CN1106470A - Quick growth method of artificial diamond film - Google Patents
Quick growth method of artificial diamond film Download PDFInfo
- Publication number
- CN1106470A CN1106470A CN 94105416 CN94105416A CN1106470A CN 1106470 A CN1106470 A CN 1106470A CN 94105416 CN94105416 CN 94105416 CN 94105416 A CN94105416 A CN 94105416A CN 1106470 A CN1106470 A CN 1106470A
- Authority
- CN
- China
- Prior art keywords
- diadust
- diamond film
- artificial diamond
- toluene
- gas
- 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.)
- Pending
Links
Images
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
The quick growing method of artificial diamond film includes grinding workpiece made of Mo or Ti, coating the mixture of catalyst and micro diamond powder, putting it in vacuum reaction region in diamond film synthesizer, vacuumizing, and inducting hydrogen and then methane gas or hydrocarbon while microwave discharge for 1 hr for electrolytic dissociation to decompose hydrocarbon or methane gas, resulting in an artificial diamond film (1.5 mm in thickness) thermally deposited.
Description
The present invention relates to a kind of artificial diamond film method of growth fast, belong to the chemical vapour deposition field.
Adamantine physics, electricity, gas, light, heat and characteristic electron all are better than other material in many aspects, and its most significant characteristic comprises other high several magnitude of coated material and high mobility of high heat conductance, hardness ratio.The application of diamond thin is very extensive; spread over every field; particularly the artificial diamond film technology causes that countries in the world pay attention to widely in recent years; flourish situation appears; current diamond synthetic method has a variety of; mainly be to protecting plasma generation chamber and reaction chamber importing under the decompression to contain hydrocarbon or the film forming gas of carbonoxide, apply magnetic field and microwave electric power, making it 10 from the outside to this gas
-5Pa all can grow into diamond film under normal pressure, the chemical vapor deposition (CVD) of immediate development that Here it is is made the method for diamond thin, and the total overall reaction process is finished in microwave plasma CVD equipment.Japanese kokai publication hei 5-5179 discloses with vacuumizing heated parts, feeds plasma gas and hydrocarbon gas and forms deposit film.European patent 923036909 discloses to vacuumize and has fed plasma body hydrocarbon gas and powder metal or non-metallic material formation film.Japanese kokai publication hei 4-280894 discloses on workpiece and to have applied the micro mist metal or non-metallic material form film, these method ubiquity film formation times long (10 μ m/h), and the cost height, coat combines insecure with metalwork, and is difficult to defective such as suitability for industrialized production.
The objective of the invention is to overcome the defective that prior art exists, provide a kind of new artificial diamond film quick growing technology, employing is in the agent of workpiece surface carbon coating hydride catalytic, when sedimentation velocity can reach 1.5mm/, workpiece surface temperature also drops to 700 ℃ by the past hot conditions, reduced cost, made PCVD technology step major step to practicability.
Realize that technical scheme of the present invention is:
1. preparation contains the catalyst-coated material
Catalyzer toluene and polyethylene are carried out miscible, the diadust that adds granularity＜1.5 μ m then fully stirs and makes its mixing, and its ratio toluene, polyethylene, diadust are 7～9.5: 3～0.5: 1～4.
2. the quick growth technique of diamond thin
Metallic substance molybdenum, titanium workpiece, with the diadust of granularity＜1.5 μ m its surface of polishing, remove greasy dirt and strengthen sticking power, be coated with the coating material that catalyzer toluene, polyethylene and diadust mix then, workpiece after applying is put into the vacuum reaction district of microwave plasma synthesis of diamond film device, vacuumizes to make its vacuum tightness reach Pa
-1After, oxygen content in the system must not surpass 0.05 ‰, charge into hydrogen earlier, feed methane gas or hydrocarbon polymer again, its ratio hydrogen: methane gas or hydrocarbon polymer are 99～99.8: 1～0.2, open microwave power supply microwave discharge, and ionization takes place in reaction chamber, methane gas or hydrocarbons decompose, and mixed gas flow is 0.3～0.5m
3/ minute, the pressure of reaction zone is 0.3Pa, workpiece surface temperature is 700～1050 ℃, and 1 hour ionized reaction times, put into the workpiece surface of reaction chamber, the heat sink thick artificial diamond film of 1.5mm of going up, sedimentation velocity is 1.5mm/h.
3. microwave plasma CVD equipment
The MWPCVD equipment that the present invention selects for use is instrumentation center, Chinese Academy of Sciences Shenyang product, the key technical indexes:
Base vacuum degree: 6.6 * 10
-3Pa
Working vacuum degree: 1-10
-4Pa
The main gas of working: hydrogen, hydrocarbons, methane gas.
This equipment is referring to synoptic diagram 1, a quartz glass discharge vessel (1) is inserted in the microwave resonator (2), coaxial with circular waveguide resonator cavity (2), an end face in chamber is a tunable piston (3), and microwave power is by coupling mechanism input resonator (2).The one end input reactant gases (4) of discharge tube, the other end communicates with reaction chamber (5), and facing to the workpiece on the workpiece table top (6), reaction chamber (5) is connected with vacuum system (7), before injecting reactant gases, system vacuumizes, injecting gas (8) afterwards, the vacuum system pumping speed is controlled the operating pressure of discharge tube and reaction chamber with two factors of injecting gas flow.
The present invention compared with prior art has following advantage:
1. production technique of the present invention adopts the agent of carbon containing hydride catalytic to be coated with and is contained in workpiece surface, can reach 1.5mm/h by microwave chemical vapour deposition production diamond like carbon film sedimentation velocity.
2. its workpiece surface temperature of production technique of the present invention drops to 700 ℃ by the past hot conditions, has reduced cost.
3. PCVD technology of the present invention, sedimentary on metal molybdenum, titanium part is hard formation deposition method based on amorphous diamond, improve the parts surface performance greatly, particularly improved its wear resistance or erosion resistance, be fit to industrial sector scale operation.
4. production technique of the present invention can be widely used in industrial all departments, cuts tool, internal combustion turbine piston, cylinder body, dies cavity protective layer, mechanical transmission component anti-wear position, synthetic glass anti-wear protective layer etc. as five metals cutter, abrasive material.
Accompanying drawing:
Fig. 1: microwave plasma gas aggradation equipment synoptic diagram
Diagram: the 1-quartz discharge Fig. 2-tunable piston of resonator cavity 3-
4-reaction gas inlet 5-reactor 6-chip bench
7-connects vacuum system 8-gas inlet
Embodiment:
At first prepare coating material, take by weighing toluene 900 grams, polyethylene 100 grams make it miscible, add granularity＜1.5 μ m diadusts, 200 grams then, fully stir to make it even.
Second step above-mentioned coating material of application on 200 * 10 * 5 molybdenum steel bar, it is indoor to put into the PCVD device reaction, vacuumizes, and oxygen content is no more than 0.05 ‰ in the vacuum chamber, is 2 * 10 at vacuum pressure
-3T is at 1kg/cm
2Pressure under, feed hydrogen earlier, hydrogen is with 20 liters/minute flow velocity, feed methane gas again and enter vacuum chamber with 0.5 liter/minute flow velocity, open the microwave power supply heating, temperature is not higher than 1050 ℃, vacuum pressure maintains 100t, under 700 ℃ of the maintenance workpiece surface temperatures, 1 hour reaction times, the thick artificial diamond film of workpiece surface deposition 1.5mm.
Claims (5)
1, a kind of artificial diamond film method for fast growing, system is with surface treated metal works, carry out the method for chemical vapour deposition man-made diamond by the microwave plasma discharge device, it is characterized in that metallic substance molybdenum, titanium workpiece, remove greasy dirt with diadust its surface of polishing, be coated with the coating material that catalyzer and diadust mix then, put into the vacuum reaction district of microwave plasma synthetic diamond thin machine, be evacuated to vacuum tightness and reach Pa
-1After, charge into hydrogen earlier, feed methane gas or hydrocarbon polymer again, open the microwave power supply heating, temperature is not higher than 1050 ℃, reacts 1 hour, puts into the heat sink thick artificial diamond film of 1.5mm/h of going up of workpiece surface of reaction chamber.
2, the method for claim 1 is characterized in that described catalyzer is toluene and poly mixed solvent, and its ratio is a toluene 7～9.5, polyethylene 3～0.5.
3, the method for claim 1, it is characterized in that described coating material is diadust to be put into the catalyzer stirring be modulated into pasty state, its ratio: toluene, polyethylene, diadust are 7～9.5: 0.5～3: 1～4, and the granularity of diadust＜1.5 μ m.
4, the method for claim 1 is characterized in that reaction zone is evacuated to Pa
-1After, feed earlier hydrogen, after fill methane gas or hydrocarbon polymer, ratio is 99～99.8: 1～0.2.
5, the method for claim 1, after it is characterized in that feeding gas, the pressure of reaction zone is 0.3Pa, 700～1050 ℃ of workpiece surface temperatures, optimum temps is 700 ℃, mixed gas flow is 0.3～0.5m
3/ minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94105416 CN1106470A (en) | 1994-07-15 | 1994-07-15 | Quick growth method of artificial diamond film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94105416 CN1106470A (en) | 1994-07-15 | 1994-07-15 | Quick growth method of artificial diamond film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1106470A true CN1106470A (en) | 1995-08-09 |
Family
ID=5032051
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94105416 Pending CN1106470A (en) | 1994-07-15 | 1994-07-15 | Quick growth method of artificial diamond film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1106470A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065573C (en) * | 1996-08-19 | 2001-05-09 | 时至准钟表股份有限公司 | Guide bush and method of forming hard carbon film over inner surface of guide bush |
| CN100370281C (en) * | 2006-01-24 | 2008-02-20 | 东北大学 | Method for depositing carbon film on resin lens |
| CN103752640A (en) * | 2013-12-29 | 2014-04-30 | 湖南中航超强金刚石膜高科技有限公司 | Manufacturing method of extrusion punching head of diamond film piston pin |
| CN106637143A (en) * | 2016-09-23 | 2017-05-10 | 常州大学 | Preparation method of MPCVD diamond film |
| CN109295434A (en) * | 2018-11-27 | 2019-02-01 | 江苏沃德赛模具科技有限公司 | Micropore surface nano-diamond coating |
-
1994
- 1994-07-15 CN CN 94105416 patent/CN1106470A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065573C (en) * | 1996-08-19 | 2001-05-09 | 时至准钟表股份有限公司 | Guide bush and method of forming hard carbon film over inner surface of guide bush |
| CN100370281C (en) * | 2006-01-24 | 2008-02-20 | 东北大学 | Method for depositing carbon film on resin lens |
| CN103752640A (en) * | 2013-12-29 | 2014-04-30 | 湖南中航超强金刚石膜高科技有限公司 | Manufacturing method of extrusion punching head of diamond film piston pin |
| CN103752640B (en) * | 2013-12-29 | 2018-10-12 | 武汉世纪中航超强金刚石膜高科技有限公司 | A kind of production method of diamond film piston pin extrusion punch |
| CN106637143A (en) * | 2016-09-23 | 2017-05-10 | 常州大学 | Preparation method of MPCVD diamond film |
| CN109295434A (en) * | 2018-11-27 | 2019-02-01 | 江苏沃德赛模具科技有限公司 | Micropore surface nano-diamond coating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5433977A (en) | Enhanced adherence of diamond coatings by combustion flame CVD | |
| US4985227A (en) | Method for synthesis or diamond | |
| US5846613A (en) | Method for depositing a hard protective coating | |
| Scott et al. | Kinetics and mechanism of amorphous hydrogenated silicon growth by homogeneous chemical vapor deposition | |
| US5674572A (en) | Enhanced adherence of diamond coatings employing pretreatment process | |
| EP0327110B1 (en) | Method for producing sintered hard metal with diamond film | |
| CN1057869A (en) | Isotopic pure single crystal epitaxial diamond films and preparation method thereof | |
| CN1106470A (en) | Quick growth method of artificial diamond film | |
| US5358596A (en) | Method and apparatus for growing diamond films | |
| Schenk et al. | The origin of reduced chemical erosion of graphite based materials induced by boron doping | |
| US6558742B1 (en) | Method of hot-filament chemical vapor deposition of diamond | |
| JPS60210597A (en) | Gas phase synthesizing method of diamond | |
| Pierson | Chemical vapor deposition of nonsemiconductor materials | |
| JP2754259B2 (en) | Combustion Flame Synthesis Method for Transparent Diamond | |
| RU2254397C2 (en) | Method of production of the diamond-like film | |
| JPH0481552B2 (en) | ||
| JPH0869997A (en) | Semiconductor device with passivation layer | |
| US20220195593A1 (en) | Method for producing N-doped carbon nanomesh | |
| CN102304696B (en) | Preparation method of diamond | |
| JPH0427690B2 (en) | ||
| Bonetti | Protective CVD Coatings–Going from High Temperature Processes to Plasma Activation | |
| JPS60231822A (en) | Production of carbonaceous fiber | |
| JP2619557B2 (en) | Synthesis method of vapor phase diamond | |
| Rudder et al. | Formation of diamond films from low pressure radio frequency induction discharges | |
| JPS62218576A (en) | Plasma cvd method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |