CN103834930B - The fixture of a kind of internal coating diamond film and technique - Google Patents
The fixture of a kind of internal coating diamond film and technique Download PDFInfo
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- CN103834930B CN103834930B CN201310736149.1A CN201310736149A CN103834930B CN 103834930 B CN103834930 B CN 103834930B CN 201310736149 A CN201310736149 A CN 201310736149A CN 103834930 B CN103834930 B CN 103834930B
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Abstract
The present invention discloses the fixture of a kind of interior punch die depositing diamond film and utilizes the technique of this fixture depositing diamond film, grinds workpiece by cleaning-drying, pre-treatment, throwing, with step deposition coating diamond films such as HF CVD depositing device shape core, growths. The diamond film of the present invention's deposition has following feature: vickers hardness number is about HV9000, and diamond film coating layer shape looks are continuous, even, fine and close, excellent radiation performance.
Description
Technical field
The present invention relates to the frock clamp of interior punch die depositing diamond film, and utilize the processing method of this frock clamp depositing diamond film.
Background technology
Interior punch die mainly contains the classifications such as wortle, punch die, extrusion die, be big batch, industrialization make welding wire, welding rod, stainless steel, cold steel, copper, aluminium, steel alloy, tungsten, etc. wire rod and the essential mould of pipe drawing, it is necessary to possess long service life, dimensional precision height, wire rod or the measured effect of tube surfaces matter.
But the cold extension of metallic substance, orientation is drawn, is pulled out, as: the drawing of pipe, line, diameter tolerance height, accuracy requirement is stable, surface smoothness is good, produce continuous operation in batches requires just higher to the mold use life-span, and owing to metallic substance its rigidity is just high, the making of mould just must use superhard material.
The mould that current wire rod and tubing industry use is sintered-carbide die and natural diamond, polycrystalline diamond mould, diamond thick-film cutting blade mainly. Sintered-carbide die is with low cost, and early application is extensive, but the sintered-carbide die life-span is short, easy sizing, and production efficiency is low, and work piece tolerance of dimension is unstable; Natural diamond mould hardness height, wear resistance are good, but all to there is fragility big for natural diamond and polycrystalline diamond and diamond thick-film, and difficulty of processing is big, expensive, and size and area little, be used for the interior punch die of footpath below 2mm.
The interior punch die being greater than more than 2mm has been used in the advanced technologies method of hard alloy substrate inwall depositing diamond film. Because in such diamond film coating, hole mould has possessed the high tenacity of Wimet and diamond high rigidity simultaneously, the characteristic of super abrasive be a kind of desirable improve in the effective means of punch die performance.
But a hole depositing diamond film and to be produced in batches to realize industrialization by no means easy in realizing on CVD coating apparatus! The inner hole wall deposition tool high rigidity making diameter very little, high adhesive force, low-friction coefficient and the uniform diamond rete of thickness, just the heated filament of temperatures as high more than 2000 �� must be passed in the middle of interior hole, heated filament energising must connect the battery lead rod at chip bench two ends, and heated filament diameter is 0.2-0.6mm only, will produce extension (elongation) sagging after heating, span is more big, sagging more serious.Have high temperature, high pressure heated filament once the sagging workpiece inner wall that touches will burn out mould. This is exactly the technical barrier that interior punch die depositing diamond film film realizes industrialization and is difficult to go beyond.
Also there is mould is parallel, vertical, to tilt the methods such as installation patent of invention before. But these patent fixtures do not have the reliability that can realize industrialization. Described parallel and tilt the mode that can only realize single-piece or 1-2 part and produce is installed. Installation method take into account the requirement of batch production, but also can only realize monofilament multimode (maximum 3-4 part), and vertically to connect electrode be very unrealistic at the two ends being achieved many heated filaments in coating apparatus narrow of excessive temperature and the metal space of conduction, therefore, multifibres multimode can only be a kind of good hope.
Summary of the invention
The present invention provides the fixture of a kind of large span, automatically compensation, high efficiency mould orate depositing diamond film and utilizes the interior punch die mass production processes of this fixture depositing diamond film. Hole depositing diamond film in wortle can be realized and automatically to center, automatically compensation heated filament drawing, and can realize batch production.
Above-mentioned purpose is achieved through the following technical solutions:
The fixture of a kind of internal coating diamond film, comprise V-type copper pad, battery lead rod, heated filament pressure pin, heated filament pull bar, spring suppport, steam line and the several heated filaments through mould orate, described heated filament is arranged in parallel on heated filament pressure pin and heated filament pull bar, described heated filament pressure pin is connected with battery lead rod respectively with heated filament pull bar, one end of described heated filament is fixed in the heated filament groove of heated filament pull bar, the other end is fixed on the spring of spring suppport, described spring suppport becomes the angle of 30 �� with horizontal plane, described spring suppport one end is arranged on heated filament pressure pin by ceramic jacket, the other end is provided with a spring by ceramic jacket, described V-type copper pad is arranged on the underface of heated filament, and the V-groove medullary ray of described V-type copper pad is parallel with heated filament, bottom and the chip bench of described V-type copper pad link together.
Described V-type copper pad is also provided with steam line, one end that described steam line is just bigger to mould diameter of bore, the less one end of mould diameter of bore, towards vacuum pump bleeding point, makes suction that mixed gas makes full use of vacuum pump be transported in each mould orate by the gas required for carbon source and deposition growing diamond film.
Described battery lead rod, chip bench inside are equipped with cooling water circulation pipe, it is ensured that the heat cooled water heat radiation in time that many heated filaments of arrangement are high-power produced with use.
The processing method step utilizing the interior punch die of this fixture depositing diamond film to produce in batches is as follows:
The first step: cleaning-drying: cleaning with raw spirit and remove workpiece surface slushing oil, then the workpiece of cleaning is put into thermostatic drying chamber, at 1-2 minute inner drying, temperature controlled at 50-60 DEG C;
2nd step: pre-treatment: etch workpiece surface in Ultrasonic Cleaners with preprocessing solution and namely carry out " pre-treatment " 50-60min, dries, in order to increase the nucleation density of diamond film deposition;
Described preprocessing solution is: with Na2Fe04 (Na2FeO4), potassium hydroxide (KOH), water (H4O2) formulated by weight the ratio of 1:2:20;
3rd step: throw and grind workpiece: throw with W6 diadust and grind the pretreated workpiece of upper step, make matrix form frame foundation before coating diamond film;
4th step: again clean: use acetone+dehydrated alcohol (3:7 proportioning) again to carry out degreasing, decontamination, cleaning, drying in Ultrasonic Cleaners;
5th step: workpiece heats: be placed in by the workpiece that upper step is dried on the chip bench of above-mentioned fixture, arranges heated filament, and being evacuated to thermocouple meter registration is 5-6Pa, 40-45min, regulates the electric current and voltage of battery lead rod that heated filament is progressively heated to 2000-2500 DEG C; The ratio of 2:2:1 inputs C, H2 and Ar to 1-2Pa from steam line simultaneously by volume;
6th step: shape core stage: after above step heating completes, regulates the electric current and voltage of battery lead rod to be progressively heated to 2800 DEG C, and the ratio of 2:2:1 inputs C, H and Ar to 1-2Pa simultaneously by volume, nucleated time 50min;
7th step: growth, depositional phase: after above step shape core completes, the electric current and voltage of battery lead rod is regulated progressively to be heated to 3000 DEG C, the ratio of 2:2:1 inputs C, H and Ar simultaneously by volume, form room, input chamber, gas mixture source, workpiece is added negative bias 4A, regulating vacuum pressure to 110KPa, deposit 5-7 hour, deposition of diamond thin films is complete.
The positively effect of the present invention is:
Present clip is combined by spring suppport, the angle of keep-spring pulling force and 30 ��, horizontal plane, by the roller slip effect of leverage and heated filament pressure pin, make to be energized heated filament in distance 250mm span by battery lead rod, it is heated to 3000 degree of high temperature, the extension produced is elongated and is compensated, and heated filament (12 hours) in whole coating required time is not sagging, remains on the straight medullary ray being arranged in mould orate. The invention solves in prior art and to produce to extend sagging after heated filament heats and sometimes burn out this technical barrier of mould, it may be achieved hole depositing diamond film in wortle also can automatically to center, automatic compensation heated filament drawing.
The present invention adopts multifibres, multiple-grooved (V-type copper pad) to arrange, it is ensured that every stove time can punch die in coating in a large number. For the chip bench of diameter �� 200mm, every stove can process 60-100 part, effectively reduces production cost, makes the industrial scale of mould orate depositing diamond film, industrialization turn into reality.
The present invention has following feature: 1, hardness: microhardness value is about HV9000, and this is that ordinary rigid alloy mold does not reach; 2, diamond film coating layer shape looks are continuous, even, fine and close; 3, excellent radiation performance: test proves, under identical working condition, in diamond film face, thermograde is little, and temperature distribution evenness is good, surface maximum temperature difference is only the half of copper. It thus is seen that use punch die ratio in the diamond film coating of the present invention to use ordinary rigid alloy mold, it may also be useful to life-span and efficiency can improve 8-10 doubly; 5-8 can be improved doubly than sintered-carbide die work-ing life and the efficiency of NCr coating.
Accompanying drawing explanation
Fig. 1 is the front view of the fixture of interior hole depositing diamond film.
Fig. 2 is the vertical view of the fixture of interior hole depositing diamond film.
Fig. 3 is interior punch die depositing diamond film production technological process.
In accompanying drawing: 1 ceramic jacket, 2 springs, 3 spring suppports, 4 battery lead rods, 5 V-type copper pads, 6 chip bench, 7 moulds, 8 heated filament pressure pins, 9 heated filaments, 10 heated filament pull bars, 11 steam lines, 12 vacuum pump bleeding points.
Embodiment
As shown in Figure 1 and Figure 2, the fixture of a kind of internal coating diamond film, comprises V-type copper pad 5, battery lead rod 4, heated filament pressure pin 8, heated filament pull bar 10, spring suppport 3, steam line and the several heated filaments 9 through hole in mould 7.Described heated filament 9 is arranged in parallel on heated filament pressure pin 8 and heated filament pull bar 10, described heated filament pressure pin 8 is connected with battery lead rod 4 respectively with heated filament pull bar 10, one end of described heated filament 9 is fixed in heated filament 9 groove of heated filament pull bar 10, the other end is fixed on the spring 2 of spring suppport 3, described spring suppport 3 becomes the angle of 30 �� with horizontal plane, described spring suppport 3 one end is arranged on heated filament pressure pin 8 by ceramic jacket 1, and the other end is provided with a spring 2 by ceramic jacket 1. Described spring suppport 3 is acted on by spring 2 and the roller slip effect of heated filament pressure pin 8, heated filament 9 is compensated adding thermogenetic extension elongation, heated filament 9 is not sagging in whole coating institute is free, remains on the straight medullary ray being arranged in hole in mould 7.
Described V-type copper pad 5 is arranged on the underface of heated filament 9, and the V-groove medullary ray of described V-type copper pad 5 is parallel with heated filament 9, and bottom and the chip bench 6 of described V-type copper pad 5 link together.
Described V-type copper pad 5 is also provided with steam line 11, one end that described steam line 11 is just bigger to mould 7 diameter of bore, the less one end of mould 7 diameter of bore, towards vacuum pump bleeding point 12, makes suction that mixed gas makes full use of vacuum pump be transported in each mould 7 in hole by the gas required for carbon source and deposition growing diamond film.
Described battery lead rod 4, chip bench 6 inside are equipped with cooling water circulation pipe, it is ensured that many heated filaments of arrangement 9 and use the cooled water heat radiation in time of high-power produced heat, it is ensured that equipment operating safety and chamber temp controlled, adjustable.
Embodiment 1:
For 60 interior hole �� 5mm wortles (being called for short " workpiece ") internal coating diamond film:
1, cleaning removal workpiece surface slushing oil with raw spirit, then the workpiece of cleaning is put into thermostatic drying chamber, at 1 minute inner drying, temperature controlled at 50 DEG C;
2, etching matrix surface in Ultrasonic Cleaners with preprocessing solution and namely carry out " pre-treatment " 50min, dry, in order to increase the nucleation density of diamond film deposition, preprocessing solution is: with Na2Fe04 (Na2FeO4), potassium hydroxide (KOH), water (H4O2) formulated by weight the ratio of 1:2:20;
3, then grind the pretreated workpiece of upper step with the throwing of W6 diadust, make workpiece form frame foundation before coating diamond film;
4, again clean: Ultrasonic Cleaners uses acetone+dehydrated alcohol (3:7 proportioning) again carry out degreasing, decontamination, cleaning, drying;
5, then the workpiece that upper step is dried is placed on chip bench, chip bench diameter �� 200mm; Battery lead rod and chip bench cold water circulating cooling. Equipment minimum power 12KVA;
6, heated filament pressure pin, heated filament pull bar are arranged on the battery lead rod at chip bench two ends respectively; Multiple-grooved V-type copper pad is arranged on chip bench with laser alignment instrument check and correction adjustment, makes V-groove medullary ray and heated filament pressure pin, heated filament pull bar heated filament groove coincidence and parallel;
7, after calibration, steady brace is installed, tightens screw. (if fixing punch die coating in a device-specific, as long as calibration once just can be reused); Mould to be coated carries out cleaning, pre-treatment, oven dry;
8, according to mould orate, this example wortle diameter of bore �� 5mm, selects heated filament diameter �� 0.4 tantalum silk, 60 workpiece are by 6 one rows, and arrangement 10 is arranged, and 10 heated filaments are through inner hole of workpiece, adjust equipment hoisting appliance according to internal bore radius, heated filament is overlapped with inner hole of workpiece medullary ray;
9, adjusting steam line makes steam line arrangement direction towards the bigger one end of the opening of mould, and alignment hydraucone is arranged in order;
10, operating equipment presses processing parameter heating heated filament to 2000 DEG C, the mixed gass such as input C, H2, Ar; By processing step: shape core, deposition (growth) diamond film.
Embodiment 2:
With 40 interior hole �� 10mm drawing dies (being called for short " workpiece "), in the equipment of embodiment 1 and the fixture coating of calibration V-type cushion block medullary ray, hole diamond film is example:
1, cleaning removal workpiece surface slushing oil with raw spirit, then the workpiece of cleaning is put into thermostatic drying chamber, at 1 minute inner drying, temperature controlled at 60 DEG C;
2, following preprocessing solution etches matrix surface in Ultrasonic Cleaners and namely carries out " pre-treatment " 50min, dries, and in order to increase the nucleation density of diamond film deposition, preprocessing solution is: with Na2Fe04 (Na2FeO4), potassium hydroxide (KOH), water (H4O2) formulated by weight the ratio of 1:2:20;
Then throw with W6 diadust and grind the pretreated workpiece of upper step, make workpiece form frame foundation before coating diamond film;
3, again clean: Ultrasonic Cleaners uses acetone+dehydrated alcohol (3:7 proportioning) again carry out degreasing, decontamination, cleaning, drying; Then the workpiece that upper step is dried is placed on HF CVD depositing device chip bench;
Using punch die coating in the device-specific on the same stage of embodiment 1, fixture has been calibrated and once just can have been reused; Mould to be coated carries out cleaning, pre-treatment, oven dry; According to this example mould diameter of bore �� 10mm, selecting �� 0.6mm heated filament, 40 workpiece, by 5 one rows, can distribute 8 rows, and heated filament, through inner hole of workpiece, adjusts equipment hoisting appliance according to internal bore radius, heated filament is overlapped with inner hole of workpiece medullary ray; Adjustment steam line makes steam line arrangement direction towards the bigger one end of the opening of mould;
4, operating equipment presses processing parameter heating heated filament to 2500 DEG C, the mixed gass such as input C, H2, Ar; By processing step: shape core, deposition (growth) diamond film.
Claims (1)
1. the technique of an internal coating diamond film, it is characterised in that comprise the steps:
The first step: cleaning-drying: cleaning with raw spirit and remove workpiece surface slushing oil, then the workpiece of cleaning is put into thermostatic drying chamber, at 1-2 minute inner drying, temperature controlled at 50-60 DEG C;
2nd step: pre-treatment: etch workpiece surface in Ultrasonic Cleaners with preprocessing solution and namely carry out " pre-treatment " 50-60min, dries, in order to increase the nucleation density of diamond film deposition;
Described preprocessing solution is: with Na2Fe04, potassium hydroxide, water, and the ratio by weight 1:2:20 is formulated;
3rd step: throw and grind workpiece: throw with W6 diadust and grind the pretreated workpiece of upper step, make matrix form frame foundation before coating diamond film;
4th step: again clean: use proportioning again to carry out degreasing, decontamination, cleaning, drying for 3:7 acetone+ethanol solution in Ultrasonic Cleaners;
5th step: workpiece heats: be placed on the chip bench of fixture of internal coating diamond film by the workpiece of upper step drying, arrange heated filament, being evacuated to thermocouple meter registration is 5-6Pa, 40-45min, regulates the electric current and voltage of battery lead rod that heated filament is progressively heated to 2000-2500 DEG C; The ratio of 2:2:1 inputs C, H from steam line simultaneously by volume2With Ar to 1-2Pa;
6th step: shape core stage: after above step heating completes, regulates the electric current and voltage of battery lead rod to be progressively heated to 2800 DEG C, and the ratio of 2:2:1 inputs C, H simultaneously by volume2With Ar to 1-2Pa, nucleated time 50min;
Described shape core, must knit the framework of diamond crystalline by structure before being the diamond film of deposition compact;
7th step: growth, depositional phase: after the 6th step shape core completes, regulates the electric current and voltage of battery lead rod to be progressively heated to 3000 DEG C, and the ratio of 2:2:1 inputs C, H simultaneously by volume2And Ar, forming room, input chamber, gas mixture source, workpiece is added negative bias 4A, regulate vacuum pressure to 110KPa, deposit 5-7 hour, deposition of diamond thin films is complete.
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| CN103834930B true CN103834930B (en) | 2016-06-08 |
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| CN107400874B (en) * | 2017-07-03 | 2019-04-09 | 浙江工业大学 | A method of diamond thin is prepared in stainless steel surface |
| CN108103477A (en) * | 2018-01-29 | 2018-06-01 | 珠海中纳金刚石有限公司 | The automatic center alignment device and method of a kind of HF CVD chemical vapor deposition |
| CN108660433B (en) * | 2018-05-13 | 2023-10-10 | 太原师范学院 | Device and method for preparing diamond film |
| CN109371380A (en) * | 2018-12-05 | 2019-02-22 | 中国科学院金属研究所 | A kind of hot-wire chemical gas-phase deposition device of Multifunctional diamond film |
| CN113549894B (en) * | 2021-07-29 | 2023-07-04 | 久钻科技(成都)有限公司 | Diamond coating wire drawing mould processingequipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4970986A (en) * | 1989-08-03 | 1990-11-20 | General Electric Company | Apparatus for synthetic diamond deposition including spring-tensioned filaments |
| US5833753A (en) * | 1995-12-20 | 1998-11-10 | Sp 3, Inc. | Reactor having an array of heating filaments and a filament force regulator |
| CN1060537C (en) * | 1998-06-12 | 2001-01-10 | 上海交通大学 | Diamond-coated wire-drawing die |
| CN2672082Y (en) * | 2003-06-24 | 2005-01-19 | 中国科学院物理研究所 | Heater in hot lamp filament chemical gas phase deposition device |
| KR100688838B1 (en) * | 2005-05-13 | 2007-03-02 | 삼성에스디아이 주식회사 | Apparatus for catalyst enhanced chemical vapor deposition and the catalyst enhanced chemical vapor deposition method |
| CN100400706C (en) * | 2006-03-27 | 2008-07-09 | 南京航空航天大学 | Heater array electrode system used for stable growth of diamond membrane with large area |
| CN201103987Y (en) * | 2007-10-10 | 2008-08-20 | 珠海格力电器股份有限公司 | Separation and floor type air conditioner |
| CN101280422B (en) * | 2008-04-02 | 2010-12-15 | 四川中物超硬材料有限公司 | Device for lot manufactureof diamond coating drawing die |
| CN102634770A (en) * | 2012-05-06 | 2012-08-15 | 北京科技大学 | Hot filament rack for large-area deposited diamond film and manufacturing method of hot filament rack |
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Effective date of registration: 20160519 Address after: 430040 East Lake new sun Technology Development Zone, Wuhan, Hubei, Gezhouba Dam Applicant after: WUHAN CENTURY ZHONGHANG SUPERPOWER DIAMOND FILM HIGH-TECH CO., LTD. Address before: Changde Hunan City Industrial Park 415200 Anfu county of Linli Province Applicant before: HUNAN ZHONGHANG SUPER DIAMOND FILM HIGH-TECH CO., LTD. |
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