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Preparation method of low-internal stress and high-hardness DLC/a-CNx nano multilayer film

A DLC film and nano-multi-layer technology, applied in the field of material friction and wear, can solve the problems of reduced hardness and wear resistance, complicated preparation process, unfavorable practical application, etc., and achieve high hardness and elastic modulus, good combination, and excellent friction The effect of academic performance

Inactive Publication Date: 2017-11-17
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, the residual stress of the DLC film prepared by the transition layer method is still close to 1GPa, and the preparation process is relatively complicated, so it is necessary to find a more suitable transition layer; and the DLC film prepared by the doping method, element doping The internal stress of the film is significantly reduced, but the internal stress is still relatively high, the hardness and wear resistance are often significantly reduced, and most of the element doping has harsh process conditions, complicated preparation process, and high cost, which is not conducive to practical application.

Method used

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  • Preparation method of low-internal stress and high-hardness DLC/a-CNx nano multilayer film

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Experimental program
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Effect test

Embodiment 1

[0035] (1) Substrate pretreatment: put the monocrystalline silicon wafer in an ultrasonic cleaning instrument, and wash it with 10% hydrofluoric acid solution-acetone-absolute ethanol in turn for 15 minutes to make the surface clean. After cleaning, use hot air Blow dry and install on the sample stage of the magnetron sputtering chamber.

[0036] (2) Experiment preparation: put the graphite target and the pretreated single crystal silicon wafer into the multi-target magnetron sputtering deposition chamber, adjust the base distance of the targets to 70 mm, and pump the air pressure in the deposition chamber to 1.5×10 -3 After Pa, the single crystal silicon wafer is heated to stabilize the temperature at 200°C.

[0037] (3)DLC / a-CN x Preparation of nano-multilayer film: Introduce working gas into the magnetron sputtering chamber, deposit DLC film layer in Ar gas, graphite target sputtering power is 65W; 2 Deposition of a-CN in mixed gas (flow ratio 4:1) x film layer, graphite...

Embodiment 2

[0039] (1) substrate pretreatment: with embodiment 1

[0040] (2) Experimental preparation: with embodiment 1

[0041] (3)DLC / a-CN x Preparation of nano-multilayer film: Introduce working gas into the magnetron sputtering chamber, deposit DLC film layer in Ar gas, graphite target sputtering power is 65W; 2 Deposition of a-CN in mixed gas (flow ratio 4:1) x film layer, graphite target sputtering power is 75W. Among them, the sputtering working pressure is 0.6Pa, and the negative bias voltage is 50V. Control the rotation of the sample stage and the residence time above the target, and alternately deposit 10nm DLC layers (residence time 314s) and 1nm a-CN x layer (residence time 19.6s). The bottom layer is DLC, and the top layer is a-CN x , cycled 59 times, and the thickness of the obtained nanometer multilayer film was about 650nm.

Embodiment 3

[0043] (1) substrate pretreatment: with embodiment 1

[0044] (2) Experimental preparation: with embodiment 1

[0045] (3)DLC / CN x Preparation of nano-multilayer film: Introduce working gas into the magnetron sputtering chamber, deposit DLC film layer in Ar gas, graphite target sputtering power is 65W; 2 Deposition of a-CN in mixed gas (flow ratio 4:1) x film layer, graphite target sputtering power is 75W. Among them, the sputtering working pressure is 0.6Pa, and the negative bias voltage is 50V. Control the rotation of the sample stage and the residence time above the target, and alternately deposit 10nm DLC layers (residence time 314s) and 1.5nm a-CN x layer (residence time 29.5s). The bottom layer is DLC, and the top layer is a-CN x , cycled 56 times, and the thickness of the obtained nanometer multilayer film was about 650nm.

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Abstract

The invention discloses a preparation method of a low-internal stress and high-hardness DLC / a-CNx nano multilayer film. The method comprises the steps that (1) a monocrystalline silicon wafer matrix is put into a hydrofluoric acid solution to be cleaned, the monocrystalline silicon wafer matrix is cleaned with acetone and absolute ethyl alcohol, the surface is clean, and roughness is not higher than Ra 0.1; (2) a graphite target and the pretreated monocrystalline silicon wafer matrix are put into a multi-target magnetron sputtering deposition chamber, the target-matrix distance is adjusted to be 60 mm to 80 mm, air pressure in the deposition chamber is adjusted to be (1.5 * 10<-3>) Pa or below, and the temperature of the matrix is adjusted to be 100 DEG C to 250 DEG C; and (3) periodic retention time of the matrix on the graphite target is controlled, DLC films and a-CNx films with certain thicknesses are alternately deposited on the surface of the matrix layer by layer in alternately switched deposition atmospheres, a nano multilayer structure of which the bottommost layer is the DLC film and the uppermost layer is the a-CNx film is obtained, and after cooling, the DLC / a-CNx nano multilayer film is obtained. According to the preparation method, good combination of the DLC films and the a-CNx films, reduction of film internal stress and a strong interface strengthening effect are achieved, and the nano multilayer film with excellent performance is obtained.

Description

technical field [0001] The invention relates to a preparation method of magnetron sputtering wear-resistant thin film material, especially a method based on diamond-like carbon (DLC) and amorphous carbon nitride (a-CN x ) composed of nanometer multilayer films, belonging to the field of material friction and wear. Background technique [0002] The performance of DLC film depends heavily on the preparation technology, and most of its hardness is distributed in the range of 12-50GPa. Due to its high hardness, low friction coefficient in the atmosphere and good wear resistance, it can be used in machinery, electronics, medical, aerospace and other fields. At present, the methods for preparing DLC ​​films mainly include pulsed laser deposition, chemical vapor deposition, and magnetron sputtering deposition. DLC films by pulsed laser deposition and chemical vapor deposition usually have a high degree of densification, sp 3 With high C content, it has high hardness; while the D...

Claims

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Application Information

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IPC IPC(8): C23C14/35C23C14/06
CPCC23C14/352C23C14/0073C23C14/0605C23C14/0658C23C14/345
Inventor 杨芳儿常新新郑晓华林玲玲龚润泽王贵葱
Owner ZHEJIANG UNIV OF TECH
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