CN101619455A - Super lubricating Si-doped diamond film preparation method - Google Patents
Super lubricating Si-doped diamond film preparation method Download PDFInfo
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- CN101619455A CN101619455A CN200810150286A CN200810150286A CN101619455A CN 101619455 A CN101619455 A CN 101619455A CN 200810150286 A CN200810150286 A CN 200810150286A CN 200810150286 A CN200810150286 A CN 200810150286A CN 101619455 A CN101619455 A CN 101619455A
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Abstract
The invention discloses a super lubricating Si-doped diamond film preparation technology with very low friction coefficient and wear rate in water environment. The invention adopts methane and argon gas as feed gas and a compound deposition technology combined by radio frequency plasma enhanced chemical vapor deposition and mid-frequency sputtering silicon target to deposit the super lubricating Si-doped diamond film on the surface of stainless steel. The film shows good wear resistant and lubricating property in water environment and has very low friction coefficient (0.005-0.009) and wear rate (1.71-8.41*10<-8>mm<3>/Nm) in a big range of load and velocity. In addition, the technology has accessible raw materials, simple devices and processes, high efficiency, fast operation, and high yield and the technology can protect the environment, save the energy and reduce the cost. The technology is estimated to have important application prospect in mechanical friction, food industry and the like.
Description
Technical field
The present invention relates to a kind of preparation method who in water surrounding, has the super lubricating Si-doped diamond film of utmost point low-friction coefficient and wear rate.
Background technology
The fast development of modern high technology industry is more and more higher to the requirement that is equipped in precision, sensitivity, reliability and transmission efficiency aspect, thereby the super lubrication technology with extremely low friction and wear behavior has also been proposed more and more urgent demand.Diamond like carbon film is as a kind of novel composite lubricating film material, have the hardness height, excellent performance such as frictional coefficient is little, friction durability is long, erosion resistance is strong, chemical stability is good, in severe rugged environment, be used as protection film and shown great application prospect as the composite lubricating film material in association areas such as precision optical machinery, micro-system, space environments.But simultaneously it has internal stress height, environmental factor dependence defectives such as strong (especially frictional coefficient be subjected to humidity effect bigger), has been subjected to very big restriction in actual applications.So that realize better application, the researchist has taked several different methods in order to overcome these limitation, as depositing transition layer, constructing gradient layer, substrate surface patterning and carry out metal and nonmetallic doping etc.Studies show that, mix the internal stress that silicon not only greatly reduces diamond like carbon film, strengthened its adaptive capacity to environment, and kept its plurality of advantages.But bibliographical information, the lubricant effect in varying environment of the diamond like carbon film of the Different Silicon content of different methods, different parameters preparation is obviously different.And, the at present domestic patent of having only dopen Nano gold and nano silicon diamond like carbon film (200310121062 and 200410011633) and steel surface plating diamond film (200710043509.4), still do not have stainless steel surface deposition Si-doped diamond film and under water surrounding the super lubricated report of realization.Thereby, by selecting certain method, optimize parameters, prepare and realize that under certain condition super lubricated Si-doped diamond film has important significance for theories and practical value.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who in water surrounding, has the siliceous diamond like carbon film of super lubricity.
The present invention is a unstripped gas with methane and argon gas, and the composite deposition technology that adopts radio-frequency plasma enhancing chemical vapour deposition and intermediate frequency sputter silicon target to combine is at stainless steel surface deposition super lubricating Si-doped diamond film.The present invention adopts silicon target, and used pulsed bias power supply and intermediate frequency shielding power supply output frequency are 20～100kHz, and used radio-frequency power supply output frequency is 13.56MHz.
A kind of preparation method of super lubricating Si-doped diamond film is characterized in that this method may further comprise the steps:
A, activation clean surface: be evacuated to 1.0 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-3Pa～1.0 * 10
-2Pa feeds argon gas to 1.5～3.0Pa; Open pulsed bias power supply, voltage transfers to-400～-1200V, dutycycle is 30～80%, with argon plasma the stainless steel substrates surface is activated cleaning;
B, plating silicon transition layer: clean finish after, ar pressure is transferred to 0.25～1.0Pa, open shielding power supply, sputtering current is transferred to 3.0～20.0A, simultaneously pulsed bias transfer to-200～-1000V, dutycycle is 30～80%, deposits 5～20 minutes;
C, deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 0.5～4.0Pa; Radio-frequency power supply power is 400～1500W, and sputtering current is 2.0～15.0A, pulsed bias is-200～-1200V, dutycycle is 30%～80%, deposits 120-160 minute.
In the C step, the mass flux ratio of argon gas and methane is 3: 1～1: 4.
The main performance index such as the table 1 of the composite lubricating film of making by the present invention:
Table 1
Advantage of the present invention is that the film preparation process is simple, and each preparation parameter is easily controlled.Applied environment requires low (open environment need not to keep vacuum or gas shield), promptly uses tap water also can obtain low-friction coefficient (can reach 0.005 and curve steady) and low wear rate (10
-8Mm
3/ Nm magnitude); And do not produce any hazardous and noxious substances in the application process, meet green, environmental protection, energy-conservation theory fully.
This film is used in hydraulic efficiency system; water is cooked lubricant and is realized super lubricated; not only greatly reduce cost; avoided the pollution that lubricating grease itself is caused in the greasing; and improved the operational paradigm of system greatly; reduced energy consumption and emission of carbon-dioxide, helped protection physical environment.In addition, this film also can be used for foodstuff production and processing industry, and water is cooked lubricant, thereby lubricating oil is to the pollution of food, for the healthy of people given security in the minimizing production process.
Embodiment
Embodiment 1:
Activation clean surface: be evacuated to 1.0 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-3Pa feeds argon gas to 1.5Pa.Open pulsed bias power supply, voltage transfers to-400V, and dutycycle is 80%, with argon plasma the stainless steel substrates surface is activated cleaning.
Plating silicon transition layer: after cleaning finishes, ar pressure is transferred to 0.25Pa, open shielding power supply, sputtering current is transferred 3.0A, pulsed bias transfers to-200V simultaneously, and dutycycle is 80%, deposits 20 minutes.
The deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 0.5Pa, and the mass flux ratio of argon gas and methane is 3: 1.Radio-frequency power supply power is 400W, and sputtering current is 2.0A, and pulsed bias is-200V that dutycycle is 80%, deposits 150 minutes.
Embodiment 2:
Activation clean surface: be evacuated to 1.0 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-2Pa feeds argon gas to 3.0Pa.Open pulsed bias power supply, voltage transfers to-1200V, and dutycycle is 30%, with argon plasma the stainless steel substrates surface is activated cleaning.
Plating silicon transition layer: after cleaning finishes, ar pressure is transferred to 1.0Pa, open shielding power supply, sputtering current is transferred to 20.0A, pulsed bias transfers to-1000V simultaneously, and dutycycle is 30%, deposits 5 minutes.
The deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 4.0Pa, and the mass flux ratio of argon gas and methane is 1: 4.Radio-frequency power supply power is 1500W, and sputtering current is 15.0A, and pulsed bias is-1200V that dutycycle is 30%, deposits 150 minutes.
Embodiment 3:
Activation clean surface: be evacuated to 5.2 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-3Pa feeds argon gas to 2.0Pa.Open pulsed bias power supply, voltage transfers to-1200V, and dutycycle is 40%, with argon plasma the stainless steel substrates surface is activated cleaning.
Plating silicon transition layer: after cleaning finishes, ar pressure is transferred to 0.8Pa, open shielding power supply, sputtering current is transferred to 10.0A, pulsed bias transfers to-600V simultaneously, and dutycycle is 60%, deposits 20 minutes.
The deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 0.8Pa, and the mass flux ratio of argon gas and methane is 1: 2.Radio-frequency power supply power is 1200W, and sputtering current is 5.0A, and pulsed bias is-1200V that dutycycle is 40%, deposits 150 minutes.
Embodiment 4
Activation clean surface: be evacuated to 2.8 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-3Pa feeds argon gas to 2.5Pa.Open pulsed bias power supply, voltage transfers to-500V, and dutycycle is 70%, with argon plasma the stainless steel substrates surface is activated cleaning.
Plating silicon transition layer: after cleaning finishes, ar pressure is transferred to 0.4Pa, open shielding power supply, sputtering current is transferred to 12.0A, pulsed bias transfers to-800V simultaneously, and dutycycle is 40%, deposits 10 minutes.
The deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 0.5Pa, and the mass flux ratio of argon gas and methane is 3: 4.Radio-frequency power supply power is 1000W, and sputtering current is 6.0A, and pulsed bias is-800V that dutycycle is 50%, deposits 150 minutes.
Claims (2)
1, a kind of preparation method of super lubricating Si-doped diamond film is characterized in that this method may further comprise the steps:
A, activation clean surface: be evacuated to 1.0 * 10 after will the stainless steel substrates of ultrasonic mistake places the sample chamber in acetone and ethanol
-3Pa～1.0 * 10
-2Pa feeds argon gas to 1.5～3.0Pa; Open pulsed bias power supply, voltage transfers to-400～-1200V, dutycycle is 30～80%, with argon plasma the stainless steel substrates surface is activated cleaning;
B, plating silicon transition layer: clean finish after, ar pressure is transferred to 0.25～1.0Pa, open shielding power supply, sputtering current is transferred to 3.0～20.0A, simultaneously pulsed bias transfer to-200～-1000V, dutycycle is 30～80%, deposits 5～20 minutes;
C, deposition Si-doped diamond film: feed the mixed gas of argon gas and methane, making its total pressure is 0.5～4.0Pa; Radio-frequency power supply power is 400～1500W, and sputtering current is 2.0～15.0A, pulsed bias is-200～-1200V, dutycycle is 30%～80%, deposits 120-160 minute.
2, the method for claim 1 is characterized in that: in the C step, the mass flux ratio of argon gas and methane is 3: 1～1: 4.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831625A (en) * | 2010-05-28 | 2010-09-15 | 江苏南晶红外光学仪器有限公司 | Process for forming diamond-like carbon film on surface of infrared optical element |
| CN101880876A (en) * | 2010-07-06 | 2010-11-10 | 星弧涂层科技(苏州工业园区)有限公司 | Compressor sliding blade and surface coating layer treatment method thereof |
| CN102190421A (en) * | 2010-02-05 | 2011-09-21 | 富士胶片株式会社 | Mold for forming optical component, optical component thereof and manufacturing method of the optical component |
| CN102261347A (en) * | 2010-05-25 | 2011-11-30 | 沈阳鼓风机集团股份有限公司 | Application of diamond-like film on impeller |
| CN102352510A (en) * | 2011-10-19 | 2012-02-15 | 济南安塞自动化技术有限公司 | Method for preparing high-performance silicon-doped type diamond film layer on magnesium alloy at low temperature |
| CN102477540A (en) * | 2010-11-27 | 2012-05-30 | 中国科学院兰州化学物理研究所 | Method for preparing doped diamond-like carbon and grease composite lubricating film |
| CN102822546A (en) * | 2010-03-30 | 2012-12-12 | Ntn株式会社 | Anti-friction bearing |
| CN109023292A (en) * | 2018-09-26 | 2018-12-18 | 佳木斯大学 | A kind of Mg alloy surface DLC protective coating preparation method |
| CN109811322A (en) * | 2018-12-20 | 2019-05-28 | 兰州空间技术物理研究所 | A kind of super lubricating solid film with space environment adaptability |
| CN114196937A (en) * | 2021-12-16 | 2022-03-18 | 浙江大学杭州国际科创中心 | Hydrophilic amorphous carbon film and preparation method thereof |
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2008
- 2008-07-03 CN CN200810150286A patent/CN101619455A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102190421A (en) * | 2010-02-05 | 2011-09-21 | 富士胶片株式会社 | Mold for forming optical component, optical component thereof and manufacturing method of the optical component |
| CN102190421B (en) * | 2010-02-05 | 2014-08-27 | 富士胶片株式会社 | Mold for forming optical component, optical component thereof and manufacturing method of the optical component |
| CN102822546A (en) * | 2010-03-30 | 2012-12-12 | Ntn株式会社 | Anti-friction bearing |
| CN102822546B (en) * | 2010-03-30 | 2015-10-14 | Ntn株式会社 | Rolling bearing |
| US9051653B2 (en) | 2010-03-30 | 2015-06-09 | Ntn Corporation | Rolling bearing |
| CN102261347A (en) * | 2010-05-25 | 2011-11-30 | 沈阳鼓风机集团股份有限公司 | Application of diamond-like film on impeller |
| CN101831625A (en) * | 2010-05-28 | 2010-09-15 | 江苏南晶红外光学仪器有限公司 | Process for forming diamond-like carbon film on surface of infrared optical element |
| CN101880876B (en) * | 2010-07-06 | 2012-01-25 | 星弧涂层科技(苏州工业园区)有限公司 | Compressor sliding blade and surface coating layer treatment method thereof |
| CN101880876A (en) * | 2010-07-06 | 2010-11-10 | 星弧涂层科技(苏州工业园区)有限公司 | Compressor sliding blade and surface coating layer treatment method thereof |
| CN102477540A (en) * | 2010-11-27 | 2012-05-30 | 中国科学院兰州化学物理研究所 | Method for preparing doped diamond-like carbon and grease composite lubricating film |
| CN102352510A (en) * | 2011-10-19 | 2012-02-15 | 济南安塞自动化技术有限公司 | Method for preparing high-performance silicon-doped type diamond film layer on magnesium alloy at low temperature |
| CN109023292A (en) * | 2018-09-26 | 2018-12-18 | 佳木斯大学 | A kind of Mg alloy surface DLC protective coating preparation method |
| CN109811322A (en) * | 2018-12-20 | 2019-05-28 | 兰州空间技术物理研究所 | A kind of super lubricating solid film with space environment adaptability |
| CN114196937A (en) * | 2021-12-16 | 2022-03-18 | 浙江大学杭州国际科创中心 | Hydrophilic amorphous carbon film and preparation method thereof |
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Open date: 20100106 |