US20070009374A1 - Heat-resistant composite diamond sintered product and method for production thereof - Google Patents

Heat-resistant composite diamond sintered product and method for production thereof Download PDF

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US20070009374A1
US20070009374A1 US10/539,507 US53950703A US2007009374A1 US 20070009374 A1 US20070009374 A1 US 20070009374A1 US 53950703 A US53950703 A US 53950703A US 2007009374 A1 US2007009374 A1 US 2007009374A1
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diamond
sintered body
pressure
grain size
heat
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Minoru Akaishi
Keigo Kawamura
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Japan Science and Technology Agency
National Institute for Materials Science
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Japan Science and Technology Agency
National Institute for Materials Science
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Assigned to NATIONAL INSTITUTE FOR MATERIALS SCIENCE, JAPAN SCIENCE AND TECHNOLOGY AGENCY reassignment NATIONAL INSTITUTE FOR MATERIALS SCIENCE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KAWAMURA, KEIGO, AKAISHI, MINORU
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/427—Diamond
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/781—Nanograined materials, i.e. having grain sizes below 100 nm
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the present invention relates to a heat-resistant diamond composite sintered body, and a production method thereof.
  • the inventors reported a method for producing a fine-grain diamond sintered body, which comprises adding oxalic acid dihydrate serving as a source of a CO 2 —H 2 O fluid phase into carbonate to prepare a mixed powder, and applying a natural diamond powder having a grading range (distribution range of particle diameter) of zero to 1 ⁇ m, onto the mixed powder to form a layered structure (see the following Patent Publication 3 and Non-Patent Publications 2 and 3).
  • this production method essentially requires a high temperature of 2000° C. or more.
  • the inventors also reported a method similar to the above method, which comprises sintering a finer-grain diamond powder, for example, having a grading range of zero to 0.1 ⁇ m (see the following Non-Patent Publication 4). In this case, any high-hardness diamond sintered body could not be obtained due to occurrence of abnormal grain growth in diamond.
  • Parent Publication 1 Japanese Patent Publication No. 52-012126
  • Parent Publication 2 Japanese Patent Publication No. 04-050270
  • Parent Publication 3 Japanese Patent Laid-Open Publication No. 2002-187775
  • Non-Patent Publication 1 Diamond and Related Mater., Vol. 5, pp 34-37, Elsevier Science S. A., 1996
  • Non-Patent Publication 2 Journal of the 41st High Pressure Symposium, p 108, the Japan Society of High Pressure Science and Technology, 2000
  • Non-Patent Publication 3 Proceedings of the 8th NIRIM International Symposium on Advanced Materials, pp 33-34, the National Institute for Research in Inorganic Materials, 2001
  • Non-Patent Publication 4 Journal of the 42nd High Pressure Symposium, p 89, the Japan Society of High Pressure Science and Technology, 2001
  • Non-Patent Publication 5 T. Irifune et al., “Characterization of polycrystalline diamonds synthesized by direct conversion of graphite using multi anvil apparatus, 6th High Pressure Mineral Physics Seminar, 28 Aug., 2002, Verbania, Italy
  • a high-hardness diamond sintered body has been produced through a high-pressure/high-temperature sintering treatment under an ultrahigh pressure condition of 5.5 to 7.7 GPa.
  • a material used as the sintered body inevitably remains as a solid in a sintered body after the high-pressure/high-temperature sintering treatment to cause decrease in bonding area between diamond grains.
  • diamond sintered body with the sintering aid is liable to have a lower hardness, and poor properties due to a chemical reaction between diamond and the sintering aid remaining in the sintered body.
  • the conventional sintered body synthetic method using no sintering aid requires an extremely high pressure and temperature.
  • the inventors attempted to synthesize a diamond sintered body by applying a synthetic hydrogen-terminated diamond power with an average grain size of 100 nm, onto a sintering aid consisting of a carbonate-C—H fluid phase to form a layered structure, and subjecting the layered structure to a sintering treatment under high-pressure/high-temperature conditions.
  • a recovered sample had layer-like cracks and carbonate partway infiltrated, homogenous infiltration of the carbonate-C—H fluid phase as a sintering aid could not be achieved.
  • the inventions attempted to sinter a natural diamond powder having a grading range of zero to 0.1 ⁇ m under the conditions of 7.7 GPa and 2300° C. for 15 minutes. In the result, it was proven that a high-hardness diamond sintered body is hardly synthesized from the natural diamond powder having a grading range of zero to 0.1 ⁇ m.
  • the inventors found that the above problem does not unexpectedly occur when a synthetic diamond powder having an average grain size of 200 nm or less is used as a starting material, and sintered under high-pressure/high-temperature conditions equivalent to those in the conventional method for producing a diamond sintered body using a sintering aid, such as carbonate. Based on this knowledge, the inventors finally achieved to synthesize a heat-resistant and time-grained diamond sintered body without use of sintering aid.
  • a sintered body obtained through this production method contains a minute amount of non-diamond carbon as a product. That is, this sintered body is formed as a composite sintered body of a diamond crystal and a non-diamond carbon, and electric conductivity is created therein. This non-diamond carbon would be derived from graphitization in a part of diamond powder as a starting material. Thus, the obtained composite sintered body having electric conductivity can be subjected to an electric discharge machining process. Furthermore, the composite sintered body has luster and glaze which cannot be seen in conventional diamond sintered bodies.
  • the present invention provides a heat-resistant diamond composite sintered body prepared by sintering an ultrafine-grain synthetic diamond powder having an average grain size of 200 nm or less, without using a sintering aid.
  • the composite sintered body comprises a diamond crystal and a minute amount of non-diamond carbon as a product, and has a Vickers hardness of 85 GPa or more.
  • the present invention also provides a method of producing the above heat-resistant diamond composite sintered body, which comprises enclosing a synthetic diamond powder having an average grain size of 200 nm or less, in a capsule made of Ta or Mo, and heating and pressurizing using an ultrahigh-pressure synthesizing apparatus under thermodynamically stable conditions including a temperature of 2100° C. or more and a pressure of 7.7 GPa or more.
  • a synthetic diamond powder is subject to plastic deformation.
  • a powder having a large grain size distribution a powder having a less grain size distribution would have a smaller size distribution in the inter-grain space.
  • a synthetic diamond powder having an approximately even grain size and the smallest possible average grain size is used as a starting material, a heat-resistant diamond composite sintered body would be synthesized without any sintering aid by utilizing plastic deformation easily occurring in diamond grains, and large surface energy inherent in small diamond grain, as a driving force.
  • the heat-resistant diamond composite sintered body synthesized by the production method of the present invention can be used not only for industrial purposes, such as a high-performance tool in cutting tool fields, and oil bits requiring high heat resistance, but also for jewelry items by taking advantage of high refractive index inherent in diamond, luster peculiar to a sintering agent-free diamond sintered body and producibility of a large sintered body.
  • the production method of the present invention can be implemented under pressure/temperature conditions equivalent to those in the conventional method for producing a diamond sintered body using carbonate as a sintering aid.
  • FIG. 1 is a sectional view conceptually showing one example of a sintered-body synthesis capsule which is filled a diamond powder to be sintered through a production method of the present invention.
  • FIG. 2 is a graph showing an X-ray diffraction pattern of a sintered body obtained in Inventive Example 1 ((a): before a heat treatment, (b): after the treatment).
  • FIG. 3 is an electron micrograph of a fracture surface of the sintered body obtained in Inventive Example 1.
  • FIG. 1 is a sectional view showing one example of a sintered-body synthesis capsule which is filled a diamond powder to be sintered through a production method of the present invention.
  • a cylindrical-shaped capsule 3 made of Ta has a graphite disc 4 A attached to the bottom thereof to prevent the deformation of the capsule.
  • a diamond powder layer 2 A is formed on the graphite disc 4 A through a Ta or Mo foil 1 A under a given compacting pressure.
  • the Ta or Mo foil is used for separating diamond powder layers from each other to synthesize a sintered body having a desired thickness, separating the graphite discs from the diamond powder layer, preventing a pressure medium from getting in the capsule, and sealing a fluid phase.
  • a Ta or Mo foil 1 B is placed on the diamond powder layer 2 A.
  • second, three diamond powder layers 2 B, 2 C, 2 D are formed while interposing Ta or Mo foils 1 C, 1 D therebetween.
  • a Ta or Mo foil 1 E is placed on the diamond powder layer 2 D, and a graphite disc 4 B is placed on the Ta or Mo foil 1 E to prevent the deformation of the capsule.
  • This capsule is placed in a pressure medium, and pressurized up to 7.7 GPa or more at room temperature by use of an ultrahigh-pressure apparatus based on a static compression process, such as a belt-type ultrahigh-pressure synthesizing apparatus. Then, under this pressure, the capsule is heated up to a given temperature of 2100° C. or more to perform a sintering treatment. If the pressure is less than 7.7 GPa, a desired heat-resistant sintered body cannot be obtained even if the temperature is equal to or greater than 2100° C. Further, if the temperature is less than 2100° C., a desired heat-resistant sintered body cannot be obtained even if the pressure is equal to or greater than 7.7 GPa. It is desirable to limit the temperature and pressure to a bare minimum in consideration of the capacity of the apparatus, because excessive temperature or pressure simply leads to deterioration in energy efficiency.
  • a synthetic diamond powder having an average grain size of 200 nm or less is obtained by grinding a synthetic diamond powder having a large grain size and classifying the ground powder.
  • the grain size herein is a measured value using a Microtrac UPA particle size analyzer. This measurement method is publicly known (see, for example, Japanese Patent Laid-Open Publication No. 2002-35636).
  • Such a synthetic diamond powder is commercially available (for example, Trade Name: MD200 (average grain size: 200 nm); MD 100 (average grain size: 100 nm) manufactured by Tomei Diamond Co., Ltd.)
  • a commercially-available synthetic diamond powder having an average grain size of 100 nm was used as a starting material.
  • a cylindrical-shaped Ta capsule having a wall thickness of 0.8 mm and an outer diameter of 11.6 mm was prepared, and a graphite disc having a thickness of 2.6 mm was attached to the bottom of the capsule to prevent the deformation of the capsule.
  • 250 mg of the diamond powder was placed on the graphite disc through a Ta foil, and pressed at a compacting pressure of 100 MPa to form a diamond powder layer.
  • a Ta foil was placed on the diamond powder layer, and then a graphite disc having a thickness of 2.6 mm was placed on this Ta foil to prevent the deformation of the capsule.
  • the capsule was subjected to pressure forming, and then an excess part of the upper graphite disc was chipped off.
  • the capsule was placed in a pressure medium of NaCl-10% ZrO 2 , and subjected to a sintering treatment under a pressure of 7.7 GPa at a temperature of 2200° C. for 30 minutes, using a belt-type ultrahigh pressure synthesizing apparatus. After completion of the sintering treatment, the capsule was taken out of the capsule.
  • a product, such as TaC, formed on the surface of the sintered body was removed using a hydrofluoric acid-nitric acid solution, and each of top and bottom surfaces of the sintered body was ground using a diamond wheel to flatten the surfaces.
  • the sintered body has a high grinding resistance, and the sintered body after the grinding had an average value of Vickers hardness of 90 GPa or more.
  • FIG. 2 An X-ray diffraction pattern of the obtained sintered body is shown in FIG. 2 .
  • FIG. 2 ( a ) and FIG. 2 ( b ) shows an X-ray diffraction pattern before the heat treatment in vacuum at 1200° C. for 30 minutes, and an X-ray diffraction pattern after the heat treatment, respectively. As seen from the result in FIG.
  • this diffraction line has no change in position and intensity. This shows that the amount of non-diamond carbon after the heat treatment is not changed at all.
  • FIG. 3 through microscopic observation of the structure of a fracture surface of the sintered body, it was proven that the sintered body comprises fine grains having an average grain size of 80 nm.
  • the diamond sintered body of the present invention has excellent heat resistance, and high wear resistance, and high hardness.
  • this diamond sintered body when used in a finishing cutting work for a difficult-to-machine material, such as high-Si—Al alloy, or an ultraprecision machining process for metal or alloy, it can exhibit excellent cutting and wire drawing performances.
  • this diamond sintered body has sufficient heat resistance suitable for a high cutting speed in oil-drilling bits and particular automobile components.
  • non-diamond carbon is created to form a composite sintered body exhibiting electric conduction properties. The properties make it possible to use an electric discharge machining process as a cutoff process of the sintered body so as to facilitate reduction in machining cost.
  • the composite sintered body has luster and glaze which cannot be seen in conventional diamond sintered bodies.
  • the sintered body can be formed in various shapes by lasering, grinding and polishing as well as the electric discharge machining process. Therefore, it can be expected to use as black diamond for jewelry having luster and glaze which cannot be seen in conventional diamond sintered bodies.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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US10/539,507 2002-12-18 2003-11-19 Heat-resistant composite diamond sintered product and method for production thereof Abandoned US20070009374A1 (en)

Applications Claiming Priority (3)

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JP2002-121802 2002-04-24
JP2002367354A JP3877677B2 (ja) 2002-12-18 2002-12-18 耐熱性ダイヤモンド複合焼結体とその製造法
PCT/JP2003/014763 WO2004054943A1 (ja) 2002-12-18 2003-11-19 耐熱性ダイヤモンド複合焼結体とその製造法

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JP (1) JP3877677B2 (enrdf_load_stackoverflow)
KR (1) KR100642841B1 (enrdf_load_stackoverflow)
CN (1) CN1300053C (enrdf_load_stackoverflow)
RU (1) RU2312844C2 (enrdf_load_stackoverflow)
WO (1) WO2004054943A1 (enrdf_load_stackoverflow)
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US20110241266A1 (en) * 2010-03-31 2011-10-06 Mitsubishi Materials Corporation Production method of fine grain polycrystalline diamond compact
US9950960B2 (en) 2014-04-30 2018-04-24 Sumitomo Electric Industries, Ltd. Composite sintered body
US10457606B2 (en) 2014-04-30 2019-10-29 Sumitomo Electric Industries, Ltd. Composite sintered body
US10870606B2 (en) 2018-03-05 2020-12-22 Wenhui Jiang Polycrystalline diamond comprising nanostructured polycrystalline diamond particles and method of making the same
US11072008B2 (en) * 2015-10-30 2021-07-27 Sumitomo Electric Industries, Ltd. Wear-resistant tool
EP3369717B1 (en) * 2015-10-30 2021-11-03 Sumitomo Electric Industries, Ltd. Composite polycrystal and method for manufacturing same
US11383306B2 (en) * 2016-10-07 2022-07-12 Sumitomo Electric Industries, Ltd. Method for producing polycrystalline diamond body, polycrystalline diamond body, cutting tool, wear-resistance tool and grinding tool

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US9403137B2 (en) 2005-09-15 2016-08-02 Diamond Innovations, Inc. Polycrystalline diamond material with extremely fine microstructures
US20070056778A1 (en) * 2005-09-15 2007-03-15 Steven Webb Sintered polycrystalline diamond material with extremely fine microstructures
US8490721B2 (en) 2009-06-02 2013-07-23 Element Six Abrasives S.A. Polycrystalline diamond
GB0913304D0 (en) * 2009-07-31 2009-09-02 Element Six Ltd Polycrystalline diamond composite compact elements and tools incorporating same
US10287824B2 (en) 2016-03-04 2019-05-14 Baker Hughes Incorporated Methods of forming polycrystalline diamond
CN107402196B (zh) * 2016-05-18 2020-09-25 株式会社岛津制作所 X射线荧光分析仪器及用于其的样品容器
US11292750B2 (en) 2017-05-12 2022-04-05 Baker Hughes Holdings Llc Cutting elements and structures
US11396688B2 (en) 2017-05-12 2022-07-26 Baker Hughes Holdings Llc Cutting elements, and related structures and earth-boring tools
US11536091B2 (en) 2018-05-30 2022-12-27 Baker Hughes Holding LLC Cutting elements, and related earth-boring tools and methods
CN116143518B (zh) * 2021-11-23 2024-09-20 燕山大学 导电高强金刚石/非晶碳复合材料及其制备方法

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ZA200505162B (en) 2007-02-28
KR100642841B1 (ko) 2006-11-10
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RU2005121920A (ru) 2006-01-20
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