lars-Åke; Rogström, Lina; Johansson-Jöesaar, Mats P.; Ghafoor, Naureen; Odén, Magnus; Nothnagel, E.; Shepard, A.; Greer, J.; Birch, Jens

    2015-01-01

    We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (greater than50 keV), high photon flux (greater than10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (less than1 s) two-dimensional (2D) detector, permits time-resolved in situ structural analysis of thin film formation...

  5. Deep ice and salty oceans of icy worlds, how high pressures influence their thermodynamics and provide constrains on extraterrestrial habitability

    Science.gov (United States)

    Journaux, B.; Brown, J. M.; Bollengier, O.; Abramson, E.

    2017-12-01

    As in Earth arctic and Antarctic regions, suspected extraterrestrial deep oceans in icy worlds (i.e. icy moons and water-rich exoplanets) chemistry and thermodynamic state will strongly depend on their equilibrium with H2O ice and present solutes. Na-Mg-Cl-SO4 salt species are currently the main suspected ionic solutes to be present in deep oceans based on remote sensing, magnetic field measurements, cryovolcanism ice grains chemical analysis and chondritic material aqueous alteration chemical models. Unlike on our planet, deep extraterrestrial ocean might also be interacting at depth with high pressure ices (e.g. III, V, VI, VI, X) which have different behavior compared to ice Ih. Unfortunately, the pressures and temperatures inside these hydrospheres differ significantly from the one found in Earth aqueous environments, so most of our current thermodynamic databases do not cover the range of conditions relevant for modeling realistically large icy worlds interiors. Recent experimental results have shown that the presence of solutes, and more particularly salts, in equilibrium with high pressure ices have large effects on the stability, buoyancy and chemistry of all the phases present at these extreme conditions. High pressure in-situ measurements using diamond anvil cell apparatus were operated both at the University of washington and at the European Synchrotron Radiation Facility on aqueous systems phase diagrams with Na-Mg-Cl-SO4 species, salt incorporation in high pressure ices and density inversions between the solid and the fluids. These results suggest a more complex picture of the interior structure, dynamic and chemical evolution of large icy worlds hydrospheres when solutes are taken into account, compared to current models mainly using pure water. Based on our in-situ experimental measurements, we propose the existence of new liquid environments at greater depths and the possibility of solid state transport of solute through the high pressure ices

  6. Robust high pressure stability and negative thermal expansion in sodium-rich antiperovskites Na{sub 3}OBr and Na{sub 4}OI{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yonggang, E-mail: yyggwang@gmail.com, E-mail: yangwg@hpstar.ac.cn, E-mail: yusheng.zhao@unlv.edu [High Pressure Science and Engineering Center, University of Nevada, Las Vegas, Nevada 89154 (United States); Institute of Nanostructured Functional Materials, Huanghe Science and Technology College, Zhengzhou, Henan 450006 (China); High Pressure Synergetic Consortium (HPSynC), Geophysical Laboratory, Carnegie Institution of Washington, Argonne, Illinois 60439 (United States); Wen, Ting [Institute of Nanostructured Functional Materials, Huanghe Science and Technology College, Zhengzhou, Henan 450006 (China); Park, Changyong; Kenney-Benson, Curtis [High Pressure Collaborative Access Team (HPCAT), Geophysical Laboratory, Carnegie Institution of Washington, Argonne, Illinois 60439 (United States); Pravica, Michael; Zhao, Yusheng, E-mail: yyggwang@gmail.com, E-mail: yangwg@hpstar.ac.cn, E-mail: yusheng.zhao@unlv.edu [High Pressure Science and Engineering Center, University of Nevada, Las Vegas, Nevada 89154 (United States); Yang, Wenge, E-mail: yyggwang@gmail.com, E-mail: yangwg@hpstar.ac.cn, E-mail: yusheng.zhao@unlv.edu [High Pressure Synergetic Consortium (HPSynC), Geophysical Laboratory, Carnegie Institution of Washington, Argonne, Illinois 60439 (United States); Center for High Pressure Science and Technology Advanced Research (HPSTAR), Shanghai 201203 (China)

    2016-01-14

    The structure stability under high pressure and thermal expansion behavior of Na{sub 3}OBr and Na{sub 4}OI{sub 2}, two prototypes of alkali-metal-rich antiperovskites, were investigated by in situ synchrotron X-ray diffraction techniques under high pressure and low temperature. Both are soft materials with bulk modulus of 58.6 GPa and 52.0 GPa for Na{sub 3}OBr and Na{sub 4}OI{sub 2}, respectively. The cubic Na{sub 3}OBr structure and tetragonal Na{sub 4}OI{sub 2} with intergrowth K{sub 2}NiF{sub 4} structure are stable under high pressure up to 23 GPa. Although being a characteristic layered structure, Na{sub 4}OI{sub 2} exhibits nearly isotropic compressibility. Negative thermal expansion was observed at low temperature range (20–80 K) in both transition-metal-free antiperovskites for the first time. The robust high pressure structure stability was examined and confirmed by first-principles calculations among various possible polymorphisms qualitatively. The results provide in-depth understanding of the negative thermal expansion and robust crystal structure stability of these antiperovskite systems and their potential applications.

  7. Robust high pressure stability and negative thermal expansion in sodium-rich antiperovskites Na3OBr and Na4OI2

    International Nuclear Information System (INIS)

    Wang, Yonggang; Wen, Ting; Park, Changyong; Kenney-Benson, Curtis; Pravica, Michael; Zhao, Yusheng; Yang, Wenge

    2016-01-01

    The structure stability under high pressure and thermal expansion behavior of Na 3 OBr and Na 4 OI 2 , two prototypes of alkali-metal-rich antiperovskites, were investigated by in situ synchrotron X-ray diffraction techniques under high pressure and low temperature. Both are soft materials with bulk modulus of 58.6 GPa and 52.0 GPa for Na 3 OBr and Na 4 OI 2 , respectively. The cubic Na 3 OBr structure and tetragonal Na 4 OI 2 with intergrowth K 2 NiF 4 structure are stable under high pressure up to 23 GPa. Although being a characteristic layered structure, Na 4 OI 2 exhibits nearly isotropic compressibility. Negative thermal expansion was observed at low temperature range (20–80 K) in both transition-metal-free antiperovskites for the first time. The robust high pressure structure stability was examined and confirmed by first-principles calculations among various possible polymorphisms qualitatively. The results provide in-depth understanding of the negative thermal expansion and robust crystal structure stability of these antiperovskite systems and their potential applications

  8. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    International Nuclear Information System (INIS)

    Bozzini, B; D'Urzo, L; Gianoncelli, A; Kaulich, B; Kiskinova, M; Prasciolu, M; Tadjeddine, A

    2009-01-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si 3 N 4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  9. Microstructures define melting of molybdenum at high pressures

    Science.gov (United States)

    Hrubiak, Rostislav; Meng, Yue; Shen, Guoyin

    2017-03-01

    High-pressure melting anchors the phase diagram of a material, revealing the effect of pressure on the breakdown of the ordering of atoms in the solid. An important case is molybdenum, which has long been speculated to undergo an exceptionally steep increase in melting temperature when compressed. On the other hand, previous experiments showed nearly constant melting temperature as a function of pressure, in large discrepancy with theoretical expectations. Here we report a high-slope melting curve in molybdenum by synchrotron X-ray diffraction analysis of crystalline microstructures, generated by heating and subsequently rapidly quenching samples in a laser-heated diamond anvil cell. Distinct microstructural changes, observed at pressures up to 130 gigapascals, appear exclusively after melting, thus offering a reliable melting criterion. In addition, our study reveals a previously unsuspected transition in molybdenum at high pressure and high temperature, which yields highly textured body-centred cubic nanograins above a transition temperature.

  10. High-pressure structural behaviour of nanocrystalline Ge

    International Nuclear Information System (INIS)

    Wang, H; Liu, J F; He, Y; Wang, Y; Chen, W; Jiang, J Z; Olsen, J Staun; Gerward, L

    2007-01-01

    The equation of state and the pressure of the I-II transition have been studied for nanocrystalline Ge using synchrotron x-ray diffraction. The bulk modulus and the transition pressure increase with decreasing particle size for both Ge-I and Ge-II, but the percentage volume collapse at the transition remains constant. Simplified models for the high-pressure structural behaviour are presented, based on the assumption that a large fraction of the atoms reside in grain boundary regions of the nanocrystalline material. The interface structure plays a significant role in affecting the transition pressure and the bulk modulus

  11. A novel high-pressure vessel for simultaneous observations of seismic velocity and in situ CO2 distribution in a porous rock using a medical X-ray CT scanner

    Science.gov (United States)

    Jiang, Lanlan; Nishizawa, Osamu; Zhang, Yi; Park, Hyuck; Xue, Ziqiu

    2016-12-01

    Understanding the relationship between seismic wave velocity or attenuation and CO2 saturation is essential for CO2 storage in deep saline formations. In the present study, we describe a novel upright high-pressure vessel that is designed to keep a rock sample under reservoir conditions and simultaneously image the entire sample using a medical X-ray CT scanner. The pressure vessel is composed of low X-ray absorption materials: a carbon-fibre-enhanced polyetheretherketone (PEEK) cylinder and PEEK vessel closures supported by carbon-fibre-reinforced plastic (CFRP) joists. The temperature was controlled by a carbon-coated film heater and an aramid fibre thermal insulator. The assembled sample cell allows us to obtain high-resolution images of rock samples during CO2 drainage and brine imbibition under reservoir conditions. The rock sample was oriented vertical to the rotation axis of the CT scanner, and seismic wave paths were aligned parallel to the rotation axis to avoid shadows from the acoustic transducers. The reconstructed CO2 distribution images allow us to calculate the CO2 saturation in the first Fresnel zone along the ray path between transducers. A robust relationship between the seismic wave velocity or attenuation and the CO2 saturation in porous rock was obtained from experiments using this pressure vessel.

  12. Synchrotron radiation

    CERN Document Server

    Kunz, C

    1974-01-01

    The production of synchrotron radiation as a by-product of circular high-energy electron (positron) accelerators or storage rings is briefly discussed. A listing of existing or planned synchrotron radiation laboratories is included. The following properties are discussed: spectrum, collimation, polarization, and intensity; a short comparison with other sources (lasers and X-ray tubes) is also given. The remainder of the paper describes the experimental installations at the Deutsches Elektronen-Synchrotron (DESY) and DORIS storage rings, presents a few typical examples out of the fields of atomic, molecular, and solid-state spectroscopy, and finishes with an outlook on the use of synchrotron radiation in molecular biology. (21 refs).

  13. In situ synchrotron X-ray diffraction study of deformation behaviour of a metastable β-type Ti-33Nb-4Sn alloy

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Shun [Institute for Advanced Materials, Jiangsu University, Zhenjiang 212013 (China); School of Materials Science and Engineering, Beihang University, Beijing 100191 (China); Jiangsu Key Laboratory of Advanced Structural Materials and Application Technology, Nanjing 211167 (China); Shang, Yao [Institute for Advanced Materials, Jiangsu University, Zhenjiang 212013 (China); Zhang, Junsong, E-mail: zhangjunsong7397@163.com [Institute for Advanced Materials, Jiangsu University, Zhenjiang 212013 (China); Meng, Qingkun [School of Materials Science and Engineering, Beihang University, Beijing 100191 (China); School of Materials Science and Engineering, China University of Mining and Technology, Xuzhou 221116 (China); Cheng, Xiaonong [Institute for Advanced Materials, Jiangsu University, Zhenjiang 212013 (China); Zhao, Xinqing, E-mail: xinqing@buaa.edu.cn [School of Materials Science and Engineering, Beihang University, Beijing 100191 (China)

    2017-04-24

    In this study, the deformation behaviour of metastable β-type Ti-33Nb-4Sn alloys in different thermo-mechanical treatment states is investigated by tensile tests and in situ synchrotron X-ray diffraction (SXRD). In the case of solution-treated alloy, stress-induced martensitic (SIM) transformation takes place over a wide strain range of 0.5–14%. During this SIM transformation, the parameter of b{sub α′′} ([020]{sub α′′}) increases with macroscopic strain within strain range of 1.5–4.7%, giving rise to that the α′′ variants, with b{sub α′′}-axis ([020]{sub α′′}) parallel to tensile direction, are formed preferentially to accommodate the macroscopic strain during loading. Similar SIM transformation behaviour also occurs in cold-rolled alloy with the exception that the extent of SIM transformation and pre-existing α′′ variants reorientation is much slighter than that in solution-treated specimen. This slighter SIM transformation gives rise to nonlinear deformation, instead of “stress plateau”, in the cold-rolled alloy. Upon annealing, the β phase survives against SIM transformation due to the suppression effects of dislocations and grain boundaries, resulting in a huge elastic deformability. Based on the results of tensile tests and SXRD, the activation sequence of different deformation mechanisms and the regions of different deformation mechanisms of Ti-33Nb-4Sn alloys, in solution-treated, cold-rolled and annealed states, are clarified unambiguously.

  14. Synchrotron radiation

    International Nuclear Information System (INIS)

    Nave, C.; Quinn, P.; Blake, R.J.

    1988-01-01

    The paper on Synchrotron Radiation contains the appendix to the Daresbury Annual Report 1987/88. The appendix is mainly devoted to the scientific progress reports on the work at the Synchrotron Radiation Source in 1987/8. The parameters of the Experimental Stations and the index to the Scientific Reports are also included in the appendix. (U.K.)

  15. High Pressure Electrolyzer System Evaluation

    Science.gov (United States)

    Prokopius, Kevin; Coloza, Anthony

    2010-01-01

    This report documents the continuing efforts to evaluate the operational state of a high pressure PEM based electrolyzer located at the NASA Glenn Research Center. This electrolyzer is a prototype system built by General Electric and refurbished by Hamilton Standard (now named Hamilton Sunstrand). It is capable of producing hydrogen and oxygen at an output pressure of 3000 psi. The electrolyzer has been in storage for a number of years. Evaluation and testing was performed to determine the state of the electrolyzer and provide an estimate of the cost for refurbishment. Pressure testing was performed using nitrogen gas through the oxygen ports to ascertain the status of the internal membranes and seals. It was determined that the integrity of the electrolyzer stack was good as there were no appreciable leaks in the membranes or seals within the stack. In addition to the integrity testing, an itemized list and part cost estimate was produced for the components of the electrolyzer system. An evaluation of the system s present state and an estimate of the cost to bring it back to operational status was also produced.

  16. Nuclear magnetic resonance studies at high pressures

    International Nuclear Information System (INIS)

    Jonas, J.

    1980-01-01

    Recent advances in the field of NMR spectroscopy at high pressure are reviewed. After a brief discussion of two novel experimental techniques, the main focus of this review is on several specific studies which illustrate the versatility and power of this high pressure field. Experimental aspects of NMR measurements at high pressure and high temperature and the techniques for the high resolution NMR spectroscopy at high pressure are discussed. An overview of NMR studies of the dynamic structure of simple polyatomic liquids and hydrogen bonded liquids is followed by a discussion of high resolution spectroscopy at high pressure. Examples of NMR studies of disordered organic solids and polymers conclude the review. (author)

  17. High-pressure structural study of yttrium monochalcogenides from experiment and theory

    DEFF Research Database (Denmark)

    Vaitheeswaran, G.; Kanchana, V.; Svane, A.

    2011-01-01

    High-pressure powder x-ray diffraction experiments using synchrotron radiation are performed on the yttrium monochalcogenides YS, YSe, and YTe up to a maximum pressure of 23 GPa. The ambient NaCl structure is stable throughout the pressure range covered. The bulk moduli are determined to be 93, 82...

  18. Phase transitions in solids under high pressure

    CERN Document Server

    Blank, Vladimir Davydovich

    2013-01-01

    Phase equilibria and kinetics of phase transformations under high pressureEquipment and methods for the study of phase transformations in solids at high pressuresPhase transformations of carbon and boron nitride at high pressure and deformation under pressurePhase transitions in Si and Ge at high pressure and deformation under pressurePolymorphic α-ω transformation in titanium, zirconium and zirconium-titanium alloys Phase transformations in iron and its alloys at high pressure Phase transformations in gallium and ceriumOn the possible polymorphic transformations in transition metals under pressurePressure-induced polymorphic transformations in АIBVII compoundsPhase transformations in AIIBVI and AIIIBV semiconductor compoundsEffect of pressure on the kinetics of phase transformations in iron alloysTransformations during deformation at high pressure Effects due to phase transformations at high pressureKinetics and hysteresis in high-temperature polymorphic transformations under pressureHysteresis and kineti...

  19. High-pressure behavior of intermediate scapolite: compressibility, structure deformation and phase transition

    Science.gov (United States)

    Lotti, Paolo; Comboni, Davide; Merlini, Marco; Hanfland, Michael

    2018-05-01

    Scapolites are common volatile-bearing minerals in metamorphic rocks. In this study, the high-pressure behavior of an intermediate member of the scapolite solid solution series (Me47), chemical formula (Na1.86Ca1.86K0.23Fe0.01)(Al4.36Si7.64)O24[Cl0.48(CO3)0.48(SO4)0.01], has been investigated up to 17.79 GPa, by means of in situ single-crystal synchrotron X-ray diffraction. The isothermal elastic behavior of the studied scapolite has been described by a III-order Birch-Murnaghan equation of state, which provided the following refined parameters: V 0 = 1110.6(7) Å3, {K_{{V_0}}} = 70(2) GPa ({β _{{V_0}}} = 0.0143(4) GPa-1) and {K_{{V}}^' = 4.8(7). The refined bulk modulus is intermediate between those previously reported for Me17 and Me68 scapolite samples, confirming that the bulk compressibility among the solid solution increases with the Na content. A discussion on the P-induced structure deformation mechanisms of tetragonal scapolite at the atomic scale is provided, along with the implications of the reported results for the modeling of scapolite stability. In addition, a single-crystal to single-crystal phase transition, which is displacive in character, has been observed toward a triclinic polymorph at 9.87 GPa. The high-pressure triclinic polymorph was found to be stable up to the highest pressure investigated.

  20. High pressure study of water-salt systems, phase equilibria, partitioning, thermodynic properties and implication for large icy worlds hydrospheres.

    Science.gov (United States)

    Journaux, B.; Brown, J. M.; Abramson, E.; Petitgirard, S.; Pakhomova, A.; Boffa Ballaran, T.; Collings, I.

    2017-12-01

    Water salt systems are predicted to be present in deep hydrosphere inside water-rich planetary bodies, following water/rock chemical interaction during early differentiation stages or later hydrothermal activity. Unfortunately the current knowledge of the thermodynamic and physical properties of aqueous salt mixtures at high pressure and high temperature is still insufficient to allow realistic modeling of the chemical or dynamic of thick planetary hydrospheres. Recent experimental results have shown that the presence of solutes, and more particularly salts, in equilibrium with high pressure ices have large effects on the stability fields, buoyancy and chemistry of all the phases present at these extreme conditions. Effects currently being investigated by our research group also covers ice melting curve depressions that depend on the salt species and incorporation of solutes inside the crystallographic lattice of high pressure ices. Both of these could have very important implication at the planetary scale, enabling thicker/deeper liquid oceans, and allowing chemical transportation through the high pressure ice layer in large icy worlds. We will present the latest results obtained in-situ using diamond anvil cell, coupled with Synchrotron X-Ray diffraction, Raman Spectroscopy and optical observations, allowing to probe the crystallographic structure, equations of state, partitioning and phase boundary of high pressure ice VI and VII in equilibrium with Na-Mg-SO4-Cl ionic species at high pressures (1-10 GPa). The difference in melting behavior depending on the dissolved salt species was characterized, suggesting differences in ionic speciation at liquidus conditions. The solidus P-T conditions were also measured as well as an increase of lattice volumes interpreted as an outcome of ionic incorporation in HP ice during incongruent crystallization. The measured phase diagrams, lattice volumes and important salt incorporations suggest a more complex picture of the

  1. 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

  2. Damage localisation and fracture propagation in granite: 4D synchrotron x-ray microtomographic observations from an in-situ triaxial deformation experiment at SOLEIL

    Science.gov (United States)

    Cartwright-Taylor, Alexis; Fusseis, Florian; Butler, Ian; Flynn, Michael; King, Andrew

    2017-04-01

    To date, most studies of damage localisation and failure have utilised indirect techniques to visualise the pathway to failure. The advent of synchrotron tomography and x-ray transparent experimental cells provides for the first time the opportunity to image localisation and fracture propagation in-situ, in real time with spatial resolutions of a few microns. We present 4D x-ray microtomographic data collected during a triaxial deformation experiment carried out at the imaging beamline PSICHE at the French Synchrotron SOLEIL. The data document damage localisation and fracture propagation in a microgranite. The sample was deformed at 15 MPa confining pressure and 3x10-5 s-1 strain rate, in a novel, miniature, x-ray transparent, triaxial deformation apparatus, designed and built at the University of Edinburgh. We used a 2.97 mm diameter x 9.46 mm long cylindrical sample of Ailsa Craig microgranite, heat treated to 600 ˚ C to introduce flaws in the form of pervasive crack damage. As the sample was loaded to failure, 21 microtomographic volumes were acquired in intervals of 5-20 MPa (decreasing as failure approached), including one scan at peak differential stress of 200 MPa (1.4 kN end load) and three post-failure scans. The scan at peak stress contained the incipient fault, and the sample failed immediately when loading continued afterwards. During scanning, a constant stress level was maintained. Individual datasets were collected in ˜10 minutes using a white beam with an energy maximum at 66 keV in a spiral configuration. Reconstructions yielded image stacks with a dimension of 1700x1700x4102 voxels with a voxel size of 2.7 μm. We analysed damage localisation and fracture propagation in the time series data. Fractures were segmented from the image data using a Multiscale Hessian fracture filter [1] and analysed for their orientations, dimensions and spatial distributions and changes in these properties during loading. Local changes in volumetric and shear

  3. Synchrotron light

    International Nuclear Information System (INIS)

    2001-01-01

    'Synchrotron Light' is an interactive and detailed introduction to the physics and technology of the generation of coherent radiation from accelerators as well as to its widespread high-tech applications in science, medicine and engineering. The topics covered are the interaction of light and matter, the technology of synchrotron light sources, spectroscopy, imaging, scattering and diffraction of X-rays, and applications to materials science, biology, biochemistry, medicine, chemistry, food and pharmaceutical technology. All synchrotron light facilities are introduced with their home-page addresses. 'Synchrotron Light' provides an instructive and comprehensive multimedia learning tool for students, experienced practitioners and novices wishing to apply synchrotron radiation in their future work. Its multiple-entry points permit an easy exploration of the CD-Rom according to the users knowledge and interest. 2-D and 3-D animations and virtual reconstruction with computer-generated images guide visitors into the scientific and technical world of a synchrotron and into the applications of synchrotron radiation. This bilingual (English and French) CD-Rom can be used for self-teaching and in courses at various levels in physics, chemistry, engineering, and biology. (author)

  4. Correlated structural and electronic phase transformations in transition metal chalcogenide under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Li, Chunyu, E-mail: licy@hpstar.ac.cn, E-mail: yanhao@hpstar.ac.cn; Ke, Feng; Yu, Zhenhai; Chen, Zhiqiang; Yan, Hao, E-mail: licy@hpstar.ac.cn, E-mail: yanhao@hpstar.ac.cn [Center for High Pressure Science and Technology Advanced Research, Shanghai 201203 (China); Hu, Qingyang [Center for High Pressure Science and Technology Advanced Research, Shanghai 201203 (China); Geophysical Laboratory, Carnegie Institution of Washington, Washington, DC 20015 (United States); Zhao, Jinggeng [Natural Science Research Center, Academy of Fundamental and Interdisciplinary Sciences, Harbin Institute of Technology, Harbin 150080 (China)

    2016-04-07

    Here, we report comprehensive studies on the high-pressure structural and electrical transport properties of the layered transition metal chalcogenide (Cr{sub 2}S{sub 3}) up to 36.3 GPa. A structural phase transition was observed in the rhombohedral Cr{sub 2}S{sub 3} near 16.5 GPa by the synchrotron angle dispersive X-ray diffraction measurement using a diamond anvil cell. Through in situ resistance measurement, the electric resistance value was detected to decrease by an order of three over the pressure range of 7–15 GPa coincided with the structural phase transition. Measurements on the temperature dependence of resistivity indicate that it is a semiconductor-to-metal transition in nature. The results were also confirmed by the electronic energy band calculations. Above results may shed a light on optimizing the performance of Cr{sub 2}S{sub 3} based applications under extreme conditions.

  5. High pressure-temperature polymorphism of 1,1-diamino-2,2-dinitroethylene

    International Nuclear Information System (INIS)

    Bishop, M M; Dattelbaum, D M; Velisavljevic, N; Chellappa, R S; Liu, Z; Preston, D N; Sandstrom, M M; Vohra, Y K

    2014-01-01

    1,1-diamino-2,2-dinitroethylene (FOX-7) is a low sensitivity energetic material with performance comparable to commonly used secondary explosives such as RDX and HMX. At ambient pressure, FOX-7 exhibits complex polymorphism with at least three structurally distinct phases (α, β, and γ). In this study, we have investigated the high pressure-temperature stability of FOX-7 polymorphs using synchrotron mid-infrared (MIR) spectroscopy. At ambient pressure, our MIR spectra and corresponding differential scanning calorimetry (DSC) measurements confirmed the known α → β (∼110 °C) and α → β (∼160 °C) structural phase transitions; as well as, indicated an additional transition γ → (∼210 °C), with the δ phase being stable up to ∼251 °C prior to decomposition. In situ MIR spectra obtained during isobaric heating at 0.9 GPa, revealed a potential α → β transition that could occur as early as 180 °C, while β → β+δ phase transition shifted to ∼300 °C with suppression of γ phase. Decomposition was observed slightly above 325 °C at 0.9 GPa.

  6. High pressure-temperature polymorphism of 1,1-diamino-2,2-dinitroethylene

    Science.gov (United States)

    Bishop, M. M.; Chellappa, R. S.; Liu, Z.; Preston, D. N.; Sandstrom, M. M.; Dattelbaum, D. M.; Vohra, Y. K.; Velisavljevic, N.

    2014-05-01

    1,1-diamino-2,2-dinitroethylene (FOX-7) is a low sensitivity energetic material with performance comparable to commonly used secondary explosives such as RDX and HMX. At ambient pressure, FOX-7 exhibits complex polymorphism with at least three structurally distinct phases (α, β, and γ). In this study, we have investigated the high pressure-temperature stability of FOX-7 polymorphs using synchrotron mid-infrared (MIR) spectroscopy. At ambient pressure, our MIR spectra and corresponding differential scanning calorimetry (DSC) measurements confirmed the known α → β (~110 °C) and α → β (~160 °C) structural phase transitions; as well as, indicated an additional transition γ → (~210 °C), with the δ phase being stable up to ~251 °C prior to decomposition. In situ MIR spectra obtained during isobaric heating at 0.9 GPa, revealed a potential α → β transition that could occur as early as 180 °C, while β → β+δ phase transition shifted to ~300 °C with suppression of γ phase. Decomposition was observed slightly above 325 °C at 0.9 GPa.

  7. In Situ Lipolysis and Synchrotron Small-Angle X-ray Scattering for the Direct Determination of the Precipitation and Solid-State Form of a Poorly Water-Soluble Drug During Digestion of a Lipid-Based Formulation

    DEFF Research Database (Denmark)

    Khan, Jamal; Hawley, Adrian; Rades, Thomas

    2016-01-01

    In situ lipolysis and synchrotron small-angle X-ray scattering (SAXS) were used to directly detect and elucidate the solid-state form of precipitated fenofibrate from the digestion of a model lipid-based formulation (LBF). This method was developed in light of recent findings that indicate variab...... on drugs, and experimental conditions, which are anticipated to produce altered solid-state forms upon the precipitation of drug (i.e., polymorphs, amorphous forms, and salts). © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci....

  8. Synchrotron radiation

    International Nuclear Information System (INIS)

    Helliwell, J.R.; Walker, R.P.

    1985-01-01

    A detailed account of the research work associated with the Synchrotron Radiation Source at Daresbury Laboratory, United Kingdom, in 1984/85, is presented in the Appendix to the Laboratory's Annual Report. (U.K.)

  9. Synchrotron radiation

    International Nuclear Information System (INIS)

    Hallmeier, K.H.; Meisel, A.; Ranft, J.

    1982-01-01

    The physical background and the properties of synchrotron radiation are described. The radiation offers many useful applications in the fields of spectroscopy and structural investigations. Some examples are given

  10. Synchrotron radiation

    International Nuclear Information System (INIS)

    Knotek, M.L.

    1987-01-01

    Synchrotron radiation has had a revolutionary effect on a broad range of scientific studies, from physics, chemistry and metallurgy to biology, medicine and geoscience. The situation during the last decade has been one of very rapid growth, there is a great vitality to the field and a capability has been given to a very broad range of scientific disciplines which was undreamed of just a decade or so ago. Here we will discuss some of the properties of synchrotron radiation that makes it so interesting and something of the sources in existence today including the National Synchrotron Light Source (NSLS). The NSLS is one of the new facilities built specifically for synchrotron radiation research and the model that was developed there for involvement of the scientific community is a good one which provides some good lessons for these facilities and others

  11. Synchrotron radiation

    International Nuclear Information System (INIS)

    Poole, M.W.; Lea, K.R.

    1982-01-01

    A report is given on the work involving the Synchrotron Radiation Division of the Daresbury Laboratory during the period January 1981 - March 1982. Development of the source, beamlines and experimental stations is described. Progress reports from individual investigators are presented which reveal the general diversity and interdisciplinary nature of the research which benefits from access to synchrotron radiation and the associated facilities. Information is given on the organisation of the Division and publications written by the staff are listed. (U.K.)

  12. Synchrotron radiation

    International Nuclear Information System (INIS)

    Norman, D.; Walker, R.P.; Durham, P.J.; Ridley, P.A.

    1986-01-01

    The paper on synchrotron radiation is the appendix to the Daresbury (United Kingdom) annual report, 1985/86. The bulk of the volume is made up of the progress reports for the work carried out during the year under review using the Synchrotron Radiation Source (SRS) at Daresbury. The Appendix also contains: the scientific programmes at the the SRS, progress on beamlines, instrumentation and computing developments, and activities connected with accelerator development. (U.K.)

  13. High-Pressure Lightweight Thrusters

    Science.gov (United States)

    Holmes, Richard; McKechnie, Timothy; Shchetkovskiy, Anatoliy; Smirnov, Alexander

    2013-01-01

    Returning samples of Martian soil and rock to Earth is of great interest to scientists. There were numerous studies to evaluate Mars Sample Return (MSR) mission architectures, technology needs, development plans, and requirements. The largest propulsion risk element of the MSR mission is the Mars Ascent Vehicle (MAV). Along with the baseline solid-propellant vehicle, liquid propellants have been considered. Similar requirements apply to other lander ascent engines and reaction control systems. The performance of current state-ofthe- art liquid propellant engines can be significantly improved by increasing both combustion temperature and pressure. Pump-fed propulsion is suggested for a single-stage bipropellant MAV. Achieving a 90-percent stage propellant fraction is thought to be possible on a 100-kg scale, including sufficient thrust for lifting off Mars. To increase the performance of storable bipropellant rocket engines, a high-pressure, lightweight combustion chamber was designed. Iridium liner electrodeposition was investigated on complex-shaped thrust chamber mandrels. Dense, uniform iridium liners were produced on chamber and cylindrical mandrels. Carbon/carbon composite (C/C) structures were braided over iridium-lined mandrels and densified by chemical vapor infiltration. Niobium deposition was evaluated for forming a metallic attachment flange on the carbon/ carbon structure. The new thrust chamber was designed to exceed state-of-the-art performance, and was manufactured with an 83-percent weight savings. High-performance C/Cs possess a unique set of properties that make them desirable materials for high-temperature structures used in rocket propulsion components, hypersonic vehicles, and aircraft brakes. In particular, more attention is focused on 3D braided C/Cs due to their mesh-work structure. Research on the properties of C/Cs has shown that the strength of composites is strongly affected by the fiber-matrix interfacial bonding, and that weakening

  14. Trends in high pressure developments for new perspectives

    Science.gov (United States)

    Largeteau, Alain; Prakasam, Mythili

    2018-06-01

    Temperature and Pressure are two parameters in the universe, where pressure represents the largest scale in comparison to temperature. The design of high pressure equipment depends mainly on the media used which could be gas, liquid or solid and the objective could be synthesis of materials or in situ characterization. The development of new research fields requiring high pressure equipment which are currently in Bordeaux - France are based on the historical development of high pressure domain initiated by Professor Gerard DEMAZEAU and his team during the last half century, which is discussed here. The main concepts governing the effect of pressure on materials synthesis is by the combination of high pressure and high temperature which are described with apt examples. There is an upsurge in various technologies for strong development for the synthesis of materials to drive several possibilities, for example: to reach very high density to obtain optical ceramics (by conventional SPS), to diminish parameters (P, T, t) of synthesis (by HP-SPS), to sinter at low temperature thermal sensitive composition (by HyS), to consolidate porous materials (by FIP), to densify biocomposite with cold decontamination (by HHP) simultaneously, etc.

  15. High pressure effects on fruits and vegetables

    NARCIS (Netherlands)

    Timmermans, R.A.H.; Matser, A.M.

    2016-01-01

    The chapter provides an overview on different high pressure based treatments (high pressure pasteurization, blanching, pressure-assisted thermal processing, pressure-shift freezing and thawing) available for the preservation of fruits and vegetable products and extending their shelf life. Pressure

  16. In situ defect annealing of swift heavy ion irradiated CeO2 and ThO2 using synchrotron X-ray diffraction and a hydrothermal diamond anvil cell

    Energy Technology Data Exchange (ETDEWEB)

    Palomares, Raul I.; Tracy, Cameron L.; Zhang, Fuxiang; Park, Changyong; Popov, Dmitry; Trautmann, Christina; Ewing, Rodney C.; Lang, Maik

    2015-04-16

    Hydrothermal diamond anvil cells (HDACs) provide facile means for coupling synchrotron X-ray techniques with pressure up to 10 GPa and temperature up to 1300 K. This manuscript reports on an application of the HDAC as an ambient-pressure sample environment for performingin situdefect annealing and thermal expansion studies of swift heavy ion irradiated CeO2and ThO2using synchrotron X-ray diffraction. The advantages of thein situHDAC technique over conventional annealing methods include rapid temperature ramping and quench times, high-resolution measurement capability, simultaneous annealing of multiple samples, and prolonged temperature and apparatus stability at high temperatures. Isochronal annealing between 300 and 1100 K revealed two-stage and one-stage defect recovery processes for irradiated CeO2and ThO2, respectively, indicating that the morphology of the defects produced by swift heavy ion irradiation of these two materials differs significantly. These results suggest that electronic configuration plays a major role in both the radiation-induced defect production and high-temperature defect recovery mechanisms of CeO2and ThO2.

  17. Developments in time-resolved high pressure x-ray diffraction using rapid compression and decompression

    International Nuclear Information System (INIS)

    Smith, Jesse S.; Sinogeikin, Stanislav V.; Lin, Chuanlong; Rod, Eric; Bai, Ligang; Shen, Guoyin

    2015-01-01

    Complementary advances in high pressure research apparatus and techniques make it possible to carry out time-resolved high pressure research using what would customarily be considered static high pressure apparatus. This work specifically explores time-resolved high pressure x-ray diffraction with rapid compression and/or decompression of a sample in a diamond anvil cell. Key aspects of the synchrotron beamline and ancillary equipment are presented, including source considerations, rapid (de)compression apparatus, high frequency imaging detectors, and software suitable for processing large volumes of data. A number of examples are presented, including fast equation of state measurements, compression rate dependent synthesis of metastable states in silicon and germanium, and ultrahigh compression rates using a piezoelectric driven diamond anvil cell

  18. High-pressure Raman investigation of the semiconductor antimony oxide

    Energy Technology Data Exchange (ETDEWEB)

    Geng, Aihui; Cao, Lihua [State Key Lab on High Power Semiconductor Laser, Changchun University of Science and Technology, 130022 Changchun (China); Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 130012 Changchun (China); Wan, Chunming [State Key Lab on High Power Semiconductor Laser, Changchun University of Science and Technology, 130022 Changchun (China); Ma, Yanmei [Department of Agronomy, Jilin University, 130062 Changchun (China)

    2011-05-15

    The in situ high-pressure behavior of the semiconductor antimony trioxide (Sb{sub 2}O{sub 3}) has been investigated by Raman spectroscopy techniques in a diamond anvil cell up to 20 GPa at room temperature. New peaks in the external lattice mode range emerged at a pressure above 8.6-15 GPa, suggesting that the structural phase transition occurred. The pressure dependence of Raman frequencies was obtained. The band at 139 cm{sup -1} (assigned to group mode) has a pressure dependence of -0.475 cm{sup -1}/GPa and reveals significant softening at high pressure. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  19. Creep deformation of Co-Re-Ta-C alloys with varying C content-investigated in-situ by simultaneous synchrotron radiation diffraction

    Czech Academy of Sciences Publication Activity Database

    Karge, L.; Gilles, R.; Mukherji, D.; Stark, A.; Beran, Přemysl; Schell, N.; Hofmann, M.; Strunz, Pavel; Hausler, J.; Rösler, J.

    2018-01-01

    Roč. 719, č. 3 (2018), s. 124-131 ISSN 0921-5093 Institutional support: RVO:61389005 Keywords : high temperature creep * Co alloys * synchrotron diffraction * neutron diffraction * dilatometer Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.094, year: 2016

  20. SrWO{sub 4} at high pressures

    Energy Technology Data Exchange (ETDEWEB)

    Grzechnik, A. [Departamento de Fisica de la Materia Condensada, Universidad del Pais Vasco, Apdo. 644, Bilbao 48080 (Spain); European Synchrotron Radiation Facility, B.P. 220, 38043 Grenoble cedex (France); Crichton, W.A.; Hanfland, M. [European Synchrotron Radiation Facility, B.P. 220, 38043 Grenoble cedex (France)

    2005-11-01

    Room-temperature high-pressure behaviour of SrWO{sub 4} scheelite (I4{sub 1}/a, Z=4) has been studied to 20.7 GPa in a diamond anvil cell using synchrotron angle-dispersive X-ray powder diffraction. Above 10 GPa, it transforms to the fergusonite structure (I2/a, Z=4). Both scheelite and fergusonite types are ordered superstructures of fluorite (Fm anti 3m, Z=4). There is no significant volume collapse at the scheelite-fergusonite phase transition. However, the compression data including both phases of strontium tungstate cannot be fitted by a common Birch-Murnaghan equation of state. An onset of decomposition into component oxides occurs at about 15 GPa. The pressure-induced transformations are irreversible. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  1. Synthesis and properties of selenium trihydride at high pressures

    Science.gov (United States)

    Zhang, Xiao; Xu, Wan; Wang, Yu; Jiang, Shuqing; Gorelli, Federico A.; Greenberg, Eran; Prakapenka, Vitali B.; Goncharov, Alexander F.

    2018-02-01

    The chemical reaction products of molecular hydrogen (H2) with selenium (Se) are studied by synchrotron x-ray diffraction (XRD) and Raman spectroscopy at high pressures. We find that a common H2Se is synthesized at 0.3 GPa using laser heating. Upon compression at 300 K, a crystal of the theoretically predicted Cccm H3Se has been grown at 4.6 GPa. At room temperature, H3Se shows a reversible phase decomposition after laser irradiation above 8.6 GPa, but remains stable up to 21 GPa. However, at 170 K Cccm H3Se persists up to 39.5 GPa based on XRD measurements, while low-temperature Raman spectra weaken and broaden above 23.1 GPa. At these conditions, the sample is visually nontransparent and shiny suggesting that metallization occurred.

  2. JHF synchrotrons

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-03-01

    The Japan Hadron Facility (JHF) consists of two synchrotrons and an injector linac. First, we will present a brief review of the specifications and lattice of the synchrotrons; one is 3 GeV booster and the other is 50 GeV main ring. Secondly, some detailed results of design study will be discussed, together with the present status of the R and D programs in progress. Among them, an estimate of beam loss is one of critical issues in beam dynamics. The development of a high gradient RF cavity is also crucial for a high intensity machine. (author)

  3. Support for the Advanced Polymers Beamline at the National Synchrotron Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Hsiao, Benjamin S. [State Univ. of New York (SUNY), Stonybrook, NY (United States)

    2008-10-01

    The primary focus of the X27C beamline is to investigate frontier polymer science and engineering problems with emphasis on real-time studies of structures, morphologies and dynamics from atomic, nanoscopic, microscopic to mesoscopic scales using simultaneous small-angle X-ray scattering (SAXS) and wide-angle X-ray diffraction (WAXD) techniques. The scientific merit of this project is as follows. Currently, many unique sample chambers for in-situ synchrotron studies, developed by the PI (B. Hsiao) and Co-PI (B. Chu), are available for general users of X27C at NSLS. These instruments include a gel/melt spinning apparatus, a continuous fiber drawing apparatus, a tensile stretching apparatus, a high pressure X-ray cell using supercritical carbon dioxide, a parallel plate strain-controlled shear stage and a dynamic rheometer for small-strain oscillatory deformation study. Based on the use of these instruments in combination with synchrotron X-rays, many new insights into the relationships between processing and structure have been obtained in recent years. The broader impact of this project is as follows. The X27C beamline is the first synchrotron facility in the United States dedicated to chemistry/materials research (with emphasis on polymers). The major benefit of this facility to the materials community is that no extensive synchrotron experience and equipment preparation are required from general users to carry out cutting-edge experiments.

  4. Application of High Pressure in Food Processing

    Directory of Open Access Journals (Sweden)

    Herceg, Z.

    2011-01-01

    Full Text Available In high pressure processing, foods are subjected to pressures generally in the range of 100 – 800 (1200 MPa. The processing temperature during pressure treatments can be adjusted from below 0 °C to above 100 °C, with exposure times ranging from a few seconds to 20 minutes and even longer, depending on process conditions. The effects of high pressure are system volume reduction and acceleration of reactions that lead to volume reduction. The main areas of interest regarding high-pressure processing of food include: inactivation of microorganisms, modification of biopolymers, quality retention (especially in terms of flavour and colour, and changes in product functionality. Food components responsible for the nutritive value and sensory properties of food remain unaffected by high pressure. Based on the theoretical background of high-pressure processing and taking into account its advantages and limitations, this paper aims to show its possible application in food processing. The paper gives an outline of the special equipment used in highpressure processing. Typical high pressure equipment in which pressure can be generated either by direct or indirect compression are presented together with three major types of high pressure food processing: the conventional (batch system, semicontinuous and continuous systems. In addition to looking at this technology’s ability to inactivate microorganisms at room temperature, which makes it the ultimate alternative to thermal treatments, this paper also explores its application in dairy, meat, fruit and vegetable processing. Here presented are the effects of high-pressure treatment in milk and dairy processing on the inactivation of microorganisms and the modification of milk protein, which has a major impact on rennet coagulation and curd formation properties of treated milk. The possible application of this treatment in controlling cheese manufacture, ripening and safety is discussed. The opportunities

  5. Evaluation of load case ``switch-off of the high pressure pump of the emergency core cooling system``, measures of verification and in situ-test; Einstufung des Lastfalls ``Ausfall der TH-Hochdruckeinspeisepumpe``, Massnahmen zur Verifikation bis hin zum Grossversuch

    Energy Technology Data Exchange (ETDEWEB)

    Trobitz, M.; Mattheis, A. [Kernkraftwerke Gundremmingen Betriebsgesellschaft m.b.H. (Germany); Kerkhof, K.; Hippelein, K. [Stuttgart Univ. (Germany). Staatliche Materialpruefungsanstalt; Gurr-Beyer, C. [Buero fuer Baudynamik, Stuttgart (Germany); Hofstoetter, P. [Technischer Ueberwachungs-Verein Rheinland e.V., Koeln (Germany)

    1998-11-01

    Within the framework of periodic safety inspection of the Gundremmingen power station (RWE-Bayernwerk - KRB II), the load collectives used for the design of safety-relevant systems and components were checked for their consistency with latest updates of the design basis. It was found that there was no analytical information or study available describing a particular process and its effects, namely switch-off of the high-pressure feedwater pump of the emergency core cooling system. The paper reports the work performed for closing the gap, including preparatory analyses, accompanying measures such as vibration measurements during plant shut-down, as well as the preparation and performance of the in-situ test. The experimental results and the comparative evaluation of calculated and experimental data are presented. (orig./CB) [Deutsch] Im Rahmen der periodischen Sicherheitsueberpruefung des Kernkraftwerkes Gundremmingen (Kernkraftwerke RWE-Bayernwerk - KRB II) wurden u.a. die Lastkollektive, die zur Auslegung sicherheitstechnisch relevanter Systeme und Komponenten herangezogen wurden, auf Aktualitaet ueberprueft. Dabei zeigte sich, dass bislang fuer eine Betriebsweise - naemlich das Abschalten der Hochdruckeinspeisepumpe des nuklearen Not- und Nachkuehlsystems (TH-HD-Pumpe) - keine analytischen Untersuchungen vorliegen. Vorbetrachtungen fuer analytische Untersuchungen, begleitende Massnahmen wie Schwingungsmessungen waehrend des Anlagenstillstandes, sowie der Versuchsaufbau und die Versuchsdurchfuehrung des Anlagenversuches werden hier dargestellt. Die Ergebnisse und der Vergleich Rechnung-Messung zum Grossversuch werden in diesem Beitrag vorgestellt. (orig.)

  6. High pressure XAFS experiments at the XAFS beamline, INDUS-2

    International Nuclear Information System (INIS)

    Ramanan, Nitya; Lahiri, Debdutta; Garg, Nandini; Sharma, Surinder M.; Bhattacharyya, D.; Jha, S.N.; Sahoo, N.K.

    2011-01-01

    The dispersive EXAFS beamline at the INDUS-2 synchrotron source, RRCAT, Indore uses a bent Si (111) crystal as a dispersive-cum-focusing element and a position sensitive CCD detector to enable instantaneous measurement of the whole EXAFS spectrum around the absorption edge of a particular atom. One of the proposed activities with this beamline is the characterization of amorphous materials under high pressure. Polychromator-based beamline is ideal for high pressure studies using Diamond Anvil Cell (DAC) with ∼ 50 μm sample size. Larger spot size would give rise to unwanted diffraction peaks from diamond, superimposed on the XAFS data. Micro-focusing by polychromator crystal and absence of its mechanical movement (unlike monochromator-based scanning-mode beamlines), during data collection, lead to required focal spot stability for DAC experiments. Currently, the theoretically determined spot size (Horizontal x vertical) varies between 17 x 137 μm and 37 x 142 μm for the X-ray energy range 5 keV-20 keV. To reduce the vertical spot size to <50 μm, we have designed an additional focusing mirror between the polychromator and sample position. The mirror, fabricated at SESO, France will be installed shortly. Meanwhile, we have carried out preliminary XAFS experiments on Sr-compounds at ∼16 keV, under ambient conditions and inside diamond anvil cell, in order to assess the signal intensity and quality. We have obtained reasonably good signal. (author)

  7. Modeling High Pressure Micro Hollow Cathode Discharges

    National Research Council Canada - National Science Library

    Boeuf, Jean-Pierre; Pitchford, Leanne

    2004-01-01

    This report results from a contract tasking CPAT as follows: The Grantee will perform theoretical modeling of point, surface, and volume high-pressure plasmas created using Micro Hollow Cathode Discharge sources...

  8. High Pressure EVA Glove (HPEG), Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Final Frontier Design's (FFD) High Pressure EVA Glove (HPEG) is a game changing technology enabling future exploration class space missions. The high operating...

  9. High pressure structural studies on nanophase praseodymium oxide

    International Nuclear Information System (INIS)

    Saranya, L.; Chandra Shekar, N.V.; Amirthapandian, S.; Hussain, Shamima; Arulraj, A.; Sahu, P. Ch.

    2014-01-01

    The phase stability of nanocrystalline Pr 2 O 3 has been investigated under pressure by in-situ high pressure X-ray diffraction using Mao-Bell type diamond anvil cell. The ambient structure and phase of the praseodymium oxide have been resolved unambiguously using x-ray diffraction, SEM and TEM techniques. Under the action of pressure the cubic phase of the system is retained up to 15 GPa. This is unusual as other isostructural rare earth oxides show structural transformations even at lower pressures. From the best fit to the P–V data with the Murnaghan equation of state yields a bulk modulus of 171 GPa

  10. High-pressure phase transitions of strontianite

    Science.gov (United States)

    Speziale, S.; Biedermann, N.; Reichmann, H. J.; Koch-Mueller, M.; Heide, G.

    2015-12-01

    Strontianite (SrCO3) is isostructural to aragonite, a major high-pressure polymorph of calcite. Thus it is a material of interest to investigate the high-pressure phase behavior of aragonite-group minerals. SrCO3 is a common component of natural carbonates and knowing its physical properties at high pressures is necessary to properly model the thermodynamic properties of complex carbonates, which are major crustal minerals but are also present in the deep Earth [Brenker et al., 2007] and control carbon cycling in the Earth's mantle. The few available high-pressure studies of SrCO3 disagree regarding both pressure stability and structure of the post-aragonite phase [Lin & Liu, 1997; Ono et al., 2005; Wang et al. 2015]. To clarify such controversies we investigated the high-pressure behavior of synthetic SrCO3 by Raman spectroscopy. Using a diamond anvil cell we compressed single-crystals or powder of strontianite (synthesized at 4 GPa and 1273 K for 24h in a multi anvil apparatus), and measured Raman scattering up to 78 GPa. SrCO3 presents a complex high-pressure behavior. We observe mode softening above 20 GPa and a phase transition at 25 - 26.9 GPa, which we interpret due to the CO3 groups rotation, in agreement with Lin & Liu [1997]. The lattice modes in the high-pressure phase show dramatic changes which may indicate a change from 9-fold coordinated Sr to a 12-fold-coordination [Ono, 2007]. Our results confirm that the high-pressure phase of strontianite is compatible with Pmmn symmetry. References Brenker, F.E. et al. (2007) Earth and Planet. Sci. Lett., 260, 1; Lin, C.-C. & Liu, L.-G. (1997) J. Phys. Chem. Solids, 58, 977; Ono, S. et al. (2005) Phys. Chem. Minerals, 32, 8; Ono, S. (2007) Phys. Chem. Minerals, 34, 215; Wang, M. et al. (2015) Phys Chem Minerals 42, 517.

  11. High-pressure portable pneumatic drive unit.

    Science.gov (United States)

    Hete, B F; Savage, M; Batur, C; Smith, W A; Golding, L A; Nosé, Y

    1989-12-01

    The left ventricular assist device (LVAD) of the Cleveland Clinic Foundation (CCF) is a single-chamber assist pump, driven by a high-pressure pneumatic cylinder. A low-cost, portable driver that will allow cardiac care patients, with a high-pressure pneumatic ventricle assist, more freedom of movement has been developed. The compact and light-weight configuration can provide periods of 2 h of freedom from a fixed position driver and does not use exotic technology.

  12. High pressure effects on fruits and vegetables

    OpenAIRE

    Timmermans, R.A.H.; Matser, A.M.

    2016-01-01

    The chapter provides an overview on different high pressure based treatments (high pressure pasteurization, blanching, pressure-assisted thermal processing, pressure-shift freezing and thawing) available for the preservation of fruits and vegetable products and extending their shelf life. Pressure treatment can be used for product modification through pressure gelatinization of starch and pressure denaturation of proteins. Key pressure–thermal treatment effects on vitamin, enzymes, flavor, co...

  13. High pressure X-ray studies

    International Nuclear Information System (INIS)

    Sikka, S.K.

    1981-01-01

    High pressure research has already led to new insights in the physical properties of materials and at times to the synthesis of new ones. In all this, X-ray diffraction has been a valuable diagnostic experimental tool. In particular, X-rays in high pressure field have been used (a) for crystallographic identification of high pressure polymorphs and (b) for study of the effect of pressure on lattice parameters and volume under isothermal conditions. The results in the area (a) are reviewed. The techniques of applying high pressures are described. These include both static and dynamic shockwave X-ray apparatus. To illustrate the effect of pressure, some of the pressure induced phase transitions in pure metals are described. It has been found that there is a clear trend for elements in any group of the periodic table to adopt similar structures at high pressures. These studies have enabled to construct generalized phase diagrams for many groups. In the case of alloys, the high pressure work done on Ti-V alloys is presented. (author)

  14. Infrared spectroscopy by use of synchrotron radiation

    International Nuclear Information System (INIS)

    Nanba, Takao

    1991-01-01

    During five years since the author wrote the paper on the utilization of synchrotron radiation in long wavelength region, it seems to be recognized that in synchrotron radiation, the light from infrared to milli wave can be utilized, and is considerably useful. Recently the research on coherent synchrotron radiation in this region using electron linac has been developed by Tohoku University group, and the high capability of synchrotron radiation as light source is verified. This paper is the report on the infrared spectroscopic research using incoherent synchrotron radiation obtained from the deflection electromagnet part of electron storage rings. Synchrotron radiation is high luminance white light source including from X-ray to micro wave. The example of research that the author carried out at UVSOR is reported, and the perspective in near future is mentioned. Synchrotron radiation as the light source for infrared spectroscopy, the intensity and dimensions of the light source, far infrared region and mid infrared region, far infrared high pressure spectroscopic experiment, and the heightening of luminance of synchrotron radiation as infrared light source are described. (K.I.)

  15. Synthesis and stability of hydrogen selenide compounds at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Pace, Edward J.; Binns, Jack; Alvarez, Miriam Pena; Dalladay-Simpson, Philip; Gregoryanz, Eugene; Howie, Ross T. (Edinburgh); (CHPSTAR- China)

    2017-11-14

    The observation of high-temperature superconductivity in hydride sulfide (H2S) at high pressures has generated considerable interest in compressed hydrogen-rich compounds. High-pressure hydrogen selenide (H2Se) has also been predicted to be superconducting at high temperatures; however, its behaviour and stability upon compression remains unknown. In this study, we synthesize H2Se in situ from elemental Se and molecular H2 at pressures of 0.4 GPa and temperatures of 473 K. On compression at 300 K, we observe the high-pressure solid phase sequence (I-I'-IV) of H2Se through Raman spectroscopy and x-ray diffraction measurements, before dissociation into its constituent elements. Through the compression of H2Se in H2 media, we also observe the formation of a host-guest structure, (H2Se)2H2, which is stable at the same conditions as H2Se, with respect to decomposition. These measurements show that the behaviour of H2Se is remarkably similar to that of H2S and provides further understanding of the hydrogen chalcogenides under pressure.

  16. Synchrotron Radiation

    International Nuclear Information System (INIS)

    Asfour, F.I

    2000-01-01

    Synchrotron light is produced by electron accelerators combined with storage rings. This light is generated over a wide spectral region; from infra-red (IR) through the visible and vacuum ultraviolet (VUV), and into the X-ray region. For relativistic electrons (moving nearly with the speed of light), most radiation is concentrated in a small cone with an opening angle of 1/gamma(some 0.1 to 1 milliradian),where gamma is the electron energy in units of rest energy (typically 10 3 -10 4 ). In synchrotron radiation sources (storage rings) highly relativistic electrons are stored to travel along a circular path for many hours. Radiation is caused by transverse acceleration due to magnetic forces(bending magnets). The radiation is emitted in pulses of 10-20 picosecond, separated by some 2 nanosecond or longer separation

  17. Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

    Science.gov (United States)

    Ma, Yan; Song, Wenwen; Bleck, Wolfgang

    2017-09-25

    The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels-in terms of ε-martensite and α'-martensite volume fractions, the stacking fault probability, and the twin fault probability-was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α'-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.

  18. Re-investigation of the crystal structure of enstatite under high-pressure conditions

    DEFF Research Database (Denmark)

    Periotto, Benedetta; Balic Zunic, Tonci; Nestola, Fabrizio

    2012-01-01

    A synthetic single crystal of pure orthoenstatite (MgSiO3, space group Pbca) has been investigated at high pressure for structural determinations by in situ single-crystal X‑ray diffraction using a diamond-anvil cell. Ten complete intensity data collections were performed up to 9.36 GPa. This study...... with different compositions. The structural evolution determined in this work confirms the high-pressure evolution found previously for other orthopyroxenes and removes some ambiguities originating from the less accurate published data on the MgSiO3 structure at high pressure. The structural compression...

  19. The influence of methanol on the chemical state of PtRu anodes in a high-temperature direct methanol fuel cell studied in situ by synchrotron-based near-ambient pressure x-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Saveleva, Viktoriia A; Savinova, Elena R; Daletou, Maria K

    2017-01-01

    Synchrotron radiation-based near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) has recently become a powerful tool for the investigation of interfacial phenomena in electrochemical power sources such as batteries and fuel cells. Here we present an in situ NAP-XPS study of the anode of a high-temperature direct methanol fuel cell with a phosphoric acid-doped hydrocarbon membrane, which reveals an enhanced flooding of the Pt 3 Ru anode with phosphoric acid in the presence of methanol. An analysis of the electrode surface composition depending on the cell voltage and on the presence of methanol reveals the strong influence of the latter on the extent of Pt oxidation and on the transformation of Ru into Ru (IV) hydroxide. (paper)

  20. The influence of methanol on the chemical state of PtRu anodes in a high-temperature direct methanol fuel cell studied in situ by synchrotron-based near-ambient pressure x-ray photoelectron spectroscopy

    Science.gov (United States)

    Saveleva, Viktoriia A.; Daletou, Maria K.; Savinova, Elena R.

    2017-01-01

    Synchrotron radiation-based near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) has recently become a powerful tool for the investigation of interfacial phenomena in electrochemical power sources such as batteries and fuel cells. Here we present an in situ NAP-XPS study of the anode of a high-temperature direct methanol fuel cell with a phosphoric acid-doped hydrocarbon membrane, which reveals an enhanced flooding of the Pt3Ru anode with phosphoric acid in the presence of methanol. An analysis of the electrode surface composition depending on the cell voltage and on the presence of methanol reveals the strong influence of the latter on the extent of Pt oxidation and on the transformation of Ru into Ru (IV) hydroxide.

  1. Abundance and Charge State of Implanted Solar Wind Transition Metals in Individual Apollo 16 and 17 Lunar Soil Plagioclase Grains Determined In Situ Using Synchrotron X-ray Fluorescence

    International Nuclear Information System (INIS)

    Kitts, K.; Sutton, S.; Newville, M.

    2007-01-01

    We report (1) a new method for determining the relative abundances in situ of Cr, Mn, Fe and Ni in implanted solar wind in individual Apollo 16 and 17 lunar plagioclases via synchrotron X-ray fluorescence and (2) the charge states of these metals. By virture of its mass alone, the Sun provides a representative composition of the solar system and can be used as a background against which to gauge excesses or deficiencies of specific components. One way of sampling the Sun is by measuring solar wind implanted ions in lunar soil grains. Such measurements are valuable because of their long exposure ages which compliment shorter time scale collections, such as those obtained by the Genesis spacecraft. Kitts et al. sought to determine the isotopic composition of solar Cr by analyzing the solar wind implanted into plagioclase grains from Apollo 16 lunar soils. The isotopic composition of the solar wind bearing fraction was anomalous and did not match any other known Cr isotopic signature. This could only be explained by either (1) an enrichment in the solar wind of heavy Cr due to spallation in the solar atmosphere or (2) that the Earth and the various parent bodies of the meteorites are distinct from the Sun and must have formed from slightly different mixes of presolar materials. To help resolve this issue, we have developed a wholly independent method for determining the relative abundances of transition metals in the solar wind implanted in individual lunar soil grains. This method is based on in situ abundance measurements by microbeam x-ray fluorescence in both the implantation zone and bulk grains using the synchrotron x-ray microprobe at the Advanced Photon Source (GSECARS sector 13) at Argonne National Laboratory. Here, we report results for Apollo 16 and 17 plagioclase grains. Additionally, a micro-XANES technique was used to determine charge states of the implanted Cr, Mn, Fe and Ni.

  2. High pressure structural behavior of YGa2: A combined experimental and theoretical study

    International Nuclear Information System (INIS)

    Sekar, M.; Shekar, N.V. Chandra; Babu, R.; Sahu, P. Ch.; Sinha, A.K.; Upadhyay, Anuj; Singh, M.N.; Babu, K. Ramesh; Appalakondaiah, S.; Vaitheeswaran, G.; Kanchana, V.

    2015-01-01

    High pressure structural stability studies were carried out on YGa 2 (AlB 2 type structure at NTP, space group P6/mmm) up to a pressure of ~35 GPa using both laboratory based rotating anode and synchrotron X-ray sources. An isostructural transition with reduced c/a ratio, was observed at ~6 GPa and above ~17.5 GPa, the compound transformed to orthorhombic structure. Bulk modulus B 0 for the parent and high pressure phases were estimated using Birch–Murnaghan and modified Birch–Murnaghan equation of state. Electronic structure calculations based on projector augmented wave method confirms the experimentally observed two high pressure structural transitions. The calculations also reveal that the ‘Ga’ networks remains as two dimensional in the high pressure isostructural phase, whereas the orthorhombic phase involves three dimensional networks of ‘Ga’ atoms interconnected by strong covalent bonds. - Graphical abstract: High pressure X-ray diffraction patterns of YGa 2 up to ~35 GPa shows an isostructural phase transition at ~5 GPa and transition to an orthorhombic structure ~14 GPa. - Highlights: • High pressure structural stability studies were carried out on YGa 2 up to 35 GPa. • An isostructural transition with reduced c/a ratio was observed above 6 GPa. • Above 17.5 GPa, the compound transformed to orthorhombic structure. • PAW based electronic structure calculations have been carried out. • Calculations confirm the experimentally observed structural transitions

  3. On high-pressure melting of tantalum

    Science.gov (United States)

    Luo, Sheng-Nian; Swift, Damian C.

    2007-01-01

    The issues related to high-pressure melting of Ta are discussed within the context of diamond-anvil cell (DAC) and shock wave experiments, theoretical calculations and common melting models. The discrepancies between the extrapolations of the DAC melting curve and the melting point inferred from shock wave experiments, cannot be reconciled either by superheating or solid-solid phase transition. The failure to reproduce low-pressure DAC melting curve by melting models such as dislocation-mediated melting and the Lindemann law, and molecular dynamics and quantum mechanics-based calculations, undermines their predictions at moderate and high pressures. Despite claims to the contrary, the melting curve of Ta (as well as Mo and W) remains inconclusive at high pressures.

  4. High-pressure boron hydride phases

    International Nuclear Information System (INIS)

    Barbee, T.W. III; McMahan, A.K.; Klepeis, J.E.; van Schilfgaarde, M.

    1997-01-01

    The stability of boron-hydrogen compounds (boranes) under pressure is studied from a theoretical point of view using total-energy methods. We find that the molecular forms of boranes known to be stable at ambient pressure become unstable at high pressure, while structures with extended networks of bonds or metallic bonding are energetically favored at high pressures. If such structures are metastable on return to ambient pressure, they would be energetic as well as dense hydrogen storage media. An AlH 3 -like structure of BH 3 is particularly interesting in that it may be accessible by high-pressure diamond anvil experiments, and should exhibit both second-order structural and metal-insulator transitions at lower pressures. copyright 1997 The American Physical Society

  5. The pressure behaviour of actinides via synchrotron radiation

    International Nuclear Information System (INIS)

    Haire, R.G.; Heathman, S.; Le Bihan, T.; Lindbaum, A.

    2002-01-01

    Various aspects of performing high-pressure studies with radioactive f-elements using synchrotrons as sources of X-rays are discussed. For ultra-high pressures, intense well-focused beams of 10 to 30 microns in diameter and a single wavelength of 0.3 to 0.7 angstrom are desired for angle dispersive diffraction measurements. Special considerations are necessary for the studies of transuranium elements under pressure at synchrotron facilities. Normally, with these actinides the pressure cells are prepared off-site and shipped to the synchrotron for study. Approved containment techniques must be provided to assure there is not a potential for the release of sample material. The goal of these high-pressure studies is to explore the fundamental science occurring as pressure is applied to the actinide samples. One of the primary effects of pressure is to reduce interatomic distances, and the goal is to ascertain the changes in bonding and electronic nature of the system that result as atoms and electronic orbitals are forced closer together. Concepts of the science being pursued with these f-elements are outlined. A brief discussion of the behaviour of americium metal under pressure performed recently at the ESRF is provided as an example of the high-pressure research being performed with synchrotron radiation. Also discussed here is the important role synchrotrons play and the techniques/procedures employed in high-pressure studies with actinides. (authors)

  6. High pressure freon decontamination of remote equipment

    International Nuclear Information System (INIS)

    Wilson, C.E.

    1987-01-01

    A series of decontamination tests using high pressure FREON 113 was conducted in the 200 Area of the Hanford site. The intent of these tests was to evaluate the effectiveness of FREON 113 in decontamination of manipulator components, tools, and equipment items contaminated with mixed fission products. The test results indicated that high pressure FREON 113 is very effective in removing fissile material from a variety of objects and can reduce both the quantity and the volume of the radioactive waste material presently being buried

  7. Techniques in high pressure neutron scattering

    CERN Document Server

    Klotz, Stefan

    2013-01-01

    Drawing on the author's practical work from the last 20 years, Techniques in High Pressure Neutron Scattering is one of the first books to gather recent methods that allow neutron scattering well beyond 10 GPa. The author shows how neutron scattering has to be adapted to the pressure range and type of measurement.Suitable for both newcomers and experienced high pressure scientists and engineers, the book describes various solutions spanning two to three orders of magnitude in pressure that have emerged in the past three decades. Many engineering concepts are illustrated through examples of rea

  8. High pressure water jet cutting and stripping

    Science.gov (United States)

    Hoppe, David T.; Babai, Majid K.

    1991-01-01

    High pressure water cutting techniques have a wide range of applications to the American space effort. Hydroblasting techniques are commonly used during the refurbishment of the reusable solid rocket motors. The process can be controlled to strip a thermal protective ablator without incurring any damage to the painted surface underneath by using a variation of possible parameters. Hydroblasting is a technique which is easily automated. Automation removes personnel from the hostile environment of the high pressure water. Computer controlled robots can perform the same task in a fraction of the time that would be required by manual operation.

  9. High pressure water jet mining machine

    Science.gov (United States)

    Barker, Clark R.

    1981-05-05

    A high pressure water jet mining machine for the longwall mining of coal is described. The machine is generally in the shape of a plowshare and is advanced in the direction in which the coal is cut. The machine has mounted thereon a plurality of nozzle modules each containing a high pressure water jet nozzle disposed to oscillate in a particular plane. The nozzle modules are oriented to cut in vertical and horizontal planes on the leading edge of the machine and the coal so cut is cleaved off by the wedge-shaped body.

  10. High-pressure X-ray diffraction and Raman spectroscopy of CaFe2O4-type β-CaCr2O4

    Science.gov (United States)

    Zhai, Shuangmeng; Yin, Yuan; Shieh, Sean R.; Shan, Shuangming; Xue, Weihong; Wang, Ching-Pao; Yang, Ke; Higo, Yuji

    2016-04-01

    In situ high-pressure synchrotron X-ray diffraction and Raman spectroscopic studies of orthorhombic CaFe2O4-type β-CaCr2O4 chromite were carried out up to 16.2 and 32.0 GPa at room temperature using multi-anvil apparatus and diamond anvil cell, respectively. No phase transition was observed in this study. Fitting a third-order Birch-Murnaghan equation of state to the P-V data yields a zero-pressure volume of V 0 = 286.8(1) Å3, an isothermal bulk modulus of K 0 = 183(5) GPa and the first pressure derivative of isothermal bulk modulus K 0' = 4.1(8). Analyses of axial compressibilities show anisotropic elasticity for β-CaCr2O4 since the a-axis is more compressible than the b- and c-axis. Based on the obtained and previous results, the compressibility of several CaFe2O4-type phases was compared. The high-pressure Raman spectra of β-CaCr2O4 were analyzed to determine the pressure dependences and mode Grüneisen parameters of Raman-active bands. The thermal Grüneisen parameter of β-CaCr2O4 is determined to be 0.93(2), which is smaller than those of CaFe2O4-type CaAl2O4 and MgAl2O4.

  11. Synchrotron radiation

    International Nuclear Information System (INIS)

    Farge, Y.

    1982-01-01

    Synchrotron radiation is produced by electrons accelerated near the velocity of light in storage rings, which are used for high energy Physics experiments. The radiation light exhibits a wide spread continuous spectrum ranging from 01 nanometre to radiofrequency. This radiation is characterized by high power (several kilowatts) and intense brightness. The paper recalls the emission laws and the distinctive properties of the radiation, and gives some of the numerous applications in research, such as molecular spectroscopy, X ray diffraction by heavy proteins and X ray microlithography in LVSI circuit making [fr

  12. High Pressure Inactivation of HAV within Mussels

    Science.gov (United States)

    The potential of hepatitis A virus (HAV) to be inactivated within Mediterranean mussels (Mytilus galloprovincialis) and blue mussels (Mytilus edulis) by high pressure processing was evaluated. HAV was bioaccumulated within mussels to approximately 6-log10 PFU by exposure of mussels to HAV-contamina...

  13. Nucleation at high pressure I: Theoretical considerations.

    NARCIS (Netherlands)

    Luijten, C.C.M.; Dongen, van M.E.H.

    1999-01-01

    A theoretical approach is presented that accounts for the influence of high pressure background gases on the vapor-to-liquid nucleation process. The key idea is to treat the carrier gas pressure as a perturbation parameter that modifies the properties of the nucleating substance. Two important

  14. High pressure metrology for industrial applications

    Science.gov (United States)

    Sabuga, Wladimir; Rabault, Thierry; Wüthrich, Christian; Pražák, Dominik; Chytil, Miroslav; Brouwer, Ludwig; Ahmed, Ahmed D. S.

    2017-12-01

    To meet the needs of industries using high pressure technologies, in traceable, reliable and accurate pressure measurements, a joint research project of the five national metrology institutes and the university was carried out within the European Metrology Research Programme. In particular, finite element methods were established for stress-strain analysis of elastic and nonlinear elastic-plastic deformation, as well as of contact processes in pressure-measuring piston-cylinder assemblies, and high-pressure components at pressures above 1 GPa. New pressure measuring multipliers were developed and characterised, which allow realisation of the pressure scale up to 1.6 GPa. This characterisation is based on research including measurements of material elastic constants by the resonant ultrasound spectroscopy, hardness of materials of high pressure components, density and viscosity of pressure transmitting liquids at pressures up to 1.4 GPa and dimensional measurements on piston-cylinders. A 1.6 GPa pressure system was created for operation of the 1.6 GPa multipliers and calibration of high pressure transducers. A transfer standard for 1.5 GPa pressure range, based on pressure transducers, was built and tested. Herewith, the project developed the capability of measuring pressures up to 1.6 GPa, from which industrial users can calibrate their pressure measurement devices for accurate measurements up to 1.5 GPa.

  15. High-pressure differential scanning microcalorimeter.

    Science.gov (United States)

    Senin, A A; Dzhavadov, L N; Potekhin, S A

    2016-03-01

    A differential scanning microcalorimeter for studying thermotropic conformational transitions of biopolymers at high pressure has been designed. The calorimeter allows taking measurements of partial heat capacity of biopolymer solutions vs. temperature at pressures up to 3000 atm. The principles of operation of the device, methods of its calibration, as well as possible applications are discussed.

  16. High-pressure oxidation of methane

    NARCIS (Netherlands)

    Hashemi, Hamid; Christensen, Jakob M.; Gersen, Sander; Levinsky, Howard; Klippenstein, Stephen J.; Glarborg, Peter

    2016-01-01

    Methane oxidation at high pressures and intermediate temperatures was investigated in a laminar flow reactor and in a rapid compression machine (RCM). The flow-reactor experiments were conducted at 700–900 K and 100 bar for fuel-air equivalence ratios (Φ) ranging from 0.06 to 19.7, all highly

  17. Study of ceramics sintering under high pressures

    International Nuclear Information System (INIS)

    Kunrath Neto, A.O.

    1990-01-01

    A systematic study was made on high pressure sintering of ceramics in order to obtain materials with controlled microstructure, which are not accessible by conventional methods. Some aspects with particular interest were: to achieve very low porosity, with fine grains; to produce dispersed metastable and denser phases which can act as toughening agents; the study of new possibilities for toughening enhancement. (author)

  18. High Pressure Physics at Brigham Young University

    Science.gov (United States)

    Decker, Daniel

    2000-09-01

    I will discuss the high pressure research of Drs. J. Dean Barnett, Daniel L. Decker and Howard B. Vanfleet of the department of Physics and Astronomy at Brigham Young University and their many graduate students. I will begin by giving a brief history of the beginning of high pressure research at Brigham Young University when H. Tracy Hall came to the University from General Elecrtric Labs. and then follow the work as it progressed from high pressure x-ray diffraction experiments, melting curve measurements under pressure to pressure effects on tracer diffusion and Mossbauer effect spectra. This will be followed by showing the development of pressure calibration techniques from the Decker equation of state of NaCl to the ruby fluorescence spectroscopy and a short discussion of using a liquid cell for hydrostatic measurements and temperature control for precision high pressure measurements. Then I will conclude with a description of thermoelectric measuremnts, critical phenomena at the magnetic Curie point, and the tricritical point of BaTiO_3.

  19. High pressure synthesis of bismuth disulfide

    DEFF Research Database (Denmark)

    Søndergaard-Pedersen, Simone; Nielsen, Morten Bormann; Bremholm, Martin

    In this research the BiS2 compound was synthesized by a high pressure and high temperature method using a multi-anvil large volume press and the structure was solved by single crystal diffraction. The structure contains Bi atoms in distorted square-based pyramidal coordination to five surrounding...

  20. Analysis of high-pressure safety valves

    NARCIS (Netherlands)

    Beune, A.

    2009-01-01

    In presently used safety valve sizing standards the gas discharge capacity is based on a nozzle flow derived from ideal gas theory. At high pressures or low temperatures real gas effects can no longer be neglected, so the discharge coefficient corrected for flow losses cannot be assumed constant

  1. High pressure studies of planetary matter

    International Nuclear Information System (INIS)

    Ross, M.

    1989-06-01

    Those materials which are of greatest interest to the physics of the deep planetary interiors are Fe, H 2 , He and the Ices. These are sufficiently diverse and intensively studied to offer an overview of present day high pressure research. 13 refs., 1 fig

  2. In situ observation of initial rust formation process on carbon steel under Na2SO4 and NaCl solution films with wet/dry cycles using synchrotron radiation X-rays

    International Nuclear Information System (INIS)

    Yamashita, M.; Konishi, H.; Kozakura, T.; Mizuki, J.; Uchida, H.

    2005-01-01

    Atmospheric corrosion of steel proceeds under thin electrolyte film formed by rain and dew condensation followed by wet and dry cycles. It is said that rust layer formed on steel as a result of atmospheric corrosion strongly affects the corrosion behavior of steel. The effect of environmental corrosiveness on the formation process and structure of the rust layer is, however, not clear to date. In this study, in situ observation of the rusting process of a carbon steel covered with a thin film of Na 2 SO 4 or NaCl solution was performed under a wet/dry repeating condition by X-ray diffraction spectroscopy with white X-rays obtained from synchrotron radiation. The present in situ experiments successfully detected initial process of the rust formation. In the early cycles, the rust constituents were not well crystallized yet, but the presence of Fe(OH) 2 and Fe(OH) 3 was confirmed. In the subsequent cycles, two different solutions resulted in difference in preferential phase of the rust constituents. α-FeOOH was preferentially formed in the case of the Na 2 SO 4 solution film, whereas β-FeOOH appeared only under the NaCl solution film

  3. Capacity Fading Mechanism of the Commercial 18650 LiFePO4-Based Lithium-Ion Batteries: An in Situ Time-Resolved High-Energy Synchrotron XRD Study.

    Science.gov (United States)

    Liu, Qi; Liu, Yadong; Yang, Fan; He, Hao; Xiao, Xianghui; Ren, Yang; Lu, Wenquan; Stach, Eric; Xie, Jian

    2018-02-07

    In situ high-energy synchrotron XRD studies were carried out on commercial 18650 LiFePO 4 cells at different cycles to track and investigate the dynamic, chemical, and structural changes in the course of long-term cycling to elucidate the capacity fading mechanism. The results indicate that the crystalline structural deterioration of the LiFePO 4 cathode and the graphite anode is unlikely to happen before capacity fades below 80% of the initial capacity. Rather, the loss of the active lithium source is the primary cause for the capacity fade, which leads to the appearance of inactive FePO 4 that is proportional to the absence of the lithium source. Our in situ HESXRD studies further show that the lithium-ion insertion and deinsertion behavior of LiFePO 4 continuously changed with cycling. For a fresh cell, the LiFePO 4 experienced a dual-phase solid-solution behavior, whereas with increasing cycle numbers, the dynamic change, which is characteristic of the continuous decay of solid solution behavior, is obvious. The unpredicted dynamic change may result from the morphology evolution of LiFePO 4 particles and the loss of the lithium source, which may be the cause of the decreased rate capability of LiFePO 4 cells after long-term cycling.

  4. High pressure study of high-temperature superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Souliou, Sofia-Michaela

    2014-09-29

    The current thesis studies experimentally the effect of high external pressure on high-T{sub c} superconductors. The structure and lattice dynamics of several members of the high-T{sub c} cuprate and Fe-based superconductors families were investigated by means of Raman spectroscopy and X-ray diffraction under well-controlled, hydrostatic high pressure and low temperature conditions. The lattice dynamics of the high-T{sub c} superconductor YBa{sub 2}Cu{sub 3}O{sub 6+x} have been investigated systematically by Raman spectroscopy as a function of doping (x = 0.95, 0.75, 0.60, 0.55, and 0.45) and external pressure. Under ambient pressure conditions, in addition to the Raman modes expected from group theory, we observe new Raman active phonons upon cooling the underdoped samples, at temperatures well above the superconducting transition temperature. The doping dependence and the onset temperatures of the new Raman features suggest that they are associated with the incommensurate charge density wave (CDW) state recently discovered in underdoped cuprates using synchrotron X-ray scattering techniques. Under high pressure conditions (from 2 to 12 GPa), our Raman measurements on highly ordered underdoped YBa{sub 2}Cu{sub 3}O{sub 6.55} samples do not show any of the new Raman phonons seen at ambient pressure. High pressure and low temperature Raman measurements have been performed on the underdoped superconductor YBa{sub 2}Cu{sub 4}O{sub 8}. A clear renormalization of some of the Raman phonons is seen below T{sub c} as a result of the changes in the phonon self-energy upon the opening of the superconducting gap, with the most prominent one being that of the B{sub 1g}-like buckling phonon mode. The amplitude of this renormalization strongly increases with pressure, resembling the effect of hole doping in YBa{sub 2}Cu{sub 3}O{sub 6+x}. At ∝ 10 GPa, the system undergoes a reversible pressure-induced structural phase transition to a non-centrosymmmetric structure (space group

  5. High pressure study of high-temperature superconductors

    International Nuclear Information System (INIS)

    Souliou, Sofia-Michaela

    2014-01-01

    The current thesis studies experimentally the effect of high external pressure on high-T c superconductors. The structure and lattice dynamics of several members of the high-T c cuprate and Fe-based superconductors families were investigated by means of Raman spectroscopy and X-ray diffraction under well-controlled, hydrostatic high pressure and low temperature conditions. The lattice dynamics of the high-T c superconductor YBa 2 Cu 3 O 6+x have been investigated systematically by Raman spectroscopy as a function of doping (x = 0.95, 0.75, 0.60, 0.55, and 0.45) and external pressure. Under ambient pressure conditions, in addition to the Raman modes expected from group theory, we observe new Raman active phonons upon cooling the underdoped samples, at temperatures well above the superconducting transition temperature. The doping dependence and the onset temperatures of the new Raman features suggest that they are associated with the incommensurate charge density wave (CDW) state recently discovered in underdoped cuprates using synchrotron X-ray scattering techniques. Under high pressure conditions (from 2 to 12 GPa), our Raman measurements on highly ordered underdoped YBa 2 Cu 3 O 6.55 samples do not show any of the new Raman phonons seen at ambient pressure. High pressure and low temperature Raman measurements have been performed on the underdoped superconductor YBa 2 Cu 4 O 8 . A clear renormalization of some of the Raman phonons is seen below T c as a result of the changes in the phonon self-energy upon the opening of the superconducting gap, with the most prominent one being that of the B 1g -like buckling phonon mode. The amplitude of this renormalization strongly increases with pressure, resembling the effect of hole doping in YBa 2 Cu 3 O 6+x . At ∝ 10 GPa, the system undergoes a reversible pressure-induced structural phase transition to a non-centrosymmmetric structure (space group Imm2). The structural transition is clearly reflected in the high pressure

  6. Advanced Diagnostics for High Pressure Spray Combustion.

    Energy Technology Data Exchange (ETDEWEB)

    Skeen, Scott A.; Manin, Julien Luc; Pickett, Lyle M.

    2014-06-01

    The development of accurate predictive engine simulations requires experimental data to both inform and validate the models, but very limited information is presently available about the chemical structure of high pressure spray flames under engine- relevant conditions. Probing such flames for chemical information using non- intrusive optical methods or intrusive sampling techniques, however, is challenging because of the physical and optical harshness of the environment. This work details two new diagnostics that have been developed and deployed to obtain quantitative species concentrations and soot volume fractions from a high-pressure combusting spray. A high-speed, high-pressure sampling system was developed to extract gaseous species (including soot precursor species) from within the flame for offline analysis by time-of-flight mass spectrometry. A high-speed multi-wavelength optical extinction diagnostic was also developed to quantify transient and quasi-steady soot processes. High-pressure sampling and offline characterization of gas-phase species formed following the pre-burn event was accomplished as well as characterization of gas-phase species present in the lift-off region of a high-pressure n-dodecane spray flame. For the initial samples discussed in this work several species were identified, including polycyclic aromatic hydrocarbons (PAH); however, quantitative mole fractions were not determined. Nevertheless, the diagnostic developed here does have this capability. Quantitative, time-resolved measurements of soot extinction were also accomplished and the novel use of multiple incident wavelengths proved valuable toward characterizing changes in soot optical properties within different regions of the spray flame.

  7. Synchrotron radiation

    International Nuclear Information System (INIS)

    Pattison, P.; Quinn, P.

    1990-01-01

    This report details the activities in synchrotron radiation and related areas at Daresbury Laboratory during 1989/90. The number and scope of the scientific reports submitted by external users and in-house staff is a reflection of the large amount of scheduled beamtime and high operating efficiency achieved at the Synchrotron Radiation Source (SRS) during the past year. Over 4000 hours of user beam were available, equivalent to about 80% of the total scheduled time. Many of the reports collected here illustrate the increasing technical complexity of the experiments now being carried out at Daresbury. Provision of the appropriate technical and scientific infrastructure and support is a continuing challenge. The development of the Materials Science Laboratory together with the existing Biological Support Laboratory will extend the range of experiments which can be carried out on the SRS. This will particularly facilitate work in which the sample must be prepared or characterised immediately before or during an experiment. The year 1989/90 has also seen a substantial upgrade of several stations, especially in the area of x-ray optics. Many of the advantages of the High Brightness Lattice can only be exploited effectively with the use of focusing optics. As the performance of these stations improves, the range of experiments which are feasible on the SRS will be extended significantly. (author)

  8. High-pressure phase transitions of deep earth materials

    International Nuclear Information System (INIS)

    Hirose, Kei

    2009-01-01

    Recent developments in synchrotron XRD measurements combined with laser-heated diamond-anvil cell (LHDAC) techniques have enabled us to search for a novel phase transition at extremely high pressure and temperature. A phase transition from MgSiO 3 perovskite to post-perovskite was discovered through a drastic change in XRD patterns above 120 GPa and 2500 K, corresponding to the condition in the lowermost mantle (Murakami et al., 2004; Oganov and Ono, 2004). A pressure-induced phase transformation from ABO 3 -type perovskite to any denser structures was not known at that time. This new MgSiO 3 polymorph called post-perovskite has an orthorhombic symmetry (space group: Cmcm) with a sheet-stacking structure. The Mg site in post-perovskite is smaller than that in perovskite, which results in a volume reduction by 1.0-1.5% from perovskite structure. The electrical conductivity of post-perovskite is higher by three orders of magnitude than that of perovskite at similar pressure range (Ohta et al., 2008). This is likely due to a shorter Fe-Fe distance in post-perovskite structure, while conduction mechanism is yet to be further examined. Phase transition boundary between perovskite and post-perovskite has been determined in a wide temperature range up to 4400 K at 170 GPa (Tateno et al., 2008). Phase relations of Fe alloys have been also studied at core pressures (>135 GPa), although the generation of high temperature is more difficult at higher pressures. A new high-pressure B2 phase of B2 phase of FeS was recently discovered above 180 GPa (Sata et al., 2008). The Fe-Ni alloys have a wide pressure-temperature stability field of fcc phase at the core pressure range, depending on the Ni content (Kuwayama et al., 2008). (author)

  9. In-situ synchrotron X-Ray diffraction investigation of the fast recovery of microstructure during electropulse treatment of heavily cold drawn nanocrystalline Ni-Ti wires

    Czech Academy of Sciences Publication Activity Database

    Malard, B.; Pilch, Jan; Šittner, Petr; Delville, R.; Curfs, C.

    172-174, č. 6 (2011), s. 1243-1248 ISSN 1012-0394 R&D Projects: GA AV ČR(CZ) IAA200100627; GA MŠk(CZ) LA10010 Institutional research plan: CEZ:AV0Z10100520 Keywords : recovery process * electropulse treatment * in-situ analysis * superelasticity Subject RIV: BM - Solid Matter Physics ; Magnetism

  10. Magnetic and Superconducting Materials at High Pressures

    Energy Technology Data Exchange (ETDEWEB)

    Struzhkin, Viktor V. [Carnegie Inst. of Washington, Washington, DC (United States)

    2015-03-24

    The work concentrates on few important tasks in enabling techniques for search of superconducting compressed hydrogen compounds and pure hydrogen, investigation of mechanisms of high-Tc superconductivity, and exploring new superconducting materials. Along that route we performed several challenging tasks, including discovery of new forms of polyhydrides of alkali metal Na at very high pressures. These experiments help us to establish the experimental environment that will provide important information on the high-pressure properties of hydrogen-rich compounds. Our recent progress in RIXS measurements opens a whole field of strongly correlated 3d materials. We have developed a systematic approach to measure major electronic parameters, like Hubbard energy U, and charge transfer energy Δ, as function of pressure. This technique will enable also RIXS studies of magnetic excitations in iridates and other 5d materials at the L edge, which attract a lot of interest recently. We have developed new magnetic sensing technique based on optically detected magnetic resonance from NV centers in diamond. The technique can be applied to study superconductivity in high-TC materials, to search for magnetic transitions in strongly correlated and itinerant magnetic materials under pressure. Summary of Project Activities; development of high-pressure experimentation platform for exploration of new potential superconductors, metal polyhydrides (including newly discovered alkali metal polyhydrides), and already known superconductors at the limit of static high-pressure techniques; investigation of special classes of superconducting compounds (high-Tc superconductors, new superconducting materials), that may provide new fundamental knowledge and may prove important for application as high-temperature/high-critical parameter superconductors; investigation of the pressure dependence of superconductivity and magnetic/phase transformations in 3d transition metal compounds, including

  11. The increase in T sub c for MgB sub 2 superconductor under high pressure

    CERN Document Server

    Liu, Z X; You, J Y; Li, S C; Zhu, J L; Yu, R C; Li, F Y; Su, S K

    2002-01-01

    We report in situ high-pressure studies up to 1.0 GPa on MgB sub 2 superconductor which had been synthesized at high pressure. The as-prepared sample is of high quality as regards having a sharp superconducting transition (T sub c) at 39 K. The in situ high-pressure measurements were carried out using a Be-Cu piston-cylinder-type instrument with a mixed oil as the pressure-transmitting medium, which provides a quasi-hydrostatic pressure environment at low temperature. The superconducting transitions were measured using the electrical conductance method. It is found that T sub c increases with pressure in the initial pressure range, leading to a parabolic-like T sub c -P evolution.

  12. The increase in Tc for MgB2 superconductor under high pressure

    International Nuclear Information System (INIS)

    Liu, Z-X; Jin, C-Q; You, J-Y; Li, S-C; Zhu, J-L; Yu, R-C; Li, F-Y; Su, S-K

    2002-01-01

    We report in situ high-pressure studies up to 1.0 GPa on MgB 2 superconductor which had been synthesized at high pressure. The as-prepared sample is of high quality as regards having a sharp superconducting transition (T c ) at 39 K. The in situ high-pressure measurements were carried out using a Be-Cu piston-cylinder-type instrument with a mixed oil as the pressure-transmitting medium, which provides a quasi-hydrostatic pressure environment at low temperature. The superconducting transitions were measured using the electrical conductance method. It is found that T c increases with pressure in the initial pressure range, leading to a parabolic-like T c -P evolution

  13. Inspection technology for high pressure pipes

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jae H.; Lee, Jae C.; Eum, Heung S.; Choi, Yu R.; Moon, Soon S.; Jang, Jong H

    2000-02-01

    Various kinds of defects are likely to be occurred in the welds of high pressure pipes in nuclear power plants. Considering the recent accident of Zuruga nuclear power plant in Japan, reasonable policy is strongly requested for the high pressure pipe integrity. In this study, we developed the technologies to inspect pipe welds automatically. After development of scanning robot prototype in the first research year, we developed and implemented the algorithm of automatic tracking of the scanning robot along the weld line of the pipes. We use laser slit beam on weld area and capture the image using digital camera. Through processing of the captures image, we finally determine the weld line automatically. In addition, we investigated a new technology on micro systems for developing micro scanning robotic inspection of the pipe welds. The technology developed in this study is being transferred to the industry. (author)

  14. Radioresistance increase in polymers at high pressures

    International Nuclear Information System (INIS)

    Milinchuk, V.; Kirjukhin, V.; Klinshpont, E.

    1977-01-01

    The effect was studied of very high pressures ranging within 100 and 2,700 MPa on the radioresistance of polytetrafluoroethylene, polypropylene and polyethylene in gamma irradiation. For experiments industrial polymers in the shape of blocks, films and fibres were used. It is shown that in easily breakable polymers, such as polytetrafluoroethylene and polypropylene 1.3 to 2 times less free radicals are formed as a result of gamma irradiation and a pressure of 150 MPa than at normal pressure. The considerably reduced radiation-chemical formation of radicals and the destruction suppression by cross-linking in polymers is the evidence of the polymer radioresistance in irradiation at high pressures. (J.B.)

  15. High-pressure oxidation of methane

    DEFF Research Database (Denmark)

    Hashemi, Hamid; Christensen, Jakob Munkholt; Gersen, Sander

    2016-01-01

    Methane oxidation at high pressures and intermediate temperatures was investigated in a laminar flow reactor and in a rapid compression machine (RCM). The flow-reactor experiments were conducted at 700–900 K and 100 bar for fuel-air equivalence ratios (Φ) ranging from 0.06 to 19.7, all highly...... diluted in nitrogen. It was found that under the investigated conditions, the onset temperature for methane oxidation ranged from 723 K under reducing conditions to 750 K under stoichiometric and oxidizing conditions. The RCM experiments were carried out at pressures of 15–80 bar and temperatures of 800......–1250 K under stoichiometric and fuel-lean (Φ=0.5) conditions. Ignition delays, in the range of 1–100 ms, decreased monotonically with increasing pressure and temperature. A chemical kinetic model for high-pressure methane oxidation was established, with particular emphasis on the peroxide chemistry...

  16. High pressure photoinduced ring opening of benzene

    International Nuclear Information System (INIS)

    Ciabini, Lucia; Santoro, Mario; Bini, Roberto; Schettino, Vincenzo

    2002-01-01

    The chemical transformation of crystalline benzene into an amorphous solid (a-C:H) was induced at high pressure by employing laser light of suitable wavelengths. The reaction was forced to occur at 16 GPa, well below the pressure value (23 GPa) where the reaction normally occurs. Different laser sources were used to tune the pumping wavelength into the red wing of the first excited singlet state S 1 ( 1 B 2u ) absorption edge. Here the benzene ring is distorted, presenting a greater flexibility which makes the molecule unstable at high pressure. The selective pumping of the S 1 level, in addition to structural considerations, was of paramount importance to clarify the mechanism of the reaction

  17. Foaming Glass Using High Pressure Sintering

    DEFF Research Database (Denmark)

    Østergaard, Martin Bonderup; Petersen, Rasmus Rosenlund; König, Jakob

    Foam glass is a high added value product which contributes to waste recycling and energy efficiency through heat insulation. The foaming can be initiated by a chemical or physical process. Chemical foaming with aid of a foaming agent is the dominant industrial process. Physical foaming has two...... to expand. After heat-treatment foam glass can be obtained with porosities of 80–90 %. In this study we conduct physical foaming of cathode ray tube (CRT) panel glass by sintering under high pressure (5-25 MPa) using helium, nitrogen, or argon at 640 °C (~108 Pa s). Reheating a sample in a heating...... variations. One way is by saturation of glass melts with gas. The other involves sintering of powdered glass under a high gas pressure resulting in glass pellets with high pressure bubbles entrapped. Reheating the glass pellets above the glass transition temperature under ambient pressure allows the bubbles...

  18. High pressure injection injuries: an overview.

    Science.gov (United States)

    Fialkov, J A; Freiberg, A

    1991-01-01

    Injuries resulting from the use of high pressure injectors and spray guns are relatively rare; however, the potential tissue damage caused by the injury as well as the extent of the injury itself may go unrecognized by the primary physician. The purpose of this paper is to inform the emergency physician of the nature and standard management of this type of injury. A basic understanding of the pathophysiology of the high pressure injection injury (HPII) is essential in avoiding the mistakes in management that have been reported in the literature. The emergency management of the HPII includes: evaluation and immobilization, tetanus and antimicrobial prophylaxis, supportive and resuscitative measures, analgesia, and minimizing the time to definitive surgical treatment.

  19. Stress concentration effects in high pressure components

    International Nuclear Information System (INIS)

    Aller, J.E.

    1990-01-01

    This paper examines the stress concentration effects of sideholes in thick walled, high pressure cylinders. It has been shown that the theoretical stress concentration factor at the intersection of a small crossbore in a closed end, thick walled cylinder varies between 3.0 and 4.0. Tests have shown that this effect can be greatly reduced in practice by carefully radiusing the bore intersection and autofrettaging the cylinder. It has also been shown that the minimum stress concentration factor occurs when the main bore and sidehole or crossbore have the same diameter, and the radius of the intersection is approximately equal to the sidehole radius. When the bore and sidehole intersection angle decreases from 90 degrees, the stress concentration factor increases significantly. Knowledge of these fundamental relationships can be used in maintaining, as well ad designing, high pressure equipment

  20. High-pressure torsion of hafnium

    International Nuclear Information System (INIS)

    Edalati, Kaveh; Horita, Zenji; Mine, Yoji

    2010-01-01

    Pure Hf (99.99%) is processed by high-pressure torsion (HPT) under pressures of 4 and 30 GPa to form an ultrafine-grained structure with a gain size of ∼180 nm. X-ray diffraction analysis shows that, unlike Ti and Zr, no ω phase formation is detected after HPT processing even under a pressure of 30 GPa. A hydride formation is detected after straining at the pressure of 4 GPa. The hydride phase decomposes either by application of a higher pressure as 30 GPa or by unloading for prolong time after HPT processing. Microhardness, tensile and bending tests show that a high hardness (360 Hv) and an appreciable ductility (8%) as well as high tensile and bending strength (1.15 and 2.75 GPa, respectively) are achieved following the high-pressure torsion.

  1. Hydrogen - High pressure production and storage

    International Nuclear Information System (INIS)

    Lauretta, J.R

    2005-01-01

    The development of simple, safe and more and more efficient technologies for the production and the storage of hydrogen is necessary condition for the transition towards the economy of hydrogen.In this work the hydrogen production studies experimentally to high pressure by electrolysis of alkaline solutions without the intervention of compressing systems and its direct storage in safe containers.The made tests show that the process of electrolysis to high pressure is feasible and has better yield than to low pressure, and that is possible to solve the operation problems, with relatively simple technology.The preliminary studies and tests indicate that the system container that studied is immune to the outbreak and can have forms and very different sizes, nevertheless, to reach or to surpass the efficiency of storage of the conventional systems the investments necessary will be due to make to be able to produce aluminum alloy tubes of high resistance

  2. New Developments in Deformation Experiments at High Pressure

    International Nuclear Information System (INIS)

    Durham, W B; Weidner, D J; Karato, S; Wang, Y

    2004-01-01

    Although the importance of rheological properties in controlling the dynamics and evolution of the whole mantle of Earth is well-recognized, experimental studies of rheological properties and deformation-induced microstructures have mostly been limited to low-pressure conditions. This is mainly a result of technical limitations in conducting quantitative rheological experiments under high-pressure conditions. A combination of factors is changing this situation. Increased resolution of composition and configuration of Earth's interior has created a greater demand for well-resolved laboratory measurement of the effects of pressure on the behavior of materials. Higher-strength materials have become readily available for containing high-pressure research devices, and new analytical capabilities--in particular very bright synchrotron X-ray sources--are now readily available to high-pressure researchers. One of the biggest issues in global geodynamics is the style of mantle convection and the nature of chemical differentiation associated with convectional mass transport. Although evidence for deep mantle circulation has recently been found through seismic tomography (e.g., van der Hilst et al. (1997)), complications in convection style have also been noted. They include (1) significant modifications of flow geometry across the mantle transition zone as seen from high resolution tomographic studies (Fukao et al. 1992; Masters et al. 2000; van der Hilst et al. 1991) and (2) complicated patterns of flow in the deep lower mantle (∼1500-2500 km), perhaps caused by chemical heterogeneity (Kellogg et al. 1999; van der Hilst and Karason 1999). These studies indicate that while large-scale circulation involving the whole mantle no doubt occurs, significant deviations from simple flow geometry are also present. Two mineral properties have strong influence on convection: (1) density and (2) viscosity (rheology) contrasts. In the past, the effects of density contrast have been

  3. Raman spectroscopy of triolein under high pressures

    Science.gov (United States)

    Tefelski, D. B.; Jastrzębski, C.; Wierzbicki, M.; Siegoczyński, R. M.; Rostocki, A. J.; Wieja, K.; Kościesza, R.

    2010-03-01

    This article presents results of the high pressure Raman spectroscopy of triolein. Triolein, a triacylglyceride (TAG) of oleic acid, is an unsaturated fat, present in natural oils such as olive oil. As a basic food component and an energy storage molecule, it has considerable importance for food and fuel industries. To generate pressure in the experiment, we used a high-pressure cylindrical chamber with sapphire windows, presented in (R.M. Siegoczyński, R. Kościesza, D.B. Tefelski, and A. Kos, Molecular collapse - modification of the liquid structure induced by pressure in oleic acid, High Press. Res. 29 (2009), pp. 61-66). Pressure up to 750 MPa was applied. A Raman spectrometer in "macro"-configuration was employed. Raman spectroscopy provides information on changes of vibrational modes related to structural changes of triolein under pressure. Interesting changes in the triglyceride C‒H stretching region at 2650-3100 cm-1 were observed under high-pressures. Changes were also observed in the ester carbonyl (C˭ O) stretching region 1700-1780 cm-1 and the C‒C stretching region at 1050-1150 cm-1. The overall luminescence of the sample decreased under pressure, making it possible to set longer spectrum acquisition time and obtain more details of the spectrum. The registered changes suggest that the high-pressure solid phase of triolein is organized as β-polymorphic, as was reported in (C. Akita, T. Kawaguchi, and F. Kaneko, Structural study on polymorphism of cis-unsaturated triacylglycerol: Triolein, J. Phys. Chem. B 110 (2006), pp. 4346-4353; E. Da Silva and D. Rousseau, Molecular order and thermodynamics of the solid-liquid transition in triglycerides via Raman spectroscopy, Phys. Chem. Chem. Phys. 10 (2008), pp. 4606-4613) (with temperature-induced phase transitions). The research has shown that Raman spectroscopy in TAGs under pressure reveals useful information about its structural changes.

  4. High Pressure Multicomponent Adsorption in Porous Media

    DEFF Research Database (Denmark)

    Shapiro, Alexander; Stenby, Erling Halfdan

    1999-01-01

    We analyse adsorption of a multicomponent mixture at high pressure on the basis of the potential theory of adsorption. The adsorbate is considered as a segregated mixture in the external field produced by a solid adsorbent. we derive an analytical equation for the thickness of a multicomponent fi...... close to a dew point. This equation (asymptotic adsorption equation, AAE) is a first order approximation with regard to the distance from a phase envelope....

  5. 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

  6. High-pressure mechanical instability in rocks.

    Science.gov (United States)

    Byerlee, J D; Brace, W F

    1969-05-09

    At a confining pressure of a few kilobars, deformation of many sedimentary rocks, altered mafic rocks, porous volcanic rocks, and sand is ductile, in that instabilities leading to audible elastic shocks are absent. At pressures of 7 to 10 kilobars, however, unstable faulting and stick-slip in certain of these rocks was observed. This high pressure-low temperature instability might be responsible for earthquakes in deeply buried sedimentary or volcanic sequences.

  7. observed by high pressure NMR and NQR

    Indian Academy of Sciences (India)

    Akogun, Hyogo 678-1297, Japan. ∗. Email: kohara@sci.himeji tech.ac.jp. Abstract. NMR and NQR studies on two interesting systems (URu2Si2, CeTIn5) were performed under high pressure. (1) URu2Si2: In the pressure range 3.0 to 8.3 kbar, we have observed new 29Si. NMR signals arising from the antiferromagnetic ...

  8. High-Pressure Polymorphism in Orthoamphiboles

    Science.gov (United States)

    Finkelstein, G. J.; Zhang, D.; Shelton, H.; Dera, P.

    2017-12-01

    Amphiboles are double-chain silicate minerals that are the structurally hydrated counterpart to single-chain, anhydrous pyroxenes. They may play an important role in the earth as a carrier for volatiles in subduction zones, as well as a generator for seismic anisotropy in the upper mantle. Recent work has described previously unrecognized high-pressure polymorphism at low temperatures in a variety of pyroxene minerals, which may be relevant for the structure and dynamics of thick, cold, subducted slabs. However, high-pressure polymorphism in amphiboles above a few GPa in pressure has not been well explored, and if similar polymorphism to pyroxenes exists in this mineral family, it may affect the extent and depth of volatile transport in amphiboles, as well as their rheological properties. At low temperatures and high pressures, orthopyroxenes undergo crystal structure transitions at lower pressures than clinopyroxenes (10-30 GPa vs. > 50 GPa), so for this study we have investigated polymorphism in the anthophyllite-gedrite (Al-free and Al rich) orthoamphibole solid solution series. Using neon gas-loaded diamond anvil cells, we compressed both phases to a maximum pressure of 31 GPa, and observed transitions to new monoclinic structures in both endmembers. In this presentation, we will discuss the details of these transitions and implications for the earth's interior.

  9. Raman study of opal at high pressure

    Science.gov (United States)

    Farfan, G.; Wang, S.; Mao, W. L.

    2011-12-01

    More commonly known for their beauty and lore as gemstones, opals are also intriguing geological materials which may have potential for materials science applications. Opal lacks a definite crystalline structure, and is composed of an amorphous packing of hydrated silica (SiO2) spheroids, which provides us with a unique nano-scaled mineraloid with properties unlike those of other amorphous materials like glass. Opals from different localities were studied at high pressure using a diamond anvil cell to apply pressure and Raman spectroscopy to look at changes in bonding as pressure was increased. We first tested different samples from Virgin Valley, NV, Spencer, ID, Juniper Ridge, OR, and Australia, which contain varying amounts of water at ambient conditions, using Raman spectroscopy to determine if they were opal-CT (semicrystalline cristobalite-trydimite volcanic origin) or opal-A (amorphous sedimentary origin). We then used x-ray diffraction and Raman spectroscopy in a diamond anvil cell to see how their bonding and structure changed under compression and to determine what effect water content had on their high pressure behavior. Comparison of our results on opal to other high pressure studies of amorphous materials like glass has implications from a geological and materials science standpoint.

  10. Rare-earth-metal nitridophosphates through high-pressure metathesis

    International Nuclear Information System (INIS)

    Kloss, Simon David; Schnick, Wolfgang

    2015-01-01

    Developing a synthetic method to target an broad spectrum of unknown phases can lead to fascinating discoveries. The preparation of the first rare-earth-metal nitridophosphate LiNdP_4N_8 is reported. High-pressure solid-state metathesis between LiPN_2 and NdF_3 was employed to yield a highly crystalline product. The in situ formed LiF is believed to act both as the thermodynamic driving force and as a flux to aiding single-crystal formation in dimensions suitable for crystal structure analysis. Magnetic properties stemming from Nd"3"+ ions were measured by SQUID magnetometry. LiNdP_4N_8 serves as a model system for the exploration of rare-earth-metal nitridophosphates that may even be expanded to transition metals. High-pressure metathesis enables the systematic study of these uncharted regions of nitride-based materials with unprecedented properties. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  11. High pressure structural studies on nanophase praseodymium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Saranya, L. [Jamal Mohamed College, Tiruchirapalli 620020, Tamil Nadu (India); Chandra Shekar, N.V., E-mail: chandru@igcar.gov.in [Condensed Matter Physics Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamil Nadu (India); Amirthapandian, S. [Materials Physics Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamil Nadu (India); Hussain, Shamima [UGC-DAE-CSR node, Kokilamedu 603103, Tamil Nadu (India); Arulraj, A.; Sahu, P. Ch. [Condensed Matter Physics Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamil Nadu (India)

    2014-09-15

    The phase stability of nanocrystalline Pr{sub 2}O{sub 3} has been investigated under pressure by in-situ high pressure X-ray diffraction using Mao-Bell type diamond anvil cell. The ambient structure and phase of the praseodymium oxide have been resolved unambiguously using x-ray diffraction, SEM and TEM techniques. Under the action of pressure the cubic phase of the system is retained up to 15 GPa. This is unusual as other isostructural rare earth oxides show structural transformations even at lower pressures. From the best fit to the P–V data with the Murnaghan equation of state yields a bulk modulus of 171 GPa.

  12. Structural analysis with high brilliance synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ohno, Hideo [Japan Atomic Energy Research Inst., Kamigori, Hyogo (Japan). Kansai Research Establishment

    1997-11-01

    The research subjects in diffraction and scattering of materials with high brilliance synchrotron radiation such as SPring-8 (Super Photon ring 8 GeV) are summarized. The SPring-8 project is going well and 10 public beamlines will be opened for all users in October, 1997. Three JAERI beamlines are also under construction for researches of heavy element science, physical and structural properties under extreme conditions such as high temperature and high pressure. (author)

  13. In situ study the effect of refiner on the microstructure evolution of variable cross-section structure by synchrotron X-ray radiography

    Science.gov (United States)

    Li, Faguo; Zhang, Jiao; Dai, Yongbing; Bian, Fenggang; Fu, Yanan; Yin, Fucheng; Sun, Baode

    2015-10-01

    The formation of microstructures during solidification is strongly affected by the interaction that occurs between factors, such as heat field, melt flow, solute distribution, and number of effective nucleation cores. In this study, the microstructure evolution of a high-purity hypoeutectic Al-Cu alloy at its region of variable cross-section was studied using synchrotron radiation imaging. The characteristics of the thermal field, solute field, and flow field were analyzed according to these radiographs. The results showed that the region of variable cross-section is the site that is more prone to dendrite arms fracture. These dendrites spread radially from the center of the thin wall and the isotherms distribute as an arc-shape. These are the main reasons for the uneven distribution of the microstructure, which lead to undesirable phase formation and aggregation at the region of variable cross-section. The microstructure can be significantly refined and solute enrichment can be eliminated by adding refiners to alloys. Comparing these two conditions, it can be concluded that the solute and flow field distribution at the variable cross-section region is significantly affected, uniformity of the solidification microstructure is improved, and undesirable phases are eliminated by increase in effective heterogeneous nucleation cores.

  14. Solid-state reactivity explored in situ by synchrotron radiation on single crystals: from SrFeO2.5 to SrFeO3 via electrochemical oxygen intercalation

    International Nuclear Information System (INIS)

    Maity, A; Dutta, R; Penkala, B; Ceretti, M; Letrouit-Lebranchu, A; Perichon, A; Paulus, W; Chernyshov, D; Piovano, A; Bossak, A; Meven, M

    2015-01-01

    In this study we demonstrate the feasibility of following up a chemical reaction by single crystal x-ray (synchrotron) diffraction under operando conditions, carried out in a specially designed electrochemical cell mounted on the BM01A at the European Synchrotron Radiation Facility (ESRF). We investigated in detail the electrochemical oxidation of SrFeO 2.5 to SrFeO 3 on a spherical single crystal of 70 µm diameter by in situ diffraction at an ambient temperature. Complete data sets were obtained by scanning the whole reciprocal space using a 2M Pilatus detector, resulting in 3600 frames with a resolution of 0.1° per data set, each obtained in 18 min. The crystal was mounted in a specially designed electrochemical cell with 1N KOH used as the electrolyte. During the electrochemical oxidation, the reaction proceeds following the phase sequence SrFeO 2.5 /SrFeO 2.75 /SrFeO 2.875 /SrFeO 3 , structurally accompanied by establishing a complex series of long-range oxygen vacancy ordering, which gets instantly organized at ambient temperature. The topotactic reaction pathway is discussed in terms of the evolution of the twin domain structure. The formation of SrFeO 2.875 is accompanied by the formation of diffuse streaks along the [1 0 0]-direction of the perovskite cell, reaching high d-spacings. The diffuse streaks are discussed and are thought to originate from a modified twin structure induced by the SrFeO 2.75 to SrFeO 2.875 transition, and the associated changes in the domain structure, developed during the oxygen intercalation. We equally analysed and discussed in detail the twin structure of all the title compounds. We confirm the ground state of SrFeO 2.5 is able to adopt the Imma space group symmetry, showing stacking faults of the tetrahedral layers along the stacking axis of the brownmillerite unit cell, indicated by the 1D diffuse rods. We showed that in situ single crystal diffraction has huge potential in the study of non-stoichiometric compounds

  15. Solid-state reactivity explored in situ by synchrotron radiation on single crystals: from SrFeO2.5 to SrFeO3 via electrochemical oxygen intercalation

    Science.gov (United States)

    Maity, A.; Dutta, R.; Penkala, B.; Ceretti, M.; Letrouit-Lebranchu, A.; Chernyshov, D.; Perichon, A.; Piovano, A.; Bossak, A.; Meven, M.; Paulus, W.

    2015-12-01

    In this study we demonstrate the feasibility of following up a chemical reaction by single crystal x-ray (synchrotron) diffraction under operando conditions, carried out in a specially designed electrochemical cell mounted on the BM01A at the European Synchrotron Radiation Facility (ESRF). We investigated in detail the electrochemical oxidation of SrFeO2.5 to SrFeO3 on a spherical single crystal of 70 µm diameter by in situ diffraction at an ambient temperature. Complete data sets were obtained by scanning the whole reciprocal space using a 2M Pilatus detector, resulting in 3600 frames with a resolution of 0.1° per data set, each obtained in 18 min. The crystal was mounted in a specially designed electrochemical cell with 1N KOH used as the electrolyte. During the electrochemical oxidation, the reaction proceeds following the phase sequence SrFeO2.5/SrFeO2.75/SrFeO2.875/SrFeO3, structurally accompanied by establishing a complex series of long-range oxygen vacancy ordering, which gets instantly organized at ambient temperature. The topotactic reaction pathway is discussed in terms of the evolution of the twin domain structure. The formation of SrFeO2.875 is accompanied by the formation of diffuse streaks along the [1 0 0]-direction of the perovskite cell, reaching high d-spacings. The diffuse streaks are discussed and are thought to originate from a modified twin structure induced by the SrFeO2.75 to SrFeO2.875 transition, and the associated changes in the domain structure, developed during the oxygen intercalation. We equally analysed and discussed in detail the twin structure of all the title compounds. We confirm the ground state of SrFeO2.5 is able to adopt the Imma space group symmetry, showing stacking faults of the tetrahedral layers along the stacking axis of the brownmillerite unit cell, indicated by the 1D diffuse rods. We showed that in situ single crystal diffraction has huge potential in the study of non-stoichiometric compounds under operando

  16. Energy Systems High-Pressure Test Laboratory | Energy Systems Integration

    Science.gov (United States)

    Facility | NREL Energy Systems High-Pressure Test Laboratory Energy Systems High-Pressure Test Laboratory In the Energy Systems Integration Facility's High-Pressure Test Laboratory, researchers can safely test high-pressure hydrogen components. Photo of researchers running an experiment with a hydrogen fuel

  17. 7 CFR 58.219 - High pressure pumps and lines.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false High pressure pumps and lines. 58.219 Section 58.219....219 High pressure pumps and lines. High pressure lines may be cleaned-in-place and shall be of such construction that dead ends, valves and the high pressure pumps can be disassembled for hand cleaning. The high...

  18. Structural phase transitions in Iron - based superconductors BaFe2-xCrxAs2 under high pressure

    International Nuclear Information System (INIS)

    Uhoya, W.O.; Montgomery, J.M.; Samudrala, G.K.; Tsoi, G.M.; Vohra, Y.K.; Sefar, A.S.

    2011-01-01

    Pure BaFe 2 As 2 with the ThCr 2 Si 2 -type crystal structure under ambient conditions is known to superconduct under high pressure and undergo an isostructural phase transition from tetragonal to collapsed tetragonal phase which is accompanied by anomalous compressibility effects. Presently, there is no reported work on the crystal structure on any of the chemically doped 122- iron based superconductors under high pressure. We have carried out the electrical resistance measurements and high pressure X-ray diffraction studies on Chromium doped samples of BaFe 2-x Cr x As 2 (x = 0, 0.05, 0.15, 0.4, 0.61) to a pressure of 75 GPa and a temperature of 10K using a synchrotron source and designer diamond anvils, so as to investigate the influence of chemical doping and high pressure on crystal structure and superconductivity

  19. Synchrotron-radiation research

    International Nuclear Information System (INIS)

    Cunningham, J.E.

    1982-01-01

    The use of radiation from synchrotron sources has started a renaissance in materials, physics, chemistry, and biology. Synchrotron radiation has advantages over conventional x rays in that its source brightness is a thousand times greater throughout a continuous energy spectrum, and resonances are produced with specific electron energy levels. Two major synchrotron radiation sources are operated by DOE: the Stanford Synchrotron Radiation Laboratory at SLAC, and the National Synchrotron Light Source at Brookhaven

  20. In Situ Characterization Techniques Based on Synchrotron Radiation and Neutrons Applied for the Development of an Engineering Intermetallic Titanium Aluminide Alloy

    Directory of Open Access Journals (Sweden)

    Petra Erdely

    2016-01-01

    Full Text Available Challenging issues concerning energy efficiency and environmental politics require novel approaches to materials design. A recent example with regard to structural materials is the emergence of lightweight intermetallic TiAl alloys. Their excellent high-temperature mechanical properties, low density and high stiffness constitute a profile perfectly suitable for their application as advanced aero-engine turbine blades or as turbocharger turbine wheels in next-generation automotive engines. As the properties of TiAl alloys during processing as well as during service are dependent on the phases occurring, detailed knowledge of their volume fractions and distribution within the microstructure is of paramount importance. Furthermore, the behavior of the individual phases during hot deformation and subsequent heat treatments is of interest to define reliable and cost-effective industrial production processes. In situ high-energy X-ray diffraction methods allow tracing the evolution of phase fractions over a large temperature range. Neutron diffraction unveils information on order-disorder transformations in TiAl alloys. Small-angle scattering experiments offer insights into the materials’ precipitation behavior. This review attempts to shine a light on selected in situ diffraction and scattering techniques and the ways in which they promoted the development of an advanced engineering TiAl alloy.

  1. Synchrotron radiation

    International Nuclear Information System (INIS)

    Seddon, E.A.; Reid, R.J.

    1992-01-01

    Work at the Daresbury SRS has of necessity been interrupted this year (1991/92) due to the incorporation of Wiggler II. However, considerable beamtime was awarded before the shutdown and the major part of this appendix is concerned with the progress reports of the research undertaken then. The reports have been organised under the following broad headings: Molecular Science (19 papers), Surface and Materials Science (169 papers), Biological Science (85 papers), Instrumental and Technique Developments (13 papers) and Accelerator Physics (3 papers). It is hoped that in time the number of contributions on accelerator physics will grow to reflect the in-house activity on, for example, accelerator improvement and design. The research reports are preceded by the Annual Report of the Synchrotron Radiation Facilities Committee, which outlines the research highlights identified by that Committee (also included are details of the current membership of the SRFC and the chairmen of the Beamtime Allocation Panels). Following the reports are the specifications for the beamlines and stations. This year Section 3 contains 289 reports (nearly 100 more than last year) and the number of publications, generated by scientists and engineers who have used or are associated with Daresbury Laboratory facilities, has topped 500 for the first time. (author)

  2. HIGH PRESSURE COAL COMBUSTON KINETICS PROJECT

    Energy Technology Data Exchange (ETDEWEB)

    Stefano Orsino

    2005-03-30

    As part of the U.S. Department of Energy (DoE) initiative to improve the efficiency of coal-fired power plants and reduce the pollution generated by these facilities, DOE has funded the High-Pressure Coal Combustion Kinetics (HPCCK) Projects. A series of laboratory experiments were conducted on selected pulverized coals at elevated pressures with the specific goals to provide new data for pressurized coal combustion that will help extend to high pressure and validate models for burnout, pollutant formation, and generate samples of solid combustion products for analyses to fill crucial gaps in knowledge of char morphology and fly ash formation. Two series of high-pressure coal combustion experiments were performed using SRI's pressurized radiant coal flow reactor. The first series of tests characterized the near burner flame zone (NBFZ). Three coals were tested, two high volatile bituminous (Pittsburgh No.8 and Illinois No.6), and one sub-bituminous (Powder River Basin), at pressures of 1, 2, and 3 MPa (10, 20, and 30 atm). The second series of experiments, which covered high-pressure burnout (HPBO) conditions, utilized a range of substantially longer combustion residence times to produce char burnout levels from 50% to 100%. The same three coals were tested at 1, 2, and 3 MPa, as well as at 0.2 MPa. Tests were also conducted on Pittsburgh No.8 coal in CO2 entrainment gas at 0.2, 1, and 2 MPa to begin establishing a database of experiments relevant to carbon sequestration techniques. The HPBO test series included use of an impactor-type particle sampler to measure the particle size distribution of fly ash produced under complete burnout conditions. The collected data have been interpreted with the help of CFD and detailed kinetics simulation to extend and validate devolatilization, char combustion and pollutant model at elevated pressure. A global NOX production sub-model has been proposed. The submodel reproduces the performance of the detailed chemical

  3. High-pressure oxidation of ethane

    DEFF Research Database (Denmark)

    Hashemi, Hamid; G. Jacobsen, Jon; Rasmussen, Christian T.

    2017-01-01

    Ethane oxidation at intermediate temperatures and high pressures has been investigated in both a laminar flow reactor and a rapid compression machine (RCM). The flow-reactor measurements at 600–900 K and 20–100 bar showed an onset temperature for oxidation of ethane between 700 and 825 K, depending...... on pressure, stoichiometry, and residence time. Measured ignition delay times in the RCM at pressures of 10–80 bar and temperatures of 900–1025 K decreased with increasing pressure and/or temperature. A detailed chemical kinetic model was developed with particular attention to the peroxide chemistry. Rate...

  4. New insights into the toxicity of mineral fibres: A combined in situ synchrotron μ-XRD and HR-TEM study of chrysotile, crocidolite, and erionite fibres found in the tissues of Sprague-Dawley rats.

    Science.gov (United States)

    Gualtieri, Alessandro F; Bursi Gandolfi, Nicola; Pollastri, Simone; Burghammer, Manfred; Tibaldi, Eva; Belpoggi, Fiorella; Pollok, Kilian; Langenhorst, Falko; Vigliaturo, Ruggero; Dražić, Goran

    2017-05-15

    Along the line of the recent research topic aimed at understanding the in vivo activity of mineral fibres and their mechanisms of toxicity, this work describes the morpho-chemical characteristics of the mineral fibres found in the tissues of Sprague-Dawley rats subjected to intraperitoneal/intrapleural injection of UICC chrysotile, UICC crocidolite and erionite-Na from Nevada (USA). The fibres are studied with in situ synchrotron powder diffraction and high resolution transmission electron microscopy to improve our understanding of the mechanisms of toxicity of these mineral fibres. In contact with the tissues of the rats, chrysotile fibres are prone to dissolve, with leaching of Mg and production of a silica rich relict. On the other hand, crocidolite and erionite-Na fibres are stable even for very long contact times within the tissues of the rats, showing just a thin dissolution amorphous halo. These findings support the model of a lower biopersistence of chrysotile with respect to crocidolite and erionite-Na but the formation of a silica-rich fibrous residue after the pseudo-amorphization of chrysotile may justify a higher cytotoxic potential and intense inflammatory activity of chrysotile in the short term in contact with the lung tissues. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. In situ synchrotron X-ray diffraction studies of the effect of microstructure on tensile behavior and retained austenite stability of thermo-mechanically processed transformation induced plasticity steel

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Kun [School of Mechanical, Materials and Mechatronic Engineering, University of Wollongong, NSW 2522 (Australia); Liss, Klaus-Dieter [School of Mechanical, Materials and Mechatronic Engineering, University of Wollongong, NSW 2522 (Australia); Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW 2234 (Australia); Timokhina, Ilana B. [Institute for Frontier Materials, Deakin University, Geelong, VIC 3217 (Australia); Pereloma, Elena V., E-mail: elenap@uow.edu.au [School of Mechanical, Materials and Mechatronic Engineering, University of Wollongong, NSW 2522 (Australia)

    2016-04-26

    Transmission electron microscopy and in situ synchrotron high-energy X-ray diffraction were used to investigate the martensitic transformation and lattice strains under uniaxial tensile loading of Fe-Mn-Si-C-Nb-Mo-Al Transformation Induced Plasticity (TRIP) steel subjected to different thermo-mechanical processing schedules. In contrast with most of the diffraction analysis of TRIP steels reported previously, the diffraction peaks from the martensite phase were separated from the peaks of the ferrite-bainite α-matrix. The volume fraction of retained γ-austenite, as well as the lattice strain, were determined from the diffraction patterns recorded during tensile deformation. Although significant austenite to martensite transformation starts around the macroscopic yield stress, some austenite grains had already experienced martensitic transformation. Hooke’s Law was used to calculate the phase stress of each phase from their lattice strain. The ferrite-bainite α-matrix was observed to yield earlier than austenite and martensite. The discrepancy between integrated phase stresses and experimental macroscopic stress is about 300 MPa. A small increase in carbon concentration in retained austenite at the early stage of deformation was detected, but with further straining a continuous slight decrease in carbon content occurred, indicating that mechanical stability factors, such as grain size, morphology and orientation of the retained austenite, played an important role during the retained austenite to martensite transformation.

  6. Sounding experiments of high pressure gas discharge

    International Nuclear Information System (INIS)

    Biele, Joachim K.

    1998-01-01

    A high pressure discharge experiment (200 MPa, 5·10 21 molecules/cm 3 , 3000 K) has been set up to study electrically induced shock waves. The apparatus consists of the combustion chamber (4.2 cm 3 ) to produce high pressure gas by burning solid propellant grains to fill the electrical pump chamber (2.5 cm 3 ) containing an insulated coaxial electrode. Electrical pump energy up to 7.8 kJ at 10 kV, which is roughly three times of the gas energy in the pump chamber, was delivered by a capacitor bank. From the current-voltage relationship the discharge develops at rapidly decreasing voltage. Pressure at the combustion chamber indicating significant underpressure as well as overpressure peaks is followed by an increase of static pressure level. These data are not yet completely understood. However, Lorentz forces are believed to generate pinching with subsequent pinch heating, resulting in fast pressure variations to be propagated as rarefaction and shock waves, respectively. Utilizing pure axisymmetric electrode initiation rather than often used exploding wire technology in the pump chamber, repeatable experiments were achieved

  7. High Pressure and Temperature Effects in Polymers

    Science.gov (United States)

    Bucknall, David; Arrighi, Valeria; Johnston, Kim; Condie, Iain

    Elastomers are widely exploited as the basis for seals in gas and fluid pipelines. The underlying behaviour of these elastomer at the high pressure, elevated temperatures they experience in operation is poorly understood. Consequently, the duty cycle of these materials is often deliberately limited to a few hours, and in order to prevent failure, production is stopped in order to change the seals in critical joints. The result is significant time lost due to bringing down production to change the seals as well as knock on financial costs. In order to address the fundamental nature of the elastomers at their intended operating conditions, we are studying the gas permeation behaviour of hydrogenated natural butyl rubber (HNBR) and fluorinated elastomers (FKM) at a high pressure and elevated temperature. We have developed a pressure system that permits gas permeation studies at gas pressures of up to 5000 psi and operating temperatures up to 150° C. In this paper, we will discuss the nature of the permeation behaviour at these extreme operating conditions, and how this relates to the changes in the polymer structure. We will also discuss the use of graphene-polymer thin layer coatings to modify the gas permeation behaviour of the elastomers.

  8. Dynamics of mineral crystallization at inclusion-garnet interface from precipitated slab-derived fluid phase: first in-situ synchrotron x-ray measurements

    Science.gov (United States)

    Malaspina, Nadia; Alvaro, Matteo; Campione, Marcello; Nestola, Fabrizio

    2015-04-01

    Remnants of the fluid phase at ultrahigh pressure (UHP) in subduction environments may be preserved as primary multiphase inclusions in UHP minerals. These inclusions are frequently hosted by minerals stable at mantle depths, such as garnet, and show the same textural features as fluid inclusions. The mineral infillings of the solid multiphase inclusions are generally assumed to have crystallized by precipitation from the solute load of dense supercritical fluids equilibrating with the host rock. Notwithstanding the validity of this assumption, the mode of crystallization of daughter minerals during precipitation within the inclusion and/or the mechanism of interaction between the fluid at supercritical conditions and the host mineral are still poorly understood from a crystallographic point of view. A case study is represented by garnet orthopyroxenites from the Maowu Ultramafic Complex (China) deriving from harzburgite precursors metasomatised at ~ 4 GPa, 750 °C by a silica- and incompatible trace element-rich fluid phase. This metasomatism produced poikilitic orthopyroxene and inclusion-rich garnet porphyroblasts. Solid multiphase primary inclusions in garnet display a size within a few tens of micrometers and negative crystal shapes. Infilling minerals (spinel: 10-20 vol.%; amphibole, chlorite, talc, mica: 80- 90 vol.%) occur with constant volume ratios and derive from trapped solute-rich aqueous fluids. To constrain the possible mode of precipitation of daughter minerals, we performed for the first time a single-crystal X-ray diffraction experiment by means of Synchrotron Radiation at DLS-Diamond Light Source. In combination with electron probe microanalyses, this measurement allowed the unique identification of each mineral phase and their reciprocal orientations. We demonstrated the epitaxial relationship between spinel and garnet and between some hydrous minerals. Epitaxy drives a first-stage nucleation of spinel under near-to-equilibrium conditions

  9. High-pressure U3O8 with the fluorite-type structure

    International Nuclear Information System (INIS)

    Zhang, F.X.; Lang, M.; Wang, J.W.; Li, W.X.; Sun, K.; Prakapenka, V.; Ewing, R.C.

    2014-01-01

    A new high-pressure phase of U 3 O 8 , which has a fluorite-type structure, forms at pressures greater than ∼8.1 GPa that was confirmed by in situ x-ray diffraction (XRD) measurements. The fluorite-type U 3 O 8 is stable at pressures at least up to ∼40 GPa and temperatures to 1700 K, and quenchable to ambient conditions. Based on the XRD analysis, there is a huge volume collapse (>20%) for U 3 O 8 during the phase transition and the quenched high-pressure phase is 28% denser than the initial orthorhombic phase at ambient conditions. The high-pressure phase has a very low compressibility comparing with the starting orthorhombic phase. - Graphical abstract: α-U 3 O 8 is in a layered structure with orthorhombic symmetry, at high pressures, it transformed to a fluorite-type cubic structure. There are a lot of defects in the cubic structure, and it is a new kind of hyperstoichiometric uranium oxide, which is stable at ambient conditions. - Highlights: • A new fluorite-type high-pressure phase was found in hyperstoichometric UO 2 +x (x∼0.8). • The new high-pressure structure is quenchable to ambient conditions. • Pressure driven phase transition in orthorhombic U 3 O 8 was first found

  10. Structural phase transitions in Zn(CN)2 under high pressures

    International Nuclear Information System (INIS)

    Poswal, H.K.; Tyagi, A.K.; Lausi, Andrea; Deb, S.K.; Sharma, Surinder M.

    2009-01-01

    High pressure behavior of zinc cyanide (Zn(CN) 2 ) has been investigated with the help of synchrotron-based X-ray diffraction measurements. Our studies reveal that under pressure this compound undergoes phase transformations and the structures of the new phases depend on whether the pressure is hydrostatic or not. Under hydrostatic conditions, Zn(CN) 2 transforms from cubic to orthorhombic to cubic-II to amorphous phases. In contrast, the non-hydrostatic pressure conditions drive the ambient cubic phase to a partially disordered crystalline phase, which eventually evolves to a substantially disordered phase. The final disordered phase in the latter case is distinct from the amorphous phase observed under the hydrostatic pressures. - Graphical abstract: High pressure X-ray diffraction investigations on Zn(CN) 2 show three phase transformations i.e., cubic→orthorhombic→cubic-II→amorphous. However, the results strongly depend upon the nature of stress

  11. Anharmonic effective pair potentials of gold under high pressure and high temperature

    CERN Document Server

    Okube, M; Ohtaka, O; Fukui, H; Katayama, Y; Utsumi, W

    2002-01-01

    In order to examine the effect of pressure on the anharmonicity of Au, extended x-ray absorption fine-structure spectra near the Au L sub 3 edge were measured in the temperature range from 300 to 1100 K under pressures up to 14 GPa using large-volume high-pressure devices and synchrotron radiation. The anharmonic effective pair potentials of Au, V (u) = au sup 2 + bu sup 3 , at 0.1 MPa, 6 and 14 GPa have been calculated. The pressure dependence of the thermal expansion coefficients has also been evaluated. The reliability of the anharmonic correction proposed on the basis of the Anderson scale has been discussed.

  12. Structural and Transport Properties of the Weyl Semimetal NbAs at High Pressure

    International Nuclear Information System (INIS)

    Zhang Jun; Liu Feng-Liang; Dong Jin-Kui; Xu Yang; Li Shi-Yan; Li Na-Na; Yang Wen-Ge

    2015-01-01

    We perform a series of high-pressure synchrotron x-ray diffraction (XRD) and resistance measurements on the Weyl semimetal NbAs. The crystal structure remains stable up to 26 GPa according to the powder XRD data. The resistance of NbAs single crystal increases monotonically with pressure at low temperature. Up to 20 GPa, no superconducting transition is observed down to 0.3 K. These results show that the Weyl semimetal phase is robust in NbAs, and applying pressure may not be a good way to obtain a topological superconductor from Weyl semimetal NbAs. (paper)

  13. 'Devil's Staircase'-Type Phase Transition in NaV2O5 under High Pressure

    International Nuclear Information System (INIS)

    Ohwada, K.; Fujii, Y.; Takesue, N.; Isobe, M.; Ueda, Y.; Nakao, H.; Wakabayashi, Y.; Murakami, Y.; Ito, K.; Amemiya, Y.

    2001-01-01

    The 'devil's staircase'-type phase transition in the quarter-filled spin-ladder compound NaV 2 O 5 has been discovered at low temperature and high pressure by synchrotron radiation x-ray diffraction. A large number of transitions are found to successively take place among higher-order commensurate phases with 2a x 2b x zc type superstructures. The observed temperature and pressure dependence of modulation wave number q c , defined by 1/z, is well reproduced by the axial next nearest neighbor Ising model. The q c is suggested to reflect atomic displacements presumably coupled with charge ordering in this system

  14. Bulk moduli and high pressure phases of ThX compounds. Pt. 2

    International Nuclear Information System (INIS)

    Staun Olsen, J.; Gerward, L.; Benedict, U.; Luo, H.; Vogt, O.

    1989-01-01

    The high-pressure crystal structures of the members of the ThX series, where X = S, Se and Te, have been studied using synchrotron X-ray diffraction in the pressure range up to about 60 GPa. A distorted fcc structure is observed for ThS above 20 GPa. These transforms to the CsCl structure at 15 GPa. has the CsCl structure already at atmospheric pressure and no further phase transition has been observed. A log-log plot of bulk modulus versus specific volume gives a straight line with slope -1.85. (orig.)

  15. Diffraction studies of order-disorder at high pressures and temperatures

    International Nuclear Information System (INIS)

    Parise, John B.; Antao, Sytle M.; Martin, Charles D.; Crichton, Wilson

    2005-01-01

    Recent developments at synchrotron X-ray beamlines now allow collection of data suitable for structure determination and Rietveld structure refinement at high pressures and temperatures on challenging materials. These include materials, such as dolomite (CaMg(CO 3 ) 2 ) that tends to calcine at high temperatures, and Fe-containing materials, such as the spinel MgFe 2 O 4 , which tend to undergo changes in oxidation state. Careful consideration of encapsulation along with the use of radial collimation produced powder diffraction patterns virtually free of parasitic scattering from the cell in the case of large volume high-pressure experiments. These features have been used to study a number of phase transitions, especially those where superior signal-to-noise discrimination is required to distinguish weak ordering reflections. The structures adopted by dolomite, and CaSO4, anhydrite, were determined from 298 to 1466 K at high pressures. Using laser-heated diamond-anvil cells to achieve simultaneous high pressure and temperature conditions, we have observed CaSO 4 undergo phase transitions to the monazite type and at highest pressure and temperature to crystallize in the barite-type structure. On cooling, the barite structure distorts, from an orthorhombic to a monoclinic lattice, to produce the AgMnO 4 -type structure.

  16. Mechanism of degradation of surface hardening at elevated temperature in TiAlV-alloys by in situ synchrotron radiation diffraction

    CERN Document Server

    Berberich, F; Kreissig, U; Schell, N; Mücklich, A

    2003-01-01

    The surface hardness of the technically important alloy Ti-6Al-4V (wt.%) can be improved by nitrogen implantation. The structural mechanisms of hardening and of the stability of the improved hardness at elevated temperatures are studied. Ion implanted (II) and plasma immersion ion implanted (PII) samples were used. The formation of small TiN crystallites was detected in the as-implanted state, but only for the II samples a considerable surface hardness increase (factor 3) is observed. The in situ XRD experiments showed, that the TiN phase is stable up to temperatures of 650 deg. C for both types of implantation. At higher temperature Ti sub 2 N is formed which is stable up to 770 deg. C. ERDA results indicate a diffusion of nitrogen into the bulk material. The redistribution of N is responsible for the hardness changes: a slight decrease for II samples but an improvement by a factor of 2.5 for PII samples. The improvements/degradations of hardness and wear are discussed in correlation with the nitrogen depth ...

  17. A novel molten-salt electrochemical cell for investigating the reduction of uranium dioxide to uranium metal by lithium using in situ synchrotron radiation.

    Science.gov (United States)

    Brown, Leon D; Abdulaziz, Rema; Jervis, Rhodri; Bharath, Vidal; Mason, Thomas J; Atwood, Robert C; Reinhard, Christina; Connor, Leigh D; Inman, Douglas; Brett, Daniel J L; Shearing, Paul R

    2017-03-01

    A novel electrochemical cell has been designed and built to allow for in situ energy-dispersive X-ray diffraction measurements to be made during reduction of UO 2 to U metal in LiCl-KCl at 500°C. The electrochemical cell contains a recessed well at the bottom of the cell into which the working electrode sits, reducing the beam path for the X-rays through the molten-salt and maximizing the signal-to-noise ratio from the sample. Lithium metal was electrodeposited onto the UO 2 working electrode by exposing the working electrode to more negative potentials than the Li deposition potential of the LiCl-KCl eutectic electrolyte. The Li metal acts as a reducing agent for the chemical reduction of UO 2 to U, which appears to proceed to completion. All phases were fitted using Le Bail refinement. The cell is expected to be widely applicable to many studies involving molten-salt systems.

  18. Computer simulations of high pressure systems

    International Nuclear Information System (INIS)

    Wilkins, M.L.

    1977-01-01

    Numerical methods are capable of solving very difficult problems in solid mechanics and gas dynamics. In the design of engineering structures, critical decisions are possible if the behavior of materials is correctly described in the calculation. Problems of current interest require accurate analysis of stress-strain fields that range from very small elastic displacement to very large plastic deformation. A finite difference program is described that solves problems over this range and in two and three space-dimensions and time. A series of experiments and calculations serve to establish confidence in the plasticity formulation. The program can be used to design high pressure systems where plastic flow occurs. The purpose is to identify material properties, strength and elongation, that meet the operating requirements. An objective is to be able to perform destructive testing on a computer rather than on the engineering structure. Examples of topical interest are given

  19. Superconductivity from magnetic elements under high pressure

    International Nuclear Information System (INIS)

    Shimizu, Katsuya; Amaya, Kiichi; Suzuki, Naoshi; Onuki, Yoshichika

    2006-01-01

    Can we expect the appearance of superconductivity from magnetic elements? In general, superconductivity occurs in nonmagnetic metal at low temperature and magnetic impurities destroy superconductivity; magnetism and superconductivity are as incompatible as oil and water. Here, we present our experimental example of superconducting elements, iron and oxygen. They are magnetic at ambient pressure, however, they become nonmagnetic under high pressure, then superconductor at low temperature. What is the driving force of the superconductivity? Our understanding in the early stages was a simple scenario that the superconductive state was obtained as a consequence of an emergence of the nonmagnetic states. In both cases, we may consider another scenario for the appearance of superconductivity; the magnetic fluctuation mechanism in the same way as unconventional superconductors

  20. Urea and deuterium mixtures at high pressures

    Energy Technology Data Exchange (ETDEWEB)

    Donnelly, M., E-mail: m.donnelly-2@sms.ed.ac.uk; Husband, R. J.; Frantzana, A. D.; Loveday, J. S. [Centre for Science at Extreme Conditions and School of Physics and Astronomy, The University of Edinburgh, Erskine Williamson Building, Peter Guthrie Tait Road, The King’s Buildings, Edinburgh EH9 3FD (United Kingdom); Bull, C. L. [ISIS, Rutherford Appleton Laboratory, Oxford Harwell, Didcot OX11 0QX (United Kingdom); Klotz, S. [IMPMC, CNRS UMR 7590, Université P and M Curie, 4 Place Jussieu, 75252 Paris (France)

    2015-03-28

    Urea, like many network forming compounds, has long been known to form inclusion (guest-host) compounds. Unlike other network formers like water, urea is not known to form such inclusion compounds with simple molecules like hydrogen. Such compounds if they existed would be of interest both for the fundamental insight they provide into molecular bonding and as potential gas storage systems. Urea has been proposed as a potential hydrogen storage material [T. A. Strobel et al., Chem. Phys. Lett. 478, 97 (2009)]. Here, we report the results of high-pressure neutron diffraction studies of urea and D{sub 2} mixtures that indicate no inclusion compound forms up to 3.7 GPa.

  1. Sizing of high-pressure restriction orifices

    International Nuclear Information System (INIS)

    Casado Flores, E.

    1995-01-01

    Constant up-grading of power plants sometimes requires the modification of components which form part of suppliers' packages. In order to protect technology they have developed, however, the suppliers do not supply their calculation criteria. In order to reduce the costs of such improvements, and so as to be able to undertake the modification without having to rely on the original supplier, this paper describes the basic criteria applicable to the study of high-pressure restriction orifices, which can be considered to be representative of the components in question. The restriction orifices discussed are: - Insert - Multiplates in series with one perforation in each plate - Multiplates in series with several perforations in each plate For each type, an explanation of their sizing is given, together with the equations relating the corresponding flow and pressure drop. (Author)

  2. Recent developments in high pressure water technology

    International Nuclear Information System (INIS)

    Johnson, N.A.; Johnson, T.

    1992-01-01

    High Pressure Water Jetting has advanced rapidly in the last decade to a point where the field is splitting into specialised areas. This has left the end user or client in the dark as to whether water jetting will work and if so what equipment is best suited to their particular application. The aim of this paper is to give an overview of:-1. The way water is delivered to the surface and the parameters which control the concentration of energy available on impact. 2. The factors governing application driven selection of equipment. 3. The effects to technical advances in pumps and delivery systems on equipment selection with reference to their to their application to concrete removal and nuclear decontamination. (Author)

  3. High Pressure Quick Disconnect Particle Impact Tests

    Science.gov (United States)

    Rosales, Keisa R.; Stoltzfus, Joel M.

    2009-01-01

    NASA Johnson Space Center White Sands Test Facility (WSTF) performed particle impact testing to determine whether there is a particle impact ignition hazard in the quick disconnects (QDs) in the Environmental Control and Life Support System (ECLSS) on the International Space Station (ISS). Testing included standard supersonic and subsonic particle impact tests on 15-5 PH stainless steel, as well as tests performed on a QD simulator. This paper summarizes the particle impact tests completed at WSTF. Although there was an ignition in Test Series 4, it was determined the ignition was caused by the presence of a machining imperfection. The sum of all the test results indicates that there is no particle impact ignition hazard in the ISS ECLSS QDs. KEYWORDS: quick disconnect, high pressure, particle impact testing, stainless steel

  4. Dynamism or Disorder at High Pressures?

    Science.gov (United States)

    Angel, R. J.; Bismayer, U.; Marshall, W. G.

    2002-12-01

    Phase transitions in minerals at elevated temperatures typically involve dynamics as a natural consequence of the increase in thermal energy available to the system. Classic examples include quartz, cristobalite, and carbonates in which the high-temperature, high symmetry phase is dynamically disordered. This disorder has important thermodynamic consequences, including displacement and curvature of phase boundaries (e.g. calcite-aragonite). In other minerals such as clinopyroxenes and anorthite feldspar, the dynamic behaviour is restricted to the neighbourhood of the phase transition. The fundamental question is whether increasing pressure generally suppresses such dynamic behaviour (as in anorthite; Angel, 1988), or not. In the latter case it must be included in thermodynamic models of high-pressure phase equilibria and seismological modelling of the mantle; the potential dynamics and softening in stishovite may provide the critical observational constraint on the presence or otherwise of free silica in the lower mantle. We have continued to use the lead phosphate as a prototype ferroelastic in which to understand dynamic behaviour, simply because its dynamics and transition behaviour is far better characterised than any mineral. Furthermore, the phase transition is at a pressure where experimental difficulties do not dominate the experimental results. Our previous neutron diffraction study (Angel et al., 2001) revealed that some disorder, either dynamic or static, is retained in the high-symmetry, high-pressure phase just above the phase transition. New neutron diffraction data on the pure material now suggests that this disorder slowly decreases with increasing pressure until at twice the transition pressure it is ordered. Further data for doped material provides insights into the nature of this disorder. Angel (1988) Amer. Mineral. 73:1114. Angel et al (2001) J PhysC 13: 5353.

  5. Silver Accumulation in the Green Microalga Coccomyxa actinabiotis: Toxicity, in Situ Speciation, and Localization Investigated Using Synchrotron XAS, XRD, and TEM.

    Science.gov (United States)

    Leonardo, Thomas; Farhi, Emmanuel; Pouget, Stéphanie; Motellier, Sylvie; Boisson, Anne-Marie; Banerjee, Dipanjan; Rébeillé, Fabrice; den Auwer, Christophe; Rivasseau, Corinne

    2016-01-05

    Microalgae are good candidates for toxic metal remediation biotechnologies. This study explores the cellular processes implemented by the green microalga Coccomyxa actinabiotis to take up and cope with silver over the concentration range of 10(-7) to 10(-2) M Ag(+). Understanding these processes enables us to assess the potential of this microalga for applications for bioremediation. Silver in situ speciation and localization were investigated using X-ray absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. Silver toxicity was evaluated by monitoring microalgal growth and photochemical parameters. Different accumulation mechanisms were brought out depending on silver concentration. At low micromolar concentration, microalgae fixed all silver initially present in solution, trapping it inside the cells into the cytosol, mainly as unreduced Ag(I) bound with molecules containing sulfur. Silver was efficiently detoxified. When concentration increased, silver spread throughout the cell and particularly entered the chloroplast, where it damaged the photosystem. Most silver was reduced to Ag(0) and aggregated to form crystalline silver nanoparticles of face-centered cubic structure with a mean size of 10 nm. An additional minor interaction of silver with molecules containing sulfur indicated the concomitant existence of the mechanism observed at low concentration or nanoparticle capping. Nanoparticles were observed in chloroplasts, in mitochondria, on the plasma membrane, on cytosolic membrane structures, and in vacuoles. Above 10(-4) M Ag(+), damages were irreversible, and photosynthesis and growth were definitely inhibited. However, high silver amounts remained confined inside microalgae, showing their potential for the bioremediation of contaminated water.

  6. High pressure and synchrotron radiation studies of solid state electronic instabilities

    International Nuclear Information System (INIS)

    Pifer, J.H.; Croft, M.C.

    1992-04-01

    This report discusses Eu and General Valence Instabilities; Ce Problem: L 3 Spectroscopy Emphasis; Bulk Property Emphasis; Transition Metal Compound Electronic Structure; Electronic Structure-Phonon Coupling Studies; High Temperature Superconductivity and Oxide Materials; and Novel Materials Collaboration with Chemistry

  7. 30 CFR 56.13021 - High-pressure hose connections.

    Science.gov (United States)

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false High-pressure hose connections. 56.13021... and Boilers § 56.13021 High-pressure hose connections. Except where automatic shutoff valves are used, safety chains or other suitable locking devices shall be used at connections to machines of high-pressure...

  8. 76 FR 38697 - High Pressure Steel Cylinders From China

    Science.gov (United States)

    2011-07-01

    ... imports from China of high pressure steel cylinders, provided for in subheading 7311.00.00 of the... threatened with material injury by reason of LTFV and subsidized imports of high pressure steel cylinders... contained in USITC Publication 4241 (July 2011), entitled High Pressure Steel Cylinders from China...

  9. 77 FR 37712 - High Pressure Steel Cylinders From China

    Science.gov (United States)

    2012-06-22

    ...), that an industry in the United States is materially injured by reason of imports of high pressure steel... preliminary determinations by Commerce that imports of high pressure steel cylinders from China were... Publication 4328 (June 2012), entitled High Pressure Steel Cylinders from China: Investigation Nos. 701-TA-480...

  10. 30 CFR 57.13021 - High-pressure hose connections.

    Science.gov (United States)

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false High-pressure hose connections. 57.13021... Air and Boilers § 57.13021 High-pressure hose connections. Except where automatic shutoff valves are...-pressure hose lines of 3/4-inch inside diameter or larger, and between high-pressure hose lines of 3/4-inch...

  11. High pressure effect for high-Tc superconductors

    International Nuclear Information System (INIS)

    Takahashi, Hiroki; Tomita, Takahiro

    2011-01-01

    A number of experimental and theoretical studies have been performed to understand the mechanism of high-T c superconductivity and to enhance T c . High-pressure techniques have played a very important role for these studies. In this paper, the high-pressure techniques and physical properties of high-T c superconductor under high pressure are presented. (author)

  12. Salt partitioning between water and high-pressure ices. Implication for the dynamics and habitability of icy moons and water-rich planetary bodies

    Science.gov (United States)

    Journaux, Baptiste; Daniel, Isabelle; Petitgirard, Sylvain; Cardon, Hervé; Perrillat, Jean-Philippe; Caracas, Razvan; Mezouar, Mohamed

    2017-04-01

    Water-rich planetary bodies including large icy moons and ocean exoplanets may host a deep liquid water ocean underlying a high-pressure icy mantle. The latter is often considered as a limitation to the habitability of the uppermost ocean because it would limit the availability of nutrients resulting from the hydrothermal alteration of the silicate mantle located beneath the deep ice layer. To assess the effects of salts on the physical properties of high-pressure ices and therefore the possible chemical exchanges and habitability inside H2O-rich planetary bodies, we measured partitioning coefficients and densities in the H2O-RbI system up to 450 K and 4 GPa; RbI standing as an experimentally amenable analog of NaCl in the H2O-salt solutions. We measured the partitioning coefficient of RbI between the aqueous fluid and ices VI and VII, using in-situ Synchrotron X-ray Fluorescence (XRF). With in-situ X-ray diffraction, we measured the unit-cell parameters and the densities of the high-pressure ice phases in equilibrium with the aqueous fluid, at pressures and temperatures relevant to the interior of planetary bodies. We conclude that RbI is strongly incompatible towards ice VI with a partitioning coefficient Kd(VI-L) = 5.0 (± 2.1) ṡ10-3 and moderately incompatible towards ice VII, Kd(VII-L) = 0.12 (± 0.05). RbI significantly increases the unit-cell volume of ice VI and VII by ca. 1%. This implies that RbI-poor ice VI is buoyant compared to H2O ice VI while RbI-enriched ice VII is denser than H2O ice VII. These new experimental results might profoundly impact the internal dynamics of water-rich planetary bodies. For instance, an icy mantle at moderate conditions of pressure and temperature will consist of buoyant ice VI with low concentration of salt, and would likely induce an upwelling current of solutes towards the above liquid ocean. In contrast, a deep and/or thick icy mantle of ice VII will be enriched in salt and hence would form a stable chemical boundary

  13. Subnanosecond breakdown in high-pressure gases

    Science.gov (United States)

    Naidis, George V.; Tarasenko, Victor F.; Babaeva, Natalia Yu; Lomaev, Mikhail I.

    2018-01-01

    Pulsed discharges in high-pressure gases are of considerable interest as sources of nonequilibrium plasma for various technological applications: pollution control, pumping of laser media, plasma-assisted combustion, etc. Recently, attention has been attracted to the use of subnanosecond voltage fronts, producing diffuse discharges with radii of several millimeters. Such plasma structures, similar to pulsed glow discharges, are of special interest for applications due to quasi-uniformity of plasma parameters in relatively large gas volumes. This review presents the results of experimental and computational study of subnanosecond diffuse discharge formation. A description of generators of short high-voltage pulses with subnanosecond fronts and of discharge setups is given. Diagnostic methods for the measurement of various discharge parameters with high temporal and spatial resolution are described. Obtained experimental data on plasma properties for a wide range of governing factors are discussed. A review of various theoretical approaches used for computational study of the dynamics and structure of fast ionization waves is given; the applicability of conventional fluid streamer models for simulation of subnanosecond ionization waves is discussed. Calculated spatial-temporal profiles of plasma parameters during streamer propagation are presented. The efficiency of subnanosecond discharges for the production of reactive species is evaluated. On the basis of the comparison of simulation results and experimental data the effects of various factors (voltage rise time, polarity, etc.) on discharge characteristics are revealed. The major physical phenomena governing the properties of subnanosecond breakdown are analyzed.

  14. Blue emitting organic semiconductors under high pressure

    DEFF Research Database (Denmark)

    Knaapila, Matti; Guha, Suchismita

    2016-01-01

    This review describes essential optical and emerging structural experiments that use high GPa range hydrostatic pressure to probe physical phenomena in blue-emitting organic semiconductors including π-conjugated polyfluorene and related compounds. The work emphasizes molecular structure and inter......This review describes essential optical and emerging structural experiments that use high GPa range hydrostatic pressure to probe physical phenomena in blue-emitting organic semiconductors including π-conjugated polyfluorene and related compounds. The work emphasizes molecular structure...... and intermolecular self-organization that typically determine transport and optical emission in π-conjugated oligomers and polymers. In this context, hydrostatic pressure through diamond anvil cells has proven to be an elegant tool to control structure and interactions without chemical intervention. This has been...... and intermolecular interactions on optical excitations, electron–phonon interaction, and changes in backbone conformations. This picture is connected to the optical high pressure studies of other π-conjugated systems and emerging x-ray scattering experiments from polyfluorenes which provides a structure-property map...

  15. Engineering Model of High Pressure Moist Air

    Directory of Open Access Journals (Sweden)

    Hyhlík Tomáš

    2017-01-01

    Full Text Available The article deals with the moist air equation of state. There are equations of state discussed in the article, i.e. the model of an ideal mixture of ideal gases, the model of an ideal mixture of real gases and the model based on the virial equation of state. The evaluation of sound speed based on the ideal mixture concept is mentioned. The sound speed calculated by the model of an ideal mixture of ideal gases is compared with the sound speed calculated by using the model based on the concept of an ideal mixture of real gases. The comparison of enthalpy end entropy based on the model of an ideal mixture of ideal gases and the model of an ideal mixture of real gases is performed. It is shown that the model of an ideal mixture of real gases deviates from the model of an ideal mixture of ideal gases only in the case of high pressure. An impossibility of the definition of partial pressure in the mixture of real gases is discussed, where the virial equation of state is used.

  16. High Pressure Laminates with Antimicrobial Properties

    Directory of Open Access Journals (Sweden)

    Sandra Magina

    2016-02-01

    Full Text Available High-pressure laminates (HPLs are durable, resistant to environmental effects and good cost-benefit decorative surface composite materials with special properties tailored to meet market demand. In the present work, polyhexamethylene biguanide (PHMB was incorporated for the first time into melamine-formaldehyde resin (MF matrix on the outer layer of HPLs to provide them antimicrobial properties. Chemical binding of PHMB to resin matrix was detected on the surface of produced HPLs by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR. Antimicrobial evaluation tests were carried out on the ensuing HPLs doped with PHMB against gram-positive Listeria innocua and gram-negative Escherichia coli bacteria. The results revealed that laminates prepared with 1.0 wt % PHMB in MF resin were bacteriostatic (i.e., inhibited the growth of microorganisms, whereas those prepared with 2.4 wt % PHMB in MF resin exhibited bactericidal activity (i.e., inactivated the inoculated microorganisms. The results herein reported disclose a promising strategy for the production of HPLs with antimicrobial activity without affecting basic intrinsic quality parameters of composite material.

  17. High pressure phase transitions in Europous oxide

    International Nuclear Information System (INIS)

    Kremser, D.T.

    1982-01-01

    The pressure-volume relationship for EuO was investigated to 630 kilobars at room temperature with a diamond-anvil, high-pressure cell. Volumes were determined by x-ray diffraction; pressures were determined by the ruby R 1 fluorescence method. The preferred interpretation involves normal compression behavior for EuO, initially in the B1 (NaCl-type) structure, to about 280 kilobars. Between approx. =280 and approx. =350 kilobars a region of anomalous compressibility in which the volume drops continuously by approximately 2% is observed. A second-order electronic transition is proposed with the 6s band overlapping with the 4f levels, thereby reducing the volume of EuO without changing the structure. This is not a semiconductor-to-metal transition. In reflected light, this transition is correlated with a subtle and continuous change in color from brown-black to a light brown. The collapsed B1 phase (postelectronic transition) is stable between approx. =350 and approx. =400 kilobars. At about 400 kilobars the collapsed B1 structure transforms to the B2 (CsCl-type) structure, with a zero pressure-volume change of approximately 12 +/- 1.5%

  18. P–V–T equation of state of molybdenite (MoS2) by a diamond anvil cell and in situ synchrotron angle-dispersive X-ray diffraction

    International Nuclear Information System (INIS)

    Fan, Dawei; Xu, Jingui; Ma, Maining; Liu, Jing; Xie, Hongsen

    2014-01-01

    The pressure–volume–temperature (P–V–T) equation of state (EoS) of a natural molybdenite (MoS 2 ) has been measured at high temperature up to 700 K and high pressures up to 18.26 GPa, by using in situ angle-dispersive X-ray diffraction and diamond anvil cell. Analysis of room-temperature P–V data to a third-order Birch–Murnaghan EoS yields: V 0 =107.0±0.1 Å 3 , K 0 =67±2 GPa and K′ 0 =5.0±0.3. With K′ 0 fixed to 4.0, we obtained: V 0 =106.7±0.1 Å 3 and K 0 =74.5±0.8 GPa. Fitting of our P–V–T data by means of the high-temperature third order Birch–Murnaghan equations of state, gives the thermoelastic parameters: V 0 =107.0±0.1 Å 3 , K 0 =69±2 GPa, K′ 0 =4.7±0.2, (∂K/∂T) P =−0.021±0.003 GPa K −1 , a=(2.2±0.7)×10 −5 K −1 and b=(2.9±0.8)×10 −8 K −2 . The temperature derivative of the bulk modulus and thermal expansion coefficient of MoS 2 are obtained for the first time. Present results are also compared with previously studies determined the elastic properties of MoS 2 and WS 2

  19. P–V–T equation of state of molybdenite (MoS{sub 2}) by a diamond anvil cell and in situ synchrotron angle-dispersive X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Dawei, E-mail: fandawei@vip.gyig.ac.cn [Laboratory for High Temperature and High Pressure Study of the Earth’s Interior of Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550002 (China); Xu, Jingui [Laboratory for High Temperature and High Pressure Study of the Earth’s Interior of Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550002 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Ma, Maining [University of Chinese Academy of Sciences, Beijing 100049 (China); Key Laboratory of Computational Geodynamics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Jing [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Xie, Hongsen [Laboratory for High Temperature and High Pressure Study of the Earth’s Interior of Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550002 (China)

    2014-10-15

    The pressure–volume–temperature (P–V–T) equation of state (EoS) of a natural molybdenite (MoS{sub 2}) has been measured at high temperature up to 700 K and high pressures up to 18.26 GPa, by using in situ angle-dispersive X-ray diffraction and diamond anvil cell. Analysis of room-temperature P–V data to a third-order Birch–Murnaghan EoS yields: V{sub 0}=107.0±0.1 Å{sup 3}, K{sub 0}=67±2 GPa and K′{sub 0}=5.0±0.3. With K′{sub 0} fixed to 4.0, we obtained: V{sub 0}=106.7±0.1 Å{sup 3} and K{sub 0}=74.5±0.8 GPa. Fitting of our P–V–T data by means of the high-temperature third order Birch–Murnaghan equations of state, gives the thermoelastic parameters: V{sub 0}=107.0±0.1 Å{sup 3}, K{sub 0}=69±2 GPa, K′{sub 0}=4.7±0.2, (∂K/∂T){sub P}=−0.021±0.003 GPa K{sup −1}, a=(2.2±0.7)×10{sup −5} K{sup −1} and b=(2.9±0.8)×10{sup −8} K{sup −2}. The temperature derivative of the bulk modulus and thermal expansion coefficient of MoS{sub 2} are obtained for the first time. Present results are also compared with previously studies determined the elastic properties of MoS{sub 2} and WS{sub 2}.

  20. Recent progress in high-pressure studies on organic conductors

    Directory of Open Access Journals (Sweden)

    Syuma Yasuzuka and Keizo Murata

    2009-01-01

    Full Text Available Recent high-pressure studies of organic conductors and superconductors are reviewed. The discovery of the highest Tc superconductivity among organics under high pressure has triggered the further progress of the high-pressure research. Owing to this finding, various organic conductors with the strong electron correlation were investigated under high pressures. This review includes the pressure techniques using the cubic anvil apparatus, as well as high-pressure studies of the organic conductors up to 10 GPa showing extraordinary temperature and pressure dependent transport phenomena.

  1. High-pressure structural behavior of the double perovskite Sr2CrReO6: an experimental and theoretical study

    DEFF Research Database (Denmark)

    Olsen, J.S.; Gerward, Leif; Vaitheeswaran, G.

    2009-01-01

    The high-pressure structural behavior of Sr2CrReO6 has been studied experimentally using synchrotron radiation and the diamond anvil cell and theoretically using density functional theory. The experimental zero-pressure bulk modulus is B0=1704GPa and the pressure derivative is B0'=4.71.0. These r...

  2. The third generation French synchrotron

    International Nuclear Information System (INIS)

    Anon.

    1997-01-01

    This short paper gives a concise presentation of the SOLEIL project of the LURE synchrotron radiation national laboratory at Orsay (France). This new accelerator is devoted to replace the DCI and Super ACO rings of first and second generation, respectively. The main research domains of this project concern: the micro-fluorescence and micro-diffraction characterization of materials, and in particular the electronic components; the study of matter in extreme conditions (high temperature and high pressure); the bio-crystallography; the study of aggregates; and the manufacturing of micro-instruments for micro-electronics or medical applications. SOLEIL will be equipped with special magnetic wigglers to obtain very high brightness sources. The source will be a 336 m circumference ring for 2.5 GeV electron storage, able to produce a large spectrum synchrotron radiation. The injection system will comprise a low energy-high current linear electron accelerator and two electron beam transport lines. The installation will be buried at a 4 m depth to ensure the environmental protection and to limit vibrations. (J.S.)

  3. Phase diagram and equation of state of TiH2 at high pressures and high temperatures

    International Nuclear Information System (INIS)

    Endo, Naruki; Saitoh, Hiroyuki; Machida, Akihiko; Katayama, Yoshinori; Aoki, Katsutoshi

    2013-01-01

    Highlights: ► We determined the phase diagram of TiH 2 at high pressures and high temperatures. ► Compression induced stain inhibited the phase transition from the bct to fcc phase. ► The phase boundary was appropriately determined using a sample with heat treatment. ► The high temperature Birch–Murnaghan equation of state of fcc TiH 2 was firstly determined. - Abstract: We determined the phase diagram and the equation of state (EoS) of TiH 2 at high pressures up to 8.7 GPa and high temperatures up to 600 °C by in situ synchrotron radiation X-ray diffraction measurements. Compression induced strain inhibited the phase transition from the low-temperature bct phase to the high-temperature fcc phase, making the phase diagram difficult to determine. However, heating around 600 °C relieved the strain, and the phase boundary between the bct and fcc phases was elucidated. The phase transition temperature at ambient pressure increased from around room temperature to 200 °C at 8.7 GPa. The high temperature Birch–Murnaghan EoS was determined for the fcc phase. With the pressure derivative of the bulk modulus K′ 0 = 4.0, the following parameters were obtained: ambient bulk modulus K 0 = 97.7 ± 0.2 GPa, ambient unit cell of the fcc phase V 0 = 88.57 ± 0.02 Å 3 , temperature derivative of the bulk modulus at constant pressure (∂K/∂T) P = −0.01 ± 0.02, and volumetric thermal expansivity α = a + bT with a = 2.62 ± 1.4 × 10 −5 and b = 5.5 ± 4.5 × 10 −8 . K 0 of fcc TiH 2 was close to those for pure Ti and bct TiH 2 reported in previous studies.

  4. Viscosity of liquid sulfur under high pressure

    International Nuclear Information System (INIS)

    Terasaki, Hidenori; Kato, T; Funakoshi, K; Suzuki, A; Urakawa, S

    2004-01-01

    The viscosity of liquid sulfur up to 9.7 GPa and 1067 K was measured using the in situ x-ray radiography falling sphere method. The viscosity coefficients were found to range from 0.11 to 0.69 Pa s, and decreased continuously with increasing pressure under approximately constant homologous temperature conditions. The observed viscosity variation suggests that a gradual structural change occurs in liquid sulfur with pressure up to 10 GPa. The L-L' transition in liquid sulfur proposed by Brazhkin et al (1991 Phys. Lett. A 154 413) from thermobaric measurements has not been confirmed by the present viscometry

  5. Synchrotron radiation in Australia

    International Nuclear Information System (INIS)

    Garrett, R.F.

    2002-01-01

    Full text: Synchrotron radiation research in Australia is entering a new era with the commencement of the Australian synchrotron project, which will construct a 3 GeV third generation synchrotron facility at Monash University in Victoria. To date Australian scientists have used overseas facilities, primarily those managed by the Australian Synchrotron Research Program in Japan and the USA. A fast developing and maturing Australian synchrotron user program has developed around these overseas facilities. The field of synchrotron radiation and its importance to a wide range of research will be introduced and Australia's current involvement and facilities will be described. The current status and technical specifications of the Australian synchrotron will be presented. Copyright (2002) Australian X-ray Analytical Association Inc

  6. High pressure experimental studies on Na3Fe(PO4)(CO3) and Na3Mn(PO4)(CO3): Extensive pressure behaviors of carbonophosphates family

    Science.gov (United States)

    Gao, Jing; Huang, Weifeng; Wu, Xiang; Qin, Shan

    2018-04-01

    Carbon-bearing phases in the Earth's interior have profound implications for the long-term Earth carbon cycle. Here we investigate high-pressure behaviors of carbonophosphates bonshtedtite Na3Fe(PO4)(CO3) and sidorenkite Na3Mn(PO4)(CO3) in diamond anvil cells up to ∼12 GPa at room temperature. Modifications in in situ synchrotron X-ray diffraction patterns and Raman spectra confirm the structural stability of carbonophosphates within the pressure region. Fitting the third-order Birch-Murnaghan equation of state to the volume compression curve, the isothermal bulk modulus parameters are obtained to be K0 = 56(1) GPa, K0' = 3.3(1), V0 = 303.3(3) Å3 for Na3Fe(PO4)(CO3) and K0 = 54(1) GPa, K0' = 3.4(1), V0 = 313.4(2) Å3 for Na3Mn(PO4)(CO3). Crystallographic axes exhibit an elastic anisotropy with a more compressible c-axis relative to the ab-plane. An inverse linear correlation between the K0 value and the ionic radius of M2+ (M = Mg, Fe, Mn) is well determined for carbonophosphates. The pressure-dependence responsiveness of [PO4] and [CO3] in carbonophosphates show a negative relationship to the M2+ radius. We also discussed the effect of [PO4] group on the structural variations and high-pressure behaviors of carbonates. Furthermore, the geochemical properties of carbonophosphates hold implications to diamond genesis.

  7. Pressure Dome for High-Pressure Electrolyzer

    Science.gov (United States)

    Norman, Timothy; Schmitt, Edwin

    2012-01-01

    A high-strength, low-weight pressure vessel dome was designed specifically to house a high-pressure [2,000 psi (approx. = 13.8 MPa)] electrolyzer. In operation, the dome is filled with an inert gas pressurized to roughly 100 psi (approx. = 690 kPa) above the high, balanced pressure product oxygen and hydrogen gas streams. The inert gas acts to reduce the clamping load on electrolyzer stack tie bolts since the dome pressure acting axially inward helps offset the outward axial forces from the stack gas pressure. Likewise, radial and circumferential stresses on electrolyzer frames are minimized. Because the dome is operated at a higher pressure than the electrolyzer product gas, any external electrolyzer leak prevents oxygen or hydrogen from leaking into the dome. Instead the affected stack gas stream pressure rises detectably, thereby enabling a system shutdown. All electrical and fluid connections to the stack are made inside the pressure dome and require special plumbing and electrical dome interfaces for this to be accomplished. Further benefits of the dome are that it can act as a containment shield in the unlikely event of a catastrophic failure. Studies indicate that, for a given active area (and hence, cell ID), frame outside diameter must become ever larger to support stresses at higher operating pressures. This can lead to a large footprint and increased costs associated with thicker and/or larger diameter end-plates, tie-rods, and the frames themselves. One solution is to employ rings that fit snugly around the frame. This complicates stack assembly and is sometimes difficult to achieve in practice, as its success is strongly dependent on frame and ring tolerances, gas pressure, and operating temperature. A pressure dome permits an otherwise low-pressure stack to operate at higher pressures without growing the electrolyzer hardware. The pressure dome consists of two machined segments. An O-ring is placed in an O-ring groove in the flange of the bottom

  8. Application on electrochemistry measurement of high temperature high pressure condition in PWR nuclear power plants

    International Nuclear Information System (INIS)

    Li Yuchun; Xiao Zhongliang; Jiang Ya; Yu Xiaowei; Pang Feifei; Deng Fenfang; Gao Fan; Zhou Nianguang

    2011-01-01

    High temperature high pressure electrochemistry testing system was comprehensively analyzed in this paper, according to actual status for supervision in primary and secondary circuits of PWR nuclear power plants. Three research methods were reviewed and discussed for in-situ monitor system. By combination with ECP realtime measurement it was executed for evaluation and water chemistry optimization in nuclear power plants. It is pointed out that in-situ electrochemistry measurement has great potential application for water chemistry evaluation in PWR nuclear power plants. (authors)

  9. Cobalt ferrite nanoparticles under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Saccone, F. D.; Ferrari, S.; Grinblat, F.; Bilovol, V. [Instituto de Tecnologías y Ciencias de la Ingeniería, “Ing. H. Fernández Long,” Av. Paseo Colón 850 (1063), Buenos Aires (Argentina); Errandonea, D., E-mail: daniel.errandonea@uv.es [Departamento de Fisica Aplicada, Institut Universitari de Ciència dels Materials, Universitat de Valencia, c/ Doctor Moliner 50, E-46100 Burjassot, Valencia (Spain); Agouram, S. [Departamento de Física Aplicada y Electromagnetismo, Universitat de València, 46100 Burjassot, Valencia (Spain)

    2015-08-21

    We report by the first time a high pressure X-ray diffraction and Raman spectroscopy study of cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles carried out at room temperature up to 17 GPa. In contrast with previous studies of nanoparticles, which proposed the transition pressure to be reduced from 20–27 GPa to 7.5–12.5 GPa (depending on particle size), we found that cobalt ferrite nanoparticles remain in the spinel structure up to the highest pressure covered by our experiments. In addition, we report the pressure dependence of the unit-cell parameter and Raman modes of the studied sample. We found that under quasi-hydrostatic conditions, the bulk modulus of the nanoparticles (B{sub 0} = 204 GPa) is considerably larger than the value previously reported for bulk CoFe{sub 2}O{sub 4} (B{sub 0} = 172 GPa). In addition, when the pressure medium becomes non-hydrostatic and deviatoric stresses affect the experiments, there is a noticeable decrease of the compressibility of the studied sample (B{sub 0} = 284 GPa). After decompression, the cobalt ferrite lattice parameter does not revert to its initial value, evidencing a unit cell contraction after pressure was removed. Finally, Raman spectroscopy provides information on the pressure dependence of all Raman-active modes and evidences that cation inversion is enhanced by pressure under non-hydrostatic conditions, being this effect not fully reversible.

  10. Novel high pressure hexagonal OsB2 by mechanochemistry

    Science.gov (United States)

    Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

    2014-07-01

    Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

  11. Phase relationships of the system Fe-Ni-S and structure of the high-pressure phase of (Fe1-xNix)3S2

    Science.gov (United States)

    Urakawa, Satoru; Kamuro, Ryota; Suzuki, Akio; Kikegawa, Takumi

    2018-04-01

    The phase relationships of the Fe-Ni-S system at 15 GPa were studied by high pressure quench experiments. The stability fields of (Fe,Ni)3S and (Fe,Ni)3S2 and the melting relationships of the Fe-Ni-S system were determined as a function of Ni content. The (Fe,Ni)3S solid solution is stable in the composition of Ni/(Fe + Ni) > 0.7 and melts incongruently into an Fe-Ni alloy + liquid. The (Fe,Ni)3S2 makes a complete solid solution and melts incongruently into (Fe,Ni)S + liquid, whose structure was determined to show Cmcm-orthorhombic symmetry by in situ synchrotron X-ray diffraction experiments. The eutectic contains about 30 at.% of S, and its temperature decreases with increasing Ni content with a rate of ∼5 K/at.% from 1175 K. The density of the Fe-FeS eutectic composition (Fe70S30) liquid is evaluated to be 6.93 ± 0.08 g/cm3 at 15 GPa and 1200 K based on the Clausius-Clapeyron relations and densities of subsolidus phases. The Fe-Ni-S liquids are a primary sulfur-bearing phase in the deep mantle with a reducing condition (250-660 km depth), and they would play a significant role in the carbon cycle as a carbon host as well as in the generation of diamond.

  12. PREFACE: 23rd International Conference on High Pressure Science and Technology (AIRAPT-23)

    Science.gov (United States)

    Gupta, Satish C.

    2012-07-01

    The 23rd AIRAPT International Conference on High Pressure Science and Technology was held at Bhabha Atomic Research Centre, Mumbai, from 25-30 September 2011. This conference is part of the series of AIRAPT International Conferences which are held biennially. AIRAPT is an acronym for the French title which translates as 'International Association for the Advancement of High Pressure Science and Technology'. This was the second time the AIRAPT Conference was organized in India. The first was held 20 years ago at the National Aeronautical Laboratory, Bangalore in 1991. The 23rd Conference covered many important topics in the area of both static and dynamic high pressures including theoretical and experimental investigations on the response of materials under high pressures, new developments using neutron and synchrotron sources, investigations on superconductivity under high pressure, studies of geophysical and planetary sciences, biosciences, and the synthesis of new materials. The conference program included Bridgman award lecture, Jemieson award lecture, seven plenary talks, 85 invited talks, 83 oral presentations and about 195 posters. In all there were 372 presentations. 285 scientists from 19 countries participated in the conference. The countries represented included Austria, Canada, China, Estonia, France, Germany, India, Israel, Italy, Japan, Nepal, New Zealand, Poland, Russia, South Korea, Spain, Sweden, Switzerland, Turkey, UK, Ukraine and USA. Many new developments were presented, for example, measurement techniques using the new generation synchrotron sources, more powerful neutron sources and much brighter laser sources; integration of gas-gun with synchrotron source; the achievement of multi-megabar pressures in shock-less dynamic compressions; and capabilities to synthesize centimeter size diamonds with better quality. All these developments have opened up new opportunities for understanding the physics of materials under high pressures. I would like

  13. High-pressure phase transition and properties of spinel ZnMn2O4

    DEFF Research Database (Denmark)

    Åbrink, S.; Waskowska, A.; Gerward, Leif

    1999-01-01

    to normal pressure. The c/a ratio reduces from 1.62 to 1.10 above P-c and remains nearly pressure independent in the high-pressure phase. The transition is attributed to the changes in electron configuration of the Mn3+ ions. According to the crystal field theory, the e(g) electron of octahedrally......-pressure behavior of ZnMn2O4 was investigated up to 52 GPa using the energy-dispersive x-ray diffraction technique and synchrotron radiation. The structural first-order phase transition from the body-centered to primitive-tetragonal cell takes place at P-c = 23 GPa. The high-pressure phase is metastable down...... coordinated Mn3+ is either in the d(z)(2) orbital or in the d(x2-y2). In the first configuration the MnO6 octahedron will be elongated and this is the case at normal pressure, while the second configuration gives the flattened octahedron. In the high-pressure phase some proportion of the e(g) electrons...

  14. A new paradigm for macromolecular crystallography beamlines derived from high-pressure methodology and results

    Energy Technology Data Exchange (ETDEWEB)

    Fourme, Roger, E-mail: roger.fourme@synchrotron-soleil.fr [Synchrotron SOLEIL, BP 48, Saint Aubin, 91192 Gif-sur-Yvette (France); Girard, Eric [IBS (UMR 5075 CEA-CNRS-UJF-PSB), 41 rue Jules Horowitz, 38027 Grenoble Cedex (France); Dhaussy, Anne-Claire [CRISMAT, ENSICAEN, 6 Boulevard du Maréchal Juin, 14000 Caen (France); Medjoubi, Kadda [Synchrotron SOLEIL, BP 48, Saint Aubin, 91192 Gif-sur-Yvette (France); Prangé, Thierry [LCRB (UMR 8015 CNRS), Université Paris Descartes, Faculté de Pharmacie, 4 avenue de l’Observatoire, 75270 Paris (France); Ascone, Isabella [ENSCP (UMR CNRS 7223), 11 rue Pierre et Marie Curie, 75231 Paris Cedex 05 (France); Mezouar, Mohamed [ESRF, BP 220, 38043 Grenoble (France); Kahn, Richard [IBS (UMR 5075 CEA-CNRS-UJF-PSB), 41 rue Jules Horowitz, 38027 Grenoble Cedex (France)

    2011-01-01

    Macromolecular crystallography at high pressure (HPMX) is a mature technique. Shorter X-ray wavelengths increase data collection efficiency on cryocooled crystals. Extending applications and exploiting spin-off of HPMX will require dedicated synchrotron radiation beamlines based on a new paradigm. Biological structures can now be investigated at high resolution by high-pressure X-ray macromolecular crystallography (HPMX). The number of HPMX studies is growing, with applications to polynucleotides, monomeric and multimeric proteins, complex assemblies and even a virus capsid. Investigations of the effects of pressure perturbation have encompassed elastic compression of the native state, study of proteins from extremophiles and trapping of higher-energy conformers that are often of biological interest; measurements of the compressibility of crystals and macromolecules were also performed. HPMX results were an incentive to investigate short and ultra-short wavelengths for standard biocrystallography. On cryocooled lysozyme crystals it was found that the data collection efficiency using 33 keV photons is increased with respect to 18 keV photons. This conclusion was extended from 33 keV down to 6.5 keV by exploiting previously published data. To be fully exploited, the potential of higher-energy photons requires detectors with a good efficiency. Accordingly, a new paradigm for MX beamlines was suggested, using conventional short and ultra-short wavelengths, aiming at the collection of very high accuracy data on crystals under standard conditions or under high pressure. The main elements of such beamlines are outlined.

  15. Theory and Practice - Measuring High-Pressure Electronic and Magnetic Properties

    International Nuclear Information System (INIS)

    Hemley, R.J.; Struzhkin, V.V.; Cohen, R.E.

    2008-01-01

    Measurements of the electronic and magnetic properties of Earth and planetary materials at high pressure play a crucial role in modern geoscience. There have been numerous advances in the field, primarily as a result of developments in diamond-anvil cell methods. In particular, synchrotron radiation techniques play an especially important role. The chapter begins with a short review of fundamental properties of the relevant materials, with emphasis on how these are altered under very high pressures and temperatures of the Earth's deep interior, followed by a discussion of different classes of electronic and magnetic excitations. Various techniques currently used for high-pressure studies are then described, beginning with optical spectroscopies, Moessbauer spectroscopy, elastic X-ray and neutron scattering, many new X-ray spectroscopy and inelastic scattering methods, transport techniques, and finally resonance methods. Selected examples of the techniques are given, with a common theme being the high P-T behavior of iron-containing oxides, silicates, and metals at conditions found throughout the Earth's interior. Applications to upper-mantle phases, 'simple' oxides, silicate perovskite and post-perovskite, volatiles, and iron and iron alloys are discussed, with an emphasis given to integrated studies utilizing a combination of different techniques to understand high P-T electronic and magnetic phenomena.

  16. Viscosity of komatiite liquid at high pressure and temperature

    Science.gov (United States)

    O Dwyer, L.; Lesher, C. E.; Wang, Y.

    2006-12-01

    The viscosities of komatiite liquids at high pressures and temperatures are being investigated by the in-situ falling sphere technique, using the T-25 multianvil apparatus at the GSECARS 13 ID-D beamline at the Advanced Photon Source, ANL. The refractory and fluid nature of komatiite and other ultramafic liquids relevant to the Earth's deep interior, presents unique challenges for this approach. To reach superliquidus temperatures we use a double reservoir configuration, where marker spheres are placed at the top of both a main melt reservoir and an overlying reservoir containing a more refractory composition. Using this approach, we have successfully measured the viscosity of a komatiite from Gorgona Island (GOR-94-29; MgO - 17.8 wt.%; NBO/T = 1.6) up to 6 GPa and 1900 K. Under isothermal conditions, viscosity increases with pressure, consistent with the depolymerized nature of the komatiite. At 1900 K, viscosity increases from 1.5 (+- 0.3) Pa s at 3.5 GPa to 3.4 (+- 0.3) Pa s at 6 GPa, corresponding to an activation volume of 2.2 cm3/mol. At high pressures, the viscosities of Gorgona Island komatiite melt are an order of magnitude higher than those measured by Liebske et al. (2005, EPSL, v. 240) for peridotite melt (MgO 37.1 wt.%; NBO/T = 2.5), and similar in magnitude to molten diopside (NBO/T = 2) (Reid et al. 2003, PEPI, v. 139). The positive pressure dependence is consistent with the reduction in interatomic space diminishing the free volume of the liquid as it is compressed. Above 6 GPa the free volume reduction may become less important with the production of high-coordinated network formers, as attributed to the reversal of the pressure dependence of viscosity for peridotite melt at ~8.5 GPa and diopside melt at ~10 GPa. Experiments at higher pressures are underway to determine if a similar viscosity maximum occurs for komatiite melt and whether its pressure is greater than 10 GPa, as suggested by the data for peridotite and diopside melts.

  17. Safety regulation on high-pressure gas and gas business

    International Nuclear Information System (INIS)

    Kim, Du Yeoung; An, Dae Jun

    1978-09-01

    This book is divided into two parts. The first part introduces safety regulation on high-pressure gas, enforcement ordinance on safety regulation about high-pressure gas and enforcement regulation on safety regulation about high-pressure gas. The second part indicates regulations on gas business such as general rules, gas business gas supplies, using land, supervision, supple mentary rules and penalty. It has two appendixes on expected questions and questions during last years.

  18. Synchrotron radiation facilities

    CERN Multimedia

    1972-01-01

    Particularly in the past few years, interest in using the synchrotron radiation emanating from high energy, circular electron machines has grown considerably. In our February issue we included an article on the synchrotron radiation facility at Frascati. This month we are spreading the net wider — saying something about the properties of the radiation, listing the centres where synchrotron radiation facilities exist, adding a brief description of three of them and mentioning areas of physics in which the facilities are used.

  19. Proposed dedicated high pressure beam lines at CHESS

    International Nuclear Information System (INIS)

    Ruoff, A.L.; Vohra, Y.K.; Bassett, W.A.; Batterman, B.W.; Bilderback, D.H.

    1988-01-01

    An instrumentation proposal for dedicated high pressure beam lines at CHESS is described. It is the purpose of this proposed program to provide researchers in high pressure science with beam lines for X-ray diffraction studies in the megabar regime. This will involve radiation from a bending magnet as well as from a wiggler. Examples of the high pressure results up to 2.16 Mbar are shown. Diffraction patterns from bending magnet and wiggler beams are shown and compared. The need for this facility by the high pressure community is discussed. (orig.)

  20. Elastic Wave Velocity Measurements on Mantle Peridotite at High Pressure and Temperature

    Science.gov (United States)

    Mistler, G. W.; Ishikawa, M.; Li, B.

    2002-12-01

    With the success of conducting ultrasonic measurements at high pressure and high temperature in large volume high pressure apparatus with in-situ measurement of the sample length by X-ray imaging, it is now possible to measure elastic wave velocities on aggregate samples with candidate compositions of the mantle to the conditions of the Earth's transition zone in the laboratory. These data can be directly compared with seismic data to distinguish the compositional models in debate. In this work, we carried out velocity measurements on natural peridotite KLB-1 at the conditions of the Earth's upper mantle. Fine powered sample of natural KLB-1 was used as starting material. Specimens for ultrasonic measurements were hot-pressed and equilibrated at various pressure and temperature conditions along geotherm up to the transition zone. The recovered samples were characterized with density measurement, X-ray diffraction and microprobe analysis. Bench top P and S wave velocities of KLB-1 sample sintered at 3-4 GPa and 1400 degree centigrade showed a very good agreement with the VRH average of pyrolite. High pressure and high temperature measurements was conducted up to 7 GPa and 800 degree centigrade using ultrasonic interferometric method in a DIA-type high pressure apparatus in conjunction with X-ray diffraction and X-ray imaging. The utilization of X-ray imaging technique provides direct measurements of sample lengths at high pressure and high temperature, ensuring a precise determination of velocities. The results of P and S wave velocities at high pressure and high temperature as well as their comparison with calculated pyrolite model will be presented.

  1. High-resolution X-ray crystal structure of bovine H-protein using the high-pressure cryocooling method

    International Nuclear Information System (INIS)

    Higashiura, Akifumi; Ohta, Kazunori; Masaki, Mika; Sato, Masaru; Inaka, Koji; Tanaka, Hiroaki; Nakagawa, Atsushi

    2013-01-01

    Using the high-pressure cryocooling method, the high-resolution X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. This is the first ultra-high-resolution structure obtained from a high-pressure cryocooled crystal. Recently, many technical improvements in macromolecular X-ray crystallography have increased the number of structures deposited in the Protein Data Bank and improved the resolution limit of protein structures. Almost all high-resolution structures have been determined using a synchrotron radiation source in conjunction with cryocooling techniques, which are required in order to minimize radiation damage. However, optimization of cryoprotectant conditions is a time-consuming and difficult step. To overcome this problem, the high-pressure cryocooling method was developed (Kim et al., 2005 ▶) and successfully applied to many protein-structure analyses. In this report, using the high-pressure cryocooling method, the X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. Structural comparisons between high- and ambient-pressure cryocooled crystals at ultra-high resolution illustrate the versatility of this technique. This is the first ultra-high-resolution X-ray structure obtained using the high-pressure cryocooling method

  2. Elasticity of stishovite at high pressure

    Science.gov (United States)

    Li, Baosheng; Rigden, Sally M.; Liebermann, Robert C.

    1996-08-01

    The elastic-wave velocities of stishovite, the rutile-structured polymorph of SiO 2, were measured to 3 GPa at room temperature in a piston cylinder apparatus using ultrasonic interferometry on polycrystalline samples. These polycrystalline samples (2-3 mm in length and diameter) were hot-pressed at 14 GPa and 1050°C in a 2000 ton uniaxial split-sphere apparatus (USSA-2000) using fused silica rods as starting material. They were characterized as low porosity (less than 1%), single phase, fine grained, free of cracks and preferred orientation, and acoustically isotropic by using density measurement, X-ray diffraction, scanning electron microscopy, and bench-top velocity measurements. On the basis of subsequent in situ X-ray diffraction study at high P and T on peak broadening on similar specimens, it is evident that the single crystal grains within these polycrystalline aggregates are well equilibrated and that these specimens are free of residual strain. P- and S-wave velocities measured at 1 atm are within 1.5% of the Hashin-Shtrikman bounds calculated from single-crystal elastic moduli. Measured pressure derivatives of the bulk and shear moduli, K' 0 = 5.3 ± 0.1 and G' 0 = 1.8 ± 0.1, are not unusual compared with values measured for other transition zone phases such as silicate spinel and majorite garnet. Isothermal compression curves calculated with the measured values of K0 and K' 0 agree well with experimental P-V data to 16 GPa. The experimental value of dG /dP is in excellent agreement with predictions based on elasticity systematics. Theoretical models are not yet able to replicate the measured values of K' 0 and G' 0.

  3. Anomalous perovskite PbRuO3 stabilized under high pressure

    Science.gov (United States)

    Cheng, J.-G.; Kweon, K. E.; Zhou, J.-S.; Alonso, J. A.; Kong, P.-P.; Liu, Y.; Jin, Changqing; Wu, Junjie; Lin, Jung-Fu; Larregola, S. A.; Yang, Wenge; Shen, Guoyin; MacDonald, A. H.; Manthiram, Arumugam; Hwang, G. S.; Goodenough, John B.

    2013-01-01

    Perovskite oxides ABO3 are important materials used as components in electronic devices. The highly compact crystal structure consists of a framework of corner-shared BO6 octahedra enclosing the A-site cations. Because of these structural features, forming a strong bond between A and B cations is highly unlikely and has not been reported in the literature. Here we report a pressure-induced first-order transition in PbRuO3 from a common orthorhombic phase (Pbnm) to an orthorhombic phase (Pbn21) at 32 GPa by using synchrotron X-ray diffraction. This transition has been further verified with resistivity measurements and Raman spectra under high pressure. In contrast to most well-studied perovskites under high pressure, the Pbn21 phase of PbRuO3 stabilized at high pressure is a polar perovskite. More interestingly, the Pbn21 phase has the most distorted octahedra and a shortest Pb—Ru bond length relative to the average Pb—Ru bond length that has ever been reported in a perovskite structure. We have also simulated the behavior of the PbRuO3 perovskite under high pressure by first principles calculations. The calculated critical pressure for the phase transition and evolution of lattice parameters under pressure match the experimental results quantitatively. Our calculations also reveal that the hybridization between a Ru:t2g orbital and an sp hybrid on Pb increases dramatically in the Pbnm phase under pressure. This pressure-induced change destabilizes the Pbnm phase to give a phase transition to the Pbn21 phase where electrons in the overlapping orbitals form bonding and antibonding states along the shortest Ru—Pb direction at P > Pc. PMID:24277807

  4. Advances in high pressure science and technology: proceedings of the fourth national conference on high pressure science and technology

    International Nuclear Information System (INIS)

    Yousuf, Mohammad; Subramanian, N.; Govinda Rajan, K.

    1997-09-01

    The proceedings of the fourth National Conference on High Pressure Science and Technology covers a wide area of research and development activities in the field of high pressure science and technology, broadly classified into the following themes: mechanical behaviour of materials; instrumentation and methods in high pressure research; pressure calibration, standards and safety aspects; phase transitions; shock induced reactions; mineral science, geophysics, geochemistry and planetary sciences; optical, electronic and transport properties; synthesis of materials; soft condensed matter physics and liquid crystals; computational methods in high pressure research. Papers relevant to INIS are indexed separately

  5. The World of Synchrotrons

    Indian Academy of Sciences (India)

    de Ciencias Fisicas,. Universidad Nacional. Autonoma de Mexico. Sameen Ahmed Khan. A summary of results on synchrotron radiation is presented along with notes on its properties and applications. Quantum aspects are briefly mentioned. Synchrotron radiation facilities are described briefly with a detailed coverage of ...

  6. Synchrotron radiation sources

    Energy Technology Data Exchange (ETDEWEB)

    van Steenbergen, A.

    1979-01-01

    As a result of the exponential growth of the utilization of synchrotron radiation for research in the domain of the material sciences, atomic and molecular physics, biology and technology, a major construction activity has been generated towards new dedicated electron storage rings, designed optimally for synchrotron radiation applications, also, expansion programs are underway at the existing facilities, such as DORIS, SPEAR, and VEPP. In this report the basic properties of synchrotron radiation will be discussed, a short overview will be given of the existing and new facilities, some aspects of the optimization of a structure for a synchrotron radiation source will be discussed and the addition of wigglers and undulators for spectrum enhancement will be described. Finally, some parameters of an optimized synchrotron radiation source will be given.

  7. Synchrotron radiation from protons

    International Nuclear Information System (INIS)

    Dutt, S.K.

    1992-12-01

    Synchrotron radiation from protons, though described by the same equations as the radiation from electrons, exhibits a number of interesting features on account of the parameters reached in praxis. In this presentation, we shall point out some of the features relating to (i) normal synchrotron radiation from dipoles in proton machines such as the High Energy Booster and the Superconducting Super Collider; (ii) synchrotron radiation from short dipoles, and its application to light monitors for proton machines, and (iii) synchrotron radiation from undulators in the limit when, the deflection parameter is much smaller than unity. The material for this presentation is taken largely from the work of Hofmann, Coisson, Bossart, and their collaborators, and from a paper by Kim. We shall emphasize the qualitative aspects of synchrotron radiation in the cases mentioned above, making, when possible, simple arguments for estimating the spectral and angular properties of the radiation. Detailed analyses can be found in the literature

  8. Ionic conduction in sodium azide under high pressure: Experimental and theoretical approaches

    Science.gov (United States)

    Wang, Qinglin; Ma, Yanzhang; Sang, Dandan; Wang, Xiaoli; Liu, Cailong; Hu, Haiquan; Wang, Wenjun; Zhang, Bingyuan; Fan, Quli; Han, Yonghao; Gao, Chunxiao

    2018-04-01

    Alkali metal azides can be used as starting materials for the synthesis of polymeric nitrogen, a potential material of high energy density. In this letter, we report the ionic transport behavior in sodium azide under high pressure by in situ impedance spectroscopy and density functional theory calculations. The ionic transportation consists of ion transfer and Warburg diffusion processes. The ionic migration channels and barrier energy were given for the high-pressure phases. The enhanced ionic conductivity of the γ phase with pressure is because of the formation of space charge regions in the grain boundaries. This ionic conduction and grain boundary effect in NaN3 under pressures could shed light on the better understanding of the conduction mechanism of alkali azides and open up an area of research for polymeric nitrogen in these compounds and other high-energy-density polynitrides.

  9. Principles and application of high pressure-based technologies in the food industry.

    Science.gov (United States)

    Balasubramaniam, V M Bala; Martínez-Monteagudo, Sergio I; Gupta, Rockendra

    2015-01-01

    High pressure processing (HPP) has emerged as a commercially viable food manufacturing tool that satisfies consumers' demand for mildly processed, convenient, fresh-tasting foods with minimal to no preservatives. Pressure treatment, with or without heat, inactivates pathogenic and spoilage bacteria, yeast, mold, viruses, and also spores and extends shelf life. Pressure treatment at ambient or chilled temperatures has minimal impact on product chemistry. The product quality and shelf life are often influenced more by storage conditions and packaging material barrier properties than the treatment itself. Application of pressure reduces the thermal exposure of the food during processing, thereby protecting a variety of bioactive compounds. This review discusses recent scientific advances of high pressure technology for food processing and preservation applications such as pasteurization, sterilization, blanching, freezing, and thawing. We highlight the importance of in situ engineering and thermodynamic properties of food and packaging materials in process design. Current and potential future promising applications of pressure technology are summarized.

  10. Energy dispersive X-ray diffraction at high pressure in CHESS

    International Nuclear Information System (INIS)

    Ruoff, A.L.; Baublitz, M.A. Jr.

    1981-01-01

    Energy dispersive X-ray techniques were used with a diamond anvil cell in the Cornell High Energy Synchrotron Source (CHESS). It was shown that quantitative relative intensity measurement could be made when the pressure was hydrostatic and the crystals were relatively defect free. The crystal structures of the high pressure polymorphs of Ge, GaAs, GaP, and AlSb were studied. Ge exhibits the β-tetragonal structure as found by Jamieson; however, the transition pressure is 80 +- 5 kbars. GaAs exhibits an orthorhombic structure above 172 +- 7 kbars, GaP the β-Sn structure above 215 +- 8 kbars, and AlSb an orthorhombic structure above 77 +- 5 kbars. (Auth.)

  11. Phase stability of TiH{sub 2} under high pressure and temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Selva Vennila, R.; Durygin, A.; Saxena, S.K. [Center for Study of Matter at Extreme Conditions (CeSMEC), Florida International University, VH-150, University Park, Miami, FL 33199 (United States); Merlini, Marco [European Synchrotron Radiation Facility (ESRF), Grenoble 38043 (France); Wang, Zhongwu [Cornell High Energy Synchrotron Source (CHESS), Wilson Laboratory, Cornell University, Ithaca, NY 14853 (United States)

    2008-11-15

    Phase stability of titanium hydride (TiH{sub 2}) was studied at high pressure-high temperature conditions using synchrotron radiation under non-hydrostatic conditions. Resistive heating method was used to heat the sample to a maximum temperature of 873 K in a diamond anvil cell (DAC) under pressure up to 12 GPa. Pressure-temperature behavior was studied by varying the temperature upto 823 K in steps of 50 K with pressure variations within 3 GPa. Structural phase transformation from tetragonal (I4/mmm) to cubic (Fm-3 m) was observed with increase in temperature. Tetragonal phase was found to be stabilized when the sample was subjected to pressure and temperature cycle. (author)

  12. Hardness of high-pressure high-temperature treated single-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Kawasaki, S.; Nojima, Y.; Yokomae, T.; Okino, F.; Touhara, H.

    2007-01-01

    We have performed high-pressure high-temperature (HPHT) treatments of high quality single-walled carbon nanotubes (SWCNTs) over a wide pressure-temperature range up to 13 GPa-873 K and have investigated the hardness of the HPHT-treated SWCNTs using a nanoindentation technique. It was found that the hardness of the SWCNTs treated at pressures greater than 11 GPa and at temperatures higher than 773 K is about 10 times greater than that of the SWCNTs treated at low temperature. It was also found that the hardness change of the SWCNTs is related to the structural change by the HPHT treatments which was based on synchrotron X-ray diffraction measurements

  13. Compressibility of the high-pressure rocksalt phase of ZnO

    DEFF Research Database (Denmark)

    Recio, J.M.; Blanco, M.A.; Luana, V.

    1998-01-01

    We report the results of a combined experimental and theoretical investigation on the stability and the volume behavior under hydrostatic pressure of the rocksalt (B1) phase of ZnO. Synchrotron-radiation x-ray powder-diffraction data are obtained from 0 to 30 GPa. Static simulations of the ZnO B1...... phase are performed using the ab initio perturbed ion method and the local and nonlocal approximations to the density-functional theory. After the pressure induced transition from the wurtzite phase, we have found that a large fraction of the B1 high-pressure phase is retained when pressure is released....... The metastability of this ZnO polymorph is confirmed through the theoretical evaluation of the Hessian eigenvalues of a nine-parameter potential energy surface. This allows us to treat the experimental and theoretical pressure-volume data on an equal basis. In both cases, we have obtained values of the bulk modulus...

  14. Chemistry with synchrotron radiation

    International Nuclear Information System (INIS)

    Preses, J.; Grover, J.R.; White, M.G.; Kvick, A.

    1990-01-01

    An accidental by-product of high-energy physics, synchrotron radiation, has emerged as one of the most powerful tools for the understanding of chemical reactions. Advances made by using synchrotron radiation in physical chemistry are reviewed herein. Descriptions of experiments exploiting the many ways that synchrotron radiation can be manipulated are presented. These manipulations include intensification of the radiation and compression or shifting of its spectral structure. Combinations of the use of synchrotron radiation, which provides access to very short wavelengths and is, at the same time, continuously and easily tunable, with laser radiation, which offers much higher resolution and much more intense radiation per pulse, but is difficult to tune in the ultraviolet region of the spectra, gives the chemist a way to map a molecule's potential energy curve, to note the lengths and strengths of chemical bonds, and to predict and explain novel reactions of more complex molecules. The use of diffraction of x-rays to study the spacing of atoms in crystals is discussed. Various applications of synchrotron radiation to studies of the fluorescence of hydrocarbons and to the chiral dichroism studies of other natural products like DNA and RNA are described. Methods for enhancing synchrotron light sources by insertion devices, such as wigglers and undulators, that increase the available photo flux and construction of new sources of synchrotron radiation are mentioned

  15. Safety analysis of high pressure gasous fuel container punctures

    Energy Technology Data Exchange (ETDEWEB)

    Swain, M.R. [Univ. of Miami, Coral Gables, FL (United States)

    1995-09-01

    The following report is divided into two sections. The first section describes the results of ignitability tests of high pressure hydrogen and natural gas leaks. The volume of ignitable gases formed by leaking hydrogen or natural gas were measured. Leaking high pressure hydrogen produced a cone of ignitable gases with 28{degrees} included angle. Leaking high pressure methane produced a cone of ignitable gases with 20{degrees} included angle. Ignition of hydrogen produced larger overpressures than did natural gas. The largest overpressures produced by hydrogen were the same as overpressures produced by inflating a 11 inch child`s balloon until it burst.

  16. Safety supervision on high-pressure gas regulations

    International Nuclear Information System (INIS)

    Lee, Won Il

    1991-01-01

    The first part lists the regulation on safety supervision of high-pressure gas, enforcement ordinance on high-pressure gas safety supervision and enforcement regulations about high-pressure gas safety supervision. The second part indicates safety regulations on liquefied petroleum gas and business, enforcement ordinance of safety on liquefied petroleum gas and business, enforcement regulation of safety supervision over liquefied petroleum gas and business. The third part lists regulation on gas business, enforcement ordinance and enforcement regulations on gas business. Each part has theory and explanation for questions.

  17. Synchrotron radiation at Trieste

    Energy Technology Data Exchange (ETDEWEB)

    Anon.

    1986-06-15

    The fast developing field of synchrotron radiation has its origins in the mastery of storage rings in high energy physics and is a prime example of spinoff from pure science. Intense electromagnetic radiation streams off when beams of high energy electrons are bent or shaken. This synchrotron radiation was once an annoying waste of energy in particle storage rings, but now the wheel has turned full circle, with dedicated machines supplying this radiation for a wide range of science. The astonishing growth rate in this field was highlighted at an International Conference on Synchrotron Radiation, held at the International Centre for Theoretical Physics (ICTP), Trieste, Italy from 7-11 April.

  18. National Synchrotron Light Source

    International Nuclear Information System (INIS)

    van Steenbergen, A.

    1979-01-01

    The National Synchrotron Light Source comprises two high intensity electron storage rings for the generation of intense fluxes of synchrotron radiation in the vuv wavelength domain (700 MeV e - ring) and in the x-ray wavelength domain (2.5 GeV e - ring). A description is presented of the basic facility and the characteristics of the synchrotron radiation sources. The present plans for specific beam lines will be enumerated and the planned use of beam wigglers and undulators will be discussed

  19. Synchrotron radiation at Trieste

    International Nuclear Information System (INIS)

    Anon.

    1986-01-01

    The fast developing field of synchrotron radiation has its origins in the mastery of storage rings in high energy physics and is a prime example of spinoff from pure science. Intense electromagnetic radiation streams off when beams of high energy electrons are bent or shaken. This synchrotron radiation was once an annoying waste of energy in particle storage rings, but now the wheel has turned full circle, with dedicated machines supplying this radiation for a wide range of science. The astonishing growth rate in this field was highlighted at an International Conference on Synchrotron Radiation, held at the International Centre for Theoretical Physics (ICTP), Trieste, Italy from 7-11 April

  20. High pressure antiferrodistortive phase transition in mixed crystals of EuTiO{sub 3} and SrTiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Parisiades, Paraskevas, E-mail: paraskevas.parisiadis@univ-paris-diderot.fr [Laboratoire Matériaux et Phénoménes Quantiques (UMR 7162 CNRS), Université Paris Diderot-Paris 7, Paris Cedex 13 (France); ID27 Beamline, European Synchrotron Radiation Facility, 71 Avenue des Martyrs, 38000 Grenoble (France); Saltarelli, Francesco [Sapienza University of Rome, Physics Dept., Piazzale Aldo Moro 5, 00185 Roma (Italy); Liarokapis, Efthymios [Department of Physics, National Technical University of Athens, GR-15780 Athens (Greece); Köhler, Jürgen; Bussmann-Holder, Annette [Max-Planck-Institute for Solid State Research, Heisenbergstrasse 1, D-70569 Stuttgart (Germany)

    2016-06-15

    We report a detailed high pressure study on Eu{sub 1−x}Sr{sub x}TiO{sub 3} polycrystalline samples using synchrotron x-ray diffraction. We have observed a second-order antiferrodistortive phase transition for all doping levels which corresponds to the transition that has been previously explored as a function of temperature. The analysis of the compression mechanism by calculating the lattice parameters, spontaneous strains and tilt angles of the TiO{sub 6} octahedra leads to a high pressure phase diagram for Eu{sub 1−x}Sr{sub x}TiO{sub 3}.

  1. High-pressure, high-temperature magic angle spinning nuclear magnetic resonance devices and processes for making and using same

    Science.gov (United States)

    Hu, Jian Zhi; Hu, Mary Y.; Townsend, Mark R.; Lercher, Johannes A.; Peden, Charles H. F.

    2015-10-06

    Re-usable ceramic magic angle spinning (MAS) NMR rotors constructed of high-mechanic strength ceramics are detailed that include a sample compartment that maintains high pressures up to at least about 200 atmospheres (atm) and high temperatures up to about least about 300.degree. C. during operation. The rotor designs minimize pressure losses stemming from penetration over an extended period of time. The present invention makes possible a variety of in-situ high pressure, high temperature MAS NMR experiments not previously achieved in the prior art.

  2. High-pressure phase transition of alkali metal-transition metal deuteride Li2PdD2

    Science.gov (United States)

    Yao, Yansun; Stavrou, Elissaios; Goncharov, Alexander F.; Majumdar, Arnab; Wang, Hui; Prakapenka, Vitali B.; Epshteyn, Albert; Purdy, Andrew P.

    2017-06-01

    A combined theoretical and experimental study of lithium palladium deuteride (Li2PdD2) subjected to pressures up to 50 GPa reveals one structural phase transition near 10 GPa, detected by synchrotron powder x-ray diffraction, and metadynamics simulations. The ambient-pressure tetragonal phase of Li2PdD2 transforms into a monoclinic C2/m phase that is distinct from all known structures of alkali metal-transition metal hydrides/deuterides. The structure of the high-pressure phase was characterized using ab initio computational techniques and from refinement of the powder x-ray diffraction data. In the high-pressure phase, the PdD2 complexes lose molecular integrity and are fused to extended [PdD2]∞ chains. The discovered phase transition and new structure are relevant to the possible hydrogen storage application of Li2PdD2 and alkali metal-transition metal hydrides in general.

  3. Electron spin transition causing structure transformations of earth's interiors under high pressure

    Science.gov (United States)

    Yamanaka, T.; Kyono, A.; Kharlamova, S.; Alp, E.; Bi, W.; Mao, H.

    2012-12-01

    To elucidate the correlation between structure transitions and spin state is one of the crucial problems for understanding the geophysical properties of earth interiors under high pressure. High-pressure studies of iron bearing spinels attract extensive attention in order to understand strong electronic correlation such as the charge transfer, electron hopping, electron high-low spin transition, Jahn-Teller distortion and charge disproponation in the lower mantle or subduction zone [1]. Experiment Structure transitions of Fe3-xSixO4, Fe3-xTixO4 Fe3-xCrxO4 spinel solid solution have been investigated at high pressure up to 60 GPa by single crystal and powder diffraction studies using synchrotron radiation with diamond anvil cell. X-ray emission experiment (XES) at high pressure proved the spin transition of Fe-Kβ from high spin (HS) to intermediate spin state (IS) or low spin state (LS). Mössbauer experiment and Raman spectra study have been also conducted for deformation analysis of Fe site and confirmation of the configuration change of Fe atoms. Jahn-Teller effect A cubic-to-tetragonal transition under pressure was induced by Jahn-Teller effect of IVFe2+ (3d6) in the tetrahedral site of Fe2TiO4 and FeCr2O4, providing the transformation from 43m (Td) to 42m (D2d). Tetragonal phase is formed by the degeneracy of e orbital of Fe2+ ion. Their c/a ratios are c/adisordered in the M2 site. At pressures above 53 GPa, Fe2TiO4 structure further transforms to Pmma. This structure change results in the order-disorder transition [2]. New structure of Fe2SiO4 The spin transition exerts an influence to Fe2SiO4 spinel structure and triggers two distinct curves of the lattice constant in the spinel phase. The reversible structure transition from cubic to pseudo-rhombohedral phase was observed at about 45 GPa. This transition is induced by the 20% shrinkage of ionic radius of VIFe2+at the low sin state. Laser heating experiment at 1500 K has confirmed the decomposition from the

  4. Spin crossover and Mott—Hubbard transition under high pressure and high temperature in the low mantle of the Earth

    Science.gov (United States)

    Ovchinnikov, S. G.; Ovchinnikova, T. M.; Plotkin, V. V.; Dyad'kov, P. G.

    2015-11-01

    Effect of high pressure induced spin crossover on the magnetic, electronic and structural properties of the minerals forming the Earth's low mantle is discussed. The low temperature P, T phase diagram of ferropericlase has the quantum phase transition point Pc = 56 GPa at T = 0 confirmed recently by the synchrotron Mössbauer spectroscopy. The LDA+GTB calculated phase diagram describes the experimental data. Its extension to the high temperature resulted earlier in prediction of the metallic properties of the Earth's mantle at the depth 1400 km insulator transition and compare them with the experimental seismic and geomagnetic field data.

  5. X-ray diffraction study of WO3 at high pressure

    International Nuclear Information System (INIS)

    Bouvier, P.; Crichton, W.A.; Boulova, M.; Lucazeau, G.

    2002-01-01

    The high-pressure behaviour of microcrystalline tungsten oxide (WO 3 ) has been investigated with angle-dispersive synchrotron x-ray powder diffraction in a diamond anvil cell up to 40 GPa at room temperature. Up to 21 GPa, the pressure dependence of the volume of the monoclinic high-pressure (P2 1 /c) phase is described by a third-order Birch-Murnaghan equation of state with parameters V 0 =210.9(7)A 3 , K T =27(2)GP a and K'=9.4(5). At 24 GPa, a first-order phase transition occurs with an approximate Δ V of 7.4% to a monoclinic P2 1 /a unit cell with a=6.1669(8)A, b=4.5758(6)A, c=5.3159(6)A, β=101.440(9) deg. A second transition is observed at pressures higher than 31 GPa with an approximate Δ V of 12% to a phase described by a third monoclinic unit cell, with a=10.3633(22)A, b=3.9065(8)A, c=9.3459(18)A and β=98.539(14) deg. (author)

  6. X-ray diffraction study of WO{sub 3} at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Bouvier, P. [ESRF, Grenoble (France); Laboratoire d' Electrochimie et de Physico-Chimie des Materiaux et des Interfaces UMR 5631 CNRS-INPG, St. Martin d' Heres (France); Crichton, W.A. [ESRF, Grenoble (France); Boulova, M. [Laboratoire d' Electrochimie et de Physico-Chimie des Materiaux et des Interfaces UMR 5631 CNRS-INPG, St. Martin d' Heres (France); Chemistry Department, Moscow State University, Moscow (Russian Federation); Lucazeau, G. [Laboratoire d' Electrochimie et de Physico-Chimie des Materiaux et des Interfaces UMR 5631 CNRS-INPG, St. Martin d' Heres (France)

    2002-07-08

    The high-pressure behaviour of microcrystalline tungsten oxide (WO{sub 3}) has been investigated with angle-dispersive synchrotron x-ray powder diffraction in a diamond anvil cell up to 40 GPa at room temperature. Up to 21 GPa, the pressure dependence of the volume of the monoclinic high-pressure (P2{sub 1}/c) phase is described by a third-order Birch-Murnaghan equation of state with parameters V{sub 0}=210.9(7)A{sup 3}, K{sub T}=27(2)GP a and K'=9.4(5). At 24 GPa, a first-order phase transition occurs with an approximate {delta} V of 7.4% to a monoclinic P2{sub 1}/a unit cell with a=6.1669(8)A, b=4.5758(6)A, c=5.3159(6)A, {beta}=101.440(9) deg. A second transition is observed at pressures higher than 31 GPa with an approximate {delta} V of 12% to a phase described by a third monoclinic unit cell, with a=10.3633(22)A, b=3.9065(8)A, c=9.3459(18)A and {beta}=98.539(14) deg. (author)

  7. A high pressure x-ray diffraction study of titanium disulfide

    International Nuclear Information System (INIS)

    Aksoy, Resul; Selvi, Emre; Knudson, Russell; Ma Yanzhang

    2009-01-01

    A high pressure angle dispersive synchrotron x-ray diffraction study of titanium disulfide (TiS 2 ) was carried out to pressures of 45.5 GPa in a diamond-anvil cell. We observed a phase transformation of TiS 2 beginning at about 20.7 GPa. The structure of the high pressure phase needs further identification. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus, K 0T , was determined to be 45.9 ± 0.7 GPa with its pressure derivative, K' 0T , being 9.5 ± 0.3 at pressures lower than 17.8 GPa. It was found that the compression behavior of TiS 2 is anisotropic along the different axes. The compression ratio of the c-axis is about nine times larger than the a-axis when pressures are lower than 1 GPa. It suddenly decreases to three times larger at pressures of about 3 GPa. This ratio shows a linear decrease with a slope of negative 0.048 at pressures below phase transformation.

  8. High pressure processing reaches the U.S. market

    International Nuclear Information System (INIS)

    Mermelstein, N.H.

    1997-01-01

    The first food product commercially produced by a U.S. company using high-pressure processing has had successful test market results. High-pressure processing permits food to be preserved by subjecting it to pressures in the range of 60,000-100,000 psi for a short time instead of exposing the food to heat, freezing, chemicals, or irradiation. To produce Classic Guacamole, Avomex of Keller, Texas, uses a batch isostatic press to deactivate the enzymes in the avocado and to kill bacteria, obtaining a refrigerated shelf life of over 30 days. The guacamole is then vacuum packed and processed again. The product undergoes no heat treatment and does not contain preservatives, and the high pressure does not affect its texture, color, or taste. Meanwhile, a continuous system for high-pressure processing of pumpable foods is currently being developed by Flow International of Kent, Washington, and will be used for testing and applications work at Oregon State University

  9. Baking and coking properties of hard coal under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Beyer, H.D.

    1981-09-01

    For a better assessment of the baking and coking properties of hard coal under high pressure as in modern coal beneficiation processes, the determination of the swelling index and the dilatation curve are investigated.

  10. High pressure orthorhombic structure of CuInSe2

    International Nuclear Information System (INIS)

    Bovornratanaraks, T; Saengsuwan, V; Yoodee, K; McMahon, M I; Hejny, C; Ruffolo, D

    2010-01-01

    The structural behaviour of CuInSe 2 under high pressure has been studied up to 53 GPa using angle-dispersive x-ray powder diffraction techniques. The previously reported structural phase transition from its ambient pressure tetragonal structure to a high pressure phase with a NaCl-like cubic structure at 7.6 GPa has been confirmed. On further compression, another structural phase transition is observed at 39 GPa. A full structural study of this high pressure phase has been carried out and the high pressure structure has been identified as orthorhombic with space group Cmcm and lattice parameters a = 4.867(8) A, b = 5.023(8) A and c = 4.980(3) A at 53.2(2) GPa. This phase transition behaviour is similar to those of analogous binary and trinary semiconductors, where the orthorhombic Cmcm structure can also be viewed as a distortion of the cubic NaCl-type structure.

  11. The high pressure gas Cerenkov counter at the Omega Facility.

    CERN Multimedia

    1975-01-01

    The high-pressure gas Cerenkov was used to measure reactions as pion (or kaon)- hydrogen --> forward proton - X. It was built by the Ecole Polytechnique (Palaiseu). Here Peter Sonderegger and Patrick Fleury,

  12. Bio-Hemostat-Acute Treatment Modality for High Pressure Hemorrhage

    National Research Council Canada - National Science Library

    Carr, Marcus

    2002-01-01

    Bleeding from an artery is difficult to control due to the high pressures found in the arterial system Hemorrhage is especially problematic in penetrating wounds where the bleeding source may not be...

  13. Applicable technical method for freeze-substitution of high pressure ...

    African Journals Online (AJOL)

    bmshsj

    2011-11-02

    Quintana, 1994) are available for the microscopic visualization of intracellular organelles. Cryo- fixation, plunge freezing, propane jet freezing, cold metal block freezing, and high pressure freezing provide advantages over chemical ...

  14. Beam steering effects in turbulent high pressure flames

    Energy Technology Data Exchange (ETDEWEB)

    Hemmerling, B; Kaeppeli, B [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-06-01

    The propagation of a laser beam through a flame is influenced by variations of the optical density. Especially in turbulent high pressure flames this may seriously limit the use of laser diagnostic methods. (author) 1 fig., 2 refs.

  15. High Pressure Electrochemical Oxygen Generation for ISS, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Giner, Inc. has developed an advanced high pressure electrochemical oxygen concentrator (EOC) that offers a simple alternative to the use of pressure swing...

  16. National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Hulbert, S.L.; Lazarz, N.M.

    1991-04-01

    This report discussion research being conducted at the National Synchrotron light source. In particular, this report contains operations summaries; symposia, workshops, and projects; NSLS highlights; and abstracts of science at the NSLS

  17. Uses of synchrotron radiation

    International Nuclear Information System (INIS)

    Gordon, B.M.

    1982-01-01

    X-ray fluorescence has long been used as a technique for elemental analysis. X-ray fluorescence techniques have a number of features that make them attractive for application to biomedical samples. In the past few years synchrotron radiation x-ray sources have been developed and, because of their properties, their use can improve the sensitivity for trace element analysis by two to three orders of magnitude. Also, synchrotron radiation will make possible an x-ray microprobe with resolution in the micrometer range. The National Synchrotron Light Source (NSLS), a dedicated synchrotron radiation source recently built at Brookhaven National Laboratory, will have a facility for trace element analysis by x-ray fluorescence and will be available to all interested users

  18. The Australian synchrotron

    International Nuclear Information System (INIS)

    Farhi, R.

    2005-06-01

    This document recalls the historical aspects of the Australian Synchrotron which will be implemented in 2007. It presents then the objectives of this program, the specifications of the ring and the light lines. (A.L.B.)

  19. Inauguration of Proton Synchrotron

    CERN Multimedia

    1960-01-01

    On 5 February 1960, the Proton Synchrotron (PS) was formally inaugurated. The great Danish physicist, Niels Bohr, releases a bottle of champagne against a shielding block to launch the PS on its voyage in physics.

  20. Model of Structural Fragmentation Induced by High Pressure Torsion

    Czech Academy of Sciences Publication Activity Database

    Kratochvíl, J.; Kružík, Martin; Sedláček, R.

    2010-01-01

    Roč. 25, č. 1 (2010), s. 88-98 ISSN 1606-5131 Institutional research plan: CEZ:AV0Z10750506 Keywords : High-pressure torsion * intergranular glide * homogeneous deformation mode Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.649, year: 2010 http://library.utia.cas.cz/separaty/2010/MTR/kruzik-model of structural fragmentation induced by high pressure torsion.pdf

  1. Thermal neutron scattering studies of condensed matter under high pressures

    International Nuclear Information System (INIS)

    Carlile, C.J.; Salter, D.C.

    1978-01-01

    Although temperature has been used as a thermodynamic variable for samples in thermal neutron scattering experiments since the inception of the neutron technique, it is only in the last decade that high pressures have been utilised for this purpose. In the paper the problems particular to this field of work are outlined and a review is made of the types of high-pressure cells used and the scientific results obtained from the experiments. 103 references. (author)

  2. Practical conditions in the neutron diffraction under high pressure

    International Nuclear Information System (INIS)

    Kamigaki, Kazuo; Ohashi, Masayoshi

    1993-01-01

    Practical analysis is made on some conditions in utilizing neutrons for the study of atomistic structure of materials under high pressure. Investigation is made on the geometrical conditions; size of the specimen, width of slits, and the rate of extra-scattering. Experiments are performed on the effects of absorption by high pressure cell and the disturbance due to an overlapping of diffraction peaks. An observation is presented on the pressure-induced transformation in RbBr. (author)

  3. High pressure discharges in cavities formed by microfabrication techniques

    International Nuclear Information System (INIS)

    Khan, B.A.; Cammack, D.A.; Pinker, R.D.; Racz, J.

    1997-01-01

    High pressure discharges are the basis of small high intensity light sources. In this work, we demonstrate the formation of high pressure discharges, in cavities formed by applying micromachining and integrated circuit techniques to quartz substrates. Cavities containing varying amounts of mercury and argon were fabricated to obtain high pressure discharges. A high pressure mercury discharge was formed in the electrodeless cavities by exciting them with a microwave source, operating at 2.45 GHz and in the electroded cavities by applying a dc voltage. The contraction of the discharge into a high pressure arc was observed. A broad emission spectrum due to self-absorption and collisions between excited atoms and normal atoms, typical of high pressure mercury discharges, was measured. The light output and efficacy increased with increasing pressure. The measured voltage was used to estimate the pressure within the electroded cavities, which is as high as 127 atm for one of the two cavities discussed in this work. Efficacies over 40 lumens per watt were obtained for the electrodeless cavities and over 50 scr(l)m/W for the electroded cavities. copyright 1997 American Institute of Physics

  4. High pressure study of a highly energetic nitrogen-rich carbon nitride, cyanuric triazide

    Energy Technology Data Exchange (ETDEWEB)

    Laniel, Dominique; Desgreniers, Serge [Laboratoire de physique des solides denses, University of Ottawa, Ottawa, Ontario K1N 6N5 (Canada); Downie, Laura E. [Department of Physics and Atmospheric Science, Dalhousie University, Halifax, Nova Scotia B3H 4R2 (Canada); Smith, Jesse S. [High Pressure Collaborative Access Team, Carnegie Institution of Washington, Argonne, Illinois 60439 (United States); Savard, Didier; Murugesu, Muralee [Department of Chemistry, University of Ottawa, Ottawa, Ontario K1N 6N5 (Canada)

    2014-12-21

    Cyanuric triazide (CTA), a nitrogen-rich energetic material, was compressed in a diamond anvil cell up to 63.2 GPa. Samples were characterized by x-ray diffraction, Raman, and infrared spectroscopy. A phase transition occurring between 29.8 and 30.7 GPa was found by all three techniques. The bulk modulus and its pressure derivative of the low pressure phase were determined by fitting the 300 K isothermal compression data to the Birch-Murnaghan equation of state. Due to the strong photosensitivity of CTA, synchrotron generated x-rays and visible laser radiation both lead to the progressive conversion of CTA into a two dimensional amorphous C=N network, starting from 9.2 GPa. As a result of the conversion, increasingly weak and broad x-ray diffraction lines were recorded from crystalline CTA as a function of pressure. Hence, a definite structure could not be obtained for the high pressure phase of CTA. Results from infrared spectroscopy carried out to 40.5 GPa suggest the high pressure formation of a lattice built of tri-tetrazole molecular units. The decompression study showed stability of the high pressure phase down to 13.9 GPa. Finally, two CTA samples, one loaded with neon and the other with nitrogen, used as pressure transmitting media, were laser-heated to approximately 1100 K and 1500 K while compressed at 37.7 GPa and 42.0 GPa, respectively. In both cases CTA decomposed resulting in amorphous compounds, as recovered at ambient conditions.

  5. Phase transformations in cerium and thorium metals at ultra high pressures

    International Nuclear Information System (INIS)

    Vohra, Y.K.

    1991-01-01

    This paper reports on the role of pressure variable in phase transformation which has not been fully exploited in metallic elements and their alloys. The static compression of over 50% in volume can readily be obtained in most metals and this tremendous change in inter-atomic distances can lead to the formation of new exotic crystal structures. The pressure-induced electron transfer amongst existing electronic energy bands and the occupation of new bands are the driving forces in a rich variety of phase transformations. The modern high pressure diamond anvil cell techniques can produce calibrated static pressures of over 300 to 400 GPa range and this technology, when interfaced with the synchrotron radiation sources, can yield rapid structural information (1-3). These capabilities have given new impetus for investigation of phase transformations in metallic systems at extreme conditions of temperatures and pressures and in establishing phase boundaries at high pressures and high temperatures. Cerium (Ce) and thorium (Th) metals occupy special positions in the periodic table at the beginning of the 4-f lanthanide and 5-f, actinide series, respectively. Ce has one electron in the localized 4-f shell, apart from the three valence electrons. Th metal, on the other hand, has four valence electrons and an unoccupied 5-f band above the Fermi-energy at ambient conditions. In view of the unoccupied 5-f band, Th metal is normally regarded as a tetravalent transition metal like Ti, Zr, and Hf and its bonding and other electronic properties can be explained within the tetravalent transition metal framework. However, the application of ultra-high pressures causes the delocalization of the 4-f shell in Ce and it is believed that Ce above 0.8 GPa pressure is a 4-f band metal

  6. Novel high pressure hexagonal OsB2 by mechanochemistry

    International Nuclear Information System (INIS)

    Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

    2014-01-01

    Hexagonal OsB 2 , a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB 2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB 2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB 2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from −225 °C to 1050 °C. The hexagonal OsB 2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB 2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods. - Graphical abstract: High resolution transmission electron micrograph of hexagonal OsB 2 nanocrystallite with corresponding fast Fourier transform and simulated diffraction pattern. - Highlights: • Hexagonal OsB 2 has been synthesized for the first time by mechanochemical method. • Hexagonal OsB 2 crystallizes in P63/mmc space group (No. 194), a=2.916 Å and c=7.376 Å. • The hexagonal structure was confirmed by a transmission electron microscope. • No phase transformation was observed after being annealed at 1050 °C for 6 days. • 20 wt% of h-OsB 2 was transformed to o-OsB 2 after being sintered at 1500 °C for 5 min

  7. European Synchrotron Radiation Facility

    International Nuclear Information System (INIS)

    Buras, B.

    1985-01-01

    How a European Synchrotron Radiation Facility has developed into a detailed proposal recently accepted as the basis for construction of the facility at Grenoble is discussed. In November 1977, the General Assembly of the European Science Foundation (ESF) approved the report of the ESF working party on synchrotron radiation entitled Synchrotron Radiation - a Perspective View for Europe. This report contained as one of its principal recommendations that work should commence on a feasibility study for a European synchrotron radiation laboratory having a dedicated hard X-ray storage ring and appropriate advanced instrumentation. In order to prepare a feasibility study the European Science Foundation set up the Ad-hoc Committee on Synchrotron Radiation, which in turn formed two working groups: one for the machine and another for instrumentation. This feasibility study was completed in 1979 with the publication of the Blue Book describing in detail the so called 1979 European Synchrotron Radiation Facility. The heart of the facility was a 5 GeV electron storage ring and it was assumed that mainly the radiation from bending magnets will be used. The facility is described

  8. A multi-probe thermophoretic soot sampling system for high-pressure diffusion flames

    Energy Technology Data Exchange (ETDEWEB)

    Vargas, Alex M.; Gülder, Ömer L. [Institute for Aerospace Studies, University of Toronto, Toronto, Ontario M3H 5T6 (Canada)

    2016-05-15

    Optical diagnostics and physical probing of the soot processes in high pressure combustion pose challenges that are not faced in atmospheric flames. One of the preferred methods of studying soot in atmospheric flames is in situ thermophoretic sampling followed by transmission electron microscopy imaging and analysis for soot sizing and morphology. The application of this method of sampling to high pressures has been held back by various operational and mechanical problems. In this work, we describe a rotating disk multi-probe thermophoretic soot sampling system, driven by a microstepping stepper motor, fitted into a high-pressure chamber capable of producing sooting laminar diffusion flames up to 100 atm. Innovative aspects of the sampling system design include an easy and precise control of the sampling time down to 2.6 ms, avoidance of the drawbacks of the pneumatic drivers used in conventional thermophoretic sampling systems, and the capability to collect ten consecutive samples in a single experimental run. Proof of principle experiments were performed using this system in a laminar diffusion flame of methane, and primary soot diameter distributions at various pressures up to 10 atm were determined. High-speed images of the flame during thermophoretic sampling were recorded to assess the influence of probe intrusion on the flow field of the flame.

  9. Experimental studies on radiation effects under high pressure oxygen

    Energy Technology Data Exchange (ETDEWEB)

    Fujimura, E [Osaka Univ. (Japan). School of Dentistry

    1974-06-01

    The effect of oxygen tension on the radiosensitivity of tumor cells is well known, but its clinical application for radiotherapy is not yet established. Rabbits with V x 2 carcinoma in the maxilla were irradiated by /sup 60/Co under high pressure oxygen (experimental group), and compared with those treated in air (control group). For the purpose of examining the clinical effects of high pressure oxygen, an experiment was made in vivo. The following items were compared respectively: a) Tumor regression effect b) Tumor clearance rate c) Survival days d) Half size reduction time e) Inhibition of DNA synthesis in the tumor tissue. Results obtained were as follows: a) 56 per cent of animals showed tumor regression in the experimental group, whereas it occured 26 per cent in the control group. b) 53 per cent of animals showed tumor disappearance in the experimental group, while it was observed only in 13 per cent in the control group. c) Only 2 of 30 rabbits irradiated in air survived over 180 days, whereas 11 of 30 rabbits survived meanwhile in the group irradiated under high pressure oxygen. d) About 11 days were necessary to reduce the tumor size by half after irradiation in the group under high pressure oxygen, while it took 17 days in the group treated in normal air. e) DNA synthesis was inhibited more prominently in the group irradiated under high pressure oxygen in normal air.

  10. Decomposition of silicon carbide at high pressures and temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Daviau, Kierstin; Lee, Kanani K. M.

    2017-11-01

    We measure the onset of decomposition of silicon carbide, SiC, to silicon and carbon (e.g., diamond) at high pressures and high temperatures in a laser-heated diamond-anvil cell. We identify decomposition through x-ray diffraction and multiwavelength imaging radiometry coupled with electron microscopy analyses on quenched samples. We find that B3 SiC (also known as 3C or zinc blende SiC) decomposes at high pressures and high temperatures, following a phase boundary with a negative slope. The high-pressure decomposition temperatures measured are considerably lower than those at ambient, with our measurements indicating that SiC begins to decompose at ~ 2000 K at 60 GPa as compared to ~ 2800 K at ambient pressure. Once B3 SiC transitions to the high-pressure B1 (rocksalt) structure, we no longer observe decomposition, despite heating to temperatures in excess of ~ 3200 K. The temperature of decomposition and the nature of the decomposition phase boundary appear to be strongly influenced by the pressure-induced phase transitions to higher-density structures in SiC, silicon, and carbon. The decomposition of SiC at high pressure and temperature has implications for the stability of naturally forming moissanite on Earth and in carbon-rich exoplanets.

  11. High pressure apparatus for neutron scattering at low temperature

    International Nuclear Information System (INIS)

    Munakata, Koji; Uwatoko, Yoshiya; Aso, Naofumi

    2010-01-01

    Effects of pressure on the physical properties are very important for understanding highly correlated electron systems, in which pressure-induced attractive phenomena such as superconductivity and magnetically ordered non-Fermi liquid have been observed. Up to now, many scientists have developed a lot of high pressure apparatus for each purpose. The characteristic features of various materials and pressure transmitting media for use of high pressure apparatus are reported. Then, two kinds of clamp type high-pressure cell designed for low-temperature neutron diffraction measurements are shown; one is a piston cylinder type high-pressure cell which can be attached to the dilution refrigerator, and the other one is a newly-developed cubic anvil type high-pressure cell which can generate pressure above 7GPa. We also introduce the results of magnetic neutron scattering under pressure on a pressure-induced superconducting ferromagnet UGe 2 in use of the piston cylinder type clamp cell, and those on an iron arsenide superconductor SrFe 2 As 2 in use of the cubic anvil type clamp cell. (author)

  12. Transportable, small high-pressure preservation vessel for cells

    International Nuclear Information System (INIS)

    Kamimura, N; Sotome, S; Shimizu, A; Nakajima, K; Yoshimura, Y

    2010-01-01

    We have previously reported that the survival rate of astrocytes increases under high-pressure conditions at 4 0 C. However, pressure vessels generally have numerous problems for use in cell preservation and transportation: (1) they cannot be readily separated from the pressurizing pump in the pressurized state; (2) they are typically heavy and expensive due the use of materials such as stainless steel; and (3) it is difficult to regulate pressurization rate with hand pumps. Therefore, we developed a transportable high-pressure system suitable for cell preservation under high-pressure conditions. This high-pressure vessel has the following characteristics: (1) it can be easily separated from the pressurizing pump due to the use of a cock-type stop valve; (2) it is small and compact, is made of PEEK and weighs less than 200 g; and (3) pressurization rate is regulated by an electric pump instead of a hand pump. Using this transportable high-pressure vessel for cell preservation, we found that astrocytes can survive for 4 days at 1.6 MPa and 4 0 C.

  13. Designing high pressure containers for research- principles and applications

    International Nuclear Information System (INIS)

    Anandkumar, V.

    1997-01-01

    The high pressure scientist looks for a well engineered pressure apparatus for high pressure experiments for 1 kbar (0.1 GPa) and above. Often, a variety of difficulties including the choice of materials, design configuration, optimum utilisation of the strength of materials used in the design, are encountered. This article is intended to help the high pressure scientist to select the design approach for pressure retaining container. The limitations imposed by the strength of available materials and engineering standards in building high pressure containers are discussed. Engineering solutions to overcome these limitations with optimal utilisation of the strength of the materials are also discussed. Novel methods to boost up the pressure retaining capacity like multilayered design and autofrettaging are compared along with their relative advantages and disadvantages. Special methods by which it is possible to attain pressures which are several times the yield strength of the materials of construction are presented. In this aspects such as the basis of the codes and their relevance in the design of high pressure equipment will also be described. Discussions are centered around the methods to tackle situations where experimental constraints dictate requirements of pressures higher than those permitted by design codes. Safety features are also discussed. (author)

  14. Future Synchrotron Radiation Sources

    CERN Document Server

    Winick, Herman

    2003-01-01

    Sources of synchrotron radiation (also called synchrotron light) and their associated research facilities have experienced a spectacular growth in number, performance, and breadth of application in the past two to three decades. In 1978 there were eleven electron storage rings used as light sources. Three of these were small rings, all below 500 mega-electron volts (MeV), dedicated to this purpose; the others, with energy up to 5 giga-electron volts (GeV), were used parasitically during the operation of the ring for high energy physics research. In addition, at that time synchrotron radiation from nine cyclic electron synchrotrons, with energy up to 5 GeV, was also used parasitically. At present no cyclic synchrotrons are used, while about 50 electron storage rings are in operation around the world as fully dedicated light sources for basic and applied research in a wide variety of fields. Among these fields are structural molecular biology, molecular environmental science, materials, analytic chemistry, micr...

  15. Australian synchrotron radiation science

    International Nuclear Information System (INIS)

    White, J.W.

    1996-01-01

    Full text: The Australian Synchrotron Radiation Program, ASRP, has been set up as a major national research facility to provide facilities for scientists and technologists in physics, chemistry, biology and materials science who need access to synchrotron radiation. Australia has a strong tradition in crystallography and structure determination covering small molecule crystallography, biological and protein crystallography, diffraction science and materials science and several strong groups are working in x-ray optics, soft x-ray and vacuum ultra-violet physics. A number of groups whose primary interest is in the structure and dynamics of surfaces, catalysts, polymer and surfactant science and colloid science are hoping to use scattering methods and, if experience in Europe, Japan and USA can be taken as a guide, many of these groups will need third generation synchrotron access. To provide for this growing community, the Australian National Beamline at the Photon Factory, Tsukuba, Japan, has been established since 1990 through a generous collaboration with Japanese colleagues, the beamline equipment being largely produced in Australia. This will be supplemented in 1997 with access to the world's most powerful synchrotron x-ray source at the Advanced Photon Source, Argonne National Laboratory, USA. Some recent experiments in surface science using neutrons as well as x-rays from the Australian National Beamline will be used to illustrate one of the challenges that synchrotron x-rays may meet

  16. High Pressure Scanning Tunneling Microscopy Studies of AdsorbateStructure and Mobility during Catalytic Reactions: Novel Design of anUltra High Pressure, High Temperature Scanning Tunneling MicroscopeSystem for Probing Catalytic Conversions

    Energy Technology Data Exchange (ETDEWEB)

    Tang, David Chi-Wai [Univ. of California, Berkeley, CA (United States)

    2005-05-16

    The aim of the work presented therein is to take advantage of scanning tunneling microscope’s (STM) capability for operation under a variety of environments under real time and at atomic resolution to monitor adsorbate structures and mobility under high pressures, as well as to design a new generation of STM systems that allow imaging in situ at both higher pressures (35 atm) and temperatures (350 °C).

  17. Evaluation of high pressure Freon decontamination. I. Preliminary tests

    International Nuclear Information System (INIS)

    Rankin, W.N.

    1983-01-01

    High-pressure Freon blasting techniques are being evaluated for applications involving the removal of non-adherent radioactive particulate contamination at SRP. Very little waste is generated by this technique because the used Freon can be easily distilled and reused. One of the principle advantages of this technique is that decontaminated electrical equipment can be returned to service immediately without drying, unlike high-pressure water blasting techniques. Preliminary scoutin tests evaluating high-pressure Freon blasting for decontamination at SRP were carried out at Quadrex Co., Oak Ridge, TN, October 12 and 13. DWPF-type contamination (raw sludge plus volatiles) and separations area-type contamination (diluted boiling point (47.6 0 C) allow it to rapidly separate from higher boiling contaminants via distillation with filtration to remove particulate material, and distillation with condensation, the solvent may be recovered for indefinite reuse while reducing the radioactive waste to a minimum. 3 references, 5 figures, 6 tables

  18. Diamonds: powerful tools for high-pressure physics

    International Nuclear Information System (INIS)

    Anon.

    1983-01-01

    Diamond-anvil high-pressure studies have progressed to the point where they complement shock-wave studies. Because they operate at static high pressure, they permit time-consuming procedures, such as x-ray diffraction measurements for determining crystal structure. The sample material is completely recoverable and the method is adaptable to minute advantage when dealing with rare or hazardous materials. One of our goals in investigating the high-pressure behavior of iridium was to test the theoretical prediction that iridium would exhibit a phase transformation from the face-centered cubic crystal structure at about 9 GPa. Our finding that no such transformation takes place even at pressures up to 30 GPa will need to be taken into account by physicsts working to improve solid-state theory

  19. Confinement of hydrogen at high pressure in carbon nanotubes

    Science.gov (United States)

    Lassila, David H [Aptos, CA; Bonner, Brian P [Livermore, CA

    2011-12-13

    A high pressure hydrogen confinement apparatus according to one embodiment includes carbon nanotubes capped at one or both ends thereof with a hydrogen-permeable membrane to enable the high pressure confinement of hydrogen and release of the hydrogen therethrough. A hydrogen confinement apparatus according to another embodiment includes an array of multi-walled carbon nanotubes each having first and second ends, the second ends being capped with palladium (Pd) to enable the high pressure confinement of hydrogen and release of the hydrogen therethrough as a function of palladium temperature, wherein the array of carbon nanotubes is capable of storing hydrogen gas at a pressure of at least 1 GPa for greater than 24 hours. Additional apparatuses and methods are also presented.

  20. Modification of enzymes by use of high-pressure homogenization.

    Science.gov (United States)

    Dos Santos Aguilar, Jessika Gonçalves; Cristianini, Marcelo; Sato, Helia Harumi

    2018-07-01

    High-pressure is an emerging and relatively new technology that can modify various molecules. High-pressure homogenization (HPH) has been used in several studies on protein modification, especially in enzymes used or found in food, from animal, plant or microbial resources. According to the literature, the enzymatic activity can be modulated under pressure causing inactivation, stabilization or activation of the enzymes, which, depending on the point of view could be very useful. Homogenization can generate changes in the structure of the enzyme modifying various chemical bonds (mainly weak bonds) causing different denaturation levels and, consequently, affecting the catalytic activity. This review aims to describe the various alterations due to HPH treatment in enzymes, to show the influence of high-pressure on proteins and to report the HPH effects on the enzymatic activity of different enzymes employed in the food industry and research. Copyright © 2018 Elsevier Ltd. All rights reserved.

  1. Security of bottle to fill in a high pressure air

    Science.gov (United States)

    Todic, M.; Latinovic, T.; Golubovic-Bugarski, V.; Majstorovic, A.

    2018-01-01

    Charging the bottle of high pressure air isolation devices is performed by a high-pressure compressor. The charging time is in function of the compressor capacity and the intensity of the nominal pressure of the air in the bottle. However, in accident situations this time is long and therefore high-pressure accumulators are used where the filling time of the bottle of isolation apparatus has been drastically reduced. Due to the short filling time of the bottle through the air flow, there is a thermodynamic load of bottle material that could endanger the safety of users and other participants in the area. It is therefore necessary to determine the critical parameters of the rapid charge and their intensity.

  2. High pressure common rail injection system modeling and control.

    Science.gov (United States)

    Wang, H P; Zheng, D; Tian, Y

    2016-07-01

    In this paper modeling and common-rail pressure control of high pressure common rail injection system (HPCRIS) is presented. The proposed mathematical model of high pressure common rail injection system which contains three sub-systems: high pressure pump sub-model, common rail sub-model and injector sub-model is a relative complicated nonlinear system. The mathematical model is validated by the software Matlab and a virtual detailed simulation environment. For the considered HPCRIS, an effective model free controller which is called Extended State Observer - based intelligent Proportional Integral (ESO-based iPI) controller is designed. And this proposed method is composed mainly of the referred ESO observer, and a time delay estimation based iPI controller. Finally, to demonstrate the performances of the proposed controller, the proposed ESO-based iPI controller is compared with a conventional PID controller and ADRC. Copyright © 2016 ISA. Published by Elsevier Ltd. All rights reserved.

  3. High-pressure phase transition in Ho2O3

    International Nuclear Information System (INIS)

    Lonappan, Dayana; Shekar, N.V. Chandra; Ravindran, T.R.; Sahu, P. Ch.

    2010-01-01

    High-pressure X-ray diffraction and Raman studies on holmium sesquioxide (Ho 2 O 3 ) have been carried out up to a pressure of ∼17 GPa in a diamond-anvil cell at room temperature. Holmium oxide, which has a cubic or bixbyite structure under ambient conditions, undergoes an irreversible structural phase transition at around 9.5 GPa. The high-pressure phase has been identified to be low symmetry monoclinic type. The two phases coexist to up to about 16 GPa, above which the parent phase disappears. The high-pressure laser-Raman studies have revealed that the prominent Raman band ∼370 cm -1 disappears around the similar transition pressure. The bulk modulus of the parent phase is reported.

  4. Bonding pathways of high-pressure chemical transformations

    International Nuclear Information System (INIS)

    Hu Anguang; Zhang Fan

    2013-01-01

    A three-stage bonding pathway towards high-pressure chemical transformations from molecular precursors or intermediate states has been identified by first-principles simulations. With the evolution of principal stress tensor components in the response of chemical bonding to compressive loading, the three stages can be defined as the van der Waals bonding destruction, a bond breaking and forming reaction, and equilibrium of new bonds. The three-stage bonding pathway leads to the establishment of a fundamental principle of chemical bonding under compression. It reveals that during high-pressure chemical transformation, electrons moving away from functional groups follow anti-addition, collision-free paths to form new bonds in counteracting the local stress confinement. In applying this principle, a large number of molecular precursors were identified for high-pressure chemical transformations, resulting in new materials. (fast track communication)

  5. Diagnostics and modeling of high pressure streamer induced discharges

    International Nuclear Information System (INIS)

    Marode, E.; Dessante, P.; Deschamps, N.; Deniset, C.

    2001-01-01

    A great variety of diagnostic has been applied to gain information on basic parameter governing high pressure nonthermal filamentary plasmas (and namely streamer induced filamentary discharges). Apart from electrical diagnostics, gas discharge, in contrast with solid state physics, can greatly benefit from all optical techniques owing to its ''transparent'' state. Emission and absorption spectroscopy, as well as LIF or CARS (talk are given during this meeting on these two techniques) are among such specific possibilities. The figures gained from these diagnostic measurements has generally no meaning by itself. They must be worked out, by means of calibrated former results, and/or by using them as input in high pressure plasma modeling. Mixing experimental and modeling approach is necessary for reaching relevant physical knowledge of the high pressure filamentary discharges processes. It is shown that diffusion, and thermal space and time distribution, must fully be taken into account

  6. Transformations in refractory compounds, caused by high pressures and temperatures

    International Nuclear Information System (INIS)

    Zajnulin, Yu.G.; Alyamovskij, S.I.; Shvejkin, G.P.

    1979-01-01

    Considered is the effect of high pressures and temperatures on structural features of refractory carbides, nitrides and monooxides of transition metals. The results are discussed on the basis of one component of the theory on daltonides and bertollides by N.S. Kurnakov - the theory of imaginary compounds, developed by G.B. Bokij. Several new ideas, resulting from this consideration, are formulated, It is shown that at high pressures and temperatures it is possible to obtain new electron modifications of compounds and to expand sufficiently the region of the existance of variable composition phases. The concept on imaginary compounds is shown to be true. A supposition is made on realization of numerous imaginary compounds at high pressures and temperatures. Other ways of production of imaginary compounds are recommended

  7. Electronic structure and optical properties of AIN under high pressure

    International Nuclear Information System (INIS)

    Li Zetao; Dang Suihu; Li Chunxia

    2011-01-01

    We have calculated the electronic structure and optical properties of Wurtzite structure AIN under different high pressure with generalized gradient approximation (GGA) in this paper. The total energy, density of state, energy band structure and optical absorption and reflection properties under high pressure are calculated. By comparing the changes of the energy band structure, we obtained AIN phase transition pressure for 16.7 GPa, which is a direct band structure transforming to an indirect band structure. Meanwhile, according to the density of states distribution and energy band structure, we analyzed the optical properties of AIN under high-pressure, the results showed that the absorption spectra moved from low-energy to high-energy. (authors)

  8. Precision synchrotron radiation detectors

    International Nuclear Information System (INIS)

    Levi, M.; Rouse, F.; Butler, J.

    1989-03-01

    Precision detectors to measure synchrotron radiation beam positions have been designed and installed as part of beam energy spectrometers at the Stanford Linear Collider (SLC). The distance between pairs of synchrotron radiation beams is measured absolutely to better than 28 /mu/m on a pulse-to-pulse basis. This contributes less than 5 MeV to the error in the measurement of SLC beam energies (approximately 50 GeV). A system of high-resolution video cameras viewing precisely-aligned fiducial wire arrays overlaying phosphorescent screens has achieved this accuracy. Also, detectors of synchrotron radiation using the charge developed by the ejection of Compton-recoil electrons from an array of fine wires are being developed. 4 refs., 5 figs., 1 tab

  9. A 2 TiO 5 (A = Dy, Gd, Er, Yb) at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    Park, Sulgiye [Department of Geological Science, Stanford University, Stanford, California 94305, United States; Rittman, Dylan R. [Department of Geological Science, Stanford University, Stanford, California 94305, United States; Tracy, Cameron L. [Department of Geological Science, Stanford University, Stanford, California 94305, United States; Chapman, Karena W. [X-ray Science Division, Advanced Photon; Zhang, Fuxiang [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States; Park, Changyong [HPCAT, Carnegie Institution of Washington, Argonne, Illinois 60439, United States; Tkachev, Sergey N. [Center for Advanced Radiation Sources, University of Chicago, Chicago, Illinois 60637, United States; O’Quinn, Eric [Department of Nuclear Engineering, University of Tennessee, Knoxville, Tennessee 37996, United States; Shamblin, Jacob [Department of Nuclear Engineering, University of Tennessee, Knoxville, Tennessee 37996, United States; Lang, Maik [Department of Nuclear Engineering, University of Tennessee, Knoxville, Tennessee 37996, United States; Mao, Wendy L. [Department of Geological Science, Stanford University, Stanford, California 94305, United States; Stanford; amp, Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States; Ewing, Rodney C. [Department of Geological Science, Stanford University, Stanford, California 94305, United States

    2018-02-07

    The structural evolution of lanthanide A2TiO5 (A = Dy, Gd, Yb, and Er) at high pressure is investigated using synchrotron X-ray diffraction. The effects of A-site cation size and of the initial structure are systematically examined by varying the composition of the isostructural lanthanide titanates, and the structure of dysprosium titanate polymorphs (orthorhombic, hexagonal and cubic), respectively. All samples undergo irreversible high pressure phase transformations, but with different onset pressures depending on the initial structure. While individual phase exhibits different phase transformation histories, all samples commonly experience a sluggish transformation to a defect cotunnite-like (Pnma) phase for a certain pressure range. Orthorhombic Dy2TiO5 and Gd2TiO5 form P21am at pressures below 9 GPa and Pnma above 13 GPa. Pyrochlore-type Dy2TiO5 and Er2TiO5 as well as defect-fluorite-type Yb2TiO5 form Pnma at ~ 21 GPa, followed by Im-3m. Hexagonal Dy2TiO5 forms Pnma directly, although a small amount of remnants of hexagonal Dy2TiO5 is observed even at the highest pressure (~ 55 GPa) reached, indicating a kinetic limitations in the hexagonal Dy2TiO5 phase transformations at high pressure. Decompression of these materials leads to different metastable phases. Most interestingly, a high pressure cubic X-type phase (Im-3m) is confirmed using highresolution transmission electron microscopy on recovered pyrochlore-type Er2TiO5. The kinetic constraints on this metastable phase yield a mixture of both the X-type phase and amorphous domains upon pressure release. This is the first observation of an X-type phase for an A2BO5 composition at high pressure.

  10. Effect of Nb additions on the microstructure, thermal stability and mechanical behavior of high pressure Zr phases under ambient conditions

    International Nuclear Information System (INIS)

    Zhilyaev, A.P.; Sabirov, I.; Gonzalez-Doncel, G.; Molina-Aldareguia, J.; Srinivasarao, B.; Perez-Prado, M.T.

    2011-01-01

    Research highlights: → We analyze the influence of Nb additions on the shear-induced α → ω → β phase transformations in pure Zr by high pressure torsion (HPT). → Nb reduces the transition pressures and increases the transformation kinetics. → High pressure phases are retained under ambient conditions due to the presence of an internal stress. → Post-HPT annealing allows to fabricate bimodal/biphase nanostructures with enhanced mechanical behavior. - Abstract: This paper analyzes the influence of Nb on the shear-induced α → ω → β transformation taking place when processing Zr by high pressure torsion (HPT) under suitable conditions of pressure and shear. With that purpose, pure Zr and Zr-2.5%Nb were processed by HPT at room temperature and at pressures ranging from 0.25 to 6 GPa using 5 anvil turns. Nb causes a further reduction of the transition pressures, which are already lower when applying shear besides pressure. Thus, the transition pressure to the β phase is reduced at least 100 times in the Zr-Nb alloy. Alloying with Nb decreases the grain size of the transformed phases, significantly enhances their thermal stability and increases their UTS and elongation to failure. Selected post-HPT annealing treatments lead to the development of very tough, multiphase Zr and Zr-Nb with bimodal grain size distributions. The retention of the high pressure phases under ambient conditions is explained by the development of a high internal stress during processing. This stress is measured by synchrotron radiation diffraction at HZB-BESSY II. It is proposed that the presence of Nb reduces the internal stress level required for the retention of the high pressure phases.

  11. High-pressure test loop design and application

    International Nuclear Information System (INIS)

    Burnette, R.D.; Graves, J.N.; Blair, P.G.; Baldwin, N.L.

    1980-07-01

    A high-pressure test loop (HPTL) has been constructed for the purpose of performing a number of chemistry experiments at simulated HTGR conditions of temperature, pressure, flow, and impurity content. The HPTL can be used to develop, modify, and verify computer codes for a variety of chemical processes involving gas phase transport in the reactor. Processes such as graphite oxidation, fission product transport, fuel reactions, purification systems, and dust entrainment can be studied at high pressure, which would largely eliminate difficulties in correlating existing laboratory data and reactor conditions

  12. Radioresistance increase in polymers at high pressures. [. gamma. rays

    Energy Technology Data Exchange (ETDEWEB)

    Milinchuk, V; KIRJUKHIN, V; KLINSHPONT, E

    1977-06-01

    The effect was studied of very high pressures ranging within 100 and 2,700 MPa on the radioresistance of polytetrafluoroethylene, polypropylene and polyethylene in gamma irradiation. For experiments industrial polymers in the shape of blocks, films and fibers were used. It is shown that in easily breakable polymers, such as polytetrafluoroethylene and polypropylene, 1.3 to 2 times less free radicals are formed as a result of gamma irradiation and a pressure of 150 MPa than at normal pressure. The considerably reduced radiation-chemical formation of radicals and the destruction suppression by cross-linking in polymers is the evidence of the polymer radioresistance in irradiation at high pressures.

  13. Very high pressure Moessbauer spectroscopy using diamond anvil cells

    International Nuclear Information System (INIS)

    Pasternak, M.P.; Taylor, R.D.

    1988-01-01

    The technique of generating very high pressure by means of Diamond Anvil Cells (DAC) for Mossbauer Effect applications is outlined. A comprehensive description is presented of the principles of DAC, modification for the use in M/umlt o/ssbauer Spectroscopy (MS), the Merrill--Bassett and Bassett cells, of pressure measurements, of gasketing and collimation, and of hydrostatic media. Examples of 151 Eu, 119 Sn and 129 I are given showing the feasibility of DAC applications in MS. Other isotopes with potential use for high pressure MS using DAC are suggested. 27 refs., 9 figs

  14. Calculation of cooling tower plumes for high pressure wintry situations

    International Nuclear Information System (INIS)

    Gassmann, F.; Tinguely, M.; Haschke, D.

    1982-12-01

    The diffusion of the plumes of the projected nuclear power plants at Kaiseraugst and Schwoerstadt, during high pressure wintry conditions, has been examined using a mathematical model to simulate the plumes. For these calculations, microaerological measurements were made in the proximity of Kaiseraugst and Schwoerstadt. These give a typical image of the weather during high pressure wintry conditions, which is normally associated with an inversion, sometimes strong, at a low height. Dry cooling towers with natural draught, which offer an alternative solution to the wet cooling towers proposed for Kasieraugst, are examined equally. (Auth./G.T.H.)

  15. Infrared spectra of hexamethylbenzene—tetracyanoethylene complexes at high pressures

    Science.gov (United States)

    Yamada, Haruka; Saheki, Masao

    Infrared spectra of hexamethylbenzene(HMB)—tetracyanoethylene(TCNE), 1:1 and 2:1, complexes were measured under high pressures, 11˜4,000 bar. It was found that the CC stretching (A g) band of TCNE became much stronger at high pressures than at 1 bar and that the intensity increase of this band was especially large for both of the complexes. Based on these facts the strong appearance of the CC band at 1 bar, which is inconsistent with the symmetry consideration derived from X-ray analysis, can be discussed.

  16. High-pressure cell for simultaneous dielectric and neutron spectroscopy

    DEFF Research Database (Denmark)

    Sanz, Alejandro; Hansen, Henriette Wase; Jakobsen, Bo

    2018-01-01

    In this article, we report on the design, manufacture, and testing of a high-pressure cell for simultaneous dielectric and neutron spectroscopy. This cell is a unique tool for studying dynamics on different time scales, from kilo- to picoseconds, covering universal features such as the α relaxation......, a cylindrical capacitor is positioned within the bore of the high-pressure container. The capacitor consists of two concentric electrodes separated by insulating spacers. The performance of this setup has been successfully verified by collecting simultaneous dielectric and neutron spectroscopy data...

  17. Magnetization at high pressure in CeP

    Science.gov (United States)

    Naka, T.; Matsumoto, T.; Okayama, Y.; Môri, N.; Haga, Y.; Suzuki, T.

    1995-02-01

    We have investigated the pressure dependence of magnetization below 60 K up to 1.6 GPa in the low-carrier concentration system CeP showing two step transitions at T = TL and TH under high pressure. At high pressure, M( P, T) exhibits a maximum at around the lower transition temperature TL. This behavior implies that the magnetic state changes at TL. The pressure dependence of isothermal magnetization M( P) is different above and below TL. In fact, M( P) below TL exhibits a maximum at around 1.4 GPa, whereas M( P) above TL increases steeply with pressure up to 1.6 GPa.

  18. High pressure studies of fluorenone emission in plastic media

    International Nuclear Information System (INIS)

    Mitchell, D.J.; Schuster, G.B.; Drickamer, H.G.

    1977-01-01

    The energy and the quantum efficiency for fluorenone fluorescence in the crystalline state and in polymeric matrices was measured as a function of external pressure over the range 0--140 kbar. The application of high pressure induces changes in the quantum yield, which ranges from 0.001 at low pressure to a maximum of approx.0.1 at high pressure in hydrocarbon plastics. These results are interpreted as arising from the decrease in the energy of the lowest ππ excited singlet state relative to other relevant states as the external pressure is increased

  19. New problems in solid-state chemistry solved by high pressure conditions: an exciting perspective for preparing new materials

    OpenAIRE

    Demazeau , Gérard

    1988-01-01

    International audience; The high-pressure technique is an efficient tool in solid-state chemistry for preparing new materials of low stability or metastable character. During the last 20 years, this technique has been used and developed especially in three principal areas : synthesis of new materials, either for a better basic approach of scientific problems or for industrial applications studies of structural transformations in situ evolution of some physical properties of materials under pr...

  20. A high-pressure thermal gradient block for investigating microbial activity in multiple deep-sea samples

    DEFF Research Database (Denmark)

    Kallmeyer, J.; Ferdelman, TG; Jansen, KH

    2003-01-01

    Details about the construction and use of a high-pressure thermal gradient block for the simultaneous incubation of multiple samples are presented. Most parts used are moderately priced off-the-shelf components that easily obtainable. In order to keep the pressure independent of thermal expansion....... Sulfate reduction rates increase with increasing pressure and show maximum values at pressures higher than in situ. (C) 2003 Elsevier Science B.V. All rights reserved....

  1. Properties of synchrotron radiation

    International Nuclear Information System (INIS)

    Materlik, G.

    1982-01-01

    This paper forms the introductory chapter to a book concerning the use of synchrotron radiation for investigation of the structure and mechanism of biological macromolecules. After a historical section, the physics of synchrotron radiation is summarized so that the most promising experiments may be extrapolated. Irradiated power and intensity, polarization and angular distribution, brilliance of a real source, and developments such as wigglers and undulators are briefly dealt with. The paper includes a tabulated compilation of proposed and operating machines in 1982, with some of their characteristics. (U.K.)

  2. High-pressure structural behavior of nanocrystalline Ge

    DEFF Research Database (Denmark)

    Wang, H.; Liu, J. F.; Yan, H.

    2007-01-01

    The equation of state and the pressure of the I-II transition have been studied for nanocrystalline Ge using synchrotron x-ray diffraction. The bulk modulus and the transition pressure increase with decreasing particle size for both Ge-I and Ge-II, but the percentage volume collapse at the transi...

  3. Effect of high pressure hydrogen on low-cycle fatigue

    International Nuclear Information System (INIS)

    Rie, K.T.; Kohler, W.

    1979-01-01

    It has been shown that the fatigue life can be influenced in low-cycle range by high pressure hydrogen while the effect of high pressure hydrogen on high-cycle fatigue will not be as significant. The paper reports the details and the results of the investigations of the effect of high pressure hydrogen on the low-cycle endurance of commercially pure titanium. The results of this study indicate that: 1. The degradation of the fatigue life in low-cycle region for commercially pure titanium under high pressure hydrogen can be described by Nsub(cr)sup(α x Δepsilon)sub(pl)sup(=c) 2. The fatigue life decreases with decreasing strain rate. 3. The fatigue life decreases with increasing hydrogen pressure. It was found that the semilogarithmic plot of the fatigue life versus the hydrogen pressure gives a linear relationship. The Sievert's law does not hold in low-cycle fatigue region. 4. HAC in titanium in low-cycle fatigue region is the result of the disolution of hydrogen at the crack tip and of the strain-induced hybride formation. (orig.) 891 RW/orig. 892 RKD [de

  4. Pneumomediastinum following high pressure air injection to the hand.

    LENUS (Irish Health Repository)

    Kennedy, J

    2012-02-01

    We present the case of a patient who developed pneumomediastinum after high pressure air injection to the hand. To our knowledge this is the first reported case of pneumomediastinum where the gas injection site was the thenar eminence. Fortunately the patient recovered with conservative management.

  5. High-pressure applications in medicine and pharmacology

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Jerson L; Foguel, Debora; Suarez, Marisa; Gomes, Andre M O; Oliveira, Andrea C [Centro Nacional de Ressonancia Magnetica Nuclear, Departamento de Bioquimica Medica, Instituto de Ciencias Biomedicas, Universidade Federal do Rio de Janeiro, Rio de Janeiro, RJ 21941-590 (Brazil)

    2004-04-14

    High pressure has emerged as an important tool to tackle several problems in medicine and biotechnology. Misfolded proteins, aggregates and amyloids have been studied, which point toward the understanding of the protein misfolding diseases. High hydrostatic pressure (HHP) has also been used to dissociate non-amyloid aggregates and inclusion bodies. The diverse range of diseases that result from protein misfolding has made this theme an important research focus for pharmaceutical and biotech companies. The use of high pressure promises to contribute to identifying the mechanisms behind these defects and creating therapies against these diseases. High pressure has also been used to study viruses and other infectious agents for the purpose of sterilization and in the development of vaccines. Using pressure, we have detected the presence of a ribonucleoprotein intermediate, where the coat protein is partially unfolded but bound to RNA. These intermediates are potential targets for antiviral compounds. The ability of pressure to inactivate viruses, prions and bacteria has been evaluated with a view toward the applications of vaccine development and virus sterilization. Recent studies demonstrate that pressure causes virus inactivation while preserving the immunogenic properties. There is increasing evidence that a high-pressure cycle traps a virus in the 'fusion intermediate state', not infectious but highly immunogenic.

  6. Effect of high pressure on physicochemical properties of meat.

    Science.gov (United States)

    Buckow, Roman; Sikes, Anita; Tume, Ron

    2013-01-01

    The application of high pressure offers some interesting opportunities in the processing of muscle-based food products. It is well known that high-pressure processing can prolong the shelf life of meat products in addition to chilling but the pressure-labile nature of protein systems limits the commercial range of applications. High pressure can affect the texture and gel-forming properties of myofibrillar proteins and, hence, has been suggested as a physical and additive-free alternative to tenderize and soften or restructure meat and fish products. However, the rate and magnitude at which pressure and temperature effects take place in muscles are variable and depend on a number of circumstances and conditions that are still not precisely known. This review provides an overview of the current knowledge of the effects of high pressure on muscle tissue over a range of temperatures as it relates to meat texture, microstructure, color, enzymes, lipid oxidation, and pressure-induced gelation of myofibrillar proteins.

  7. Strength-toughness requirements for thick walled high pressure vessels

    International Nuclear Information System (INIS)

    Kapp, J.A.

    1990-01-01

    The strength and toughness requirements of materials for use in high pressure vessels has been the subject of some discussion in the meetings of the Materials Task Group of the Special Working Group High Pressure Vessels. A fracture mechanics analysis has been performed to theoretically establish the required toughness for a high pressure vessel. This paper reports that the analysis performed is based on the validity requirement for plane strain fracture of fracture toughness test specimens. This is that at the fracture event, the crack length, uncracked ligament, and vessel length must each be greater than fifty times the crack tip plastic zone size for brittle fracture to occur. For high pressure piping applications, the limiting physical dimension is the uncracked ligament, as it can be assumed that the other dimensions are always greater than fifty times the crack tip plastic zone. To perform the fracture mechanics analysis several parameters must be known: these include vessel dimensions, material strength, degree of autofrettage, and design pressure. Results of the analysis show, remarkably, that the effects of radius ratio, pressure and degree of autofrettage can be ignored when establishing strength and toughness requirements for code purposes. The only parameters that enter into the calculation are yield strength, toughness and vessel thickness. The final results can easily be represented as a graph of yield strength against toughness on which several curves, one for each vessel thickness, are plotted

  8. High pressure processing inactivates human norovirus within oysters

    Science.gov (United States)

    Consumption of raw bivalve mollusks can result in norovirus infection. One potential intervention for virus-contaminated shellfish is high pressure processing (HPP). Currently HPP is known to inactivate Vibrio bacteria, hepatitis A virus, and murine norovirus within oysters. To evaluate the potentia...

  9. Magnetism in UPtAl under high pressure

    Czech Academy of Sciences Publication Activity Database

    Honda, F.; Eto, T.; Oomi, G.; Sechovský, V.; Andreev, Alexander V.; Takeshita, N.; Môri, N.

    2002-01-01

    Roč. 52, č. 2 (2002), s. 263-266 ISSN 0011-4626. [Czech and Slovak Conference on Magnetism /11./. Košice, 20.08.2001-23.08.2001] Institutional research plan: CEZ:AV0Z1010914 Keywords : UPtAl * high pressure * electrical resistivity Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.311, year: 2002

  10. Growth and high pressure studies of zirconium sulphoselenide ...

    Indian Academy of Sciences (India)

    Growth and high pressure studies of zirconium sulphoselenide single ... tance was monitored in a Bridgman opposed anvil set-up up to 8 GPa pressure to identify .... The optical band gaps of the as-grown crystals were obtained by optical ab-.

  11. Crosslinking polymerization of tetraethylene glycol dimethacrylate under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Kaminski, K; Paluch, M; Ziolo, J [Institute of Physics, Silesian University, Uniwersytecka 4, 40-007 Katowice (Poland); Bogoslovov, R; Roland, C M [Chemistry Division, Code 6120, Naval Research Laboratory, Washington DC 20375-5342 (United States)], E-mail: kaminski@us.edu.pl

    2008-07-15

    The polymerization reaction of tetraethylene glycol dimethacrylate was induced by application of high pressure. Broadband dielectric spectroscopy was employed to investigate dielectric properties of the produced polymers. Additionally swelling experiment was performed to determine the degree of crossliniking of the polymers.

  12. Screening of hydrogen storage media applying high pressure thermogravimetry

    DEFF Research Database (Denmark)

    Bentzen, J.J.; Pedersen, Allan Schrøder; Kjøller, J.

    2001-01-01

    A number of commercially available hydride-forming alloys of the MmNi5–xSnx (Mm=mischmetal, a mixture of lanthanides) type were examined using a high pressure, high temperature microbalance,scanning electron microscopy and X-ray diffraction. Activation conditions, reversible storage capacity...

  13. High-pressure physical properties of magnesium silicate post ...

    Indian Academy of Sciences (India)

    MgSiO3) post-perovskite at high pressure are investigated with quasi-harmonic Debye model and ab initio method based on the density functional theory (DFT). The calculated structural parameters of MgSiO3 post-perovskite are consistent with the ...

  14. Pneumomediastinum following high pressure air injection to the hand.

    LENUS (Irish Health Repository)

    Kennedy, J

    2010-04-01

    We present the case of a patient who developed pneumomediastinum after high pressure air injection to the hand. To our knowledge this is the first reported case of pneumomediastinum where the gas injection site was the thenar eminence. Fortunately the patient recovered with conservative management.

  15. Effect of high pressurized carbon dioxide on Escherichia coli ...

    African Journals Online (AJOL)

    Carbon dioxide at high pressure can retard microbial growth and sometimes kill microorganisms depending on values of applied pressure, temperature and exposure time. In this study the effect of high pressurised carbon dioxide (HPCD) on Escherichia coli was investigated. Culture of E. coli was subjected to high ...

  16. A high pressure sample facility for neutron scattering

    International Nuclear Information System (INIS)

    Carlile, C.J.; Glossop, B.H.

    1981-06-01

    Commissioning tests involving deformation studies and tests to destruction as well as neutron diffraction measurements of a standard sample have been carried out on the SERC high pressure sample facility for neutron scattering studies. A detailed description of the pressurising equipment is given. (author)

  17. Investigation of Acrylic Acid at High Pressure using Neutron Diffraction

    DEFF Research Database (Denmark)

    Johnston, Blair F.; Marshall, William G.; Parsons, Simon

    2014-01-01

    This article details the exploration of perdeuterated acrylic acid at high pressure using neutron diffraction. The structural changes that occur in acrylic acid-d4 are followed via diffraction and rationalised using the Pixel method. Acrylic acid undergoes a reconstructive phase transition to a new...

  18. Effects of high pressures on magnetism in UNiGa

    Czech Academy of Sciences Publication Activity Database

    Míšek, M.; Sechovský, V.; Kamarád, Jiří; Prokleška, J.

    2010-01-01

    Roč. 30, č. 1 (2010), 8-11 ISSN 0895-7959 Grant - others:GAUK(CZ) 129009 Institutional research plan: CEZ:AV0Z10100521 Keywords : high pressure * uniaxial stress * magnetism Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.995, year: 2010

  19. High pressure and foods -fruit/vegetable juices

    Czech Academy of Sciences Publication Activity Database

    Houška, M.; Strohalm, J.; Kocurová, K.; Totušek, J.; Lefnerová, D.; Tříska, Jan; Vrchotová, Naděžda; Fiedlerová, V.; Holasová, M.; Gabrovská, D.; Paulíčková, I.

    2006-01-01

    Roč. 77, č. 3 (2006), s. 386-398 ISSN 0260-8774 R&D Projects: GA MZe(CZ) QF3287 Institutional research plan: CEZ:AV0Z60870520 Keywords : high-pressure pasteurisation * Foods * Broccoli juice Subject RIV: GM - Food Processing Impact factor: 1.696, year: 2006

  20. Investigation of Methacrylic Acid at High Pressure Using Neutron Diffraction

    DEFF Research Database (Denmark)

    Marshall, William G.; Urquhart, Andrew; Oswald, Iain D. H.

    2015-01-01

    This article shows that pressure can be a low-intensity route to the synthesis of polymethacrylic acid. The exploration of perdeuterated methacrylic acid at high pressure using neutron diffraction reveals that methacrylic acid exhibits two polymorphic phase transformations at relatively low...

  1. Learning by Practice, High-Pressure Student Ateliers

    NARCIS (Netherlands)

    Timmermans, W.; Cilliers, J.; Garcia, A.; Koolen, A.; Woudstra, A.; Dijk, van T.

    2014-01-01

    Two international and interdisciplinary high pressure student ateliers have been done and evaluated, one to explore possible future scenario’s for Strofylia (Greece) as requested by local and regional authorities and stakeholders, the other to put urban agriculture on the Lugo (Galicia, Spain)

  2. A high-pressure MWPC detector for crystallography

    DEFF Research Database (Denmark)

    Ortuno-Prados, F.; Bazzano, A.; Berry, A.

    1999-01-01

    The application of the Multi-Wire Proportional Counter (MWPC) as a potential detector for protein crystallography and other wide-angle diffraction experiments is presented. Electrostatic problems found with our large area MWPC when operated at high pressure are discussed. We suggest that a solution...

  3. Propane Oxidation at High Pressure and Intermediate Temperatures

    DEFF Research Database (Denmark)

    Hashemi, Hamid; Christensen, Jakob Munkholt; Glarborg, Peter

    Propane oxidation at intermediate temperatures (500—900 K) and high pressure (100 bar) has been characterized by conducting experiments in a laminar flow reactor over a wide range of stoichiometries. The onset of fuel oxidation was found to be 600—725 K, depending on mixture stoichiometry...

  4. International Space Station (ISS) Oxygen High Pressure Storage Management

    Science.gov (United States)

    Lewis, John R.; Dake, Jason; Cover, John; Leonard, Dan; Bohannon, Carl

    2004-01-01

    High pressure oxygen onboard the ISS provides support for Extra Vehicular Activities (EVA) and contingency metabolic support for the crew. This high pressure 02 is brought to the ISS by the Space Shuttle and is transferred using the Oxygen Recharge Compressor Assembly (ORCA). There are several drivers that must be considered in managing the available high pressure 02 on the ISS. The amount of O2 the Shuttle can fly up is driven by manifest mass limitations, launch slips, and on orbit Shuttle power requirements. The amount of 02 that is used from the ISS high pressure gas tanks (HPGT) is driven by the number of Shuttle docked and undocked EVAs, the type of EVA prebreath protocol that is used and contingency use of O2 for metabolic support. Also, the use of the ORCA must be managed to optimize its life on orbit and assure that it will be available to transfer the planned amount of O2 from the Shuttle. Management of this resource has required long range planning and coordination between Shuttle manifest on orbit plans. To further optimize the situation hardware options have been pursued.

  5. High pressure gas laser technology for atmospheric remote sensing

    Science.gov (United States)

    Javan, A.

    1980-01-01

    The development of a fixed frequency chirp-free and highly stable intense pulsed laser made for Doppler wind velocity measurements with accurate ranging is described. Energy extraction from a high pressure CO2 laser at a tunable single mode frequency is also examined.

  6. Variable high pressure processing sensitivities for GII human noroviruses

    Science.gov (United States)

    Human norovirus (HuNoV) is the leading cause of foodborne diseases worldwide. High pressure processing (HPP) is one of the most promising non-thermal technologies for decontamination of viral pathogens in foods. However, the survival of HuNoVs by HPP is poorly understood because these viruses cann...

  7. High-pressure applications in medicine and pharmacology

    International Nuclear Information System (INIS)

    Silva, Jerson L; Foguel, Debora; Suarez, Marisa; Gomes, Andre M O; Oliveira, Andrea C

    2004-01-01

    High pressure has emerged as an important tool to tackle several problems in medicine and biotechnology. Misfolded proteins, aggregates and amyloids have been studied, which point toward the understanding of the protein misfolding diseases. High hydrostatic pressure (HHP) has also been used to dissociate non-amyloid aggregates and inclusion bodies. The diverse range of diseases that result from protein misfolding has made this theme an important research focus for pharmaceutical and biotech companies. The use of high pressure promises to contribute to identifying the mechanisms behind these defects and creating therapies against these diseases. High pressure has also been used to study viruses and other infectious agents for the purpose of sterilization and in the development of vaccines. Using pressure, we have detected the presence of a ribonucleoprotein intermediate, where the coat protein is partially unfolded but bound to RNA. These intermediates are potential targets for antiviral compounds. The ability of pressure to inactivate viruses, prions and bacteria has been evaluated with a view toward the applications of vaccine development and virus sterilization. Recent studies demonstrate that pressure causes virus inactivation while preserving the immunogenic properties. There is increasing evidence that a high-pressure cycle traps a virus in the 'fusion intermediate state', not infectious but highly immunogenic

  8. Ultra-high pressure water jet: Baseline report

    International Nuclear Information System (INIS)

    1997-01-01

    The ultra-high pressure waterjet technology was being evaluated at Florida International University (FIU) as a baseline technology. In conjunction with FIU's evaluation of efficiency and cost, this report covers the evaluation conducted for safety and health issues. It is a commercially available technology and has been used for various projects at locations throughout the country. The ultra-high pressure waterjet technology acts as a cutting tool for the removal of surface substrates. The Husky trademark pump feeds water to a lance that directs the high pressure water at the surface to be removed. The safety and health evaluation during the testing demonstration focused on two main areas of exposure. These were dust and noise. The dust exposure was found to be minimal, which would be expected due to the wet environment inherent in the technology, but noise exposure was at a significant level. Further testing for noise is recommended because of the outdoor environment where the testing demonstration took place. In addition, other areas of concern found were arm-hand vibration, ergonomics, heat stress, tripping hazards, electrical hazards, lockout/tagout, fall hazards, slipping hazards, hazards associated with the high pressure water, and hazards associated with air pressure systems

  9. In situ x-ray diffraction of an arc weld showing the phase transformations of Ti and Fe as a function of position in the weld performed at a synchrotron

    International Nuclear Information System (INIS)

    Wong, J.; Elmer, J.W.; Waide, P.A.

    1994-01-01

    The synchrotron x-ray source provides a unique opportunity to observe open-quotes in-situclose quotes processes. The formation of the open-quotes short-livedclose quotes intermediate species, Ta 2 C, during the combustion synthesis of TaC, has been observed and reported by monitoring the Bragg diffraction peaks of the reactants and products. Similarly, the synthesis of the ferroelectric material, BaTiO 3 , and subsequent phase transformation from cubic to tetragonal have also been investigated. These experiments would not have been possible without the high incident x-ray flux available at a synchrotron source. The physical and mechanical properties of a weld join are highly independent upon the thermal history of the weld. Factors such as grain size, which increases with annealing, influence the tensile strength of the weld. This work presents the results of an investigation of the phase changes in two materials, titanium and stainless steel, which occur during the welding process. 4 refs., 3 figs

  10. Temperature control for high pressure processes up to 1400 MPa

    International Nuclear Information System (INIS)

    Reineke, K; Mathys, A; Knorr, D; Heinz, V

    2008-01-01

    Pressure- assisted sterilisation is an emerging technology. Hydrostatic high pressure can reduce the thermal load of the product and this allows quality retention in food products. To guarantee the safety of the sterilisation process it is necessary to investigate inactivation kinetics especially of bacterial spores. A significant roll during the inactivation of microorganisms under high pressure has the thermodynamic effect of the adiabatic heating. To analyse the individual effect of pressure and temperature on microorganism inactivation an exact temperature control of the sample to reach ideal adiabatic conditions and isothermal dwell times is necessary. Hence a heating/cooling block for a high pressure unit (Stansted Mini-Food-lab; high pressure capillary with 300 μL sample volume) was constructed. Without temperature control the sample would be cooled down during pressure built up, because of the non-adiabatic heating of the steel made vessel. The heating/cooling block allows an ideal adiabatic heat up and cooling of the pressure vessel during compression and decompression. The high pressure unit has a pressure build-up rate up to 250 MPa s -1 and a maximum pressure of 1400 MPa. Sebacate acid was chosen as pressure transmitting medium because it had no phase shift over the investigate pressure and temperature range. To eliminate the temperature difference between sample and vessel during compression and decompression phase, the mathematical model of the adiabatic heating/cooling of water and sebacate acid was implemented into a computational routine, written in Test Point. The calculated temperature is the setpoint of the PID controller for the heating/cooling block. This software allows an online measurement of the pressure and temperature in the vessel and the temperature at the outer wall of the vessel. The accurate temperature control, including the model of the adiabatic heating opens up the possibility to realise an ideal adiabatic heating and cooling

  11. Reflectometry with synchrotron radiation

    International Nuclear Information System (INIS)

    Krumrey, Michael; Cibik, Levent; Fischer, Andreas; Gottwald, Alexander; Kroth, Udo; Scholze, Frank

    2014-01-01

    The measurement of the reflectivity for VUV, XUV, and X-radiation at the PTB synchrotron radiation sources is described. The corresponding data of the used beams are presented. Results of experiments on a Cu-Ni double-layer, SiO 2 , Si, and MgF 2 are presented. (HSI)

  12. Coherent synchrotron radiation

    International Nuclear Information System (INIS)

    Agoh, Tomonori

    2006-01-01

    This article presents basic properties of coherent synchrotron radiation (CSR) with numerical examples and introduces the reader to important aspects of CSR in future accelerators with short bunches. We show interesting features of the single bunch instability due to CSR in storage rings and discuss the longitudinal CSR field via the impedance representation. (author)

  13. Characteristics of synchrotron radiation

    International Nuclear Information System (INIS)

    Brown, G.S.

    1984-01-01

    The characteristics and production of synchrotron radiation are qualitatively discussed. The spectral properties of wigglers and undulators are briefly described. Possible applications in condensed matter physics are outlined. These include atomic and molecular studies, crystallography, impurities in solids and radiographic imaging

  14. Ignition during hydrogen release from high pressure into the atmosphere

    Science.gov (United States)

    Oleszczak, P.; Wolanski, P.

    2010-12-01

    The first investigations concerned with a problem of hydrogen jet ignition, during outflow from a high-pressure vessel were carried out nearly 40 years ago by Wolanski and Wojcicki. The research resulted from a dramatic accident in the Chorzow Chemical Plant Azoty, where the explosion of a synthesis gas made up of a mixture composed of three moles of hydrogen per mole of nitrogen, at 300°C and 30 MPa killed four people. Initial investigation had excluded potential external ignition sources and the main aim of the research was to determine the cause of ignition. Hydrogen is currently considered as a potential fuel for various vehicles such as cars, trucks, buses, etc. Crucial safety issues are of potential concern, associated with the storage of hydrogen at a very high pressure. Indeed, the evidence obtained nearly 40 years ago shows that sudden rupture of a high-pressure hydrogen storage tank or other component can result in ignition and potentially explosion. The aim of the present research is identification of the conditions under which hydrogen ignition occurs as a result of compression and heating of the air by the shock wave generated by discharge of high-pressure hydrogen. Experiments have been conducted using a facility constructed in the Combustion Laboratory of the Institute of Heat Engineering, Warsaw University of Technology. Tests under various configurations have been performed to determine critical conditions for occurrence of high-pressure hydrogen ignition. The results show that a critical pressure exists, leading to ignition, which depends mainly on the geometric configuration of the outflow system, such as tube diameter, and on the presence of obstacles.

  15. Synchrotron radiation research

    International Nuclear Information System (INIS)

    Markus, N.

    1995-01-01

    In the many varied application fields of accelerators, synchrotron radiation ranks as one of the most valuable and widely useful tools. Synchrotron radiation is produced in multi-GeV electron synchrotrons and storage rings, and emerges tangentially in a narrow vertical fan. Synchrotron radiation has been used extensively for basic studies and, more recently, for applied research in the chemical, materials, biotechnology and pharmaceutical industries. Initially, the radiation was a byproduct of high energy physics laboratories but the high demand soon resulted in the construction of dedicated electron storage rings. The accelerator technology is now well developed and a large number of sources have been constructed, with energies ranging from about 1.5 to 8 GeV including the 6 GeV European Synchrotron Radiation Facility (ESRF) source at Grenoble, France. A modern third-generation synchrotron radiation source has an electron storage ring with a complex magnet lattice to produce ultra-low emittance beams, long straights for 'insertion devices', and 'undulator' or 'wiggler' magnets to generate radiation with particular properties. Large beam currents are necessary to give high radiation fluxes and long beam lifetimes require ultra high vacuum systems. Industrial synchrotron radiation research programmes use either Xray diffraction or spectroscopy to determine the structures of a wide range of materials. Biological and pharmaceutical applications study the functions of various proteins. With this knowledge, it is possible to design molecules to change protein behaviour for pharmaceuticals, or to configure more active proteins, such as enzymes, for industrial processes. Recent advances in molecular biology have resulted in a large increase in protein crystallography studies, with researchers using crystals which, although small and weakly diffracting, benefit from the high intensity. Examples with commercial significance include the study of

  16. 76 FR 33239 - High Pressure Steel Cylinders From the People's Republic of China; Initiation of Countervailing...

    Science.gov (United States)

    2011-06-08

    ... DEPARTMENT OF COMMERCE International Trade Administration [C-570-978] High Pressure Steel... countervailing duty (``CVD'') petition concerning imports of high pressure steel cylinders (``steel cylinders... of Antidumping Duties and Countervailing Duties on High Pressure Steel Cylinders from the People's...

  17. High-resolution X-ray crystal structure of bovine H-protein using the high-pressure cryocooling method.

    Science.gov (United States)

    Higashiura, Akifumi; Ohta, Kazunori; Masaki, Mika; Sato, Masaru; Inaka, Koji; Tanaka, Hiroaki; Nakagawa, Atsushi

    2013-11-01

    Recently, many technical improvements in macromolecular X-ray crystallography have increased the number of structures deposited in the Protein Data Bank and improved the resolution limit of protein structures. Almost all high-resolution structures have been determined using a synchrotron radiation source in conjunction with cryocooling techniques, which are required in order to minimize radiation damage. However, optimization of cryoprotectant conditions is a time-consuming and difficult step. To overcome this problem, the high-pressure cryocooling method was developed (Kim et al., 2005) and successfully applied to many protein-structure analyses. In this report, using the high-pressure cryocooling method, the X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. Structural comparisons between high- and ambient-pressure cryocooled crystals at ultra-high resolution illustrate the versatility of this technique. This is the first ultra-high-resolution X-ray structure obtained using the high-pressure cryocooling method.

  18. 3D IMAGING USING COHERENT SYNCHROTRON RADIATION

    Directory of Open Access Journals (Sweden)

    Peter Cloetens

    2011-05-01

    Full Text Available Three dimensional imaging is becoming a standard tool for medical, scientific and industrial applications. The use of modem synchrotron radiation sources for monochromatic beam micro-tomography provides several new features. Along with enhanced signal-to-noise ratio and improved spatial resolution, these include the possibility of quantitative measurements, the easy incorporation of special sample environment devices for in-situ experiments, and a simple implementation of phase imaging. These 3D approaches overcome some of the limitations of 2D measurements. They require new tools for image analysis.

  19. High pressure inactivation of human norovirus-like particles: evidence that the capsid of human norovirus is highly pressure resistant

    Science.gov (United States)

    High pressure processing (HPP) is a promising non-thermal technology to inactivate foodborne viruses. However, the effectiveness of HPP on inactivating human norovirus (HuNoV), the leading cause of acute gastroenteritis, is unknown because it cannot be propagated in cell culture. Therefore, developi...

  20. Experiments on aerosol removal by high-pressure water spray

    Energy Technology Data Exchange (ETDEWEB)

    Corno, Ada del, E-mail: delcorno@rse-web.it [RSE, Power Generation Technologies and Materials Dept, via Rubattino 54, I-20134 Milano (Italy); Morandi, Sonia, E-mail: morandi@rse-web.it [RSE, Power Generation Technologies and Materials Dept, via Rubattino 54, I-20134 Milano (Italy); Parozzi, Flavio, E-mail: parozzi@rse-web.it [RSE, Power Generation Technologies and Materials Dept, via Rubattino 54, I-20134 Milano (Italy); Araneo, Lucio, E-mail: lucio.araneo@polimi.it [Politecnico di Milano, Department of Energy, via Lambruschini 4A, I-20156 Milano (Italy); CNR-IENI, via Cozzi 53, I-20125 Milano (Italy); Casella, Francesco, E-mail: francesco2.casella@mail.polimi.it [Politecnico di Milano, Department of Energy, via Lambruschini 4A, I-20156 Milano (Italy)

    2017-01-15

    Highlights: • Experimental research to measure the efficiency of high-pressure sprays in capturing aerosols if applied to a filtered containment venting system in case of severe accident. • Cloud of monodispersed SiO{sub 2} particles with sizes 0.5 or 1.0 μm and initial concentration in the range 2–90 mg/m{sup 3}. • Carried out in a chamber 0.5 × 1.0 m and 1.5 m high, with transparent walls equipped with a high pressure water spray with single nozzle. • Respect to low-pressure sprays, removal efficiency turned out significant: the half-life for 1 μm particles with a removal high-pressure spray system is orders of magnitude shorter than that with a low-pressure sprays system. - Abstract: An experimental research was managed in the framework of the PASSAM European Project to measure the efficiency of high-pressure sprays in capturing aerosols when applied to a filtered containment venting system in case of severe accident. The campaign was carried out in a purposely built facility composed by a scrubbing chamber 0.5 × 1.0 m and 1.5 m high, with transparent walls to permit the complete view of the aerosol removal process, where the aerosol was injected to form a cloud of specific particle concentration. The chamber was equipped with a high pressure water spray system with a single nozzle placed on its top. The test matrix consisted in the combination of water pressure injections, in the range 50–130 bar, on a cloud of monodispersed SiO{sub 2} particles with sizes 0.5 or 1.0 μm and initial concentration ranging between 2 and 99 mg/m{sup 3}. The spray was kept running for 2 min and the efficiency of the removal was evaluated, along the test time, using an optical particle sizer. With respect to low-pressure sprays, the removal efficiency turned out much more significant: the half-life for 1 μm particles with a removal high-pressure spray system is orders of magnitude shorter than that with a low-pressure spray system. The highest removal rate was