US3647331A - Ultrahigh pressure-temperature apparatus - Google Patents

Ultrahigh pressure-temperature apparatus Download PDF

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Publication number
US3647331A
US3647331A US18143A US3647331DA US3647331A US 3647331 A US3647331 A US 3647331A US 18143 A US18143 A US 18143A US 3647331D A US3647331D A US 3647331DA US 3647331 A US3647331 A US 3647331A
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Prior art keywords
adiabatic
thermostable
pressure
discs
electrically conductive
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Expired - Lifetime
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US18143A
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English (en)
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Tatsuo Kuratomi
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/065—Presses for the formation of diamonds or boronitrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/06—Heating or cooling methods or arrangements specially adapted for performing forging or pressing operations
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S425/00—Plastic article or earthenware shaping or treating: apparatus
    • Y10S425/026—High pressure

Definitions

  • Ultra-high-pressure-temperature apparatus capable of producing and maintaining pressures of the order of 40,000 to 100,000 atmospheres and temperatures of the order of 1,000 to 2,500 C. is desirable to effect, control and study reactions occurring under these conditions.
  • the reactions of various materials subjected to such pressures and temperatures can be employed for research study purposes or to obtain physical and chemical changes which desirably alter the characteristics of the materials.
  • new compounds are known to be formed by subjecting old materials to very high pressures.
  • Ultra-high-pressure-temperature apparatus is also useful for studying the changes in phase of various materials which occur at very high pressures, or for studying the compressibility or electrical, optical or magnetic properties of various materials.
  • An example of a change occurring under these conditions which is of considerable practical utility is the catalytic conversion of nondiamond carbon to the diamond form.
  • Prior art high-pressure-temperature apparatus of this type comprises generally (1) a pair of opposed punch assemblies, each of the punch assemblies terminating in a tapered electrically conductive piston; (2) means for exerting pressure on the punch assemblies, whereby an electrically conductive object positioned between the opposed pistons can be subjected to high pressure; (3) a lateral pressure-resisting annulus, positioned between the opposed pistons and provided with a substantially central aperture circumferentially surrounding the object to be subjected to high pressure, the annulus having a pressure-resisting inner wall surface; (4) means for passing electrical current through the pistons and the object to be subjected to high pressure, whereby to produce a high temperature within the object simultaneously with the high pressure; and (5) thermal and electrical insulating gaskets positioned in the aperture of the lateral pressure-resisting annulus and circumferentially surrounding the tapered pistons.
  • FIG. 1 A typical prior art apparatus is illustrated in FIG. 1, wherein a lateral pressure-resisting annulus 4 having apressure-resisting inner wall surface 5 is shown surrounding object 7.
  • Opposed tapered electrically conductive pistons 6 and 6 are urged toward object 7 by conventional means (not shown) to produce high pressure in object 7.
  • Thermally and electrically insulating gaskets 8 and 8 are provided to separate pistons 6 and 6 from annulus 4, but not from object 7. Electricity is then passed through piston 6, object 7 and piston 6, thus heating object 7 by internal resistance heating.
  • Annulus 4 is strengthened and reinforced with several layers of steel rings.
  • Apparatus of this type is frequently capable of pressures in excess of 80,000 atmospheres and temperatures in excess of 2,000 C., and further details of its construction and operation are described in the prior art, for example US. Pat. No. 2,941,248.
  • Such apparatus is subject to the disadvantage, however, that the pressure-resisting annulus 4 and pistons 6 and 6 bear much of the pressure and heat of the reaction within object 7, with the result that these parts are subject to fracture and frequently need replacement.
  • FIG. 1 is a sectional schematic diagram of the central portion of conventional high-pressure-temperature apparatus as described above.
  • FIG. 2 is a sectional schematic diagram of the central portion of apparatus according to the present invention.
  • FIG. 3 is a sectional view of the apparatus of FIG. 2, taken along line 3-3 ofFIG. 2.
  • FIGS. 2 and 3 of the drawings the apparatus of the present invention will now be described in detail.
  • Lateral pressure-resisting annulus l 1 having a vertical cylindrical shape for its pressure-resisting inner wall surface surrounds circumferentially the object 20 to be subjected to high pressure.
  • Materials which can be used for annulus 11 include ultrahard alloys, high-speed steel and die steel; these materials themselves are known in the art.
  • Above and below object 20 are opposed punch assemblies (not shown), terminating in tapered electrically conductive pistons 12 and 12'. It should be noted that references herein to above,” below, lateral"and the like are merely indicative of orientation when the apparatus is arranged with the pistons 12 and 12' in a vertical configuration, and the apparatus need not be so arranged. This designation is convenient, however, in indicating the relative orientation of the various parts of the apparatus herein described.
  • Materials which can be used for pistons 12 and 12' include die steels and ultrahard alloys such as cemented tungsten carbide. One such alloy which is commercially available contains 94 percent tungsten carbide and 6 percent cobalt.
  • thermostable hollow cylinder 15 Within the aperture of lateral pressure-resisting annulus 11 and circumferentially surrounding object 20 is an adiabatic, electrically nonconductive, thermostable hollow cylinder 15.
  • Preferred materials for cylinder 15 include thorium oxide, zirconium oxide, hafnium oxide and mixtures thereof. In order that temperatures of 2,500 C. can be generated within object 20, the material for hollow cylinder 15 must have a melting point of at least 2,600 C. and be adiabatic and electrically nonconductive. Materials with sufficiently high melting points and electrical resistivities include the following:
  • Calcium oxide and magnesium oxide are not preferred because of their comparatively high thermal conductivities.
  • Calcium oxide has the further disadvantage of reacting with carbon at temperatures above 2,000 C. to form calcium carbide. The carbonization reaction advances rapidly and continuously, whereas the carbides of thorium and zirconium, for example, form thin filmy protective coatings on the inner face of hollow cylinder 15, so that further carbonization does not occur.
  • a pair of adiabatic thermostable discs 19 and 19' disc 19 being positioned above object 20, between object 20 and piston 12; and disc 19' being positioned below object 20, between object 20 and piston 12'.
  • Discs 19 and 19' are of such diameter, however, as to allow the passage of electrical current from one piston to the other piston'through object 20.
  • Discs l8 and 18 are simultaneously in electrical contact with rings 17 and 17', respectively, on the one hand, and object 20 on the other.
  • electrical current can pass from piston 12 to ring 17 to disc 18 to object 20 to disc 18 to ring 17 to piston 12, while pistons 12 and 12' are shielded by adiabatic thermostable discs 19 and 19 from the heat and pressure generated in object 20.
  • Preferred materials for adiabatic thermostable discs 19 and 19 include thorium oxide, zirconium oxide, hafnium oxide, and mixtures thereof.
  • a still more preferred embodiment of this invention includes a second adiabatic, electrically nonconductive, thermostable, hollow cylinder 14 positioned within the aperture of the lateral pressurerresisting annulus 1 l, and circumferentially surrounding (l) the first adiabatic, electrically nonconductive, thermostable, hollow cylinder 15; (2) the adiabatic, thermostable discs 19 and 19'; (3) the electrically conductive rings 17 and 17'; (4) the electrically conductive discs 18 and 18'; and (5) the object 20 to be subjected to high pressure,
  • Preferred materials for adiabatic, electrically nonconductive, thermostable, hollow cylinder 14 include zirconium oxide, pyrophyllite, and mixtures thereof.
  • a still more preferred embodiment of this invention includes a metallic hollow cylinder 13, positioned within the aperture of the lateral pressure-resisting annulus 11 and circumferentially surrounding the second adiabatic, electrically nonconductive, thermostable, hollow cylinder 14.
  • Cylinder 13 should be of a metallic material of great hardness and tenacity so as to reduce the high pressures-generated within the apparatus (by urging pistons 12 and 12' towards object 20), and thereby subject annulus 11 to less stress than would otherwise be the case.
  • annulus 11 is able to maintain its hardness and tenacity without being melted or worsened in quality by the full heat and pressures generated within object 20.
  • Preferred materials for cylinder 13 include ultrahard alloys, high-speed steel, die steel and ceramic-metallic (cermet) alloys.
  • cylindrical shapes for the pressure-resisting inner wall surface of pressure-resisting annulus 11 and for cylinders l3, l4 and 15, these innermost parts which bear the greatest heat and pressure of the apparatus can easily be replaced, if need be.
  • the cylindrical shape also aids in the transmission of pressures from pistons 12 and 12 to object 20.
  • Thermal and electrical insulating gaskets l6 and 16 preferably of pyrophyllite, surround pistons 12 and 12', respectively, to complete the portion of the apparatus shown.
  • a high-pressure-temperature apparatus for subjecting an object to high pressure, comprising: (a) a pair of opposed,
  • the invention which comprises the provision of a vertical cylindrical shape for the pressure-resisting inner wall surface of the pressure-resisting annulus, and in combination therewith l) a first adiabatic, electrically nonconductive, thermostable, hollow cylinder, positioned within the aperture of the lateral, pressure-resisting annulus, and circumferentially surrounding the object to be subjected to high pres sure, said first adiabatic, electrically nonconductive, thermostable, hollow cylinder consisting essentially of thorium oxide, zirconium
  • thermostable discs consist essentially of hafnium oxide.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
US18143A 1969-03-10 1970-03-10 Ultrahigh pressure-temperature apparatus Expired - Lifetime US3647331A (en)

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JP44017548A JPS503025B1 (da) 1969-03-10 1969-03-10

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US00204414A Expired - Lifetime US3727028A (en) 1969-03-10 1971-12-03 Ultra high pressure-temperature apparatus

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DE (1) DE2011010A1 (da)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4284398A (en) * 1979-02-02 1981-08-18 Metzeler Schaum Gmbh Apparatus for the manufacture of a foam material ball with an embossed surface
US4475880A (en) * 1980-03-27 1984-10-09 Manesty Machines Limited Tabletting machines
US4927345A (en) * 1988-03-03 1990-05-22 Ohwada Carbon Industrial Co., Ltd. Press cylinder for high-temperature, high-pressure pressing machine
US5244368A (en) * 1991-11-15 1993-09-14 Frushour Robert H High pressure/high temperature piston-cylinder apparatus
WO2013154952A1 (en) * 2012-04-09 2013-10-17 Smith International Inc. High-pressure high-temperature cell
US10239273B2 (en) 2012-04-09 2019-03-26 Smith International, Inc. Thermal insulation layer and pressure transfer medium for high-pressure high-temperature cell

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2220349C3 (de) * 1972-04-26 1975-02-27 Fried. Krupp Gmbh, 4300 Essen Vorrichtung zur Erzeugung von hohen Drücken und Temperaturen
GB1506308A (en) * 1975-06-12 1978-04-05 Kennametal Inc High temperature high pressure apparatus having a ductile driver element
FI53085C (da) * 1975-12-23 1978-02-10 Levanto Oy L A
US4097208A (en) * 1976-01-02 1978-06-27 Hiroshi Ishizuka Ultrahigh pressure apparatus for diamond synthesis
DE2600395C3 (de) * 1976-01-07 1982-04-29 Hiroshi Tokyo Ishizuka Ultrahochdruck-Apparat
JPS6059008B2 (ja) * 1980-04-18 1985-12-23 博 石塚 改良超高圧装置
JPS61133135A (ja) * 1984-11-29 1986-06-20 Kobe Steel Ltd 固体超高圧加圧装置
US5308688A (en) * 1992-12-28 1994-05-03 Hughes Missile Systems Company Oxidation resistant diamond composite and method of forming the same
US20040126480A1 (en) * 2002-12-26 2004-07-01 Unilever Bestfoods North America Food process

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2941252A (en) * 1957-03-20 1960-06-21 Gen Electric Reaction vessel
US3061877A (en) * 1959-11-05 1962-11-06 Adamant Lab Proprietary Ltd High-pressure die
US3096544A (en) * 1960-06-17 1963-07-09 Asea Ab High pressure vessel with punch
US3201828A (en) * 1961-12-27 1965-08-24 Asea Ab High pressure apparatus
US3249964A (en) * 1963-09-09 1966-05-10 Stackpole Carbon Co Producing dense articles from powdered carbon and other materials
US3313004A (en) * 1965-06-14 1967-04-11 Fred W Vahldiek High pressure electrical resistance cell
US3350743A (en) * 1964-11-04 1967-11-07 Ishizuka Hiroshi High temperature and high pressure apparatus
US3383737A (en) * 1966-05-05 1968-05-21 Herbert H. Greger Apparatus for pressure sintering ceramic material
US3407445A (en) * 1966-03-02 1968-10-29 Gen Electric High pressure reaction vessel for the preparation of diamond

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1220376A (en) * 1967-05-04 1971-01-27 Hiroshi Ishizuka Improvements in or relating to a high temperature high pressure apparatus

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2941252A (en) * 1957-03-20 1960-06-21 Gen Electric Reaction vessel
US3061877A (en) * 1959-11-05 1962-11-06 Adamant Lab Proprietary Ltd High-pressure die
US3096544A (en) * 1960-06-17 1963-07-09 Asea Ab High pressure vessel with punch
US3201828A (en) * 1961-12-27 1965-08-24 Asea Ab High pressure apparatus
US3249964A (en) * 1963-09-09 1966-05-10 Stackpole Carbon Co Producing dense articles from powdered carbon and other materials
US3350743A (en) * 1964-11-04 1967-11-07 Ishizuka Hiroshi High temperature and high pressure apparatus
US3313004A (en) * 1965-06-14 1967-04-11 Fred W Vahldiek High pressure electrical resistance cell
US3407445A (en) * 1966-03-02 1968-10-29 Gen Electric High pressure reaction vessel for the preparation of diamond
US3383737A (en) * 1966-05-05 1968-05-21 Herbert H. Greger Apparatus for pressure sintering ceramic material

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4284398A (en) * 1979-02-02 1981-08-18 Metzeler Schaum Gmbh Apparatus for the manufacture of a foam material ball with an embossed surface
US4475880A (en) * 1980-03-27 1984-10-09 Manesty Machines Limited Tabletting machines
US4927345A (en) * 1988-03-03 1990-05-22 Ohwada Carbon Industrial Co., Ltd. Press cylinder for high-temperature, high-pressure pressing machine
US5244368A (en) * 1991-11-15 1993-09-14 Frushour Robert H High pressure/high temperature piston-cylinder apparatus
WO2013154952A1 (en) * 2012-04-09 2013-10-17 Smith International Inc. High-pressure high-temperature cell
CN104220216A (zh) * 2012-04-09 2014-12-17 史密斯国际有限公司 高压高温单元
US9586376B2 (en) 2012-04-09 2017-03-07 Smith International, Inc. High pressure high temperature cell
US10239273B2 (en) 2012-04-09 2019-03-26 Smith International, Inc. Thermal insulation layer and pressure transfer medium for high-pressure high-temperature cell

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Publication number Publication date
US3727028A (en) 1973-04-10
DE2011010A1 (de) 1970-09-17
JPS503025B1 (da) 1975-01-30

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