CN101736323B - Device for preparing boron-doped diamond composite coating on surface of cutter - Google Patents
Device for preparing boron-doped diamond composite coating on surface of cutter Download PDFInfo
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- CN101736323B CN101736323B CN2009103118979A CN200910311897A CN101736323B CN 101736323 B CN101736323 B CN 101736323B CN 2009103118979 A CN2009103118979 A CN 2009103118979A CN 200910311897 A CN200910311897 A CN 200910311897A CN 101736323 B CN101736323 B CN 101736323B
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- Prior art keywords
- temperature resistant
- resistant spring
- cutter
- drilling bit
- heat wire
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 49
- 239000010432 diamond Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- 239000011248 coating agent Substances 0.000 title claims abstract description 7
- 238000000576 coating method Methods 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 229910000714 At alloy Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 19
- 239000007888 film coating Substances 0.000 abstract description 4
- 238000009501 film coating Methods 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 3
- 238000005553 drilling Methods 0.000 abstract 6
- 238000001816 cooling Methods 0.000 abstract 3
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- 238000000151 deposition Methods 0.000 description 13
- 230000008021 deposition Effects 0.000 description 12
- 239000010410 layer Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 229910017052 cobalt Inorganic materials 0.000 description 7
- 239000010941 cobalt Substances 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- HZEIHKAVLOJHDG-UHFFFAOYSA-N boranylidynecobalt Chemical compound [Co]#B HZEIHKAVLOJHDG-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000004050 hot filament vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- BYGOPQKDHGXNCD-UHFFFAOYSA-N tripotassium;iron(3+);hexacyanide Chemical compound [K+].[K+].[K+].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] BYGOPQKDHGXNCD-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
Abstract
The invention discloses a device for preparing a boron-doped diamond composite coating on the surface of a cutter, belonging to the technical field of cutters. The device comprises a reaction hood, an alloy drilling bit, a supporting table, a cooling device, a direct current voltage bias power supply, a heat wire power source, air pressure control device, a high-temperature resistant spring, a heat wire and a drilling bit bracket, wherein the alloy drilling bit and the high-temperature resistant spring are respectively and vertically arranged on the drilling bit bracket; two ends of the heat wire are respectively connected with the high-temperature resistant spring; the drilling bit bracket is fixed on the supporting table and the cooling device; the reaction device is fixed on the supporting table and the cooling device and the outer part of the drilling bit bracket is connected with the air pressure control device; the direct current voltage bias power source is respectively connected with the heat wire and the shell of the reaction hood; and the heat wire power source is respectively connected with the heat wire and the high-temperature resistant spring. The invention can ensure excellent adhesive strength between a diamond composite film and a matrix and can effectively improve the surface quality and the uniformity of the diamond film, thereby improving the service life and the cutting performance of the cutter with the diamond film coating.
Description
Technical field
What the present invention relates to is the device in a kind of cutter manufacturing technology field, specifically is a kind of cemented carbide with complicated shape device for preparing boron-doped diamond composite coating on surface of cutter that is used for.
Background technology
Diamond thin has many excellent properties near natural diamond; High like hardness, Young's modulus is big; Frictional coefficient is low, wear resistance is strong and surface chemistry stable performance etc.; Therefore, diamond thin has broad application prospects at tool and mould and wear resistant appliance field as wear-resisting, antifriction or protective coating material.Chemical Vapor deposition process (Chemical Vapor Deposition; Abbreviation CVD method) the preparation diamond thin does not receive the restriction of base shape; Can directly be deposited on the surface of complicated shape matrix, be suitable for very much preparing complicated shape diamond film coating layer cutter.Yet; The constructional feature of complex shaped cutter self and performance requriements make it to the deposition apparatus and the depositing operation of cutter matrix surface pretreatment technology, CVD diamond thin particular requirement arranged all; And the bonding phase cobalt in the inserted tool has the graphitizing of urging to diamond thin; This CVD diamond thin and adhesion strength between the matrix that has caused being deposited on the cemented carbide with complicated shape tool surface is lower; Film surface is of poor quality, and this has greatly restricted the industrialization of complicated shape diamond film coating layer cutter.
Through the retrieval of document is found, be the adhesion strength that improves between diamond thin and the hard alloy substrate, the pretreatment process that generally adopts comprises that acid etch, plasma arc etching, chemical reaction substitute, hot treat mechanically and add intermediate layer etc.Yet; Though these pretreatment processs can improve the sticking power between diamond thin and the cemented carbide with complicated shape tool matrix to a certain extent; But along with the prolongation of deposition of diamond thin films process, these methods will weaken for the restraining effect of cobalt gradually, and effect is unsatisfactory.People such as F.X.Lu have proposed in " Diamond and Related Materials " the 15th phase in 2006 the 2039th page of " Novel pretreatment of hard metal substrate for better performance of diamond coated cutting tools " literary composition of delivering through the inserted tool matrix being carried out the adhesion strength of the pretreated method raising of boronising diamond thin.This method is in the cemented carbide substrate surfaces boronising; Make the cobalt element generation chemical reaction on boron and matrix top layer generate stable boron cobalt cpd; Thereby stop the diffusion of cobalt element to the matrix top layer; Suppressing its influence to the diamond thin quality, is a kind of novel pretreatment process that improves film-Ji adhesion strength.Yet; This method is before diamond film growth, under the condition of static state, tool matrix is carried out boronising and handles, though it can suppress the inner cobalt element of tool matrix to a certain extent to surface diffusion; But should the static state boronising is pretreated need under hot conditions, carry out; Complicated operating process not only, time consumption and energy consumption, and very easily change the material property of cutter.In addition, this method can't effectively suppress the inner cobalt element of hard alloy substrate equally to the matrix surface thermodiffusion in the process of long-time high temperature deposition diamond thin.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists; A kind of device for preparing boron-doped diamond composite coating on surface of cutter is provided; Can security deposit's hard rock laminated film and matrix between have good adhesion strength; And can effectively improve the surface quality and the homogeneity of diamond thin, thereby improve the work-ing life and the cutting ability of diamond film coating layer cutter.
The present invention realizes through following technical scheme, through utilizing the hot-wire chemical gas-phase deposition device, deposited the boron-doped diamond compounded film that the diamond thin by different boron-doping concentration is composited at the cemented carbide with complicated shape matrix surface.Boron-doped diamond compounded film had both had good adhesion strength, had uniform surface quality again.
The present invention includes: reaction hood, alloy bit, brace table and refrigerating unit, dc bias power, heater supply, Pneumatic controller, high temperature resistant spring, heated filament and drill bit support; Wherein: alloy bit and high temperature resistant spring vertically are arranged on the drill bit support respectively; The two ends of heated filament are connected with high temperature resistant spring respectively; The drill bit support is fixedly set on brace table and the refrigerating unit; Reaction unit is fixedly set in the outside of brace table and refrigerating unit and drill bit support and is connected with Pneumatic controller, and dc bias power links to each other respectively at heated filament and reaction hood shell, the linking to each other with heated filament and high temperature resistant spring respectively of heater supply.
Totally two of described heated filaments, the same plane, both sides that these two heated filaments are positioned at alloy bit and become parallel equidistant arrangement, the two ends of two heated filaments are connected;
The Heating temperature of described heater supply is 2000-2400 ℃;
Described reaction hood is provided with gas inlet and viewing window, and wherein: the gas inlet is positioned at the top of reaction hood, and viewing window is positioned at the side of reaction hood.
The present invention carries out work through following steps:
The first step vertically is put in the cemented carbide with complicated shape cutter in the middle of two heated filaments, makes it parallel with two heated filaments and keep equidistantly.In deposition process; The cemented carbide with complicated shape cutter is the rotation around himself axle center under the drive of worktable; Can guarantee that like this each position, tool matrix surface has the consistent temperature field distribution; Can guarantee the homogeneity of carbon source concentration and boron source concentration around the tool matrix again, thereby, guarantee thickness, surface quality and the homogeneity of diamond thin for diamond thin provides good growing environment.
Second step; Adopt above-mentioned improved hot-wire chemical gas-phase deposition device; Mixture with hydrogen, acetone is a reactant gases, is the doped with boron source with the trimethyl borate that is dissolved in the acetone soln, on the cemented carbide with complicated shape tool matrix, deposits boron-doped diamond film.
The 3rd step; Reduce the concentration that is dissolved in the trimethyl borate in the acetone soln; Continue in-situ deposition lower concentration boron-doped diamond film on high density boron-doped diamond film surface, thereby prepared the boron-doped diamond compounded film that is composited by the different concns boron-doped diamond film in cemented carbide substrate surfaces.
The present invention is simple to operate; Convenient in application; Be applicable in cemented carbide with complicated shape tool surface deposition adhesion strength high; The surface is diamond thin uniformly, helps lend some impetus to the application of diamond thin in cemented carbide with complicated shape cutter field, has bright industrialization prospect and remarkable economic efficiency.
Description of drawings
Fig. 1 is a synoptic diagram of the present invention.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
As shown in Figure 1; This enforcement comprises: reaction hood 1, alloy bit 2, brace table and refrigerating unit 3, dc bias power 4, heater supply 5, Pneumatic controller 6, high temperature resistant spring 7, heated filament 8 and drill bit support 9; Wherein: alloy bit 2 vertically is arranged on the drill bit support 9 respectively with high temperature resistant spring 7; The two ends of heated filament 8 are connected with high temperature resistant spring 7 respectively; Drill bit support 9 is fixedly set on brace table and the refrigerating unit 3; Reaction unit is fixedly set in the outside of brace table and refrigerating unit 3 and drill bit support 9 and is connected with Pneumatic controller 6, and dc bias power 4 links to each other respectively at heated filament 8 and reaction hood 1 shell, the linking to each other with heated filament 8 and high temperature resistant spring 7 respectively of heater supply 5.
Totally two of described heated filaments 8, the same plane, both sides that these two heated filaments 8 are positioned at alloy bit 2 and become parallel equidistant arrangement, the two ends of two heated filaments 8 are connected;
The Heating temperature of described heater supply 5 is 2000-2400 ℃;
Described reaction hood 1 is provided with gas inlet 10 and viewing window 11, and wherein: gas inlet 10 is positioned at the top of reaction hood 1, and viewing window 11 is positioned at the side of reaction hood 1.
Present embodiment carries out work through following steps:
The first step: adopt the two-step acid-alkali method that the carbide drill head surface is carried out pre-treatment.At first, inserted drill is immersed in carries out ultrasonic cleaning in 30 minutes in the Murakami solution, this makes that wolfram varbide (WC) particle on wimet top layer is cracked, thereby causes the substrate surface alligatoring.The composition of Murakami solution is Pottasium Hydroxide (KOH), the Tripotassium iron hexacyanide (K
3(Fe (CN)
6)) and water (H
2O), its quality proportioning is KOH: K
3(Fe (CN)
6): H
2O=1: 1: 10.Subsequently, inserted drill is immersed in the etching of carrying out 1 minute in the Caro mixed acid solution to remove the cobalt element (Co) of underlayer surface.The composition of Caro mixed acid solution is the vitriol oil (H
2SO
4) and ydrogen peroxide 50 (H
2O
2), its volume proportion is H
2SO
4: H
2O
2=1: 10.
Second step: the carbide drill head erect is placed on the circular graphite block, and the graphite block center is drilled with circular port with fixed drill bit, and just graphite block places on the sample support frame again.Arrange according to heated filament shown in Figure 1; With two diameters is that φ 0.6mm tantalum wire is vertically placed; And it is stretching fixing with high temperature resistant spring; Keep the axle center of two heated filaments in same plane, to become parallel equidistant arrangement with the axle center of drill bit, apart from about 3-4mm, the heated filament top is higher than drill bit 5-8mm to heated filament apart from bit face.
The 3rd step: adopting hot filament CVD, is reactant gases with the mixture of hydrogen, acetone, is the doped with boron source with the trimethyl borate that is dissolved in the acetone soln, deposition high density boron-doped diamond film on the cemented carbide with complicated shape tool matrix.Deposition process parameters is: pressure 3-5KPa, and reactant gases total flux 250 ml/min, acetone/hydrogen volume is 2% than (carbon source concentration); Acetone soln mesoboric acid methyl esters concentration is 0.5%; 2200 ± 50 ℃ of hot-wire temperatures, 800 ± 50 ℃ of substrate temperatures, bias current is 1A.After 2 hours deposition, can obtain the about 4 microns high density boron-doped diamond film of thickness in cemented carbide with complicated shape bit matrix surface preparation.
In the 4th step, continue in-situ deposition lower concentration boron-doped diamond film on high density boron-doped diamond film surface.The concentration of acetone soln mesoboric acid trimethyl is reduced to 0.1%; All the other deposition parameters remain unchanged; Proceed 3 hours deposition; Can deposit the boron-doped diamond film of the about 6 microns lower concentration of a layer thickness, thereby prepare boron-doped diamond compounded film in cemented carbide substrate surfaces.
The boron-doped diamond compounded film for preparing in this instance, not only and have good adhesion strength between the cemented carbide with complicated shape matrix, and roughness of film is low, and frictional coefficient is little, and unrelieved stress further reduces.
Claims (2)
1. device for preparing boron-doped diamond composite coating on surface of cutter; Comprise: reaction hood, alloy bit, brace table and refrigerating unit, dc bias power, heater supply, Pneumatic controller, high temperature resistant spring, heated filament and drill bit support; It is characterized in that: alloy bit and high temperature resistant spring vertically are arranged on the drill bit support respectively; The two ends of heated filament are connected with high temperature resistant spring respectively; The drill bit support is fixedly set on brace table and the refrigerating unit; Reaction unit is fixedly set in the outside of brace table and refrigerating unit and drill bit support and is connected with Pneumatic controller, and dc bias power links to each other respectively at heated filament and reaction hood shell, the linking to each other with heated filament and high temperature resistant spring respectively of heater supply;
Totally two of described heated filaments, the same plane, both sides that these two heated filaments are positioned at alloy bit and become parallel equidistant arrangement, the two ends of two heated filaments are connected;
Described reaction hood is provided with gas inlet and viewing window, and wherein: the gas inlet is positioned at the top of reaction hood, and viewing window is positioned at the side of reaction hood.
2. device for preparing boron-doped diamond composite coating on surface of cutter according to claim 1 is characterized in that, the Heating temperature of described heater supply is 2000-2400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103118979A CN101736323B (en) | 2009-12-21 | 2009-12-21 | Device for preparing boron-doped diamond composite coating on surface of cutter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103118979A CN101736323B (en) | 2009-12-21 | 2009-12-21 | Device for preparing boron-doped diamond composite coating on surface of cutter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101736323A CN101736323A (en) | 2010-06-16 |
| CN101736323B true CN101736323B (en) | 2012-01-04 |
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|---|---|---|---|
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| CN (1) | CN101736323B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586762B (en) * | 2012-03-27 | 2015-08-19 | 上海交通大学 | The method of preparing diamond film through multiple-doped hot filament chemical vapor deposition |
| CN103628036B (en) * | 2013-12-12 | 2016-02-03 | 南京航空航天大学 | The preparation method of cubic boron nitride coated cutting tool |
| CN105200391B (en) * | 2014-05-29 | 2018-12-18 | 上海交友钻石涂层有限公司 | Diamond coatings drawing mould preparation method suitable for water lubrication |
| CN106119808A (en) * | 2016-08-24 | 2016-11-16 | 张家港合升进出口有限公司 | Cutter diamond coatings preparation facilities |
| CN107513696B (en) * | 2017-09-12 | 2019-08-13 | 张家港市微纳新材料科技有限公司 | Diamond coatings brill/milling cutter grinds pretreated method |
| CN108559970B (en) * | 2017-12-06 | 2019-11-01 | 上海交通大学 | The HFCVD batch preparation of complicated shape diamond-coated tools |
| CN108642562A (en) * | 2018-04-10 | 2018-10-12 | 东莞领杰金属精密制造科技有限公司 | A kind of high-accuracy processing method of graphite cutter |
| CN111304602B (en) * | 2018-12-11 | 2023-07-21 | 深圳先进技术研究院 | Super-hydrophobic diamond-like composite layer structure and preparation method thereof |
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2009
- 2009-12-21 CN CN2009103118979A patent/CN101736323B/en active Active
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