FR2969178A1 - Diamond coating of tungsten carbide tools by chemical vapor deposition without chemical preparation of carbide, comprises depositing intermediate layer of silicon carbide on tools, and microbead blasting tools with silicon carbide - Google Patents

Diamond coating of tungsten carbide tools by chemical vapor deposition without chemical preparation of carbide, comprises depositing intermediate layer of silicon carbide on tools, and microbead blasting tools with silicon carbide Download PDF

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Publication number
FR2969178A1
FR2969178A1 FR1004978A FR1004978A FR2969178A1 FR 2969178 A1 FR2969178 A1 FR 2969178A1 FR 1004978 A FR1004978 A FR 1004978A FR 1004978 A FR1004978 A FR 1004978A FR 2969178 A1 FR2969178 A1 FR 2969178A1
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France
Prior art keywords
tools
sic
carbide
layer
silicon carbide
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FR1004978A
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French (fr)
Inventor
Jacques Gaillard
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A2C SOC
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A2C SOC
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Priority to FR1004978A priority Critical patent/FR2969178A1/en
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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B27/00Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14Cutting tools of which the bits or tips or cutting inserts are of special material
    • B23B27/148Composition of the cutting inserts
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0254Physical treatment to alter the texture of the surface, e.g. scratching or polishing
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0272Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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 method of coating
    • C23C16/455Chemical 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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45595Atmospheric CVD gas inlets with no enclosed reaction chamber
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B2224/00Materials of tools or workpieces composed of a compound including a metal
    • B23B2224/28Titanium carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B2226/00Materials of tools or workpieces not comprising a metal
    • B23B2226/31Diamond
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B2226/00Materials of tools or workpieces not comprising a metal
    • B23B2226/72Silicon carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B2228/00Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/04Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner applied by chemical vapour deposition [CVD]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23BTURNING; BORING
    • B23B2228/00Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/10Coatings

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  • 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)
  • Cutting Tools, Boring Holders, And Turrets (AREA)

Abstract

The process comprises depositing an intermediate layer of silicon carbide (SiC) on the tools using low temperature plasma at atmospheric pressure, microbead blasting the tools with SiC for etching and implanting SiC microparticles (5) between carbide grains (7), coating the tools with a layer (4) of CVD SiC produced by plasma of nitrogen and methane at low temperature and atmospheric pressure. The tools are made of tungsten carbide with cobalt binder. The layer of SiC is subjected, in an ultrasonic bath, a germination operation that implements diamond grains (6) on a surface of the SiC layer. The process comprises depositing an intermediate layer of silicon carbide (SiC) on the tools using low temperature plasma at atmospheric pressure, microbead blasting the tools with SiC for etching and implanting SiC microparticles (5) between carbide grains (7), coating the tools with a layer (4) of CVD SiC produced by plasma of nitrogen and methane at low temperature and atmospheric pressure. The tools are made of tungsten carbide with cobalt binder. The layer of SiC is subjected, in an ultrasonic bath, a germination operation that implements diamond grains (6) on a surface of the SiC layer. A CVD diamond layer (1) is deposited on the layer of SiC.

Description

1 La présente invention concerne un procédé pour la réalisation de couches (1) diamantées par procédé CVD sur une couche intermédiaire en SiC (4) déposée sur les outils carbure (2) par plasma basse température et à pression atmosphérique. Le revêtement diamant CVD traditionnel des outils en carbure de tungstène est réalisé généralement, après un traitement chimique qui diminue le % du liant cobalt en surface sur la partie à revêtir. Cette opération chimique affaiblit les caractéristiques mécaniques du carbure et arrondit les arrêtes de coupe des outils.(3) Le procédé suivant l'invention permet de remédier à ces inconvénients en supprimant le traitement chimique, en conservant après revêtement diamant CVD les caractéristiques mécaniques du carbure et l'acuité des arêtes de coupe (3) des outils. Selon des modes particuliers de réalisation, les outils sont fabriqués en carbure de tungstène WcCo avec un pourcentage de cobalt qui peut varier de 3 à 12 % La granulométrie des grains de tungstène se situe entre 0,5 à 5 microns. Les carbures ne doivent pas avoir de carbure mixte dans leur composition. La surface à revêtir est microbillée avec du SiC grains 800 ,pression d'air du microbillage 2 bars distance buse/ pièce 100 mm jet perpendiculaire aux surfaces à revêtir pour implantation de grains de SiC (5) entre les grains de carbure (7) de l'outil. Les outils sont ensuite revêtus d'une couche de SiC CVD (4) par procédé plasma à basse température et à pression atmosphérique. Plasma avec N2 + CH4 (14) Proportions N2 501/mn CH4 0,51/mn. Buse (10) à 40 mm de l'outil ;Vitesse de balayage 30 m/mn, 15 passages sur l'outil. A la base de la buse( 10 ) dans le plasma (11) introduction d'un précurseur (12) du type C6H18Si2. Le débit du précurseur (12) de l'ordre de 25 ml/mn et le débit du gaz porteur (13)de 201/mn. pour la création de la couche de SiC (4) sur le carbure de tungstène. Le jet plasma (1l) est perpendiculaire à la surface à traiter (8). Ces paramètres permettent de réaliser des couches de SiC (4) d'une épaisseur (9)de 0,5 à 1 micron. Cette épaisseur est suffisante pour créer une barrière efficace 30 contre les remontées de cobalt à travers la couche de SiC . Avant le revêtement diamant CVD, les outils sont plongés dans un bain ultrasonique avec grains de diamant en suspension pour créer des zones de germination par implantations de grains de diamant (6) dans la couche de SiC (4) Cette opération grave la surface de la couche de SiC (4) et favorise l'accroche du revêtement diamant.The present invention relates to a method for producing CVD diamond layers (1) on an SiC intermediate layer (4) deposited on the carbide tools (2) by low temperature plasma and at atmospheric pressure. The traditional CVD diamond coating of tungsten carbide tools is generally performed after a chemical treatment which decreases the% of the cobalt binder at the surface on the part to be coated. This chemical operation weakens the mechanical properties of the carbide and rounds the cutting edges of the tools. (3) The method according to the invention overcomes these disadvantages by eliminating the chemical treatment, retaining after CVD diamond coating the mechanical properties of the carbide and the sharpness of the cutting edges (3) of the tools. According to particular embodiments, the tools are made of WcCo tungsten carbide with a percentage of cobalt which can vary from 3 to 12% The particle size of the tungsten grains is between 0.5 to 5 microns. Carbides should not have mixed carbide in their composition. The surface to be coated is microbilled with SiC grains 800, air pressure of the microbrilling 2 bars distance nozzle / piece 100 mm perpendicular to the surfaces to be coated for implantation of SiC grains (5) between the carbide grains (7) of the tool. The tools are then coated with a CVD (4) SiC layer by a plasma process at low temperature and at atmospheric pressure. Plasma with N2 + CH4 (14) Proportions N2 501 / min CH4 0.51 / min. Nozzle (10) at 40 mm from the tool, sweeping speed 30 m / min, 15 passes on the tool. At the base of the nozzle (10) in the plasma (11) introduction of a precursor (12) of the C6H18Si2 type. The flow rate of the precursor (12) of the order of 25 ml / min and the flow rate of the carrier gas (13) of 201 / min. for the creation of the SiC layer (4) on tungsten carbide. The plasma jet (11) is perpendicular to the surface to be treated (8). These parameters make it possible to produce SiC layers (4) with a thickness (9) of 0.5 to 1 micron. This thickness is sufficient to create an effective barrier against cobalt rising through the SiC layer. Before the CVD diamond coating, the tools are immersed in an ultrasonic bath with diamond grains in suspension to create germination zones by implantation of diamond grains (6) in the SiC layer (4). This operation engraves the surface of the layer of SiC (4) and promotes the grip of the diamond coating.

35 Le bain ultra-sons 40HZ contient un mélange de 1L d'eau DI avec 2 carats de poudre de diamant de 0,5 micron .Le temps de traitement est de 10 minutes environ. Les outils sont ensuite revêtus dans un four CVD diamant à environ 800° C. Après traitement, l'épaisseur du revêtement est typiquement de 6 microns. Le procédé suivant l'invention est destiné à revêtir les outils en carbure de tungstène avec un 40 revêtement diamant par procédé CVD .en supprimant leur préparation chimique . The 40HZ ultrasonic bath contains a mixture of 1L DI water with 2 carats of 0.5 micron diamond powder. The treatment time is about 10 minutes. The tools are then coated in a diamond CVD oven at about 800 ° C. After treatment, the coating thickness is typically 6 microns. The process according to the invention is intended to coat the tungsten carbide tools with a CVD diamond coating by removing their chemical preparation.

Claims (6)

REVENDICATIONS1) Procédé pour le revêtement diamant par CVD d'outils en carbure de tungstène sans préparation chimique du carbure, caractérisé en ce que préalablement à la réalisation du revêtement diamant par CVD, on dépose sur les outils une couche intermédiaire de SiC par plasma basse température et à pression atmosphérique. CLAIMS1) Method for CVD diamond coating tungsten carbide tools without chemical preparation of carbide, characterized in that prior to the realization of the diamond coating by CVD, is deposited on the tools an intermediate layer of SiC by low temperature plasma and at atmospheric pressure. 2) Procédé selon la revendication 1, caractérisé en ce que les outils sont fabriqués en 1 o carbure de tungstène avec liant cobalt. 2) Process according to claim 1, characterized in that the tools are made of 1 tungsten carbide with cobalt binder. 3) Procédé selon les revendications précédentes, caractérisé en ce que préalablement au dépôt de la couche intermédiaire de SiC, les outils en WC sont microbillés avec du SiC pour les décaper et y implanter des microparticules de SiC (5) entre les grains de carbure (7). 15 3) Process according to the preceding claims, characterized in that prior to the deposition of the SiC intermediate layer, the WC tools are microbilled with SiC to strip and implant SiC microparticles (5) between the carbide grains ( 7). 15 4) Procédé selon les revendications précédentes, caractérisé en ce que suite au microbillage, les outils sont revêtus d'une couche de SiC CVD (4) réalisée par plasma (11) d'azote et de méthane, à basse température et à pression atmosphérique. 4) Process according to the preceding claims, characterized in that following microbilling, the tools are coated with a layer of SiC CVD (4) made by plasma (11) of nitrogen and methane, at low temperature and at atmospheric pressure. . 5) Procédé selon les revendications précédentes, caractérisé en ce que la couche de SiC subit dans un bain à ultrasons une opération de germination qui implante des grains 20 diamant (6) sur la surface de la couche de SiC (4). 5) Method according to the preceding claims, characterized in that the SiC layer undergoes in an ultrasonic bath a germination operation which implements diamond grains (6) on the surface of the SiC layer (4). 6) Procédé selon les revendications précédentes, caractérisé en ce que la couche CVD diamant (1) est déposée sur la couche de SiC (4). 6) Method according to the preceding claims, characterized in that the diamond CVD layer (1) is deposited on the SiC layer (4).
FR1004978A 2010-12-20 2010-12-20 Diamond coating of tungsten carbide tools by chemical vapor deposition without chemical preparation of carbide, comprises depositing intermediate layer of silicon carbide on tools, and microbead blasting tools with silicon carbide Pending FR2969178A1 (en)

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FR1004978A FR2969178A1 (en) 2010-12-20 2010-12-20 Diamond coating of tungsten carbide tools by chemical vapor deposition without chemical preparation of carbide, comprises depositing intermediate layer of silicon carbide on tools, and microbead blasting tools with silicon carbide

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FR1004978A FR2969178A1 (en) 2010-12-20 2010-12-20 Diamond coating of tungsten carbide tools by chemical vapor deposition without chemical preparation of carbide, comprises depositing intermediate layer of silicon carbide on tools, and microbead blasting tools with silicon carbide

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10475619B2 (en) 2016-06-30 2019-11-12 General Electric Company Multilayer X-ray source target
US10692685B2 (en) 2016-06-30 2020-06-23 General Electric Company Multi-layer X-ray source target

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19521007A1 (en) * 1994-06-14 1995-12-21 Valenite Inc Deposition of diamond coatings on hard substrates

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19521007A1 (en) * 1994-06-14 1995-12-21 Valenite Inc Deposition of diamond coatings on hard substrates

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CABRAL G ET AL: "A study of diamond film deposition on WC-Co inserts for graphite machining: Effectiveness of SiC interlayers prepared by HFCVD", DIAMOND AND RELATED MATERIALS, ELSEVIER SCIENCE PUBLISHERS, AMSTERDAM, NL, vol. 17, no. 6, 1 June 2008 (2008-06-01), pages 1008 - 1014, XP022638724, ISSN: 0925-9635, [retrieved on 20080328], DOI: 10.1016/J.DIAMOND.2008.03.017 *
DEUERLER F ET AL: "Production, characterization, and wear behaviour of plasma jet CVD diamond films on hard metal cutting tools", PHYSICA STATUS SOLIDI A AKADEMIE VERLAG GERMANY, vol. 154, no. 1, 16 March 1996 (1996-03-16) - 16 March 1996 (1996-03-16), pages 403 - 422, XP002663617, ISSN: 0031-8965, DOI: DOI:10.1002/PSSA.2211540129 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10475619B2 (en) 2016-06-30 2019-11-12 General Electric Company Multilayer X-ray source target
US10692685B2 (en) 2016-06-30 2020-06-23 General Electric Company Multi-layer X-ray source target

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