CN1224772A - Synthesis of carbon-base film - Google Patents
Synthesis of carbon-base film Download PDFInfo
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- CN1224772A CN1224772A CN 98111833 CN98111833A CN1224772A CN 1224772 A CN1224772 A CN 1224772A CN 98111833 CN98111833 CN 98111833 CN 98111833 A CN98111833 A CN 98111833A CN 1224772 A CN1224772 A CN 1224772A
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Abstract
The present invention relates to the technology field of vacuum deposition film. By utilizing carbon as metal plasma source and nitrogen as gas plasma source, the present invention forms diamond-like film or carbon nitride film on the surface of workpiece with complicated shape. The method described in the present invention is used to synthesize film with superhigh hardness, high bonding strength, high wear resistance and high corrosion resistance on the surface of workpiece with complicated shape. The method is mainly used in the surface modification of artificial organs.
Description
The present invention relates to the vacuum deposition film technical field, particularly in the technical field of complex-shaped device surface uniform deposition carbon-base film.
Diamond thin, carboritride film and so on carbon-base film material has excellent mechanics, calorifics, electricity, optics and acoustic characteristics and the wide thin-film material of the development prospect that becomes, methods such as using plasma chemical vapour deposition, sputter, ion beam enhanced depositing and magnetic filtered arc source deposition have been synthesized diamond like carbon film and carboritride film, wherein method such as sputtering sedimentation, ion beam enhanced depositing is because sedimentary atomic ion line is a collinear, there is not diffraction, thereby can only be at planar sample surface deposition film.Though magnetic filtered arc source deposition method is because what draw is charged ion beam current, move thereby have part diffraction along power line applying under the negative bias effect line on the sample table, still can not the uniform film of acquisition to the spatial workpiece.The plasma activated chemical vapour deposition method is in the reactive plasma field owing to workpiece, thereby can obtain uniform film at the workpiece surface of complexity, but this method institute synthetic film bonding force is not really high, and because institute's synthetic film SP3 linkage content is not high, so its hardness and other performances are restricted, and, substrate material is limited to some extent because synthesis temperature is higher.Document 1 (K.C.walter, et al, Diamond-like carbon deposition for tribological applications at Los Alamos National Laboratory, MaterialsResearch Society Symposium Proceedings, Volume 383,1995) reported that the acetylene gas pulsed plasma synthesizes the method for diamond like carbon film, charge into acetylene gas in the vacuum chamber and ionization formation plasma field, apply the pulse negative high voltage on the workpiece in plasma field, carbon ion is accelerated bombardment and is deposited on workpiece surface, it is higher to obtain bonding force, uniform diamond like carbon film, but owing to exist hydrogen inevitably, the only about 25GPa of the hardness of film in the film.Do not see as yet and (be lower than 200 ℃) at a lower temperature at surperficial superhard (hardness is greater than the 40GPa) diamond like carbon film and the report of carboritride film of forming of complex part.
The vacuum deposition method that the purpose of this invention is to provide a kind of carbon-base film, it can be effectively in the synthetic equably high rigidity of complex-shaped workpiece surface, the diamond like carbon film and the carboritride film of higher bonding force are arranged with matrix.
Using plasma immersion ion implantttion technique of the present invention is implemented in the diamond like carbon film and the carboritride film of complex part surface uniform deposition ultrahigh hardness (hardness is greater than 40GPa), and its technology can realize by following scheme:
1 with graphite as cathode material, pack into the negative electrode of four uniform metallic cathode Vacuum Arc plasma sources (MEVVA source) of plasma immersion ion injection device, carbon plasma is introduced vacuum chamber, the parameter that produces and draw carbon plasma is: trigger voltage 2-12KV, electric current 200-600mA, trigger frequency 10-200Hz, pulse width 50-500 μ s, striking voltage 50-500V, electric current 10-100A, pass through the deflecting action of the outer deflection solenoid of installing of bend pipe and filter neutral atom and particle, the voltage 100-1000V of magnetic deflection coil, electric current 5-50A, and through the scanning of the scanning solenoid of bend pipe and vacuum chamber junction and enter vacuum chamber, sweep voltage is 100-2000V, and sweep current is 5-30A, and carbon plasma density is 5 * 10
8-1 * 10
10/ cm
3For making film and matrix that higher bonding force be arranged, on sample table, apply negative DC voltage earlier and make the sample table rotation, voltage magnitude is 8-10kv, deposit 5-10 minute, turn down negative DC voltage subsequently, voltage magnitude is 0.1-0.5kv, the stream of carbon ion bombardment is by force 10-100mA, the sample table speed of rotation is 0.5-10 rev/min, carbon plasma sweep beam that draw in four uniform cathode vacuum arc plasma sources around the vacuum chamber and sample table are rotated under the combined action, obtain the superhard diamond like carbon film of uniform pure carbon at the workpiece surface of complexity, and depositing of thin film speed is 1-20 dust/second.
With above-mentioned carbon plasma producing method carbon plasma is introduced vacuum chamber by metal vacuum arc plasma source, density is 5 * 10
8-1 * 10
10/ cm
3For making film and matrix that higher bonding force be arranged, on sample table, apply a pulse negative voltage earlier, voltage magnitude is 30-60kv, pulse width is 10-60 μ s, pulse-repetition frequency is 50-1000Hz, deposits 5-10 minute, turns down the pulse negative voltage subsequently, voltage magnitude is 0.1-0.5kv, the stream of carbon ion bombardment is by force 10-100mA, and depositing of thin film speed is 1-20 dust/second, obtains the superhard diamond like carbon film of uniform pure carbon on the complex part surface.
2. with above-mentioned carbon plasma producing method, with graphite as cathode material, pack into the negative electrode of four uniform metallic cathode Vacuum Arc plasma sources (MEVVA source) of plasma immersion ion injection device, carbon plasma is drawn by metallic cathode arc plasma source, filter neutral atom and particle through the deflecting action of the outer solenoid of installing of bend pipe and enter vacuum chamber through the scanning of the solenoid of bend pipe and vacuum chamber junction, carbon plasma density is 5 * 10
8-1 * 10
10/ cm
3Simultaneously charge into nitrogen in vacuum chamber, pressure is 10
-3-10
-1Pa adopts the rf (discharge) plasma source, and frequency is 13.56MHz, and discharge power is 0.3-3KW; THE FILAMENT DISCHARGE AND plasma source, sparking voltage are 50-200v, and electric current is 10-50A or microwave discharge plasma source, and frequency is 2.45GHz, and discharge power is 0.5-3kW, produces nitrogen plasma in vacuum chamber, and making nitrogen plasma density is 5 * 10
8-5 * 10
10/ cm
3For making film and matrix that higher bonding force be arranged, on sample table, apply a direct current negative voltage earlier and make the sample table rotation, voltage magnitude is 8-10kv, deposits 5-10 minute, turns down negative DC voltage subsequently, voltage magnitude is 0.1-0.5kv, the sample table velocity of rotation is 0.5-10 rev/min, can form the carboritride film at sample surfaces, and depositing of thin film speed is 1-20 dust/second.
Use above-mentioned carbon, the nitrogen plasma production method, with graphite as cathode material, pack into the negative electrode of four uniform metallic cathode Vacuum Arc plasma sources (MEVVA source) of plasma immersion ion injection device, carbon plasma is drawn by metallic cathode arc plasma source, filter neutral atom and particle through the deflecting action of the outer solenoid of installing of bend pipe and enter vacuum chamber through the scanning of the solenoid of bend pipe and vacuum chamber junction, in vacuum chamber, charge into simultaneously nitrogen, adopt the rf (discharge) plasma source, THE FILAMENT DISCHARGE AND plasma source or microwave discharge plasma source form nitrogen plasma in vacuum chamber, for making film and matrix that higher bonding force be arranged, on sample table, apply earlier a pulse negative voltage, voltage magnitude is 30-60kv, pulse width is 10-60 μ s, pulse-repetition frequency is 50-1000Hz, deposit 5-10 minute, turn down the pulse negative voltage subsequently, voltage magnitude is 0.1-0.5kv, depositing of thin film speed is 1-20 dust/second, forms the carboritride film at sample surfaces.
The present invention's advantage and effect compared with prior art is:
(1) the present invention can realize batch processing, thereby can realize industrial application at synthetic uniform diamond like carbon film of the workpiece surface of complexity and carboritride film.
(2) because the ionic fluid of institute of the present invention synthetic diamond like carbon film and carboritride depositing of thin film process is all Ionized, its energy can be regulated in a big way and control, thereby institute's synthetic film can obtain very high-load carbon-to-carbon or carbon-nitrogen-atoms bonded sp
3Key, thereby can obtain very high hardness (can greater than 40Gpa), and can make film and body material that very high bonding force is arranged, and can make workpiece in deposition process, remain on lesser temps (being lower than 200 ℃).
Description of drawings of the present invention is as follows:
Fig. 1 is the vacuum chamber A-A sectional view of equipment therefor of the present invention.
Fig. 2 is the vacuum chamber vertical view of equipment therefor of the present invention.
The invention will be further described below in conjunction with accompanying drawing:
Embodiment 1 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, and airtight vacuum chamber 1 is evacuated to air pressure less than 5 * 10
-4Pa, graphite 2 is installed in the negative electrode in metallic cathode arc plasma source 3, the extraction catheter in metallic cathode arc plasma source has magnetic deflection coil 4 outward, in junction sweep coil 5 is arranged with main vacuum chamber, open the triggering device power supply in metallic cathode arc plasma source 3, regulate trigger voltage to 6.5KV, electric current 200mA, striking voltage 120V, the voltage 200V of electric current 10A and magnetic deflection coil, electric current 10A.Carbon plasma is introduced vacuum chamber, and density is 1 * 10
9-5 * 10
9/ cm
3 Opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A makes the sample table rotation, speed 0.5-10 rev/min, applying 10Kv negative direct current high voltage deposition on the vacuum chamber sample bench 6 after 5 minutes, turn down voltage to 0.25KV, the stream of carbon ion bombardment is by force 10-100mA, behind the deposition certain hour, form diamond-film-like on workpiece 7 surfaces.
Embodiment 2 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, and airtight vacuum chamber 1 is evacuated to air pressure less than 5 * 10
-4Pa, graphite 2 is installed in the negative electrode in metallic cathode arc plasma source 3, the extraction catheter in metallic cathode arc plasma source has magnetic deflection coil 4 outward, in junction sweep coil 5 is arranged with main vacuum chamber, open the triggering device power supply in metallic cathode arc plasma source 3, regulate trigger voltage to 12KV, electric current 500mA, striking voltage 300V, the voltage 400V of electric current 30A and magnetic deflection coil, electric current 15A.Carbon plasma is introduced vacuum chamber, and density is 1 * 10
9-5 * 10
9/ cm
3 Opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A makes the sample table rotation, speed 0.5-10 rev/min, applying 8Kv negative direct current high voltage deposition on the vacuum chamber sample bench 6 after 5 minutes, turn down voltage to 0.35KV, the stream of carbon ion bombardment is by force 10-100mA, behind the deposition certain hour, form diamond-film-like on workpiece 7 surfaces.
Embodiment 3 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, take step identical and processing method and parameter that carbon plasma is introduced vacuum chamber with embodiment 1 or embodiment 2, opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A, on vacuum chamber sample bench 6, apply 40KV pulse negative high voltage, pulse width is 30 μ s, high voltage pulse repetition rate 500Hz, deposit after 5 minutes, turn down the pulse negative voltage subsequently, voltage magnitude is 0.2KV, the stream of carbon ion bombardment is by force 10-100mA, forms diamond-film-like on workpiece 7 surfaces.
Embodiment 4 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, take step identical and processing method and parameter that carbon plasma is introduced vacuum chamber with embodiment 1 or embodiment 2, opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A, on vacuum chamber sample bench 6, apply 50KV pulse negative high voltage, pulse width is 50 μ s, high voltage pulse repetition rate 1000Hz, deposit after 5 minutes, turn down the pulse negative voltage subsequently, voltage magnitude is 0.4KV, the stream of carbon ion bombardment is by force 10-100mA, forms diamond-film-like on workpiece 7 surfaces.
Embodiment 6 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, and airtight vacuum chamber 1 is evacuated to air pressure less than 5 * 10
-4Pa charges into vacuum chamber with high pure nitrogen, and pressure is 5 * 10
-1Pa, open filament plasma source 8, filament voltage 70V, electric current 20A makes to form the nitrogen plasma field in the vacuum chamber, and density is 1 * 10
9-4 * 10
9/ cm
3, open the triggering device power supply of metallic cathode arc plasma source 3 (graphite 2 being installed) at its negative electrode, take step identical and processing method and parameter that carbon plasma is introduced vacuum chamber with embodiment 1 or embodiment 2, density is 1 * 10
9-3 * 10
9/ cm
3 Opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A makes the sample table rotation, speed 0.5-10 rev/min, applying 8KV negative direct current high voltage deposition on the vacuum chamber sample bench 6 after 5 minutes, turn down voltage to 0.15KV, behind the deposition certain hour, form the carboritride film on workpiece 7 surfaces.
Embodiment 7 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, and airtight vacuum chamber 1 is evacuated to air pressure less than 5 * 10
-4Pa charges into vacuum chamber with high pure nitrogen, and pressure is 5 * 10
-1Pa opens radio frequency plasma body source 9, power 500W, and frequency 13.56MHz makes to form the nitrogen plasma field in the vacuum chamber, and density is 1 * 10
9-4 * 10
9/ cm
3, take step identical and processing method and parameter that carbon plasma is introduced vacuum chamber with embodiment 1 or embodiment 2, density is 1 * 10
9-3 * 10
9/ cm
3 Opening scanning solenoid 5 power switches simultaneously scans, voltage 1000V, electric current 20A makes the sample table rotation, speed 0.5-10 rev/min, applying 8KV negative direct current high voltage deposition on the vacuum chamber sample bench 6 after 5 minutes, turn down voltage to 0.5KV, behind the deposition certain hour, form the carboritride film on workpiece 7 surfaces.
Embodiment 9 puts into workpiece 7 on the sample bench 6 of vacuum chamber 1, and airtight vacuum chamber 1 is evacuated to air pressure less than 5 * 10
-4Pa, high pure nitrogen is charged into vacuum chamber, take step identical and processing method and parameter that ammonia plasma treatment, carbon plasma are introduced vacuum chamber with embodiment 5,6,7,8, apply 30KV pulse negative high voltage on vacuum chamber sample bench 6, pulse width is 30 μ s, high voltage pulse repetition rate 500Hz, deposit after 5 minutes, turn down the pulse negative voltage subsequently, voltage magnitude is 0.2KV, forms the carboritride film at workpiece surface.
Claims (7)
1. synthesis of carbon-base film, utilize the plasma immersion ion injection device, carbon plasma is drawn by the metal arc source, pass through the deflecting action of the outer deflection solenoid of installing of bend pipe and filter neutral atom and particle, and through the scanning of the scanning solenoid of bend pipe and vacuum chamber junction and enter vacuum chamber, it is characterized in that as material carbon plasma being introduced vacuum chamber with graphite, the parameter that produces and draw carbon plasma is: trigger voltage 2-12KV, electric current 200-600mA, trigger frequency 10-200Hz, pulse width 50-500 μ s, striking voltage 50-500V, electric current 10-100A, the voltage 100-1000V of magnetic deflection coil, electric current 5-50A, sweep voltage are 100-2000V, sweep current is 5-30A, and carbon plasma density is 5 * 10
8-1 * 10
10/ cm
3On sample table, apply a direct current negative voltage earlier and make the sample table rotation, voltage magnitude is 8-10kv, deposit 5-10 minute, turn down negative DC voltage subsequently, voltage magnitude is 0.1-0.5kv, the stream of carbon ion bombardment is by force 10-100mA, the sample table speed of rotation is 0.5-10 rev/min, and depositing of thin film speed is 1-20 dust/second, obtains the superhard diamond like carbon film of uniform pure carbon at the workpiece surface of complexity.
2. synthesis of carbon-base film according to claim 1, it is characterized in that on sample table, applying earlier a pulse negative voltage, voltage magnitude is 30-60kv, and pulse width is 10-60 μ s, and pulse-repetition frequency is 50-1000Hz, deposit 5-10 minute, turn down the pulse negative voltage subsequently, voltage magnitude is 0.1-0.5kv, and the stream of carbon ion bombardment is by force 10-100mA, depositing of thin film speed is 1-20 dust/second, obtains the superhard diamond like carbon film of uniform pure carbon on the complex part surface.
3. synthesis of carbon-base film, with graphite as cathode material, pack into the negative electrode of four uniform metallic cathode Vacuum Arc plasma sources of plasma immersion ion injection device, carbon plasma is drawn by metallic cathode arc source, filter neutral atom and particle through the deflecting action of the outer solenoid of installing of bend pipe and enter vacuum chamber through the scanning of the solenoid of bend pipe and vacuum chamber junction, adopt radio frequency plasma body source, THE FILAMENT DISCHARGE AND plasma source or microwave plasma source, it is characterized in that charging in the vacuum chamber nitrogen, pressure is 10
-3-10
-1Pa produces nitrogen plasma, and making nitrogen plasma density is 5 * 10
8-5 * 10
10/ cm
3, carbon plasma density is 5 * 10
8-1 * 10
10/ cm
3On sample table, apply a direct current negative voltage earlier and make the sample table rotation, voltage magnitude is 8-10kv, deposit 5-10 minute, turn down negative DC voltage subsequently, voltage magnitude is 0.1-0.5kv, and the sample table velocity of rotation is 0.5-10 rev/min, depositing of thin film speed is 1-20 dust/second, forms the carboritride film at sample surfaces.
4. synthesis of carbon-base film according to claim 3 is characterized in that producing nitrogen plasma with THE FILAMENT DISCHARGE AND, and voltage is 50-200v, and electric current is 10-50A.
5. synthesis of carbon-base film according to claim 3 is characterized in that producing nitrogen plasma with the radio frequency discharge of 13.56MHz, and discharge power is 0.3-3KW,
6. synthesis of carbon-base film according to claim 3 is characterized in that producing nitrogen plasma with the microwave discharge of 2.45GHz, and discharge power is 0.5-3kW,
7. synthesis of carbon-base film according to claim 3, it is characterized in that on sample table, applying earlier a pulse negative voltage, voltage magnitude is 30-60kv, pulse width is 10-60 μ s, and pulse-repetition frequency is 50-1000Hz, deposits 5-10 minute, turn down the pulse negative voltage subsequently, voltage magnitude is 0.1-0.5kv, and depositing of thin film speed is 1-20 dust/second, forms the carboritride film at sample surfaces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB98111833XA CN1141415C (en) | 1998-01-24 | 1998-01-24 | Synthesis of carbon-base film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB98111833XA CN1141415C (en) | 1998-01-24 | 1998-01-24 | Synthesis of carbon-base film |
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| Publication Number | Publication Date |
|---|---|
| CN1224772A true CN1224772A (en) | 1999-08-04 |
| CN1141415C CN1141415C (en) | 2004-03-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB98111833XA Expired - Lifetime CN1141415C (en) | 1998-01-24 | 1998-01-24 | Synthesis of carbon-base film |
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| Country | Link |
|---|---|
| CN (1) | CN1141415C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410418C (en) * | 2006-05-19 | 2008-08-13 | 哈尔滨工业大学 | Bearing outer ring ball track ion injection and deposition combined treatment method |
| CN102291922A (en) * | 2011-07-22 | 2011-12-21 | 中国科学院空间科学与应用研究中心 | Ion generating device |
| CN104945652A (en) * | 2015-07-23 | 2015-09-30 | 中国科学院理化技术研究所 | Nylon with highly hard and abrasion resistant surface and preparation method thereof |
| CN105895071A (en) * | 2016-05-27 | 2016-08-24 | 西南交通大学 | Defect-state structure acoustic metamaterial plate |
| CN111041430A (en) * | 2020-01-10 | 2020-04-21 | 安徽纯源镀膜科技有限公司 | Production process of high-temperature-resistant diamond-like carbon film layer |
| CN112376031A (en) * | 2020-11-27 | 2021-02-19 | 中国科学院兰州化学物理研究所 | Method for preparing low-friction high-wear-resistance silicone rubber surface by injecting low-temperature electron beam excited plasma into carbon nanoclusters |
| CN113293351A (en) * | 2021-06-01 | 2021-08-24 | 南京邮电大学 | Method for plating carbon on surface of copper nanowire |
| CN113549902A (en) * | 2021-07-13 | 2021-10-26 | 南京邮电大学 | Preparation device and preparation method of C/TiC/TiN/TiAlN composite coating |
-
1998
- 1998-01-24 CN CNB98111833XA patent/CN1141415C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410418C (en) * | 2006-05-19 | 2008-08-13 | 哈尔滨工业大学 | Bearing outer ring ball track ion injection and deposition combined treatment method |
| CN102291922A (en) * | 2011-07-22 | 2011-12-21 | 中国科学院空间科学与应用研究中心 | Ion generating device |
| CN102291922B (en) * | 2011-07-22 | 2013-03-20 | 中国科学院空间科学与应用研究中心 | Ion generating device |
| CN104945652A (en) * | 2015-07-23 | 2015-09-30 | 中国科学院理化技术研究所 | Nylon with highly hard and abrasion resistant surface and preparation method thereof |
| CN104945652B (en) * | 2015-07-23 | 2018-06-26 | 中国科学院理化技术研究所 | High hard wear resistant nylon in a kind of surface and preparation method thereof |
| CN105895071A (en) * | 2016-05-27 | 2016-08-24 | 西南交通大学 | Defect-state structure acoustic metamaterial plate |
| CN111041430A (en) * | 2020-01-10 | 2020-04-21 | 安徽纯源镀膜科技有限公司 | Production process of high-temperature-resistant diamond-like carbon film layer |
| CN112376031A (en) * | 2020-11-27 | 2021-02-19 | 中国科学院兰州化学物理研究所 | Method for preparing low-friction high-wear-resistance silicone rubber surface by injecting low-temperature electron beam excited plasma into carbon nanoclusters |
| CN113293351A (en) * | 2021-06-01 | 2021-08-24 | 南京邮电大学 | Method for plating carbon on surface of copper nanowire |
| CN113549902A (en) * | 2021-07-13 | 2021-10-26 | 南京邮电大学 | Preparation device and preparation method of C/TiC/TiN/TiAlN composite coating |
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| Publication number | Publication date |
|---|---|
| CN1141415C (en) | 2004-03-10 |
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