CN103114275B - Preparation method of moving core mark for micronano-diamond composite coating tube stock - Google Patents
Preparation method of moving core mark for micronano-diamond composite coating tube stock Download PDFInfo
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- CN103114275B CN103114275B CN201310083293.XA CN201310083293A CN103114275B CN 103114275 B CN103114275 B CN 103114275B CN 201310083293 A CN201310083293 A CN 201310083293A CN 103114275 B CN103114275 B CN 103114275B
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- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011248 coating agent Substances 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 229910003460 diamond Inorganic materials 0.000 title abstract description 25
- 239000010432 diamond Substances 0.000 title abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 239000000956 alloy Substances 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 238000004050 hot filament vapor deposition Methods 0.000 claims abstract description 4
- 238000007667 floating Methods 0.000 claims description 44
- 239000007789 gas Substances 0.000 claims description 20
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000002113 nanodiamond Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 230000003698 anagen phase Effects 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910009043 WC-Co Inorganic materials 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 5
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000004513 sizing Methods 0.000 description 6
- 239000006071 cream Substances 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 241001012508 Carpiodes cyprinus Species 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Chemical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a preparation method of a moving core mark for a micronano-diamond composite coating tube stock. The preparation method comprises the following steps: as a coating matrix material, the pretreated low-cobalt hard alloy moving core mark is arranged on a conical fixed clamp, the moving core mark for the micronano-diamond composite coating tube stock is prepared by adopting a hot filament chemical vapor deposition method through a spatial hot filament array. By utilizing the preparation method, the service life of the original moving core mark can be greatly prolonged, thereby having significant meaning on improving the production efficiency and the product quality.
Description
Technical field
The present invention relates to a kind of preparation method of micro-nano diamond composite coating tubing floating core head.
Background technology
Floating core head trombone slide is the production method of a kind of advanced person of current drawing pipe, ultra-long tube high-speed stretch can be realized, reduce the waste end to end of tubing, improve lumber recovery, improve quality product, expand kind, be used widely in the good metals of plasticity such as copper, aluminium, mild steel and alloy pipe are produced.
Current application the most widely floating core head material is Wimet, have that hardness is high, wear-resisting, intensity and toughness better, be easy to the characteristics such as processing, be the main raw making floating core head at present.Because Wimet is formed by hard particles WC and binding agent Co sintering, in pulling process, binding agent Co easily and metal pipe material generation adhesion effect produce adhesive wear, thus the WC particle causing hardness higher comes off, make inner hole of pipe dimension overproof, smooth finish does not reach requirement, result is that the floating core head life-span is shorter, thus add production cost, reduce production efficiency and quality product, and cause the waste of tungsten resource, seriously constrain the progress of industrial technology and the raising of industry benefit.Therefore, excellent, the long-life superhard floating core head of exploitation wear resisting property is inexorable trend, is of great significance the manufacturing fast-developing tool of promotion tubular object extruding.
Diamond has extreme hardness and chemical stability, and its wear resistance is 100 times ~ 250 times of Wimet, has the excellent properties such as strong alkali-acid resistance, is the candidate material preparing floating core head.But due to reasons such as diamond fragility, preparation cost and techniques, natural diamond and polycrystalline diamond cannot apply to the preparation of floating core head.
If with the good Wimet floating core head of toughness for matrix, the diamond thin that coating one deck wear resistance is high, unreactiveness is good, then diamond coatings floating core head has the higher-strength of Wimet and the feature of diamond super abrasive concurrently, will be a kind of means of desirable raising floating core head performance.
Literature search through prior art finds, patent ZL200510107335.4 discloses a kind of floating core head blank and manufactures the method for floating core head with this blank, and floating core head blank includes sizing and large footpath, and the center at core print two ends is provided with center hole.The method manufacturing floating core head includes grinding sizing, large footpath profile operation, and the Wimet floating core head made by this method, the right alignment in its sizing and large footpath is high.Patent ZL201110228157.6 discloses a kind of strong lubrication floating core head and preparation method thereof, strong lubrication floating core head comprises core print with shoe cream room and union lever, core print is made up of working body and lubricant body, shoe cream room is arranged in lubricant body, and working body one end is provided with the step head with shoe cream room chamber wall shrink-fit.During making, adopt principle of expanding with heat and contracting with cold to realize the shrink-fit of working body and lubricant body, technique is easy to realize, and tooling cost is low.Above patent is only in mechanical lubrication, working method has been done very large improvement, and the degree improved for floating core head use properties is little, and does not all originally improve the use properties of core print with it from floating core head material.
Chemical vapor deposition diamond film has the premium properties of many uniquenesses, it has hardness close to natural diamond and wear resistance, there is low-friction coefficient, the characteristic such as high heat conductance and high chemical stability, from the beginning of the eighties in last century, on heterogeneous matrix, successful diamond synthesis film is so far, no matter cvd diamond is from growth theory, preparation method, preparation quality and performance characterization, or all achieve huge progress from subsequent processing techniques and applied research aspect, thus make it as wear-resistant coating at cutting tool, drawing mould and wear-resistant devices field have broad application prospects, effectively can solve high rigidity, high-wearing feature and temperature resistance problem.Up to the present not yet find both at home and abroad by cvd diamond film expansive approach to the application of drawing pipes on floating core head material.
Summary of the invention
The present invention is directed to prior art above shortcomings, provide a kind of preparation method of diamond coatings tubing floating core head.
The preparation method of diamond coatings tubing floating core head of the present invention is achieved through the following technical solutions, adopt pretreated low cobalt WC-Co hard alloy, be arranged on taper stationary fixture, be placed on the water-cooled platform of reaction chamber, adopt hot filament CVD to prepare micro-nano diamond composite coating tubing floating core head by space heater array.
Described pre-treatment refers to: the hard alloy substrate as floating core head is immersed in Murakami solution, and (each volume components compares k
3[Fe (CN)]
6: KOH:H
2o=1:1:10) ultrasonic cleaning 30min in, then (each volume components compares HNO hard alloy substrate to be placed in dilute nitric acid solution
3: H
2o=1:3) in, etching 15min is to remove the cobalt element on top layer.Finally supersound process 30min in the alcohol aaerosol solution containing particle diameter 1 μm.
Described hard alloy in low cobalt refers to: containing cobalt amount lower than 8% YG series WC-Co series hard alloy, the trade mark has YG8, YG6, YG3 etc.
Described stationary fixture refers to: adopt high temperature resistant, that thermal conductivity is good miramint material, the taper position of fixture and the inner hole of floating core head end good after be fixed on cooling table.
Described space heater array refers to: it is upper and lower two right to arrange, totally four high temperature spring vertical pulling heated filaments, and heated filament is perpendicular with the floating core head be vertically placed on water-cooled worktable, and the distance on heated filament range walk core print surface is 3mm ~ 5mm.
The micro-nano diamond composite coating processing parameter of described preparation:
1) the gaseous tension 1.0kPa ~ 2.0kPa in forming core stage, the volume parts of carbon-source gas is 3% ~ 6%, time 30 min ~ 60min; 2) growth phase reaction pressure 2.0kPa ~ 4.0kPa, the volume parts of carbon-source gas is 1% ~ 3%, depositing time 5h ~ 7h; 3) the making Nano surface stage, reaction pressure 1.0kPa ~ 2.0kPa, the volume parts of carbon-source gas is 3 ~ 6%, time 30 min ~ 60min.
In three stages, reactant gases is carbon-source gas CH
4and H
2gas mixture, total flux 300 ml/min ~ 500ml/min, remains that the temperature of vertical pulling heated filament is about 2000 DEG C ~ 2300 DEG C, regulates floating core head substrate temperature scope at 800 DEG C ~ 900 DEG C according to hot-wire temperature.
The present invention adopts hot filament CVD to be realized by space heater array, can increase substantially the work-ing life of original floating core head, significant to improve production efficiency and product quality.
Accompanying drawing explanation
Fig. 1 is the preparation facilities structural representation of small aperture diamond coating wortle of the present invention;
Fig. 2 is the preparation facilities structure vertical view of small aperture diamond coating wortle of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Fig. 1 is the preparation facilities structural representation of small aperture diamond coating wortle of the present invention.Shown in Fig. 1, Wimet floating core head 1 is fixed on tapered fixture 2, according to floating core head arrangements space heater array, be made up of upper heater strip 3 and lower heater strip 4, heater strip 3,4 is fixed on high temperature spring 5 and on electrode 7, by direct supply 6 pairs of heated filament thermal degradation gases, matrix 1 prepares diamond coatings.
Fig. 2 is the preparation facilities structure vertical view of small aperture diamond coating wortle of the present invention.It is be arranged in equably around Wimet floating core head 1 in pairs that Fig. 2 shows heater strip 3,4, ensure that the homogeneity of depositing temperature, thus ensure that the homogeneity of diamond coatings.
Wimet floating core head 1 in the present invention adopts YG8 Wimet floating core head, sizing portion size is Φ 9.50mm, allowable tolerance is-0.02 ~ 0mm, the sizing Φ 9.44mm of surface after repairing reserved coat-thickness and tolerance, mould is placed on ultrasonic cleaning 30min in Murakami solution through surface decontamination cleaning, then dilute nitric acid solution (HNO3:H2O=1:3) is placed in remove the cobalt of matrix surface, take out after 15min, the acid of remained on surface is washed away with clear water, again mould is put into the diadust suspension sonic oscillation process 30min that granularity is 1 μm, take out rear deionized water and raw spirit cleaning, then be placed on the tapered fixture 2 of chemical vapor deposition reaction chamber.Arrange upper and lower two pairs of heated filaments 3 and 4, and the shortest distance of every root heated filament and heated filament is 4mm, heated filament adopts the tantalum wire of Φ 0.3mm, and one end is fixed on electrode 7, and the other end adopts high temperature spring 5 to strain.Reactant gases (H is passed into after reaction chamber vacuumizes
2, CH
4), start chemical gas-phase deposition of diamond coating after adjustment chamber pressure.Forming core stage process parameter is: pressure 1.5kPa, and reactant gases is CH4 and H2 gas mixture, and the volume parts of total flux 500ml/min, CH4 is 4%, hot-wire temperature about 2200 DEG C, time 1h.Growth phase processing parameter is: pressure 2.5kPa, and reactant gases is CH
4, H
2gas mixture, CH
4volume parts is 2%, total gas couette 500ml/min, time 6h.In the making Nano surface stage, pressure 1.5kPa, the volume parts of carbon-source gas is 5%, time 50min.Obtain about 35 μm of thick micro-nano diamond composite coatings.Sizing after coating mold polishing is Φ 9.49mm.This diamond composite coating floating core head is used for the drawing of copper pipe, and its life-span is more than 10 times of Wimet floating core head.
Claims (2)
1. the preparation method of a micro-nano diamond composite coating tubing floating core head, it is characterized in that, described preparation method comprises following content: adopt pretreated hard alloy in low cobalt floating core head as coated substrate material, be arranged on taper stationary fixture, adopt hot filament CVD to prepare micro-nano diamond composite coating tubing floating core head by space heater array;
Described pre-treatment is: the hard alloy substrate as floating core head is immersed in volume components and compares K
3[Fe (CN)]
6: KOH:H
2ultrasonic cleaning 30min in the solution of O=1:1:10, then hard alloy substrate is placed in volume components and compares HNO
3: H
215min is etched to remove the cobalt element on top layer in the dilute nitric acid solution of O=1:3; Finally supersound process 30min in the alcohol aaerosol solution containing particle diameter 1 μm;
Described hard alloy in low cobalt refer to containing cobalt amount lower than 8% WC-Co series hard alloy;
Described space heater array is: it is upper and lower two right to arrange, totally four high temperature spring vertical pulling heated filaments, and heated filament is perpendicular with the floating core head be vertically placed on water-cooled worktable, and the distance on heated filament range walk core print surface is 3mm ~ 5mm;
The micro-nano diamond composite coating processing parameter of described preparation:
1) the gaseous tension 3.0KPa ~ 5.0KPa in forming core stage, the volume parts of carbon-source gas is 3% ~ 6%, time 30 min ~ 60min; 2) growth phase reaction pressure 2.0KPa ~ 4.0KPa, the volume parts of carbon-source gas is 1% ~ 3%, depositing time 5h ~ 7h; 3) the making Nano surface stage, growth phase reaction pressure 2.0KPa ~ 4.0KPa, the volume parts of carbon-source gas is 3 ~ 6%, time 30 min ~ 60min;
In above-mentioned three stages, reactant gases is carbon-source gas CH
4and H
2gas mixture, total flux 300 ml/min ~ 500ml/min, remains that the temperature of vertical pulling heated filament is 2000 DEG C ~ 2300 DEG C, regulates floating core head substrate temperature scope at 800 DEG C ~ 900 DEG C according to hot-wire temperature.
2. preparation method according to claim 1, is characterized in that, described stationary fixture adopts the miramint material high temperature resistant, thermal conductivity is good, the taper position of fixture and the inner hole of floating core head end good after be fixed on cooling table.
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| CN201310083293.XA CN103114275B (en) | 2013-03-15 | 2013-03-15 | Preparation method of moving core mark for micronano-diamond composite coating tube stock |
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| CN201310083293.XA CN103114275B (en) | 2013-03-15 | 2013-03-15 | Preparation method of moving core mark for micronano-diamond composite coating tube stock |
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| CN103114275B true CN103114275B (en) | 2015-01-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104785560A (en) * | 2015-03-31 | 2015-07-22 | 广东龙丰精密铜管有限公司 | Traveling core head provided with high-hardness working surface |
| CN107282677A (en) * | 2017-05-25 | 2017-10-24 | 爱康企业集团(上海)有限公司 | A kind of tube extrusion mouth mold with film plating layer and preparation method thereof |
| CN108060407B (en) * | 2017-11-09 | 2021-08-06 | 上海交通大学 | A kind of preparation method of micro-nano multilayer composite diamond film |
| JP7287109B2 (en) * | 2018-05-25 | 2023-06-06 | 株式会社プロテリアル | Method for manufacturing sliding parts |
| CN110527891B (en) * | 2019-09-16 | 2021-11-02 | 东华大学 | Diamond coating on the surface of low cobalt cemented carbide and preparation method thereof |
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| CN101280423B (en) * | 2008-04-02 | 2010-04-21 | 中国工程物理研究院总体工程研究所 | Manufacturing method of small aperture diamond coating drawing die |
| CN202482433U (en) * | 2012-03-05 | 2012-10-10 | 宜兴市景程模具有限公司 | Micro-pore diamond coating device for wire-drawing dies |
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Address after: 919 box 401, box 621900, Mianyang City, Sichuan Province Co-patentee after: Sichuan jiuzuan Technology Co., Ltd. Patentee after: General Engineering Research Inst., China Engineering Physics Inst. Address before: 919 box 401, box 621900, Mianyang City, Sichuan Province Co-patentee before: Sichuan Zhongwu Ultrahard Material Co., Ltd. Patentee before: General Engineering Research Inst., China Engineering Physics Inst. |
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Effective date of registration: 20210729 Address after: 919 box 401, box 621900, Mianyang City, Sichuan Province Patentee after: GENERAL ENGINEERING RESEARCH INST., CHINA ACADEMY OF ENGINEERING PHYSICS Patentee after: Jiuzuan Technology (Chengdu) Co.,Ltd. Address before: 919 box 401, box 621900, Mianyang City, Sichuan Province Patentee before: GENERAL ENGINEERING RESEARCH INST., CHINA ACADEMY OF ENGINEERING PHYSICS Patentee before: Sichuan jiuzuan Technology Co.,Ltd. |