CN116043166A - Preparation method of high-temperature wear-resistant carbon-rich SiC film - Google Patents
Preparation method of high-temperature wear-resistant carbon-rich SiC film Download PDFInfo
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- CN116043166A CN116043166A CN202111260629.6A CN202111260629A CN116043166A CN 116043166 A CN116043166 A CN 116043166A CN 202111260629 A CN202111260629 A CN 202111260629A CN 116043166 A CN116043166 A CN 116043166A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 58
- 238000000151 deposition Methods 0.000 claims abstract description 30
- 230000007704 transition Effects 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- 238000005530 etching Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000013077 target material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
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- 238000001035 drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
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- 230000001050 lubricating effect Effects 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 6
- 238000010884 ion-beam technique Methods 0.000 abstract description 5
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 5
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation method of a high-temperature wear-resistant carbon-rich SiC film, which adopts an ion beam assisted magnetron sputtering technology and comprises the following steps: step one, conventionally cleaning a substrate; step two, further performing sputtering cleaning on the substrate, and etching the target; thirdly, depositing Cr on the surface of the substrate by utilizing direct-current magnetron sputtering to form a Cr film transition layer; and fourthly, depositing a carbon-rich SiC film on the Cr film transition layer by utilizing ion beam assisted magnetron sputtering. The preparation method adopted by the invention has simple process, low cost and large-area preparation; the SiC film prepared by the method is well combined with the substrate, the problems of insufficient toughness and the like of the SiC film are overcome, and in a high-temperature friction and wear experiment, the carbon-rich SiC film has very low friction coefficient and wear rate, has excellent high-temperature friction and wear characteristics, and provides more choices for high-temperature wear-resistant solid film lubricating materials.
Description
Technical Field
The invention belongs to the technical field of film materials, and particularly relates to a preparation method of a high-temperature wear-resistant carbon-rich SiC film.
Background
In the modern industrial field, tools and mechanical parts such as hot-working dies, cylinder liners/piston rings of internal combustion engines, cutting tools, bearings in steel-making furnace door rotary valves, magnetic heads/magnetic disks of thermally assisted magnetic recording hard disks and the like need to operate in a high-temperature environment, and the contact surfaces thereof have the problem of high-temperature friction and wear. Accordingly, the high-temperature frictional wear problem is increasingly focused by researchers, and solving the high-temperature frictional wear problem becomes a research hotspot in the current tribology field. The proper coating/film protection can improve the frictional wear characteristics of the tool and the mechanical parts without affecting the overall strength of the tool and the mechanical parts, and provides a choice for improving the frictional wear of mechanical equipment at high temperature and prolonging the service life of the mechanical equipment.
The SiC film has excellent characteristics of heat resistance, wear resistance, corrosion resistance, high mechanical strength, high-temperature oxidation resistance and the like, and has great potential and possibility as a high-temperature solid lubricating coating/film. However, the SiC film has the problems of hard brittleness, insufficient toughness and the like, and greatly limits the application of the SiC film in the field of high-temperature friction. The element doping can change the structural characteristics of the film so as to improve the performance of the film, and is one of the simplest and effective methods for improving the high-temperature tribological characteristics of the film. Research shows that Si doped into DLC film can increase coordination number of carbon atoms, form SiC with tetrahedral structure and increase sp in the film 3 The content of the polymer is used for inhibiting graphitization of the film, so that the thermal stability of the film is improved. In addition, if SiO is formed on the surface of the film x The layer also prevents further oxidation of the film, and the formation of Si-O-C also reduces the coefficient of friction of the film. Compared with an undoped DLC film (the failure temperature is lower than 200 ℃), the failure temperature of the Si-doped DLC (Si-DLC) film is increased to 400-500 ℃, and the high-temperature tribological property of the DLC film is greatly improved. The doping of the C element in the SiC film is very similar to the Si-DLC film in terms of element composition, chemical bond formation type and the like, so that the carbon-rich SiC film obtained by doping a proper amount of the C element in the SiC film can have the lubrication characteristic of the Si-DLC film while maintaining the excellent characteristic of the SiC film, and provides more choices for Gao Wenma friction materials. However, no related report has been made on the study of the high-temperature frictional wear properties of the carbon-rich SiC film.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to exert the excellent characteristics of heat resistance, abrasion resistance, corrosion resistance, high mechanical strength, high-temperature oxidation resistance and the like of the SiC film and overcome the problems of insufficient toughness and the like of the SiC film serving as a high-temperature solid lubricating coating/film; the invention provides a preparation method of a high-temperature wear-resistant carbon-rich SiC film, which can prepare a solid lubricating film material with lower friction coefficient and wear rate from room temperature to 500 ℃.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the high-temperature wear-resistant carbon-rich SiC film adopts an ion beam assisted magnetron sputtering method and specifically comprises the following steps of:
step one: cleaning a substrate
Sequentially immersing the substrate with the roughness less than 10nm into acetone, alcohol and deionized water, carrying out ultrasonic cleaning for 15-30 min, and drying.
Step two: pretreatment (etching target material, sputtering cleaning substrate)
Placing Cr target (purity is 99.95%), stoichiometric ratio SiC target (purity is 99.99%) and blow-dried substrate in corresponding position in vacuum chamber, vacuumizing the vacuum chamber to 10% -3 Pa～10 -5 Pa, then introducing argon and keeping the vacuum degree of the vacuum chamber at 0.6-1.2 Pa. The power of the Cr target is regulated to be DC 140-160W, the medium-frequency power supply current of the SiC target is regulated to be 0.3-0.6A, the duty ratio is regulated to be 50%, and the target is etched for 15-30 min. After the target material etching is finished, pulse bias voltage of-700V to-1000V is applied to the substrate, and the duty ratio is 50%; the ion source current is regulated to be 0.3-0.6A, the duty ratio is 70%, and the substrate is etched and cleaned for 15-30 min.
Step three: depositing a Cr transition layer
After pretreatment is finished, keeping the atmosphere and the air pressure of the vacuum chamber unchanged, and adjusting the pulse bias voltage of the substrate to be-500V to-700V and the duty ratio to be 50%; the power of the Cr target is DC 140-160W, the deposition time is 15-30 min, and the Cr film transition layer is formed.
Step four: deposition of carbon-rich SiC layers
After the deposition of the Cr film transition layer is finished, C2H2 and Ar are introduced into the vacuum chamber, the flow ratio is controlled to be 15-30%, and the vacuum degree of the vacuum chamber is kept to be 0.6-1.2 Pa; regulating the pulse bias voltage of the substrate to be-400V to-700V, and the duty ratio to be 30%; the current of the ion source is regulated to be 0.3 to 0.6A, and the duty ratio is regulated to be 70 percent; adjusting the intermediate frequency power supply current of the SiC target to be 0.3-0.6A, and the duty ratio to be 50%; the deposition time is 70-100 min, and the carbon-rich SiC film is obtained on the surface of the substrate.
Preferably, the substrate is free of external heating during the preparation process.
Preferably, the substrate is silicon wafer, H13 steel, 718 high-temperature alloy steel, GH4169 alloy steel or the like.
Preferably, the flow ratio of the C2H2 to the Ar is 15-30%, and the deposition air pressure is 0.6-1.2 Pa.
Preferably, the substrate pulse bias voltage is-500V to-700V.
The beneficial effects of the invention are as follows: the ion beam assisted magnetron sputtering technology is adopted to prepare the solid lubricating film material with lower friction coefficient and wear rate from room temperature to 500 ℃, and the adopted preparation technology has the advantages of simplicity, low cost, large-area deposition and the like. On one hand, a Cr transition layer is pre-deposited on the surface of the substrate, and the Cr transition layer can overcome the defects of high internal stress, poor adhesive force and the like of the SiC film, so that the bonding strength between the carbon-rich SiC film and the substrate is effectively improved, the stability of the film is improved, and the possibility is provided for practical application of the film; on the other hand, the C element is doped in the SiC film, so that the tribological property of the SiC film is effectively improved, and the excellent properties of high mechanical strength, high-temperature oxidation resistance and the like of the SiC film are maintained. In the high-temperature frictional wear experiment, the carbon-rich SiC film has very low friction coefficient and wear rate, and has excellent high-temperature frictional wear characteristics. Therefore, the invention develops a novel high-temperature wear-resistant solid film lubricating material.
Drawings
Fig. 1 is a surface SEM image of the carbon-rich SiC thin film prepared in example 1 of the present invention.
Fig. 2 is a cross-sectional SEM image of the carbon-rich SiC thin film prepared in example 1 of the present invention.
FIG. 3 is an XPS spectrum of a carbon-rich SiC film prepared in example 2 of the present invention: FIGS. 3 a-b are XPS full spectrum, C1s spectrum and Si2p, respectively.
FIG. 4 shows the friction coefficient of the carbon-rich SiC film prepared in example 3 of the present invention at different temperatures (25-500 ℃).
Detailed Description
The invention is described in further detail below with reference to the examples of the drawings, but the scope of the invention is not limited thereto:
example 1
The preparation of the high-temperature wear-resistant carbon-rich SiC film comprises the following steps:
1) Cleaning a substrate: sequentially immersing the substrate with the roughness less than 10nm into acetone, alcohol and deionized water, respectively ultrasonically cleaning for 15min to remove surface pollutants, and drying with nitrogen for later use.
2) Pretreatment (etching target, sputter cleaning substrate): placing Cr target (purity is 99.95%), stoichiometric ratio SiC target (purity is 99.99%) and blow-dried substrate in corresponding position in vacuum chamber, vacuumizing the vacuum chamber to 10% -5 Pa, argon gas was then introduced and the vacuum degree of the vacuum chamber was maintained at 0.8Pa. And adjusting the power of the Cr target to be DC140W, the medium-frequency power supply current of the SiC target to be 0.3A, and the duty ratio to be 50%, and etching the target for 15min. After the target material etching is finished, pulse bias voltage of 700V is applied to the substrate, and the duty ratio is 50%; and (3) regulating the current of the ion source to 0.6A, and etching and cleaning the substrate for 30min, wherein the duty ratio is 50%.
3) Depositing a Cr transition layer: after pretreatment is finished, keeping the atmosphere and the air pressure of the vacuum chamber unchanged, and adjusting the pulse bias voltage of the substrate to-500V and the duty ratio to 50%; the power of the Cr target is DC160W, the deposition time is 30min, and a Cr film transition layer is formed.
4) Depositing a carbon-rich SiC layer: after the deposition of the Cr film transition layer is finished, C2H2 and Ar are introduced into the vacuum chamber, the flow ratio is controlled to be 15%, and the vacuum degree of the vacuum chamber is kept to be 1.1Pa; adjusting the substrate pulse bias to-500V with a duty cycle of 30%; adjusting the ion source current to 0.4A and the duty ratio to 70%; adjusting the intermediate frequency power supply current of the SiC target to be 0.4A, and the duty ratio to be 50%; the deposition time is 70min, and the carbon-rich SiC film is obtained on the surface of the substrate.
The Cr transition layer thickness of the obtained high-temperature wear-resistant carbon-rich SiC film is 0.25mm; the thickness of the carbon-rich SiC layer is 0.85mm, and the layer contains C, si, O and trace Ar, wherein the C content is 86.6%, the Si content is 2.8%, the O content is 9.8% and the Ar content is 0.8%; the film hardness (H) was 19GPa, young's modulus (E) was 185GPa, and H/E was 0.10.
Example 2
The preparation of the high-temperature wear-resistant carbon-rich SiC film comprises the following steps:
1) Cleaning a substrate: sequentially immersing the substrate with the roughness less than 10nm into acetone, alcohol and deionized water, respectively ultrasonically cleaning for 25min to remove surface pollutants, and drying with nitrogen for later use.
2) Pretreatment (etching target, sputter cleaning substrate): placing the Cr target (purity is 99.95%), the stoichiometric ratio SiC target (purity is 99.99%) and the dried substrate at corresponding positions in a vacuum chamber, vacuumizing the vacuum chamber to 10 < -4 > Pa, introducing argon and keeping the vacuum degree of the vacuum chamber to be 0.9Pa. And (3) regulating the power of the Cr target to be DC150W, the current of the SiC target to be 0.5A, the duty ratio to be 50%, and etching the target for 25min. After the target material etching is finished, pulse bias voltage of-800V is applied to the substrate, and the duty ratio is 50%; and (3) regulating the current of the ion source to 0.5A, and etching and cleaning the substrate for 20min, wherein the duty ratio is 70%.
3) Depositing a Cr transition layer: after pretreatment is finished, keeping the atmosphere and the air pressure of the vacuum chamber unchanged, and adjusting the pulse bias voltage of the substrate to 600V with the duty ratio of 50 percent; the power of the Cr target is DC150W, the deposition time is 20min, and the Cr film transition layer is formed.
4) Depositing a carbon-rich SiC layer: after the deposition of the Cr film transition layer is finished, C is introduced into the vacuum chamber 2 H 2 Ar, controlling the flow ratio to be 20%, and keeping the vacuum degree of the vacuum chamber to be 0.9Pa; the substrate pulse bias voltage is regulated to 600V, and the duty ratio is 30%; adjusting the ion source current to 0.5A and the duty ratio to 70%; adjusting the intermediate frequency power supply current of the SiC target to 0.5A, and the duty ratio to 50%; the deposition time is 80min, and the carbon-rich SiC film is obtained on the surface of the substrate.
The Cr transition layer thickness of the obtained high-temperature wear-resistant carbon-rich SiC film is 0.3mm; the thickness of the carbon-rich SiC layer is 0.80mm, and the layer contains C, si, O and trace Ar, wherein the content of C is 87.9%, the content of Si is 1.7%, the content of O is 9.5%, and the content of Ar is 0.9%; the film hardness (H) was 20GPa, young's modulus (E) was 196GPa, and H/E was 0.10.
Example 3
The preparation of the high-temperature wear-resistant carbon-rich SiC film comprises the following steps:
1) Cleaning a substrate: sequentially immersing the substrate with the roughness less than 10nm into acetone, alcohol and deionized water, respectively ultrasonically cleaning for 30min to remove surface pollutants, and drying with nitrogen for later use.
2) Pretreatment (etching target, sputter cleaning substrate): placing Cr target (purity is 99.95%), stoichiometric ratio SiC target (purity is 99.99%) and blow-dried substrate in corresponding position in vacuum chamber, vacuumizing the vacuum chamber to 10% -3 Pa, argon gas was then introduced and the vacuum degree of the vacuum chamber was maintained at 1.1Pa. And (3) regulating the power of the Cr target to be DC160W, regulating the current of the SiC target to be 0.6A, regulating the duty ratio to be 50%, and etching the target for 30min. After the target material etching is finished, pulse bias voltage of-1000V is applied to the substrate, and the duty ratio is 50%; and (3) regulating the current of the ion source to 0.3A, and etching and cleaning the substrate for 15min, wherein the duty ratio is 70%.
3) Depositing a Cr transition layer: after pretreatment is finished, keeping the atmosphere and the air pressure of the vacuum chamber unchanged, and adjusting the pulse bias voltage of the substrate to 700V with the duty ratio of 50 percent; the power of the Cr target is DC140W, the deposition time is 15min, and the Cr film transition layer is formed.
4) Depositing a carbon-rich SiC layer: after the deposition of the Cr film transition layer is finished, C is introduced into the vacuum chamber 2 H 2 Ar, controlling the flow ratio to be 30%, and keeping the vacuum degree of the vacuum chamber to be 0.8Pa; the substrate pulse bias voltage is regulated to 700V, and the duty ratio is 30%; adjusting the ion source current to 0.6A and the duty ratio to 70%; adjusting the intermediate frequency power supply current of the SiC target to 0.6A, and the duty ratio to 50%; the deposition time is 90min, and the carbon-rich SiC film is obtained on the surface of the substrate.
The Cr transition layer thickness of the obtained high-temperature wear-resistant carbon-rich SiC film is 0.35mm; the thickness of the carbon-rich SiC layer is 0.75mm, and the layer contains C, si, O and trace Ar, wherein the content of C is 86.8%, the content of Si is 2.5%, the content of O is 10%, and the content of Ar is 0.7%; the hardness (H) of the film layer was 18GPa, young's modulus (E) was 180GPa, and H/E was 0.10.
The invention is prepared by utilizing ion beam auxiliary magnetron sputteringThe high-temperature wear-resistant carbon-rich SiC film has a flat and smooth surface, an average roughness of about 5.3nm (see figure 1), a compact film section and good adhesion with a substrate (see figure 2). The film contains Si-C, sp as main bond 2 C and sp 3 C, etc. (see fig. 3). Using a linear reciprocating ball and disc friction tester (UMT, bruker) at room temperature, 100deg.C, 200deg.C, 300deg.C, 400deg.C and 500deg.C, respectively, with Al 2 O 3 The ball was subjected to a frictional wear test for the abrasive material with an applied load of 5N, and frictional wear characteristics of example 1, example 2 and example 3 at different temperatures were evaluated, and the results are shown in table 1.
Table 1 the high temperature abrasion-resistant carbon-rich SiC films prepared by the present invention have coefficients of friction (cof) and wear rates (W) at different temperatures. The wear rate (W) is 10 -7 mm 3 /Nm。
Claims (5)
1. A preparation method of a high-temperature wear-resistant carbon-rich SiC film is characterized by comprising the following steps of: comprising the following steps:
step one: cleaning a substrate
Sequentially immersing the substrate with the roughness less than 10nm into acetone, alcohol and deionized water, carrying out ultrasonic cleaning for 15-30 min, and drying.
Step two: pretreatment (etching target material, sputtering cleaning substrate)
Placing Cr target (purity is 99.95%), stoichiometric ratio SiC target (purity is 99.99%) and blow-dried substrate in corresponding position in vacuum chamber, vacuumizing the vacuum chamber to 10% -3 Pa～10 -5 Pa, then introducing argon and keeping the vacuum degree of the vacuum chamber at 0.6-1.2 Pa. The power of the Cr target is regulated to be DC 140-160W, the current of the SiC target is regulated to be 0.3-0.6A, the duty ratio is regulated to be 50%, and the target is etched for 15-30 min. After the target material etching is finished, pulse bias voltage of-700V to-1000V is applied to the substrate, and the duty ratio is 50%; the ion source current is regulated to be 0.3-0.6A, the duty ratio is 70%, and the substrate is etched and cleaned for 15-30 min.
Step three: depositing a Cr transition layer
After pretreatment is finished, keeping the atmosphere and the air pressure of the vacuum chamber unchanged, and adjusting the pulse bias voltage of the substrate to be-500V to-700V and the duty ratio to be 50%; the power of the Cr target is DC 140-160W, the deposition time is 15-30 min, and the Cr film transition layer is formed.
Step four: deposition of carbon-rich SiC layers
After the deposition of the Cr film transition layer is finished, C is introduced into the vacuum chamber 2 H 2 Ar, controlling the flow ratio to be 15-30%, and keeping the vacuum degree of the vacuum chamber to be 0.6-1.2 Pa; regulating the pulse bias voltage of the substrate to be-400V to-700V, and the duty ratio to be 30%; adjusting the ion source current to 0.5A and the duty ratio to 70%; adjusting the intermediate frequency power supply current of the SiC target to 0.5A, and the duty ratio to 50%; the deposition time is 70-90 min, and the carbon-rich SiC film is obtained on the surface of the substrate.
2. The method for preparing a high-temperature wear-resistant carbon-rich SiC film according to claim 1, wherein the substrate is free from external heating during the preparation process.
3. The method for preparing the high-temperature wear-resistant carbon-rich SiC film according to claim 1, wherein the substrate is silicon wafer, H13 steel, 718 high-temperature alloy steel, GH4169 alloy steel or the like.
4. The method for preparing the high-temperature wear-resistant carbon-rich SiC film according to claim 1, wherein the C is as follows 2 H 2 And Ar flow ratio is 15% -30%, and deposition air pressure is 0.8-1.1 Pa.
5. The method for preparing a high-temperature wear-resistant carbon-rich SiC film according to claim 1, wherein the substrate pulse bias voltage is-500V to-600V.
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