Theory and Practice – Multianvil Cells and High-Pressure Experimental Methods

Advance of high-pressure Earth science has strongly relied on development of the high-pressure experimental technology. Multianvil apparatuses (MAAs) were invented based on the principles of high-pressure design extracted from the technologies of the opposed anvil-type high-pressure apparatuses. Due to the massive support and lateral support of the anvils, attainable pressure in MAAs far exceeds the compressive strength of the anvil material. Advantages of the MAAs over the opposed anvil apparatuses including the diamond anvil cell are larger sample volume and much higher hydrostatic compression. Following the pioneering Hall’s (1958) tetrahedral apparatus, a cubic, and an octahedral MAAs were successively developed in the late 1960s. Among them, the octahedral (Kawai-type) apparatus has been the most widely used in laboratories of Earth science for various purposes such as material synthesis, phase equilibrium, and physical property measurement. Improvements and devices in this apparatus are described, which are anvil materials, pressure media, gasket materials, the manners of pressure calibration methods for sample heating and temperature measurement. Applications to determination of phase equilibrium, crystal growth, and electrical conductivity measurement at high pressure and high temperature are also shown. The double-staged systems to compress the assembly of eight cubic anvils (the Kawai cell) via the cubic (DIA-type) guide block with the aid of a uniaxial press are interfaced with synchrotron radiation facilities. This method has made various kinds of researches under precisely controlled pressure and temperature conditions, which include determinations of phase equilibrium, equation of state, measurement of density, and viscosity of melt, etc. Experimental procedures for in situ X-ray diffraction study using energy dispersive method are described, emphasizing importance of the pressure scale. The reinvestigated α–β, β–γ transformation boundaries in Mg2SiO4 determined based on the NaCl pressure scale are generally consistent with those determined by the quench method. However, the boundary for the dissociation of γ-phase into perovskite and periclase is controversial, various locations in the P–T space being proposed. Part of the discrepancy originates from employment of the different pressure scales which are not mutually consistent. Other origins are uncertainty of temperature measurement and inherent slow reaction kinetics. Sphere falling viscometry using X-ray radiography is surveyed. Recent applications of the Kawai-type apparatus to rheological and acoustic emission studies are also briefly described. The maximum attainable pressure of the Kawai-type apparatus has reached 72 GPa by equipment of sintered diamond (SD) anvil. Pressures higher than 100 GPa may be generated near future by improvement of quality of SD. Therefore, we can more quantitatively determine the state of the Earth’s interior. Generation of pressures to 30 GPa over a volume of c. 1 cm3 or more is another direction to be proceeded. The technology can be applied to grow large crystals and to measure various properties of geophysically important materials.

[1]  S. Ono,et al.  Thermoelastic properties of the high-pressure phase of SnO2 determined by in situ X-ray observations up to 30 GPa and 1400 K , 2000 .

[2]  Numerical modelling of the growth dynamics of a simple silicic lava dome , 2003 .

[3]  Michael Sung,et al.  Carbon nitride and other speculative superhard materials , 1996 .

[4]  H. Terasaki,et al.  The effect of temperature, pressure, and sulfur content on viscosity of the Fe–FeS melt , 2001 .

[5]  Murli H. Manghnani,et al.  Pressure Measurement at High Temperature in X-Ray Diffraction Studies: Gold as a Primary Standard , 1982 .

[6]  M. Carpenter,et al.  Some simplifications to multianvil devices for high pressure experiments , 1990 .

[7]  Y. Ohishi,et al.  Letter. Stability and equation of state of MgGeO3 post-perovskite phase , 2005 .

[8]  D. C. Presnall,et al.  Melting of enstatite (MgSiO3) from 10 to 16.5 GPa and the forsterite (Mg2SiO4)‐majorite (MgSiO3) eutectic at 16.5 GPa: Implications for the origin of the mantle , 1990 .

[9]  Ashutosh Kumar Singh,et al.  The lattice strains in a specimen (cubic system) compressed nonhydrostatically in an opposed anvil device , 1993 .

[10]  Jiuhua Chen,et al.  Olivine flow mechanisms at 8 GPa , 2003 .

[11]  J. Brown The NaCl pressure standard , 1999 .

[12]  Daniel L. Decker,et al.  Equation of State of NaCl and Its Use as a Pressure Gauge in High-Pressure Research , 1965 .

[13]  H. Fujisawa,et al.  Olivine-spinel transition in the system Mg2SiO4-Fe2SiO4 at 800°C , 1966 .

[14]  T. Kikegawa,et al.  In situ X ray observation of high‐pressure phase transitions of MgSiO3 and thermal expansion of MgSiO3 perovskite at 25 GPa by double‐stage multianvil system , 1995 .

[15]  M. Murakami,et al.  In situ measurements of the majorite‐akimotoite‐perovskite phase transition boundaries in MgSiO3 , 2001 .

[16]  P. Meredith,et al.  Detection and analysis of microseismicity in multi anvil experiments , 2004 .

[17]  Y. M. Borzdov,et al.  Diamond formation through carbonate-silicate interaction , 2002 .

[18]  K. Hirose,et al.  Experimentally determined postspinel transformation boundary in Mg2SiO4 using MgO as an internal pressure standard and its geophysical implications , 2004 .

[19]  M. Walter,et al.  Melting experiments of mantle materials under lower mantle conditions with implications for magma ocean differentiation , 2004 .

[20]  A. E. Ringwood,et al.  Synthesis of majorite and other high pressure garnets and perovskites , 1971 .

[21]  E. Ito,et al.  High-pressure synthesis of ZnSiO3 ilmenite , 1974 .

[22]  A. E. Ringwood,et al.  The system Mg2SiO4Fe2SiO4 at high pressures and temperatures , 1970 .

[23]  O. Shimomura,et al.  SPring-8 Beamlines for High Pressure Science with Multi-Anvil Apparatus , 1998 .

[24]  D. Weidner,et al.  Crystal growth of MgSiO3 perovskite , 1986 .

[25]  Jiuhua Chen,et al.  Deformation experiments using synchrotron X-rays: in situ stress and strain measurements at high pressure and temperature , 2004 .

[26]  S. C. Parker,et al.  The MD simulation of the equation of state of MgO: Application as a pressure calibration standard at high temperature and high pressure , 2000 .

[27]  H. Sumiya,et al.  Formation of pure polycrystalline diamond by direct conversion of graphite at high pressure and high temperature , 2004 .

[28]  D. Rubie,et al.  A new large-volume multianvil system , 2004 .

[29]  Xu,et al.  The effect of alumina on the electrical conductivity of silicate perovskite , 1998, Science.

[30]  A. E. Ringwood,et al.  The constitution of the mantle - II. Further data on the olivine-spinel transition , 1958 .

[31]  T. Yagi,et al.  Temperature distribution in a cylindrical furnace for high‐pressure use , 1988 .

[32]  A. E. Ringwood,et al.  Phase transformations and the constitution of the mantle , 1970 .

[33]  A. Schultz,et al.  Variations in the electrical conductivity of the upper mantle beneath North America and the Pacific Ocean , 2000 .

[34]  J. Leger,et al.  X-ray diffraction study of the phase transitions and structural evolution of tin dioxide at high pressure:ffRelationships between structure types and implications for other rutile-type dioxides , 1997 .

[35]  K. Kawabe,et al.  High-pressure generation in the Kawai-type apparatus equipped with sintered diamond anvils: application to the wurtzite–rocksalt transformation in GaN , 2005 .

[36]  S. M. Stishov,et al.  Another step toward an international practical pressure scale: 2nd AIRAPT IPPS task group report , 1986 .

[37]  T. Yagi,et al.  Direct determination of coesite- stishovite transition by in-situ X-ray measurements , 1976 .

[38]  A. Kubo,et al.  Post-garnet transitions in the system Mg4Si4O12–Mg3Al2Si3O12 up to 28 GPa: phase relations of garnet, ilmenite and perovskite , 2000 .

[39]  H. Mao,et al.  Behavior of thermocouples under high pressure in a multi-anvil apparatus , 2003 .

[40]  T. Kikegawa,et al.  An in situ X ray diffraction study of the kinetics of the Ni2SiO4 olivine‐spinel transformation , 1990 .

[41]  E. Watson,et al.  Assessment of temperature gradients in multianvil assemblies using spinel layer growth kinetics , 2003 .

[42]  T. Duffy,et al.  Equation of state of gold and its application to the phase boundaries near 660 km depth in Earth’s mantle , 2002 .

[43]  K. Suito,et al.  Thermoelastic properties of periclase and magnesiowüstite under high pressure and high temperature , 1999 .

[44]  Y. Ohishi,et al.  Post-Perovskite Phase Transition in MgSiO3 , 2004, Science.

[45]  井上 勝彦 Development of high temperature and high pressure X-ray diffraction apparatus with energy dispersive technique and its geophysical applications , 1976 .

[46]  H. M. Strong,et al.  Pressure Dependence of the emf of Thermocouples to 1300°C and 50 kbar , 1965 .

[47]  N. Kawai A Static High Pressure Apparatus with Tapering Multi-Pistons Forming a Sphere. I , 1966 .

[48]  T. Katsura,et al.  A large-volume high-pressure and high-temperature apparatus for in situ X-ray observation, ‘SPEED-Mk.II’ , 2004 .

[49]  S. Ono,et al.  Post-spinel transition in Mg2SiO4 determined by high P–T in situ X-ray diffractometry , 2003 .

[50]  B. Gutenberg On the layer of relatively low wave velocity at a depth of about 80 kilometers , 1948 .

[51]  H. Sawamoto Single crystal growth of the modified spinel (β) and spinel (γ) phases of (Mg,Fe)2SiO4 and some geophysical implications , 1986 .

[52]  T. Kikegawa,et al.  HIP production of a diamond/SiC composite and application to high-pressure anvils , 2004 .

[53]  K. Suito PHASE TRANSFORMATIONS OF PURE Mg2SiO4 INTO A SPINEL STRUCTURE UNDER HIGH PRESSURES AND TEMPERATURES , 1972 .

[54]  A. Oganov,et al.  Theoretical and experimental evidence for a post-perovskite phase of MgSiO3 in Earth's D″ layer , 2004, Nature.

[55]  K. Koto,et al.  High temperature X-ray study of single crystal stishovite synthesized with Li2WO4 as flux , 1986 .

[56]  H. Mao,et al.  Quasi‐hydrostatic compression of magnesium oxide to 52 GPa: Implications for the pressure‐volume‐temperature equation of state , 2001 .

[57]  R. Liebermann,et al.  Modern techniques in measuring elasticity of Earth materials at high pressure and high temperature using ultrasonic interferometry in conjunction with synchrotron X-radiation in multi-anvil apparatus , 2004 .

[58]  P. Shearer,et al.  Global mapping of topography on transition zone velocity discontinuities by stacking SS precursors , 1998 .

[59]  R. Jeanloz,et al.  Electrical conductivity of (Mg,Fe)SiO3 perovskite and a perovskite-dominated assemblage at lower man , 1987 .

[60]  O. Anderson,et al.  Measured elastic moduli of single-crystal MgO up to 1800 K , 1989 .

[61]  E. Ito,et al.  High-pressure transformations in silicates, germanates, and titanates with ABO3 stoichiometry , 1979 .

[62]  T. Katsura,et al.  Determination of the phase boundary between the B1 and B2 phases in NaCl by in situ x-ray diffraction , 2003 .

[63]  R. Hazen,et al.  Structure and twinning of single-crystal MgSiO3 garnet synthesized at 17 GPa and 1800 oC , 1989 .

[64]  E. Ito,et al.  An ultrahigh‐pressure furnace assembly to 100 Kbar and 1500°C with minimum temperature uncertainty , 1982 .

[65]  S. Ono,et al.  In situ Observation of ilmenite‐perovskite phase transition in MgSiO3 using synchrotron radiation , 2001 .

[66]  T. Katsura,et al.  Electrical Conductivity Measurement of Minerals at High Pressures and Temperatures , 1998 .

[67]  A. Onodera,et al.  A New Device for Pressure Vessels , 1973 .

[68]  Uchida,et al.  The postspinel phase boundary in Mg2SiO4 determined by in situ X-ray diffraction , 1998, Science.

[69]  T. Kondo Ultrahigh-pressure and high-temperature generation by use of the MA8 system with sintered-diamond anvils , 1993 .

[70]  O. Nishikawa,et al.  In situ X‐ray observation of iron using Kawai‐type apparatus equipped with sintered diamond: Absence of β phase up to 44 GPa and 2100 K , 2003 .

[71]  E. Ito,et al.  Postspinel transformations in the system Mg2SiO4‐Fe2SiO4 and some geophysical implications , 1989 .

[72]  G. Kennedy,et al.  Effect of Pressure on the emf of Chromel‐Alumel and Platinum‐Platinum 10% Rhodium Thermocouples , 1970 .

[73]  Jianzhong Zhang,et al.  In situ X-ray observations of the coesite-stishovite transition: reversed phase boundary and kinetics , 1996 .

[74]  N. Olsen Long-period (30 days-1 year) electromagnetic sounding and the electrical conductivity of the lower mantle beneath Europe , 1999 .

[75]  O. Shimomura,et al.  In situ observation of the olivine‐spinel phase transformation in Fe2SiO4 using synchrotron radiation , 1987 .

[76]  Manabu Kato,et al.  The use of composite metal gaskets to improve pressure generation in multiple anvil devices , 1984 .

[77]  N. Nishiyama,et al.  Comparison between the Au and MgO pressure calibration standards at high temperature , 2002 .

[78]  H. T. Hall,et al.  High Pressure Polymorphism in Cesium , 1964, Science.

[79]  O. Anderson,et al.  Anharmonicity and the equation of state for gold , 1989 .

[80]  High-pressure behavior of MnGeO3 and CdGeO3 perovskites and the post-perovskite phase transition , 2005 .

[81]  D. Lindsley,et al.  Diopside-enstatite equilibria at 850 degrees to 1400 degrees C, 5 to 35 kb , 1976 .

[82]  T. Irifune,et al.  In situ X-ray observations of phase transitions in MgAl2O4 spinel to 40 GPa using multianvil apparatus with sintered diamond anvils , 2002 .

[83]  H. Mao,et al.  Analysis of lattice strains measured under nonhydrostatic pressure , 1998 .

[84]  Eiji Ito,et al.  MgSiO 3 (ilmenite-type); single crystal X-ray diffraction study , 1982 .

[85]  T. Katsura Phase-relation studies of mantle minerals by in situ X-ray diffraction using multianvil apparatus , 2007 .

[86]  Kazuo Inoue,et al.  A compact cubic anvil high pressure apparatus , 1964 .

[87]  S. Endo,et al.  The Generation of Ultrahigh Hydrostatic Pressures by a Split Sphere Apparatus , 1970 .

[88]  H. T. Hall,et al.  High pressure-high temperature X-ray diffraction apparatus , 1964 .

[89]  R. Ando,et al.  Viscosity of peridotite liquid up to 13 GPa: Implications for magma ocean viscosities , 2005 .

[90]  K. Hirose,et al.  A critical evaluation of pressure scales at high temperatures by in situ X-ray diffraction measurements , 2004 .

[91]  J. Poirier,et al.  Electrical conductivity of the Earth's lower mantle , 1989, Nature.

[92]  M. Rivers,et al.  In situ X-ray diffraction study of phase transitions of FeTiO3 at high pressures and temperatures using a large-volume press and synchrotron radiation , 2006 .

[93]  T. Kondo,et al.  Thermoelastic properties of MgSiO3 perovskite determined by in situ X ray observations up to 30 GPa and 2000 K , 1996 .

[94]  E. Ito,et al.  Report on the First International Pressure Calibration Workshop , 1998 .

[95]  H. T. Hall Some High‐Pressure, High‐Temperature Apparatus Design Considerations: Equipment for Use at 100 000 Atmospheres and 3000°C , 1958 .

[96]  D. Dobson,et al.  The flux growth of magnesium silicate perovskite single crystals , 2004 .

[97]  R. Roy,et al.  New High-Pressure Polymorph of Zinc Oxide , 1962, Science.

[98]  T. Yoshino,et al.  Hydrous olivine unable to account for conductivity anomaly at the top of the asthenosphere , 2006, Nature.

[99]  T. Yoshino,et al.  Olivine‐wadsleyite transition in the system (Mg,Fe)2SiO4 , 2004 .

[100]  T. Kikegawa,et al.  In situ determination of the phase boundary between Wadsleyite and Ringwoodite in Mg2SiO4 , 2000 .

[101]  F. Birch Elasticity and Constitution of the Earth's Interior , 1952 .

[102]  Kiminori Sato,et al.  Electrical conductivity of silicate perovskite at lower-mantle conditions , 1998, Nature.

[103]  H. Terasaki,et al.  Effect of pressure on the viscosity of Fe‐S and Fe‐C liquids up to 16 GPa , 2006 .

[104]  Yousheng Xu,et al.  In-situ Electrical Conductivity Measurements up to 20 GPa in the Multi-anvil Apparatus , 1998 .

[105]  T. Katsura,et al.  The system Mg2SiO4‐Fe2SiO4 at high pressures and temperatures: Precise determination of stabilities of olivine, modified spinel, and spinel , 1989 .

[106]  Katsuhiko Inoue,et al.  Cubic Anvil X-Ray Diffraction Press Up to 100 kbar and 1000°C , 1973 .

[107]  H. Jeffreys The Times of P, S and SKS, and the Velocities of P and S , 1939 .

[108]  T. Kikegawa,et al.  The Phase Boundary Between α- and β-Mg2SiO4 Determined by in Situ X-ray Observation , 1994, Science.

[109]  H. Utada,et al.  A semi‐global reference model for electrical conductivity in the mid‐mantle beneath the north Pacific region , 2003 .

[110]  T. Yagi,et al.  A new, post-stishovite highpressure polymorph of silica , 1989, Nature.

[111]  J. Leger,et al.  The high-pressure phase transition sequence from the rutile-type through to the cotunnite-type structure in , 1996 .

[112]  L. Liu A Fluorite Isotype of SnO2 and a New Modification of TiO2: Implications for the Earth's Lower Mantle. , 1978, Science.

[113]  Daniel L. Decker,et al.  High‐Pressure Equation of State for NaCl, KCl, and CsCl , 1971 .

[114]  T. Kikegawa,et al.  High‐pressure generation by a multiple anvil system with sintered diamond anvils , 1989 .

[115]  A. E. Ringwood,et al.  Synthesis of a perovskite-type polymorph of CaSiO3 , 1975 .

[116]  A. E. Ringwood,et al.  Single crystal analysis of the structure of stishovite , 1978, Nature.

[117]  N. Hamaya,et al.  Experimental Investigation on the Mechanism of Olivine → Spinel Transformation: Growth of Single Crystal Spinel from Single Crystal Olivine in Ni2SiO4 , 1982 .

[118]  Y. Sato Pressure-volume relationship of stishovite under hydrostatic compression , 1977 .

[119]  H. T. Hall Ultra‐High‐Pressure, High‐Temperature Apparatus: the ``Belt'' , 1960 .

[120]  T. Gasparik Transformation of enstatite — diopside — jadeite pyroxenes to garnet , 1989 .

[121]  H. Mao,et al.  Elasticity of MgO and a primary pressure scale to 55 GPa. , 2000, Proceedings of the National Academy of Sciences of the United States of America.

[122]  B. Gutenberg PKKP, P′P′, and the Earth's core , 1951 .

[123]  T. Tsuchiya First‐principles prediction of the P‐V‐T equation of state of gold and the 660‐km discontinuity in Earth's mantle , 2003 .