A kind of preparation method of wear-resistant tungsten disulfide film

A technology of tungsten disulfide and thin film, which is applied in metal material coating process, vacuum evaporation plating, coating, etc., can solve the problems of limited improvement of wear resistance, large increase of friction coefficient, high process cost, etc., and achieve reduction The effect of protection level, large elastic modulus and simple process

Active Publication Date: 2019-11-29
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, improving magnetron sputtering WS in humid environment 2 The methods of film friction and wear properties include: (1) in WS 2 A certain amount of metals such as Ag (Lai Deming, Acta Tribology, 2006, 26 (6): 515-518), Ti (Banerjee T, Surface and Coatings Technology, 2014, 258: 849-860), Cr (Deepthi B, Surface & Coatings Technology, 2010, 205 (2): 565-574), etc., metal particles present nanocrystalline or amorphous state in the film to improve the compactness and wear resistance of the film, but this method has high process cost and friction (2) A certain amount of other sulfides or carbon-based materials are added to form nanocomposite films, such as WS 2 / MoS 2 Composite film (Watanabe S, Surface and Coatings Technology, 2004, 188:644-648), WS 2 / MoS 2 / C composite film, etc. (Zhou Lei, Chinese Journal of Nonferrous Metals, 2010,20(3):483-487), the resulting composite film structure is dense, but the wear rate is high (about 10 -13 m 3 N -1 m -1 magnitude)

Method used

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  • A kind of preparation method of wear-resistant tungsten disulfide film
  • A kind of preparation method of wear-resistant tungsten disulfide film
  • A kind of preparation method of wear-resistant tungsten disulfide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation before coating

[0030] Take a single crystal polished silicon wafer ( or crystal orientation) with a size of 20×20×0.45mm, degrease it by ultrasonic degreasing with absolute alcohol, soak in 10% (volume fraction) hydrofluoric acid solution, deionize After washing with water, dry with hot air and set aside. Take Φ60×3mm graphite target (99.99% carbon mass fraction) and WS 2 Each piece of target (WS 2 Mass fraction 99.9%), put into the multi-target magnetron sputtering chamber together with the substrate, and vacuumize the deposition chamber to 1.0×10 -3 Pa, adjust the distance between the target and the base to 70mm, adjust the pulse DC bias power supply, so that the output amplitude of the negative bias voltage is 50V, and the duty cycle is 50%.

[0031] (2) Carbon film deposition

[0032] Introduce high-purity argon gas (flow rate 50 sccm) and stabilize the air pressure at 0.2 Pa, start heating the substrate and keep the temperature constant at 30...

Embodiment 2

[0036] (1) Preparation before coating

[0037] Same as Example 1.

[0038] (2) Carbon film deposition

[0039] Introduce high-purity argon gas (flow rate 50 sccm) and stabilize the air pressure at 0.6 Pa, start heating the substrate and keep the temperature constant at 200 ° C, turn on the graphite target sputtering power supply for sputtering (power is 65 W), and the duration is 270 min. The thickness of the carbon film is about 370nm.

[0040] (3)WS 2 thin film deposition

[0041] Keep the substrate temperature at 200°C and the deposition pressure at 0.6Pa, and turn on the WS 2 Target sputtering power supply for sputtering (power is 60W), duration is 9min, the obtained WS 2 The film thickness is about 140nm.

Embodiment 3

[0043] (1) Preparation before coating

[0044] Same as Example 1.

[0045] (2) Carbon film deposition

[0046] Introduce high-purity argon gas (flow rate 50 sccm) and stabilize the air pressure at 0.8 Pa, start heating the substrate and keep the temperature constant at 100 ° C, turn on the graphite target sputtering power supply for sputtering (power is 80 W), the duration is 118 min, and the obtained The thickness of the carbon film is about 210nm.

[0047] (3)WS 2 thin film deposition

[0048] Increase the heating temperature of the substrate and keep it at 200°C, adjust the deposition pressure to 0.6Pa, and turn on the WS 2 Target sputtering power supply for sputtering (power is 60W), duration is 33min, the obtained WS 2 The film thickness is about 515nm.

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Abstract

A preparation method of wear-proof tungsten disulfide film comprises the following steps that (1) pretreatment is conducted on a monocrystalline silicon piece, the surface of the monocrystalline silicon piece is made clean, the roughness of the surface of the monocrystalline silicon piece is made not higher than Ra 0.1, a graphite target, a WS2 target and the pretreated monocrystalline silicon piece are fed in a multi-target magnetron sputtering deposition chamber, after the air pressure in the deposition chamber is made to be 1.0*10<-3> Pa, through pumping, the target-substrate distance is adjusted to be appropriate, and pulse direct-current negative bias voltage is applied to a base material; (2) high-purity argon is fed to be used as work gas, and amorphous-state carbon film with the deposition thickness being 20-400 nm is deposited on the surface of the monocrystalline silicon piece with the graphite target as a sputtering target material; (3) the temperature of the amorphous-state carbon film obtained in the step (2) is adjusted to 200 DEG C, WS2 film is deposited on the amorphous-state carbon film with the deposit thickness being 140-740 nm with the WS2 target as a sputtering target material, and then the tungsten disulfide film is obtained. The preparation method is simple in technology, good in economical efficiency, capable of greatly improving the mechanical performance of the tungsten disulfide film and the wear-proof performance of the tungsten disulfide film in vacuum or in a humid environment.

Description

technical field [0001] The invention relates to a method for preparing a magnetron sputtering solid lubricating film, in particular to a method for preparing a tungsten disulfide thin film, and belongs to the field of material friction and wear and solid lubrication. Background technique [0002] Transition metal sulfide films, such as tungsten disulfide (WS 2 ), exhibits excellent lubricating properties due to its layered crystal structure, and has been widely used in tribological engineering fields such as metal processing, aerospace, and vacuum equipment. However, because it is easy to absorb oxygen and water vapor in a humid atmosphere, the wear resistance is greatly reduced, and the service performance and application occasions are greatly limited. Therefore, how to improve WS 2 The friction and wear properties of thin films in humid environment have received great attention, especially the magnetron sputtering WS 2 Thin films are widely used in practical application...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/06C23C14/35
CPCC23C14/0605C23C14/0623C23C14/345C23C14/352
Inventor 郑晓华杨芳儿沈靖枫徐秉政李昂鲁叶
Owner ZHEJIANG UNIV OF TECH
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