CN103160779B - Ultralow-friction silicon-aluminum double-element mixed amorphous carbon film preparing method - Google Patents
Ultralow-friction silicon-aluminum double-element mixed amorphous carbon film preparing method Download PDFInfo
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- CN103160779B CN103160779B CN201110425150.3A CN201110425150A CN103160779B CN 103160779 B CN103160779 B CN 103160779B CN 201110425150 A CN201110425150 A CN 201110425150A CN 103160779 B CN103160779 B CN 103160779B
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Abstract
The invention discloses a silicon-aluminum double-element mixed amorphous carbon film preparing method with a radio frequency magnetron sputtering physical vapor deposition technology. An ultralow-friction silicon-aluminum double-element mixed amorphous carbon film has nano hardness of 9-15 Gpa and good tribology performance, the minimum friction coefficient can reach 0.0083, and the number of reciprocating times continuously in the ultralow friction coefficient can be 18000. The film is even and compact and is firmly combined with base materials, abrasion resistance is good, the film can be widely used in a magnetic memory optical disk, a micro electronic mechanical system (MEMS) and automobile parts and other fields.
Description
Technical field
The present invention relates to a kind of method utilizing rf magnetron sputtering physical gas phase deposition technology to prepare the silicon-aluminium binary doping amorphous carbon film with excellent tribology performance.
Background technology
Amorphous carbon film material, owing to having the excellent specific properties such as higher hardness, extremely low frictional coefficient, excellent resistance to abrasion, fabulous unreactiveness and good thermostability, is therefore with a wide range of applications in fields such as machinery, tribology, protection against corrosion, aerospace.
The main method of the amorphous carbon film material of current preparation doping has physical vapor deposition, electrochemical deposition, chemical Vapor deposition process etc.In these methods, what physical vapor deposition used in the industry is particularly extensive.Usually, in d.c. sputtering physics vapour deposition system, if the electroconductibility of target is poor, then in ion bombardment process, positive charge can accumulate at target material surface, runs up to and to a certain degree then arc-over can occur, and affects the deposition of target as sputter and film.If but DC sputtering power is replaced with radio frequency or intermediate frequency power supply, this electric discharge phenomena can be avoided.On the other hand, there is the thin-film material of ultralow friction coefficient at microelectromechanical systems (MEMS), bearing aspect has significant application prospect, but the realization of ultralow friction coefficient still has very large challenge, and can continue for a long time to occur that the thin-film material of ultralow friction coefficient is of inadequate achievement especially.
Summary of the invention
Main purpose of the present invention prepares a kind of amorphous carbon film in atmospheric environment with the silicon-aluminium binary doping of ultralow friction coefficient by rf magnetron sputtering.
The amorphous carbon-film of the sial doping that the present invention adopts rf magnetron sputtering physical gas phase deposition technology to prepare, this kind of film has ultralow friction coefficient and excellent wear resistance in atmospheric environment, performance excess of export lubricity, and this film even compact, smooth surface, elasticity is good, and tack is strong, and environmental resistance is good.
Technical scheme of the present invention is, described preparation method at room temperature implements, and base material is without the need to any extra heat-processed.
A preparation method for ultra-low friction silicon-aluminium binary doping amorphous carbon film, is characterized in that the method concrete steps are:
The monocrystalline silicon piece of A ultrasonic cleaning, is then placed in the reaction chamber of magnetron sputtering deposition system, vacuumizes;
B works as vacuum tightness and reaches 5 × 10
-4during Pa, logical argon gas, in sediment chamber, is 50%-70% in dutycycle, medium-frequency pulse frequency 40KHz) carry out sputter clean silicon single crystal agreement that contracts a film or TV play to an actor or actress 10-20min with argon (Ar) plasma body under the condition of direct current (DC) bias-700 ~-1000V;
C transition layer is obtained by the twin titanium target of pure Ar plasma sputtering, preparation condition is medium-frequency pulse and frequency 40KHz electric current is 1.0-2.0A, argon flow amount is 30-60sccm, when operating pressure is 3.0-5.0Pa, substrate bias is-200V, target and monocrystalline silicon piece distance 9-10cm, depositing time is 10min;
D by methane gas and argon gas to pass in reaction chamber after the ratio mixing of 1: 7, operating pressure opens radio-frequency power supply under the condition of 0.5-1.2Pa, power is 400-700W, under the effect of self-bias, produce the plasma body containing C and Ar, above-mentioned plasma body sputters the mixing target be made up of aluminium, silicon jointly, and area ratio is A
aluminium/ A
silicon=1/8;
It is 100-200V that E opens medium-frequency pulse frequency 40KHz direct current (DC) bias, makes the hybrid plasma of above-mentioned generation accelerate to arrive monocrystalline silicon piece, and is deposited on monocrystalline silicon piece.
Magnetron sputtering deposition system of the present invention is produced by Shenyang scientific instrument company limited of the Chinese Academy of Sciences, and the trade mark is JGP-450.
The present invention has the following advantages:
(1) amorphous carbon film frictional coefficient of (relative humidity 35-50%) under atmospheric environment that prepared by this kind of method can be low to moderate 0.0083, achieve ultra-low friction, and the time length is longer;
(2) the amorphous carbon film internal stress little (stress < 0.1GPa) prepared of this kind of method, tack is good;
(3) the amorphous carbon film growth velocity prepared of this kind of method is very fast, can the deposition of Large-Area-Uniform.
(4) amorphous carbon-film prepared by the method can play very effective reduction friction resistance, reduces fret wear, as solid lubricant, can be widely used in magnetic storage CD, cutter, and the field such as automobile component.
The reason that the present invention has above-mentioned advantage is: the plasma body ionization level that radio-frequency power supply produces is higher, and plasma atmosphere is even.Silicon, aluminium regulate the hybridization state of the carbon chemical bond in amorphous carbon-film jointly, jointly facilitate the greying behavior of amorphous carbon in tribology behavior, and then effectively reduce frictional coefficient, improve the abrasion resistance of film.
Ultra-low friction silicon-aluminium binary doping amorphous carbon film has the nano hardness of 9-15GPa, and excellent tribological property, minimum frictional coefficient reaches 0.0083, and the reciprocal time continuing to be in ultralow friction coefficient reaches 18000 times.Film even compact, firm with the combination of base material, wear resistance is good, can be widely used in magnetic storage CD, the fields such as microelectromechanical systems (MEMS) and automobile component.
Embodiment
In order to understand the present invention better, be described by example.
Embodiment 1:
Cleaning substrate: use dehydrated alcohol and acetone soln ultrasonic cleaning monocrystalline silicon piece (N100 type silicon chip) each 10min first respectively, dry up with nitrogen in the reaction chamber being placed on magnetron sputtering deposition system; Vacuumize: with efficient molecular pump, reaction chamber is vacuumized; Substrate surface treatment: when vacuum tightness reaches higher than 5 × 10
-4during Pa, logical argon gas, in sediment chamber, is carry out sputter clean silicon single crystal agreement that contracts a film or TV play to an actor or actress 10-20min with argon (Ar) plasma body under the condition of 50%-70% pulse direct current bias voltage-700 ~-1000V in dutycycle, to remove zone of oxidation and other impurity on surface; Deposition: by methane gas and argon gas to pass in reaction chamber after the ratio mixing of 1: 7, operating pressure opens radio-frequency power supply (power is 400-700W) under the condition of 0.5-1.2Pa, and (area ratio is A jointly to sputter the mixing target be made up of aluminium, silicon
aluminium/ A
silicon=1/8), meanwhile, monocrystalline silicon piece applies 100-200V negative bias, deposition obtains the amorphous carbon-film of silicon-aluminium binary doping.
Raman spectroscopic data demonstrates obvious G peak, and D peak is fainter.Utilize field emission scanning electron microscope to observe thin-membrane section to find, film is even, fine and close, and base material combines good.Nanometer micro-indentation test shows, the elastic recovery properties of film is excellent, and elastic restoration ratio is up to 95%.
The film of UMT-2MT frictiograph (U.S. CE TR company) to preparation is adopted to carry out friction testing.The way of contact of film sample and mating material (diameter is the Stainless Steel Ball of 3-10mm) is ball dish contact.Gliding cable structure is 0.1m/s, and load 2N, test environment is atmospheric environment, and relative humidity is 35-50%.
Claims (1)
1. a preparation method for ultra-low friction silicon-aluminium binary doping amorphous carbon film, is characterized in that the method concrete steps are:
The monocrystalline silicon piece of A ultrasonic cleaning, is then placed in the reaction chamber of magnetron sputtering deposition system, vacuumizes;
B works as vacuum tightness and reaches 5 × 10
-4during Pa, logical argon gas, in sediment chamber, is 50%-70% in dutycycle, carries out sputter clean monocrystalline silicon piece 10-20min under the condition of medium-frequency pulse frequency 40KHz direct current (DC) bias-700 ~-1000V with argon plasma;
C transition layer is obtained by the twin titanium target of pure Ar plasma sputtering, preparation condition is medium-frequency pulse and frequency 40KHz electric current is 1.0-2.0A, argon flow amount is 30-60sccm, when operating pressure is 3.0-5.0Pa, substrate bias is-200V, target and monocrystalline silicon piece distance 9-10cm, depositing time is 10min;
D by methane gas and argon gas to pass in reaction chamber after the ratio mixing of 1: 7, operating pressure opens radio-frequency power supply under the condition of 0.5-1.2Pa, power is 400-700W, under the effect of self-bias, produce the plasma body containing C and Ar, above-mentioned plasma body sputters the mixing target be made up of aluminium, silicon jointly, and area ratio is A
aluminium/ A
silicon=1/8;
It is 100-200V that E opens medium-frequency pulse frequency 40KHz direct current (DC) bias, makes the hybrid plasma of above-mentioned generation accelerate to arrive monocrystalline silicon piece, and is deposited on monocrystalline silicon piece.
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| CN107326336B (en) * | 2017-06-29 | 2020-04-07 | 四川理工学院 | Antibacterial wear-resistant amorphous carbon coating, preparation method thereof and antibacterial wear-resistant device |
| CN114369806B (en) * | 2022-01-14 | 2023-08-29 | 深圳大学 | Method for realizing near zero running-in ultralow friction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665904A (en) * | 2008-09-04 | 2010-03-10 | 中国科学院兰州化学物理研究所 | Aluminum-containing diamond-like carbon film and method for preparing same |
| CN101787518A (en) * | 2010-03-24 | 2010-07-28 | 中国地质大学（北京） | Multi-ion-beam sputter-deposition technology for doping with diamond-like carbon (DLC) coating |
| CN101787520A (en) * | 2010-03-24 | 2010-07-28 | 中国地质大学（北京） | Tungsten-titanium co-doped diamond coating material and preparation technique thereof |
| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665904A (en) * | 2008-09-04 | 2010-03-10 | 中国科学院兰州化学物理研究所 | Aluminum-containing diamond-like carbon film and method for preparing same |
| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
| CN101787518A (en) * | 2010-03-24 | 2010-07-28 | 中国地质大学（北京） | Multi-ion-beam sputter-deposition technology for doping with diamond-like carbon (DLC) coating |
| CN101787520A (en) * | 2010-03-24 | 2010-07-28 | 中国地质大学（北京） | Tungsten-titanium co-doped diamond coating material and preparation technique thereof |
Non-Patent Citations (1)
| Title |
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| 掺硅类金刚石薄膜的制备及其微观机械性能研究;王智;《河北化工》;20110830;第34卷(第8期);1-3页 * |
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