CN1239739C - Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface - Google Patents
Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface Download PDFInfo
- Publication number
- CN1239739C CN1239739C CN 200310108305 CN200310108305A CN1239739C CN 1239739 C CN1239739 C CN 1239739C CN 200310108305 CN200310108305 CN 200310108305 CN 200310108305 A CN200310108305 A CN 200310108305A CN 1239739 C CN1239739 C CN 1239739C
- Authority
- CN
- China
- Prior art keywords
- diamond
- slimline
- coating
- self
- tubule
- 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.)
- Expired - Fee Related
Links
- 239000010432 diamond Substances 0.000 title claims abstract description 106
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 106
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 25
- 239000010937 tungsten Substances 0.000 claims abstract description 25
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 6
- 238000004050 hot filament vapor deposition Methods 0.000 claims abstract description 6
- 239000010959 steel Substances 0.000 claims abstract description 6
- 239000003822 epoxy resin Substances 0.000 claims abstract description 3
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims description 63
- 239000011248 coating agent Substances 0.000 claims description 39
- 210000005239 tubule Anatomy 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 23
- 239000011159 matrix material Substances 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000010419 fine particle Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 239000012495 reaction gas Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- 229920006332 epoxy adhesive Polymers 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 230000003628 erosive effect Effects 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 230000004907 flux Effects 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000011247 coating layer Substances 0.000 abstract 4
- 239000000853 adhesive Substances 0.000 abstract 2
- 230000001070 adhesive effect Effects 0.000 abstract 2
- 239000004411 aluminium Substances 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 4
- 239000003082 abrasive agent Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000010900 secondary nucleation Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Abstract
The present invention relates to a method for preparing a diamond composite coating layer slimline with low roughness at the inner surface. The method adopts an electronic enhancement hot filament chemical vapor deposition (CVD) method to prepare a diamond composite coating layer for a tungsten rod basal body, and the tungsten rod basal body is removed by corrosion to obtain a self supporting diamond slimline. A steel tube or an aluminium tube which is thicker than the self supporting diamond slimline is used as a casing of the slimline to be sheathed outside the self supporting diamond slimline. Modified epoxy resin adhesives are filled between the self supporting diamond slimline and the casing to form a slimline whose inner surface is composed of the diamond composite coating layer with low roughness. The method can obtain the wear resistant diamond coating layer with high adhesive strength at the inner surface of the slimline, the roughness of the inner surface of the slimline can be reduced effectively through technology control, and thereby, the frictional property is improved greatly, the service life of the slimline is extended, and the production efficiency and the machining quality are improved. The present invention has the advantages of simple operation, convenient application, bright industrial prospect and obvious economic benefit.
Description
Affiliated technical field
The present invention relates to a kind of diamond coatings elongated tubular preparation method, particularly a kind of employing electronics strengthens hot-wire chemical gas-phase deposition (CVD, Chemical Vapour Deposition) method is carried out the method for internal surface low roughness diamond composite coating elongated tubular preparation, belongs to wear resistant appliance diamond coatings preparing technical field.
Background technology
Diamond has a series of excellent properties, it has very high hardness, high Young's modulus, high thermal conductivity, low frictional coefficient, low thermal coefficient of expansion and chemical stability and fabulous antiacid, alkali resistant, anti-various corrosive gases erosive excellent properties, thereby is being widely used aspect the preparation of cutting tool and wear resistant appliance.As the external surface coating high-abrasive material, diamond thin has been successfully applied on protection of the protective layer of disk and CD, accurate punching and shearing die top coat and the motor car engine mechanical component coating easy to wear etc.In fact, diamond thin also is embodied in and is applied to the wear-resisting and lubricated occasion of many internal surfaces often requirement, as wortle, elongated tubular, nozzle etc. as optimal instrument and high-abrasive material.And in actual production process, above-mentioned instrument all can be had a strong impact on because of serious wear makes production efficiency and processing quality etc.Polycrystalline diamond and thick film gold hard rock have begun to be used for the aperture 2 millimeters preparations with interior wortle and nozzle, the polycrystalline diamond elongated tubular also has commodity to come out, wear problems is resolved, but the producing apparatus scale of investment of product is big, makes product price very expensive.Polycrystalline diamond and thick film diamond are then seldom used in preparation for wide-aperture wortle and nozzle.Increasingly mature hot-wire chemical gas-phase deposition (CVD) diamond coatings technology brings hope for the preparation of wide aperture internal surface wearing piece, it has, and area is big, shape random and low cost and other advantages, thereby is the key that realizes wide aperture internal surface wearing piece industrialization preparation.Wortle, sliding surface bearing, nozzle and elongated shape jet pipe etc. as vulnerable part, if use diamond thin as high-abrasive material, then whether the inefficacy of its function mainly depends on the degree of wear of internal surface diamond thin, thereby the friction and wear characteristic of diamond thin becomes the matter of utmost importance of care.Relevant studies show that, the friction and wear characteristic of diamond thin and the roughness of coatingsurface are closely related, and will obtain the low roughness diamond thin at internal surface of elongated tube will be a difficult problem on coating process, not have the example of successful Application at present in actual production.
Summary of the invention
When working, make the elongated tubular working life in order to overcome existing internal surface of elongated tube because of serious wear, the deficiency that production efficiency and processing quality etc. are had a strong impact on, the invention provides a kind of employing electronics and strengthen the method that hot-wire chemical gas-phase deposition (CVD) method is carried out the preparation of internal surface low roughness diamond composite coating elongated tubular, this method can not only obtain the wear-resisting diamond coatings of high-adhesion at internal surface of elongated tube, and can reduce the roughness of internal surface diamond coatings effectively by suitable processing method, thereby greatly improve its frictional behaviour, improved the elongated tubular working life, production efficiency and processing quality etc.
The technical solution adopted for the present invention to solve the technical problems is: the tungsten bar material matrix that this preparation method adopts electronics to strengthen after hot filament CVD is handled surface finish carries out the fine-particle diamond coating earlier, tungsten bar material matrix needn't strengthen the hot filament chemical vapor deposition reactor chamber from electronics and took out this moment, improve reaction gas pressure then, reduce the volume ratio of acetone/hydrogen and remove the compound coating preparation that the rare gas element argon gas carries out the coarse grain diamond coatings in position again, by obtaining the slick self-supporting diamond tubule of internal surface behind the erosion removal tungsten bar material matrix, employing is than the bigger steel pipe of self-supporting diamond tubule or the aluminum pipe shell as elongated tubular, be enclosed within outside the self-supporting diamond tubule, and between self-supporting diamond tubule and shell, fill by the epoxy adhesive of modification, form the elongated tubular that internal surface is made up of the low roughness diamond composite coating thus.
At first select the tungsten bar material of easy growing diamond of suitable diameter as matrix according to needed elongated tubular internal diameter, make that by the surface finish processing tungsten bar material matrix surface is smooth as far as possible, adopt electronics to strengthen heated filament CVD method then, use depositing operation stage by stage, tungsten bar material matrix is carried out the preparation of diamond composite coating, the diamond deposition initial stage to improve adamantine nucleation rate, by improving the concentration of carbon-source gas, reduce substrate temperature and reduce sediment chamber's air pressure to promote that second nucleation increases, grain refining, generation is based on＜100〉crystal orientation, crystalline form is relatively poor, the nanometer spheric grain that crystal grain is tiny, then to reduce the concentration of carbon-source gas in the diamond deposition middle and later periods, improve substrate temperature, in-situ deposition growth one deck＜111 again on the diamond coatings of having grown〉crystal orientation, crystal grain is sturdy, the diamond multicrystal film of good crystallinity.By above technological measure, can on tungsten bar material matrix, deposit and prepare the thick diamond composite coating of about 10～50 μ m of one deck.Adopt etch to remove tungsten bar material matrix then to prepare self-supporting diamond tubule with certain wall thickness, because tungsten bar material matrix adopts special process parameter refinement diamond crystals through the surface finish processing and at the diamond coatings deposition initial stage before depositing, thereby feasible self-supporting diamond tubule coating inner surface prepared after corroding is very smooth.To meet the steel pipe of diameter dimension requirement or aluminum pipe shell again as elongated tubular, with the preparation the self-supporting diamond tubule as inner casing, between self-supporting diamond tubule and shell, fill by the Resins, epoxy of modification, bear also release action in the external load of diamond composite coating internal surface, avoid stress to concentrate causing the diamond coatings inefficacy of breaking, form the elongated tubular that internal surface is made up of the low roughness diamond composite coating thus.
The invention has the beneficial effects as follows, this method can not only obtain the wear-resisting diamond coatings of high-adhesion at elongated tubular internal layer working face, and can reduce self-supporting diamond tubule inside surface roughness effectively by technology controlling and process, thereby greatly improve its frictional behaviour, improve elongated tubular working life, production efficiency and processing quality etc.Present method is simple to operate, application is convenient, industrialization prospect light, thereby have remarkable economic efficiency.
Embodiment
Prepare example below in conjunction with the internal surface low roughness diamond composite coating elongated tubular that obtains close grain low roughness diamond thin at internal surface, concrete enforcement of the present invention is further described.
The first step: at first the tungsten bar material of easy growing diamond of selecting respective diameters according to needed elongated tubular internal diameter is as matrix, handles making that tungsten bar material matrix surface is smooth as far as possible by surface finish.
Second step: the tungsten bar material matrix after will handling through surface finish places electronics to strengthen the CVD reaction chamber, adopts electronics to strengthen heated filament CVD method and carries out the fine-particle diamond coating.Hot filament adopts the tantalum wire of 0.6 millimeter of ф, and is stretching with high temperature resistant spring, and reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), beginning CVD deposition fine-particle diamond coating behind the adjustment chamber pressure.The coating process parameter is: pressure 0.5-2KPa, and reactant gases total flux 200-400 ml/min, the volume ratio of acetone/hydrogen (carbon source concentration) is 2%-6%, and filament temperature is 2000 ℃, and bias current is 1A, adds rare gas element argon gas (Ar), argon gas/hydrogen (Ar/H
2) volume ratio be 0.5-1.5.Traditional relatively CVD diamond coatings technology, owing to reduced reaction gas pressure, increased carbon source concentration and added rare gas element, thereby can increase the speed of diamond secondary nucleation greatly, deposition has obtained the nano diamond coating of small grains thus, the about 50-100 nanometer of crystal grain size, coatingsurface is more smooth smooth, and frictional coefficient is little, and hardness also descends to some extent.After 2 hours, obtain thick about 5 microns fine-particle diamond coating.
The 3rd step: carry out the coarse grain diamond coatings.After the fine-particle diamond coating reaches 5 microns, beginning in-situ deposition coarse grain diamond coatings.Tungsten bar material matrix needn't strengthen the heated filament CVD reaction chamber from electronics and took out this moment, only needed to change processing condition and promptly improve reaction gas pressure, reduced carbon source concentration and had removed the rare gas element argon gas just.Reaction gas pressure can be brought up to 4-10KPa, and carbon source concentration is reduced to 1-3%, removes argon gas, suitably improves filament temperature to 2200 ℃ simultaneously.Can greatly improve hydrionic concentration in the reaction atmosphere by changing above processing parameter, strengthened etchings such as graphite and decolorizing carbon in the diamond film process, thereby impelled that diamond crystals is relatively poor by crystalline form, crystal grain is tiny＜100〉crystal orientation nanometer spheric grains to crystal grain sturdy, good crystallinity＜111〉crystal orientation trilaterals (mix square is arranged) coarse grain changes.Through 4 hours the deposition after, prepare the about 15 microns coarse grain diamond coatings of a bed thickness thus, coatingsurface is very coarse, frictional coefficient is big, the hardness height helps improving the quality of diamond coatings like this, and can combine with epoxy adhesive better.
The 4th step: the tungsten bar material that will deposit diamond composite coating strengthens the heated filament CVD reaction chamber from electronics and takes out, and puts in the container that fills corrosive fluid removing tungsten bar material matrix, thereby prepares the self-supporting diamond tubule.The corrosive fluid preparation program is: proportion is that 1.19 hydrochloric acid and concentration are that the volume proportion of 30% hydrogen peroxide is 1: 1.
The 5th step: after from the container that fills corrosive fluid, taking out the self-supporting diamond tubule, for increasing the bonding force between diamond coatings and Resins, epoxy, also to carry out following surface treatment: (1) oxygen plasma surface treatment to the self-supporting diamond tubule for preparing, to remove the decolorizing carbon of coating outside surface, and, make coating mutually moistening with Resins, epoxy at regional area generation carbon-oxygen (C=O) key; (2) can generate the titanium (Ti) or chromium (Cr) metal of carbide with diamond in the sputter of coating outside surface, and apply the monoalkoxy type titanate coupling agent that contains Ti.
The 6th step: again will be than the bigger steel pipe of self-supporting diamond tubule or aluminum pipe shell as elongated tubular, be enclosed within outside the prepared self-supporting diamond tubule, between self-supporting diamond tubule and shell, fill by the Racemic glycidol ethers propane type epoxy resin of di phenolic group binding agent of modification, bear also release action in the external load of diamond composite coating internal surface, avoid stress to concentrate causing the diamond coatings inefficacy of breaking, form the elongated tubular that internal surface is made up of the low roughness diamond composite coating thus.For the thermal expansivity that reduces epoxy adhesive causes the coating stress cracking with preventing because of expansion coefficient difference is excessive, also need add silicon-dioxide (SiO in the resin formula
2) micro mist and styrenic toughner carries out modification to epoxy adhesive and handle.
Claims (2)
1. internal surface low roughness diamond composite coating elongated tubular preparation method, it is characterized in that the tungsten bar material matrix that this preparation method adopts electronics to strengthen after hot filament CVD is handled surface finish carries out the fine-particle diamond coating earlier, tungsten bar material matrix needn't strengthen the hot filament chemical vapor deposition reactor chamber from electronics and took out this moment, improve reaction gas pressure then, reduce the volume ratio of acetone/hydrogen and remove the compound coating preparation that the rare gas element argon gas carries out the coarse grain diamond coatings in position again, by obtaining the slick self-supporting diamond tubule of internal surface behind the erosion removal tungsten bar material matrix, employing is than the bigger steel pipe of self-supporting diamond tubule or the aluminum pipe shell as elongated tubular, be enclosed within outside the self-supporting diamond tubule, and between self-supporting diamond tubule and shell, fill by the epoxy adhesive of modification, form the elongated tubular that internal surface is made up of the low roughness diamond composite coating thus.
2. internal surface low roughness diamond composite coating elongated tubular preparation method according to claim 1, its feature is that also this preparation method comprises:
[1] the tungsten bar material of easy growing diamond of at first selecting respective diameters according to needed elongated tubular internal diameter is as matrix, handles making that tungsten bar material matrix surface is smooth as far as possible by surface finish;
[2] will place electronics to strengthen chemical vapor deposition reaction chamber through the tungsten bar material matrix after the surface finish processing, hot filament adopts the tantalum wire of 0.6 millimeter of ф, stretching with high temperature resistant spring, reaction chamber vacuumizes the back and feeds hydrogen and acetone, begin chemical vapour deposition fine-particle diamond coating after adjusting chamber pressure, the coating process parameter is: pressure 0.5-2KPa, reactant gases total flux 200-400 ml/min, the volume ratio of acetone/hydrogen is 2%-6%, filament temperature is 2000 ℃, bias current 1A adds rare gas element Ar, Ar/H
2Volume ratio is 0.5-1.5, after 2 hours, obtains thick 5 microns fine-particle diamond coating;
[3] after the fine-particle diamond coating reaches 5 microns, beginning in-situ deposition coarse grain diamond coatings, improve reaction gas pressure to 4-10KPa, the volume ratio that reduces acetone/hydrogen is to 1-3%, remove argon gas, improve simultaneously suitably filament temperature to 2200 ℃, through after 4 hours depositions, prepare the coarse grain diamond coatings of 15 microns of bed thickness again;
[4] the tungsten bar material that will deposit diamond composite coating takes out from electronics enhancing hot filament chemical vapor deposition reactor chamber, put in the container that fills corrosive fluid to remove tungsten bar material matrix, thereby prepare the self-supporting diamond tubule, the corrosive fluid preparation program is: proportion is that 1.19 hydrochloric acid and concentration are that the volume proportion of 30% hydrogen peroxide is 1: 1;
[5] from the container that fills corrosive fluid, take out the self-supporting diamond tubule after, for increasing the bonding force between diamond coatings and Resins, epoxy, also to carry out following surface treatment: (1) oxygen plasma surface treatment to the self-supporting diamond tubule for preparing, to remove the decolorizing carbon of coating outside surface, and, make coating mutually moistening with Resins, epoxy at regional area generation C=O key; (2) can generate the Ti or the Cr metal of carbide with diamond in the sputter of coating outside surface, and apply the monoalkoxy type titanate coupling agent that contains Ti;
[6] again will be than the bigger steel pipe of self-supporting diamond tubule or aluminum pipe shell as elongated tubular, be enclosed within outside the self-supporting diamond tubule, between self-supporting diamond tubule and shell, fill, form the elongated tubular that internal surface is made up of the low roughness diamond composite coating thus by the Racemic glycidol ethers propane type epoxy resin of di phenolic group binding agent of modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108305 CN1239739C (en) | 2003-10-30 | 2003-10-30 | Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108305 CN1239739C (en) | 2003-10-30 | 2003-10-30 | Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1540032A CN1540032A (en) | 2004-10-27 |
| CN1239739C true CN1239739C (en) | 2006-02-01 |
Family
ID=34334594
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310108305 Expired - Fee Related CN1239739C (en) | 2003-10-30 | 2003-10-30 | Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1239739C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9469918B2 (en) * | 2014-01-24 | 2016-10-18 | Ii-Vi Incorporated | Substrate including a diamond layer and a composite layer of diamond and silicon carbide, and, optionally, silicon |
| CN104032357B (en) * | 2014-05-19 | 2016-08-24 | 山东科技大学 | The preparation method of ability cathode electrophoresis resin-diamond scroll saw |
| CN104018207B (en) * | 2014-05-19 | 2016-08-24 | 山东科技大学 | The preparation of ability cathode electrophoresis resin-diamond scroll saw and ultra high pressure treatment method thereof |
| CN108660429B (en) * | 2018-03-23 | 2020-06-23 | 浙江工业大学 | Grain-close-packed n-type nano-diamond film and preparation method thereof |
| CN108823551A (en) * | 2018-07-05 | 2018-11-16 | 四川纳涂科技有限公司 | A kind of matrix self-cleaning method in cvd diamond deposition process |
| CN112126911A (en) * | 2020-09-30 | 2020-12-25 | 久钻科技(成都)有限公司 | High-performance diamond coating water jet cutting sand pipe and preparation method and preparation tool thereof |
-
2003
- 2003-10-30 CN CN 200310108305 patent/CN1239739C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1540032A (en) | 2004-10-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101818332B (en) | Super-hard self-lubricating diamond/diamond-like composite laminated coating material and preparation method thereof | |
| US5915162A (en) | Coated cutting tool and a process for the production of the same | |
| CN101487121B (en) | Diamond / W-C gradient structure composite coating and preparing method thereof | |
| CN1219109C (en) | Hard alloy matix complex shape cutter diamond coating preparation method | |
| EP0413834B1 (en) | Diamond-covered member and process for producing the same | |
| CN109930129A (en) | A kind of composite diamond coated carbides knife mold and preparation method | |
| JPWO2011055813A1 (en) | Coated tool | |
| CN106835037A (en) | A kind of high rigidity, multicomponent nitride coatings of high elastic modulus and preparation method thereof | |
| Klages et al. | Diamond coatings and cBN coatings for tools | |
| Gaydaychuk et al. | Influence of Al-Si-N interlayer on residual stress of CVD diamond coatings | |
| CN1239739C (en) | Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface | |
| You et al. | Microstructure and properties of CVD coated Ti (C, N)-based cermets with varying WC additions | |
| JPS61264171A (en) | Coated superalloy block having abrasion resistance and its production | |
| JP5424868B2 (en) | Hard material coating and method for producing a multifunctional hard material coating on a substrate | |
| JP3214891B2 (en) | Diamond coated members | |
| CN110387534A (en) | A kind of preparation method of nano diamond coating cemented carbide material | |
| US5334453A (en) | Diamond-coated bodies and process for preparation thereof | |
| CN115233067A (en) | Hard alloy for CVD diamond coating substrate and preparation method thereof | |
| JPH04507394A (en) | Transition metal carbide and nitride whiskers grown by CVD | |
| CN101967638B (en) | Preparation method of diamond film inner wall of fracture well head | |
| CN113667933B (en) | CrAlYO coated cutting tool and preparation method thereof | |
| CN113564551B (en) | Multiphase BN-Y/CrAlN composite coating and preparation method thereof | |
| JPH05209276A (en) | Manufacture of diamond coated member | |
| Singh et al. | Review on various techniques for the development of thin film boron nitride coating on metal surfaces | |
| JP3167371B2 (en) | Peel-resistant diamond-coated sintered alloy and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20041027 Assignee: CHANGZHOU HAILI TOOL Co.,Ltd. Assignor: Shanghai Jiao Tong University Contract record no.: 2018320000216 Denomination of invention: Method for preparing composite coat layer of diamond being plated slimline with low roughness in inside surface Granted publication date: 20060201 License type: Common License Record date: 20181022 |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060201 |