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WO1993024676A1 - Depot de film de diamant - Google Patents

Depot de film de diamant Download PDF

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Publication number
WO1993024676A1
WO1993024676A1 PCT/GB1993/001082 GB9301082W WO9324676A1 WO 1993024676 A1 WO1993024676 A1 WO 1993024676A1 GB 9301082 W GB9301082 W GB 9301082W WO 9324676 A1 WO9324676 A1 WO 9324676A1
Authority
WO
WIPO (PCT)
Prior art keywords
diamond
dust
shock wave
diamond dust
substrate surface
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/GB1993/001082
Other languages
English (en)
Inventor
Phillip John
John Ivor Barrett Wilson
Iain Cameron Drummond
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BTG International Ltd
Original Assignee
British Technology Group Ltd
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 British Technology Group Ltd filed Critical British Technology Group Ltd
Priority to EP93910285A priority Critical patent/EP0642599A1/fr
Publication of WO1993024676A1 publication Critical patent/WO1993024676A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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
    • C23C16/274—Diamond only using microwave discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
    • B24C11/00—Selection of abrasive materials or additives for abrasive blasts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
    • B24C3/00—Abrasive blasting machines or devices; Plants
    • B24C3/32—Abrasive blasting machines or devices; Plants designed for abrasive blasting of particular work, e.g. the internal surfaces of cylinder blocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
    • B24C5/00—Devices or accessories for generating abrasive blasts
    • B24C5/08—Devices for generating abrasive blasts non-mechanically, e.g. of metallic abrasives by means of a magnetic field or by detonating cords
    • 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
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing

Definitions

  • This Invention relates to the deposition of diamond films on surfaces of substrates of suitable materials and, in particular, to the pre-treat ent of such surfaces to prepare them for subsequent diamond film deposition by any of a number of available chemical vapour techniques such as described, for example, in a review article entitled “Diamonds from the vapour phase", by P. Bachmann, published in "Physics World”, April 1991, pages 32-36.
  • Suitable pre-treatment of a substrate surface, to enhance the nucleation density and the rate of growth during film deposition, is of paramount importance for the success of all these vapour deposition techniques.
  • Such etching or sputtering of unmasked areas of the surface reduces the nucleation density there due to the abrasion, and it 1s found that after subsequent removal of the temporary masking it is only on those parts which have been masked, so that the abrasions have remained unaffected by the 1on-beam etching step, that diamond film deposition occurs when the whole surface is submitted to the diamond deposition step.
  • the method of pre-treating a surface comprises the steps of positioning a quantity of diamond dust in relation to the surface, producing a shock wave in gas adjacent the dust, subjecting the dust to the shock wave, and thereby causing the diamond dust to impinge at high velocity on to the surface.
  • the shock wave may be produced by causing a build-up of gas under pressure contained in part by a rupturable membrane or diaphragm, and then causing the membrane or diaphragm to rupture.
  • the rupture of the membrane or diaphragm may be caused either by progressively increasing the pressure of the gas or may be initiated by piercing it with a sharp point.
  • the shock wave may be produced in the gas by other means, such as by producing an electrical spark within the gas.
  • the method may include the steps of positioning the diamond dust within a nozzle directed towards the substrate surface and causing the diamond dust to be expelled through the nozzle by the shock wave; and the diamond dust may be provided in the form of a friable pellet of compressed diamond dust.
  • the surface ⁇ or the selected part of 1t) is ready for deposition of diamond upon it by any of the known deposition techniques.
  • the invention also provides a method of depositing a diamond film on a substrate surface, comprising pre-treating the substrate surface by the method outlined above and thereafter depositing a diamond film on all or part of the pre-treated surface by any known and suitable method of deposition.
  • apparatus for pre-treating a surface prior to depositing a film of diamond thereon comprising means for holding a charge of diamond dust, means for generating a shock wave in gas adjacent the charge of diamond dust, and means for directing the shock wave at the diamond dust and causing the diamond dust to be expelled at high velocity for impingement on an adjacent surface.
  • the means for generating a shock wave comprises a burstable diaphragm and means for providing a build-up of gaseous pressure on a side of the diaphragm remote from the charge of diamond dust.
  • the apparatus shown in the drawing comprises a pressure vessel 10 composed of two stainless steel tubular sections 11 and 12 formed with respective end flanges 11a and 12a by means of which the two sections are releasably held together end-to-end by an internally threaded collar 13 and a co-operating externally threaded collar 14.
  • the sections 11 and 12 may be of about 10 mm internal diameter and of length 250 mm and 150 mm respectively.
  • the section 12 is internally threaded to receive a nozzle fitment 15 having a nozzle outlet portion 15a with an internal diameter of about 1.5 mm and a portion 15b adapted to receive and hold a friable pellet or disc 16 of compressed diamond dust.
  • the sections 11 and 12 of the device 10 are secured together with a burstable membrane or diaphragm 17 held between them so as to obturate the tubular interior.
  • the driver section 11, at its end remote from the section 12, is fitted with a high-pressure hose 18 for connection via a control valve (not shown), to a source (also not shown) of high-pressure gas, preferably nitrogen or other inert gas.
  • the device 10 is positioned with the nozzle 15a spaced, by a distance typically between 0 and 50 mm, from a surface which is to be pre-treated and which, as illustrated, may be one optically polished surface of a single crystal silicon wafer 19 of which the other face rests on a solidly mounted support 20.
  • Controlled admission of gas through the hose 18 then allows a build-up of pressure within the driver section 11 until, at a pressure determined by the choice of diaphragm 17, the diaphragm ruptures. This generates a shock wave which travels down the interior of the expansion section 12 to impact on and pulverise the disc 16 and to project the resulting diamond dust through the nozzle 15a to impact at high velocity on the opposed surface of the wafer or substrate 19.
  • the wafer 19 was then cleaned by washing with deionised water and drying under nitrogen.
  • the whole of the wafer surface to different parts of which the pre-treatments had been applied was then subjected to a diamond film deposition process using the known microwave plasma technique.
  • the wafer substrate was maintained at a temperature of 700°C while exposed within a deposition chamber to a plasma formed by subjecting a gas mixture of hydrogen with 0.5% of methane to microwave radiation while flowing through the chamber under reduced pressure.
  • the pressure employed within the chamber was 11 torr, the flow rate through the chamber was 1000 standard cubic centimetres of gas mixture per minute, and the microwave power applied was 620W with a frequency of 2.45 GHz.
  • the deposition process was continued for a period of 5.5 hours, after which the wafer was allowed to cool and was then examined. It was found that deposition of a diamond film had occurred, but only on those parts of the surface to which a pre-treatment had occurred.
  • the film thickness was greater (implying higher growth rates) for the outer regions which had been pre-treated in accordance with the invention than for the two parts of the central region which had been conventionally abraded; and, as between different areas of the outer pre-treated regions, the film thickness was greater, the higher the pressure at which the diaphragm had burst during carrying out of the pre-treatment.
  • a diaphragm 17 may be used in combination with a gas pressure which is not itself sufficient to rupture the diaphragm, some other means being provided, such as a sharp point which can be triggered to pierce the diaphragm, as a means of Initiating the rupture.
  • the shock wave may be generated by other means than a bursting diaphragm, for example by producing an electrical spark within gas adjacent the diamond powder.
  • the diamond dust is not necessarily provided in the form of a pellet or disc 16 as described above: particularly if the apparatus 10 is operated in a vertical position as illustrated 1n the drawing, the diamond dust may be provided simply as a charge of loose powder in the bore of the fitment 15, in the lower part of its portion 15b and/or in the bore of its nozzle portion 15a.
  • the discs 16 each contained 7mg of diamond dust; but it will be understood that larger or smaller quantities may also be used, whether as loose powder or formed into a disc.
  • the dust expelled from the nozzle 15a issues as a generally conically-expanding jet and impinges on a generally circular area of the substrate 19, the diameter of such area increasing with increased spacing of the nozzle from the substrate.

Landscapes

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

Abstract

L'invention concerne un procédé et un appareil améliorés destinés à prétraiter une surface (19) d'un substrat afin de la préparer à recevoir ensuite un dépôt d'un film de diamant. Le procédé de prétraitement de surface de l'invention consiste à placer une quantité de poussière de diamant (16) sur la surface, à générer une onde de choc dans la poussière adjacente au gaz, à soumettre la poussière à l'onde de choc, et à faire ainsi heurter la poussière de diamant, à grande vitesse, contre la surface. L'appareil, selon l'invention, comporte des éléments pour maintenir une charge de poussière de diamant (17), des éléments pour générer une onde de choc dans la charge de poussière de diamant (17) adjacente au gaz, et des éléments pour diriger l'onde de choc sur la poussière de diamant (12) et à faire en sorte que la poussière de diamant à expulser à grande vitesse se heurte à la surface du substrat. L'invention concerne également un procédé de dépôt d'un film de diamant sur un substrat, comprenant le prétraitement s'effectuant à l'aide du procédé et de l'appareil décrits ci-dessus.
PCT/GB1993/001082 1992-05-26 1993-05-26 Depot de film de diamant Ceased WO1993024676A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP93910285A EP0642599A1 (fr) 1992-05-26 1993-05-26 Depot de film de diamant

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9211107.9 1992-05-26
GB929211107A GB9211107D0 (en) 1992-05-26 1992-05-26 Diamond film deposition

Publications (1)

Publication Number Publication Date
WO1993024676A1 true WO1993024676A1 (fr) 1993-12-09

Family

ID=10716019

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1993/001082 Ceased WO1993024676A1 (fr) 1992-05-26 1993-05-26 Depot de film de diamant

Country Status (3)

Country Link
EP (1) EP0642599A1 (fr)
GB (1) GB9211107D0 (fr)
WO (1) WO1993024676A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997014373A1 (fr) * 1995-10-20 1997-04-24 Hickok Teresa R Procede de durcissement pour pointe de dentisterie a ultrasons
GB2334039A (en) * 1998-02-10 1999-08-11 Secr Defence Manufacture of diamond fibres incliding a pretreatment step
EP1016735A1 (fr) * 1998-12-28 2000-07-05 Siemens Aktiengesellschaft Procédé pour revêtir un objet
EP1893782A4 (fr) * 2005-05-09 2010-08-04 Univ Ottawa Procedes et dispositifs de depot de materiau

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991018991A1 (fr) * 1990-05-29 1991-12-12 E.I. Du Pont De Nemours And Company Procede et appareil ameliores d'introduction de substances biologiques dans des cellules vivantes

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991018991A1 (fr) * 1990-05-29 1991-12-12 E.I. Du Pont De Nemours And Company Procede et appareil ameliores d'introduction de substances biologiques dans des cellules vivantes

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"PROCESS FOR ENHANCED GROWTH OF DIAMOND THIN FILMS BY THE SPRAY APPLICATION OF A SEED-LAYER.", RESEARCH DISCLOSURE., MASON PUBLICATIONS, HAMPSHIRE., GB, no. 323., 1 March 1991 (1991-03-01), GB, pages 204., XP000176294, ISSN: 0374-4353 *
DATABASE WPI Section Ch, Week 2289, Derwent Publications Ltd., London, GB; Class B22, AN 89-164012 Ç22! *
PATENT ABSTRACTS OF JAPAN vol. 10, no. 366 (C-390)(2423) 6 December 1986 *
WINDISCHMANN H., EPPS G. F.: "PROPERTIES OF DIAMOND MEMBRANES FOR X-RAY LITHOGRAPHY.", JOURNAL OF APPLIED PHYSICS, AMERICAN INSTITUTE OF PHYSICS, US, vol. 68., no. 11., 1 December 1990 (1990-12-01), US, pages 5665 - 5673., XP000176495, ISSN: 0021-8979, DOI: 10.1063/1.346981 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997014373A1 (fr) * 1995-10-20 1997-04-24 Hickok Teresa R Procede de durcissement pour pointe de dentisterie a ultrasons
US5704787A (en) * 1995-10-20 1998-01-06 San Diego Swiss Machining, Inc. Hardened ultrasonic dental surgical tips and process
GB2334039A (en) * 1998-02-10 1999-08-11 Secr Defence Manufacture of diamond fibres incliding a pretreatment step
GB2334039B (en) * 1998-02-10 2002-10-30 Secr Defence Method of manufacture of diamond fibres
EP1016735A1 (fr) * 1998-12-28 2000-07-05 Siemens Aktiengesellschaft Procédé pour revêtir un objet
EP1893782A4 (fr) * 2005-05-09 2010-08-04 Univ Ottawa Procedes et dispositifs de depot de materiau

Also Published As

Publication number Publication date
EP0642599A1 (fr) 1995-03-15
GB9211107D0 (en) 1992-07-08

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