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Kinetic Study on the Crystal Structure Transformation by Time-resolved Measurement of X-ray Diffraction

Research Project

Project/Area Number 63420020
Research Category

Grant-in-Aid for General Scientific Research (A)

Allocation TypeSingle-year Grants
Research Field 鉱物学(含岩石・鉱床学)
Research InstitutionOsaka University

Principal Investigator

YAMANAKA Takamitsu  Osaka Univ. College of General Education, Professor, 教養部, 教授 (30011729)

Co-Investigator(Kenkyū-buntansha) OHTAKA Osamu  Osaka Univ. College of General Educatioin, Research Associate, 教養部, 助手 (40213748)
TAKUBO Hiroshi  Osaka Univ. College of General Education, Associate Professor, 教養部, 助教授 (80029678)
KUME Shouichi  Osaka Univ. College of General Education, Professor, 教養部, 教授 (00029604)
芦田 利文  徳島大学, 工学部, 助手 (60167905)
Project Period (FY) 1988 – 1990
Project Status Completed (Fiscal Year 1990)
Budget Amount *help
¥28,000,000 (Direct Cost: ¥28,000,000)
Fiscal Year 1990: ¥2,500,000 (Direct Cost: ¥2,500,000)
Fiscal Year 1989: ¥3,300,000 (Direct Cost: ¥3,300,000)
Fiscal Year 1988: ¥22,200,000 (Direct Cost: ¥22,200,000)
KeywordsStructure Transformation / Time resolved / X-ray diffraction / High Pressure and Temperature / In-situ Observation / kinetics / Amorphization of GeO_2 / Dehydration of Ca(OH)_2 / 転移・反応速度 / ダイアモンドアンビル油圧式高圧
Research Abstract

Research of the crystal structure and texture of the minerals are necessary for understanding the dynamical phenomena in earth sciences. A new analytical system is designed for the observation of the crystal structure change in the process of the phase transformations, decomposition, melting, recrystallizaton in response to the variation of the physical, conditions, pressure and temperature and stress surround the earth materials. For these research we have developed the following new systems :
(1) Angular dispersive measurement for time-resolved diffraction study A new system for time-resolved studies under pressure was composed of four-circle diffractometer with a position sensitive detector having an working angular region of 120^゚ and of computer aided measurement and control system. A high photon count efficiency is a large advantage for high pressure X-ray diffraction studies.
(2) High pressure apparatus A diamond anvil with an oil-pressure controller was installed on the four-circ … More le diffractometer set on the rotated anode X-ray generator. Pressure was finely controlled by a sensor and measured by the ruby fluorescence method and equation state of internal standard sample of NaCl based on the compressibility.
Result 1. Kinetics of polymorphic transition of GeO_2 from hexagonal (quartz-type P321, z=3) to tetragonal (rutile type P4/mmm, z=2) various temperatures under pressure. (1) Hexagonal GeO_2 was transformed to the amorphous phase at 7GPa and 62゚C but easily transformed to rutile structure at 85^゚C and 0.6GPa. The amorphous phase was successively retained up to 25GPa at room temperature. (2) Full width half maximums (FWHM) of the diffraction peaks became linearly broadened due to reducing crystallite size, indicating the enhancement of the finer-domain. Integrated diffraction intensities were decreased with pressure. (3) A local structure around Ge ion in the quenched amorphous phase was analyzed by EXAFS and Raman spectra at room condition. It was elucidated that amorphous phase was partly composed of 6-fold coordinated Ge ions and that the structure was quite different from that of melted-glass. (4) The amorphous phase was confirmed to be thermodynamically metastable.
2. Dehydration Process of Ca (OH) _2 and Mg (OH) _2
A time-resolved observation of the dehydration process was undertaken by energy dispersive diffraction using tungsten rotated anode X-ray and synchrotron radiation. The in situ measurements of the spectra up to 900^゚C were carried out by intrinsic Ge SSD in the energy range 10keV-40kev. Integrated intensities obtained by the profile fitting provide the mass ratio of oxide products to hydrates. Less

Report

(4 results)
  • 1990 Annual Research Report   Final Research Report Summary
  • 1989 Annual Research Report
  • 1988 Annual Research Report
  • Research Products

    (25 results)

All Other

All Publications (25 results)

  • [Publications] S.Kawasaki,T.Yamanaka,S,Kume&T.Ashida: "Crystallite size effect on the pressureーinduced phase transformation of ZrO_2." Solid State Comm.76. 527-530 (1990)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] O.Ohtaka,T.Yamanaka,S.Kume,N.Hara,H.Asano & F.Izumi: "Structure analysis of orthorhombic ZrO_2 by high resolution neutron powder diffraction." Proc.Japan Acad.66. 193-196 (1990)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] S.Kume,O.Ohtaka,T.Yamanaka & A.Navrotsky: "High pressure polymorphs in ceramics and minerals GeO_2 and ZrO_2." Solid State Ionics. 32/33. 285-287 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] H.Ozawa,R.Uno,T.Yamanaka,H.Morikawa,M.Ando & K.Ohsumi: "New Powder diffractometer for the Photon Factory." Rev.Sci.Instrum.60. 2382-2385 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] T.Ashida,S.Kume,E.Ito & A.Navrotsky: "MgSiO_3 ilumenite:heat capacity,thermal expansivity and enthalpy of transformation." Phys.Chem.Minerals.16. 239-245 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] T.Akamatsu,M.Koto,H.Sawamoto,M.Kumazawa,K.Fujino & T.Yamanaka: "Pressure and Temperature dependence of cation distribution in MgーMn olivine." Phys.Chem.Minerals.16. 105-113 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] T. Yamanaka & K. Ogata: "Structure refinement of Ge_2 polymorphs at high pressures and temperature." J. Appl. Cryst.

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] S. Kawasaki, T. Yamanaka, S. Kume & T. Ashida: "Crystallite size effect on the pressure-induced phase transformation of ZrO_2." Solid State Comm. 76. 527-530 (1990)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] O. Ohtaka, T. Yamanaka, S. Kume, N. Hara, H. Asano & F. Izumi: "Structure analysis of orthorhombic ZrO_2 by high resolution neutron powder diffraction." Proc. Japan Acad.66, B,. 193-196 (1990)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] S. Kume, O. Ohtaka, T. Yamanaka & A. Navrotsky: "High pressure polymorphs in ceramics and minerals GeO_2 and ZrO_2." Solid State Ionics. 32/33. 285-587 (1989)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] H. Ozawa, R. Uno, T. Yamanaka, H. Morikawa, M. Ando & K. Ohsumi: "New Powder diffractometer for the Photon Factory." Rev. Sci. Instrum.60. 2382-2385 (1989)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] T. Ashida, S. Kume, E. Ito & A. Navrotsky: "MgSiO_3 ilumenite : heat capacity , thermal expansivity and enthalpy of transformation." Phys. Chem. Minerals.16. 239-245 (1988)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] T. Akamatsu, M. Koto, H. Sawamoto, M. Kumazawa, K. Fujino & T. Yamanaka: "pressure and Temperature dependence of cation distribution in MgーMn olivine." Phys. Chem. Minerals. 16. 105-133 (1988)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] R. Uno H. Ozawa, T. Yamanaka, H. Morikawa, M. Ando, K. Ohsumi & K. Yukino: "Powder diffractometry at the Tsukuba Photon Factory." Aust. J. Phys.41. 133-144 (1988)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1990 Final Research Report Summary
  • [Publications] S.Kawasaki,T.Yamanaka,S,Kume & T.Ashida: "Crystallite size effect on the pressureーinduced phase transformation of ZrO_2." Solid State Comm.76. 527-530 (1990)

    • Related Report
      1990 Annual Research Report
  • [Publications] O.Ohtaka,T.Yamanaka,S.Kume,N.Hara,H.Asano & F.Izumi: "Structure analysis of orthorhombic ZrO_2 by high resolution neutron powder diffraction." Proc.Japan Acad.66. 193-196 (1990)

    • Related Report
      1990 Annual Research Report
  • [Publications] S.Kume,O.Ohtaka,T.Yamanaka & A.Navrotsky: "High pressure polymorphs in ceramics and minerals GeO_2 and ZrO_2." Solid State Ionics. 32/33. 285-287 (1989)

    • Related Report
      1990 Annual Research Report
  • [Publications] H.Ozawa,R.Uno,T.Yamanaka,H.Morikawa,M.Ando & K.Ohsumi: "New powder diffractometer for the Photon Factory." Rev.Sci.Instrum.60. 2382-2385 (1989)

    • Related Report
      1990 Annual Research Report
  • [Publications] T.Ashida,S.Kume,E.Ito & A.Navrotsky: "MgSiO_3 ilumenite:heat capacity,thermal expansivity and enthalpy of transformation." Phys.Chem.Minerals.16. 239-245 (1988)

    • Related Report
      1990 Annual Research Report
  • [Publications] T.Akamatsu,M.Koto,H.Sawamoto,M.Kumazawa,K.Fujino & T.Yamanaka: "Pressure and Temperature dependence of cation distribution in MgーMn olivine." Phys.Chem.Minerals.16. 105-113 (1988)

    • Related Report
      1990 Annual Research Report
  • [Publications] Uno,R.,Ozawa,H.,Yamanaka,T.,Morikawa,H.,Ando,M.,Ohsumi,K.&Yukino,K.: "Powder Diffractometry at the Tsukuba Photon Factory." Aust.J.Phys.41. 133-144 (1988)

    • Related Report
      1989 Annual Research Report
  • [Publications] Ozawa,H.,Uno,R.,Yamanaka,T.,Morikawa.,Ando,M.&Ohsumi,K.: "New powder diffractometer for the Photon Factory." Rev.Sci.Instrum. 60. 2382-2385 (1989)

    • Related Report
      1989 Annual Research Report
  • [Publications] Kume,S.,Ohtaka,O.,Yamanaka,T.&Navrotsky,A.: "High Pressure Polymorphs in Ceramics and Minerals GeO_2 and ZrO_2" Solid State Ionics. 32/33. 285-287 (1989)

    • Related Report
      1989 Annual Research Report
  • [Publications] Yamanaka,T.,Ogata,K.: Journal of Applied crystallography.

    • Related Report
      1988 Annual Research Report
  • [Publications] Uno,R.;Ozara,H.;Yamanaka,T;Morikawa,H;Ando,M.;Ohsumi,K.;Yukino,K.;Kawasaki,T.: Australian Journal of Physics. 41. 133-44 (1988)

    • Related Report
      1988 Annual Research Report

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Published: 1988-04-01   Modified: 2016-04-21  

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