CN103225061A - Preparation method of Ti-Si-C nanocomposite film - Google Patents
Preparation method of Ti-Si-C nanocomposite film Download PDFInfo
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- CN103225061A CN103225061A CN2013101697954A CN201310169795A CN103225061A CN 103225061 A CN103225061 A CN 103225061A CN 2013101697954 A CN2013101697954 A CN 2013101697954A CN 201310169795 A CN201310169795 A CN 201310169795A CN 103225061 A CN103225061 A CN 103225061A
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Abstract
The invention aims to provide a preparation method of a Ti-Si-C nanocomposite film having low friction coefficients in atmospheric and water environments. The Ti-Si-C nanocomposite film is prepared by utilizing an unbalanced medium-frequency magnetron sputtering technology, using a TiSi bar and a graphite bar according to different proportions to assemble a target material, treating argon as a sputtering gas, adjusting the assembly proportions of the TiSi bar and the graphite bar in the target material, the Ti-Si atom ratio in the TiSi bar and the work argon pressure, and using a medium-frequency sputtering current and a pulse bias.
Description
Technical field
[0001] the present invention relates to the technology of preparing of carbon nano compound film.
Background technology
The carbon-based nano laminated film is meant that yardstick is that hard nanometer crystal grain (TiC, TiN, WC etc.) is embedded in the film that forms two-phase or multiphase composite structure in the amorphous carbon matrix (a-C, a-C:H, a-C:Si etc.).Germany scientist S. Veprek thinks that in nano composite structure a large amount of atoms are in crystal boundary and form strong interface combination, has avoided dislocation to produce and stops crack propagation and suppress the crystal boundary slippage, and this makes film have high hardness and toughness.Simultaneously, amorphous carbon is on good terms in the film, and formation interfacial migration layer makes film have low frictional coefficient and good wear resisting property in friction process.So the carbon-based nano laminated film has epochmaking using value at machinery part surfaces such as cutter, gear, bearing and pistons as the antifriction antiwear protective coating.But the carbon-base film frictional coefficient is subjected to envrionment conditions, and particularly humidity effect is very big, and this has limited it in the more application of wide field.
Summary of the invention
Of the present inventionPurpose provides a kind of preparation method who all has the Ti-Si-C nano compound film of low-friction coefficient in atmosphere and water surrounding.
The present invention is a kind of preparation method of Ti-Si-C nano compound film, the steps include:
(1) TiSi bar and graphite bar are assembled into composition target according to 1:1～1:13 ratio;
(2) will be respectively in ethanol and acetone the silicon single crystal of ultrasonic cleaning and stainless steel substrates place non-equilibrium medium frequency magnetron sputtering thin film deposition system, be evacuated to≤3.0 * 10
-3Pa feeds argon gas and makes pressure to 0.6～1.5 Pa;
(3)Open pulsed bias power supply, regulating bias voltage is-800～-1000 V, and dutycycle 50%～80% is cleaned activation with argon plasma to silicon chip and stainless steel surface;
(4) regulating argon flow amount, to make sediment chamber's pressure be 0.5～1.0 Pa, open intermediate frequency power supply sputter composite target material, with current setting to 1.0～2.5 A, sputtering voltage is 400～500 V, at last, the regulating impulse bias voltage is-100～-1000 V, and dutycycle is 10%～80%, the preparation nano compound film.
Thin film preparation process of the present invention is simple, good reproducibility.The preparation film have higher hardness, good toughness and a film-substrate cohesion, in air and water surrounding, all have the excellent friction performance, be applicable in the complex environment of air, water surrounding and variation thereof as machinery part surface antifriction and erosion resistant coating.
Description of drawings
Fig. 1 is TiSi and a graphite splicing construction synoptic diagram in the target of the present invention.
Embodiment
The present invention is a kind of preparation method of Ti-Si-C nano compound film, the steps include:
As shown in Figure 1, at first TiSi bar and graphite bar are assembled into composition target according to 1:1～1:13 ratio;
Then, with respectively in ethanol and acetone the silicon single crystal of ultrasonic cleaning and stainless steel substrates place non-equilibrium medium frequency magnetron sputtering thin film deposition system, be evacuated to≤3.0 * 10
-3Pa feeds argon gas and makes pressure to 0.6～1.5 Pa;
Secondly,Open pulsed bias power supply, regulating bias voltage is-800～-1000 V, and dutycycle 50%～80% is cleaned activation with argon plasma to silicon chip and stainless steel surface;
Once more, it is 0.5～1.0 Pa that the adjusting argon flow amount makes sediment chamber's pressure, open intermediate frequency power supply sputter composite target material, with current setting to 1.0～2.5 A, sputtering voltage is 400～500 V, and last, the regulating impulse bias voltage is-100～-1000 V, dutycycle is 10%～80%, the preparation nano compound film.
Embodiment 1:
At first, TiSi (Ti:Si=4:1) bar and graphite bar are assembled into composition target according to the 1:1 ratio.Secondly, cleaned stainless steel is placed non-equilibrium medium frequency magnetron sputtering thin film deposition system, be evacuated to 3.0 * 10
-3Pa feeds argon gas and makes pressure to 1.0 Pa; Open pulsed bias power supply, regulating bias voltage is-800 V, and dutycycle 80% is cleaned activation with argon plasma to stainless steel surface.Then, it is 0.6 Pa that the adjusting argon flow amount makes pressure, opens intermediate frequency shielding power supply electric current to 1.2 A, and sputtering voltage is 450 V.At last, the regulating impulse bias voltage is-100 V, and dutycycle is 80%, the preparation nano compound film.
Embodiment 2:
At first, TiSi (Ti:Si=9:1) bar and graphite bar are assembled into composition target according to the 5:9 ratio.Secondly, cleaned silicon single crystal is placed non-equilibrium medium frequency magnetron sputtering thin film deposition system, be evacuated to 2.0 * 10
-3Pa feeds argon gas and makes pressure to 0.8 Pa; Open pulsed bias power supply, regulating bias voltage is-1000 V, and dutycycle 60% is cleaned activation with argon plasma to monocrystalline silicon surface.Then, it is 0.7 Pa that the adjusting argon flow amount makes pressure, opens intermediate frequency shielding power supply electric current to 1.5 A, and sputtering voltage is 500 V.At last, the regulating impulse bias voltage is-1000 V, and dutycycle is 10%, the preparation nano compound film.
The nano compound film the key technical indexes of making by the present invention is:
The range estimation laminated film is a black, and smooth surface is smooth, field emission scanning electron microscope MEASUREMENTS OF THIN thickness 0.5～1.0 μ m, and film surface is smooth, and the r.m.s. roughness is 3.5-0.4 nm, TiC grain-size 4～20 nm in calculating according to XRD.Film Ti constituent content 20-30 at.%, Si constituent content 5-15 at.%, C constituent content 75-55 at.%.The frictional coefficient of UMT-2MT type trier testing film in empty G﹠W that adopts U.S. CE TR company to make is about 0.15-0.20.Nanometer is pressed into test and shows that film hardness is 10～24 GPa.Film and stainless steel substrate caking power are 60-80 N.
Claims (1)
1. the preparation method of a Ti-Si-C nano compound film the steps include:
(1) TiSi bar and graphite bar are assembled into composition target according to 1:1～1:13 ratio;
(2) will be respectively in ethanol and acetone the silicon single crystal of ultrasonic cleaning and stainless steel substrates place non-equilibrium medium frequency magnetron sputtering thin film deposition system, be evacuated to≤3.0 * 10
-3Pa feeds argon gas and makes pressure to 0.6～1.5 Pa;
(3)Open pulsed bias power supply, regulating bias voltage is-800～-1000 V, and dutycycle 50%～80% is cleaned activation with argon plasma to silicon chip and stainless steel surface;
(4) regulating argon flow amount, to make sediment chamber's pressure be 0.5～1.0 Pa, open intermediate frequency power supply sputter composite target material, with current setting to 1.0～2.5 A, sputtering voltage is 400～500 V, at last, the regulating impulse bias voltage is-100～-1000 V, and dutycycle is 10%～80%, the preparation nano compound film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101697954A CN103225061A (en) | 2013-05-10 | 2013-05-10 | Preparation method of Ti-Si-C nanocomposite film |
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| CN2013101697954A CN103225061A (en) | 2013-05-10 | 2013-05-10 | Preparation method of Ti-Si-C nanocomposite film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087898A (en) * | 2014-07-18 | 2014-10-08 | 上海理工大学 | TiSiCN nanometer composite coating with ultrahigh hardness and low friction coefficient and preparation method of TiSiCN nanometer composite coating |
| CN107488043A (en) * | 2016-06-12 | 2017-12-19 | 中国科学院宁波材料技术与工程研究所 | Multilayer complex films, its preparation method and the application as carborundum and its composite connecting material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102650043A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院兰州化学物理研究所 | Preparation method for nano composite lubricating film |
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2013
- 2013-05-10 CN CN2013101697954A patent/CN103225061A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102650043A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院兰州化学物理研究所 | Preparation method for nano composite lubricating film |
Non-Patent Citations (1)
| Title |
|---|
| M. RESTER ET AL.: "Annealing studies of nanocomposite Ti-Si-C thin films with respect to phase stability and tribological performance", 《 MATERIALS SCIENCE AND ENGINEERING》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087898A (en) * | 2014-07-18 | 2014-10-08 | 上海理工大学 | TiSiCN nanometer composite coating with ultrahigh hardness and low friction coefficient and preparation method of TiSiCN nanometer composite coating |
| CN104087898B (en) * | 2014-07-18 | 2017-05-03 | 上海理工大学 | TiSiCN nanometer composite coating with ultrahigh hardness and low friction coefficient and preparation method of TiSiCN nanometer composite coating |
| CN107488043A (en) * | 2016-06-12 | 2017-12-19 | 中国科学院宁波材料技术与工程研究所 | Multilayer complex films, its preparation method and the application as carborundum and its composite connecting material |
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Application publication date: 20130731 |