WO2005031033A1 - Procede de production d'un diamant cvd ameliore - Google Patents

Procede de production d'un diamant cvd ameliore Download PDF

Info

Publication number
WO2005031033A1
WO2005031033A1 PCT/US2003/026986 US0326986W WO2005031033A1 WO 2005031033 A1 WO2005031033 A1 WO 2005031033A1 US 0326986 W US0326986 W US 0326986W WO 2005031033 A1 WO2005031033 A1 WO 2005031033A1
Authority
WO
WIPO (PCT)
Prior art keywords
diamond
cvd diamond
temperature
cvd
raising
Prior art date
Application number
PCT/US2003/026986
Other languages
English (en)
Inventor
Robert H. Frushour
Wei Li
Original Assignee
Diamond Innovations, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Diamond Innovations, Inc. filed Critical Diamond Innovations, Inc.
Priority to AU2003273252A priority Critical patent/AU2003273252A1/en
Priority to PCT/US2003/026986 priority patent/WO2005031033A1/fr
Publication of WO2005031033A1 publication Critical patent/WO2005031033A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/006—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterized by the colour of the layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • 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
    • B01J2203/00—Processes utilising sub- or super atmospheric pressure
    • B01J2203/06—High pressure synthesis
    • B01J2203/0605—Composition of the material to be processed
    • B01J2203/062—Diamond
    • 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
    • B01J2203/00—Processes utilising sub- or super atmospheric pressure
    • B01J2203/06—High pressure synthesis
    • B01J2203/065—Composition of the material produced
    • B01J2203/0655—Diamond
    • 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
    • B01J2203/00—Processes utilising sub- or super atmospheric pressure
    • B01J2203/06—High pressure synthesis
    • B01J2203/0675—Structural or physico-chemical features of the materials processed
    • B01J2203/069—Recrystallisation

Definitions

  • CND diamond can be classified as either single crystal or polycrystalline. Either type can be manufactured to produce materials that range from opaque to fully transparent. Typical impurities within CND diamond are graphite and hydrogen, although trace amounts of other materials may be present, such as nitrogen. In addition to impurities, there are structural defects which occur that further degrade the material and its properties as compared to a defect free natural diamond. As a result, CND diamond is often opaque or very dark Most industrial applications for diamond require high quality crystals or films. Common applications include lenses that require high optical transmission of light, heat sinks that require very high heat conductivity, and electrical insulators.
  • Synthetic diamond will change from yellow to lighter yellow. It would be advantageous if a method were found that would significantly improve the properties of CND diamond after it is grown. It would also be desirable to form CND diamond with fewer defects that serve to degrade the intrinsic properties of a perfect crystalline diamond material in order to enhance its usage in many applications.
  • a method of improving the optical, thermal, electrical, and mechanical properties of CND diamond which includes the steps of: 1. creating a reaction mass by placing the CND diamond in a pressure transmitting medium that completely encloses the diamond; and 2.
  • reaction mass subjecting the reaction mass to a temperature of at least 1500°C and, preferably, in the range of about 1800°C to about 2900°C under a pressure of at least 4.0 GPA
  • the period of time during which the sample is subjected to HPHT conditions is from less than about one minute to about 30 minutes.
  • the preferred time is between one to five minutes.
  • the actual conditions can be varied depending on the grade and the size of the CND sample.
  • the reaction mass may be subjected to any number of such treatments. Thus, if the desired results were not achieved the first time, the sample may be retreated at HPHT until such time that the desired improvement in characteristics or properties is achieved.
  • Fig. 1 is a cross sectional view of the inner portion of a high pressure cell used to treat CND diamond according to the present invention.
  • DETAILED DESCRIPTION The present invention is a process to heat treat CND diamond at high temperature and high pressure.
  • the outer body 2 is cylindrical in shape and is designed to fit within a central cavity of an ultrahigh pressure and ultrahigh temperature cell, such as that described in US Patent ⁇ os. 3,745,623 or 3,913,280.
  • the outer body 2 is composed of graphite or other material that will readily transmit pressure and remain stable and non-reactive to the CVD diamond 1 at high temperature and high pressure. Other materials for the outer body 2 include, but are not limited to, salt, MgO, or talc.
  • the CVD diamond 1 is encapsulated in the outer body 2.
  • the CVD sample 1 is a stand alone CVD diamond or a CVD coating on diamond or other materials.
  • This assembly should be consolidated to greater than 90% of its theoretical density and made to fit snugly into a HPHT reaction cell, such as that used to manufacture PCD.
  • the entire cell is subjected to pressures in excess of 4.0 GPA and heated to temperature in excess of 1500°C for a time of five minutes. Then the cell is allowed to cool enough so that the CVD diamond does not back-convert to graphite after the pressure is released.
  • the sample 1 is removed from the graphite outer body by mechanical means, such as by tapping with a mallet.
  • the sample can then be further heated in an oven to 725°C for approximately ten minutes in order to obtain a clean and smooth outer diamond surface. This treatment removes any graphite that may have adhered to the sample.
  • EXAMPLE #1 A cubed-shaped CVD coated synthetic type lb diamond, approximately one centimeter square, was encapsulated in a graphite cylinder. The CVD portion was a layer on one side of the cube-shaped natural diamond, approximately one millimeter thick and was opaque to optical transmission. The synthetic diamond substrate was light yellow.
  • the graphite cylinder was loaded into a HPHT reaction vessel that was configured for indirect heating of the reaction mass. Various reaction vessel configurations, which provide the indirect or direct heating, are disclosed in the patent literature and are also useful for carrying out the present HPHT process.
  • Reaction vessels of this type usually of a plurality of interfitting cylindrical members and end plugs or discs for containing a sample in the innermost cylinder.
  • one of the cylindrical members is made of graphite that is heated by the passage of electric current through the cylinder.
  • the reaction mass if composed of graphite, must be electrically insulated from the graphite heater tube by an insulating material, such as talc or salt, to prevent passage of electrical current through the reaction mass.
  • the insulating sleeve is not required as the sample is heated by simply passing electric current through the reaction mass provided it is composed of an electrically conducting material, such as used in this example.
  • the reaction vessel was placed in a conventional HPHT apparatus. First, the pressure was increased to 5.0 GPA, and then the temperature was rapidly brought up to 2200°C. The sample was maintained at these conditions for five minutes, then the temperature was decreased over a period of about one minute to room temperature before the pressure was released.
  • the CVD diamond-coated substrate was removed from the reaction mass and examined under an optical microscope. The opaque CVD diamond layer turned clear and remained firmly bonded to the yellow synthetic type lb diamond

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Selon l'invention, un diamant CVD est chauffé à des températures comprises entre 1500 °C et 2900 °C, et à une pression propre à empêcher une graphitisation significative. On obtient ainsi un diamant CVD présentant des propriétés optiques, électriques, thermiques et mécaniques améliorées.
PCT/US2003/026986 2003-08-26 2003-08-26 Procede de production d'un diamant cvd ameliore WO2005031033A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2003273252A AU2003273252A1 (en) 2003-08-26 2003-08-26 Method of making enhanced cvd diamond
PCT/US2003/026986 WO2005031033A1 (fr) 2003-08-26 2003-08-26 Procede de production d'un diamant cvd ameliore

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2003/026986 WO2005031033A1 (fr) 2003-08-26 2003-08-26 Procede de production d'un diamant cvd ameliore

Publications (1)

Publication Number Publication Date
WO2005031033A1 true WO2005031033A1 (fr) 2005-04-07

Family

ID=34392786

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2003/026986 WO2005031033A1 (fr) 2003-08-26 2003-08-26 Procede de production d'un diamant cvd ameliore

Country Status (2)

Country Link
AU (1) AU2003273252A1 (fr)
WO (1) WO2005031033A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8110041B2 (en) 2002-09-06 2012-02-07 Daniel James Twitchen Coloured diamond

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5011509A (en) * 1989-08-07 1991-04-30 Frushour Robert H Composite compact with a more thermally stable cutting edge and method of manufacturing the same
EP0480895A2 (fr) * 1990-10-11 1992-04-15 Sandvik Aktiebolag Outils diamantés améliorés pour le forage de roches, la coupe de métaux et des applications comme pièce d'usure
EP0671482A1 (fr) * 1994-03-11 1995-09-13 General Electric Company Diamant à tenacité élevée déposée chimiquement en phase vapeur
US5672395A (en) * 1994-05-05 1997-09-30 General Electric Company Method for enhancing the toughness of CVD diamond
WO2004022821A1 (fr) * 2002-09-06 2004-03-18 Element Six Limited Diamant colore.

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5011509A (en) * 1989-08-07 1991-04-30 Frushour Robert H Composite compact with a more thermally stable cutting edge and method of manufacturing the same
EP0480895A2 (fr) * 1990-10-11 1992-04-15 Sandvik Aktiebolag Outils diamantés améliorés pour le forage de roches, la coupe de métaux et des applications comme pièce d'usure
EP0671482A1 (fr) * 1994-03-11 1995-09-13 General Electric Company Diamant à tenacité élevée déposée chimiquement en phase vapeur
US5672395A (en) * 1994-05-05 1997-09-30 General Electric Company Method for enhancing the toughness of CVD diamond
WO2004022821A1 (fr) * 2002-09-06 2004-03-18 Element Six Limited Diamant colore.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8110041B2 (en) 2002-09-06 2012-02-07 Daniel James Twitchen Coloured diamond

Also Published As

Publication number Publication date
AU2003273252A1 (en) 2005-04-14

Similar Documents

Publication Publication Date Title
USRE41189E1 (en) Method of making enhanced CVD diamond
US7754180B2 (en) Ultrahard diamonds and method of making thereof
US5451430A (en) Method for enhancing the toughness of CVD diamond
Zhu et al. Growth and characterization of diamond films on nondiamond substrates for electronic applications
US5908503A (en) Low defect density diamond single crystal and a process for the production of the same
US4226900A (en) Manufacture of high density, high strength isotropic graphite
JP2010540399A (ja) ダイヤモンドを低圧でアニールする方法
KR100310317B1 (ko) 실리콘 단결정 추출 장치
EP0272418B1 (fr) Appareil et procède pour la condensation de diamant
CA2763652A1 (fr) Procede de cementation d'un element en tantale et element en tantale
JPS61201607A (ja) 熱分解窒化ホウ素物品およびその製造方法
US5882807A (en) Jig for heat treatment and process for fabricating the jig
CN113816737A (zh) 一种高效制备透明金刚石材料的方法
CN111348650A (zh) 碳化钽材的制造方法
WO2005031033A1 (fr) Procede de production d'un diamant cvd ameliore
US8110171B1 (en) Method for decolorizing diamonds
JPS62502043A (ja) シリコン・カ−バイド半導体デバイスのためのウェ−ハ・ベ−ス
Catledge et al. Homoepitaxial diamond films on diamond anvils with metallic probes: the diamond/metal interface up to 74 GPa
KR20170001636A (ko) 탄탈륨 단편 또는 탄탈륨 합금 단편의 처리 방법
CN111659318B (zh) 一种cvd培育金刚石高温高压改性用组装块及改性方法
US20020071803A1 (en) Method of producing silicon carbide power
CN115142039A (zh) Cvd钻石及其制作方法、改进钻石光学性质的方法
JP2013202446A (ja) 単結晶ダイヤモンドおよびその製造方法
FR2658753A1 (fr) Dispositif de moulage en materiau composite pour le pressage a chaud de pieces en materiau refractaire.
RU2201797C1 (ru) Способ обработки алмаза и реакционная ячейка многопуансонного аппарата для его осуществления

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SY TJ TM TN TR TT TZ UA UG UZ VC VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LU MC NL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
122 Ep: pct application non-entry in european phase
NENP Non-entry into the national phase

Ref country code: JP