CN112795882A - High-hardness wear-resistant fullerene-like carbon film and preparation method thereof - Google Patents
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
Abstract
The invention provides a high-hardness wear-resistant fullerene-like carbon film which sequentially comprises a fullerene-like carbon layer, a CrN/Cr soft-hard alternating transition layer and a metal substrate from top to bottom; the CrN/Cr soft-hard alternating transition layer is used as the intermediate transition layer, so that the stress between the fullerene-like carbon layer film and the metal substrate can be reduced, the adhesive force and the overall toughness of the fullerene-like carbon layer film are improved, and the overall toughness of the film can be improved by depositing the fullerene-like carbon film on the surface of the fullerene-like carbon layer film; therefore, the fullerene-like carbon film has the characteristics of high hardness, good toughness and excellent wear resistance, and is particularly suitable for being applied to wear-resistant parts; the invention also provides a preparation method of the high-hardness wear-resistant fullerene-like carbon film, which adopts a composite technology of magnetron sputtering and Plasma Enhanced Chemical Vapor Deposition (PECVD), so that the temperature in the whole film preparation and deposition process is obviously reduced and is lower than 150 ℃, and the annealing of metal materials caused by high temperature is avoided.
Description
Technical Field
The invention belongs to the technical field of surface engineering, and particularly relates to a high-hardness wear-resistant fullerene-like carbon film and a preparation method thereof.
Background
The fullerene-like carbon film has excellent characteristics similar to those of diamond, such as extremely high hardness and elastic modulus, high wear resistance, good corrosion resistance and chemical inertness, and has good application prospects in the fields of aerospace, cutters, molds and the like, but the fullerene-like film with high hardness and high stress is easy to cause peeling failure of the film in the using process.
The current common method has the problems that the preparation of the fullerene-like film by adopting magnetron sputtering needs higher temperature, and the energy and the density of the plasma of the direct current or radio frequency plasma enhanced chemical vapor deposition fullerene-like carbon-based film can not be independently controlled.
Disclosure of Invention
In order to solve the problems, the invention provides the high-hardness wear-resistant fullerene-like carbon film and the preparation method thereof, the high-hardness wear-resistant fullerene-like carbon film has the advantage of low deposition temperature, and the obtained film has the characteristics of high hardness and high toughness and good tribological performance.
A high-hardness wear-resistant fullerene-like carbon film sequentially comprises a fullerene-like carbon layer, a CrN/Cr soft-hard alternating transition layer and a metal substrate from top to bottom.
Further, the metal matrix is 9Cr18 stainless steel material or GCr15 stainless steel material.
Further, the CrN/Cr soft-hard alternating transition layer is obtained by magnetron sputtering deposition, and the fullerene-like carbon layer is obtained by PECVD technology deposition.
Furthermore, the thickness of the CrN/Cr soft-hard alternating transition layer is 0.3-0.5 μm, and the thickness of the fullerene-like carbon film is 1.2-1.5 μm.
A preparation method of a high-hardness wear-resistant fullerene-like carbon film comprises the following steps:
and 7, stopping coating until the temperature in the coating vacuum chamber is reduced to be below 80 ℃ to obtain the metal substrate coated with the fullerene-like carbon layer and the CrN/Cr soft-hard alternating transition layer.
Furthermore, the anode layer ion beam source voltage in the step 1 is 1000V-1200V, and meanwhile, a pulse bias voltage of-600V-1000V is applied on the metal substrate.
Further, the purity of the Cr target was 99.99%.
Further, the duty ratio of the direct current pulse power supply in the step 5 is 0.4-0.7, and the frequency is 20 kHz-40 kHz.
Has the advantages that:
1. the invention provides a high-hardness wear-resistant fullerene-like carbon film which sequentially comprises a fullerene-like carbon layer, a CrN/Cr soft-hard alternating transition layer and a metal substrate from top to bottom; the CrN/Cr soft-hard alternating transition layer is used as the intermediate transition layer, so that the stress between the fullerene-like carbon layer film and the metal substrate can be reduced, the adhesive force and the overall toughness of the fullerene-like carbon layer film are improved, and the overall toughness of the film can be improved by depositing the fullerene-like carbon film on the surface of the fullerene-like carbon layer film; therefore, the fullerene-like carbon film has the characteristics of high hardness, good toughness and excellent wear resistance, and is particularly suitable for being applied to wear-resistant parts.
2. The invention provides a preparation method of a high-hardness wear-resistant fullerene-like carbon film, which comprises the following steps: plasma cleaning the surface of a substrate, magnetron sputtering deposition of a CrN/Cr soft-hard alternating transition layer, and plasma enhanced chemical vapor deposition of a fullerene-like carbon film; therefore, the invention adopts the composite technology of magnetron sputtering and Plasma Enhanced Chemical Vapor Deposition (PECVD), so that the temperature in the whole film preparation and deposition process is obviously reduced and is lower than 150 ℃, thereby avoiding the annealing of metal materials caused by high temperature, and having high hardness, good adhesive force and excellent wear resistance.
Drawings
FIG. 1 is a schematic structural diagram of a high-hardness wear-resistant fullerene-like carbon film according to the present invention;
FIG. 2 is a top view of the apparatus structure for preparing a fullerene-like carbon film by combining magnetron sputtering and plasma enhanced chemical vapor deposition provided by the present invention;
1-radio frequency power supply, 2-upper polar plate, 3-magnetic control Cr target, 4-workpiece table, 5-lower polar plate and 6-direct current pulse power supply.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application.
Example one
As shown in FIG. 1, the high-hardness wear-resistant fullerene-like carbon film comprises a fullerene-like carbon layer, a CrN/Cr soft-hard alternating transition layer and a metal substrate in sequence from top to bottom. The CrN/Cr soft-hard alternating transition layer can enable the hardness and the stress of the film layer to be well matched with each other from the base material, the soft-hard alternating transition layer and the fullerene-like carbon layer.
The whole thickness of the film is 1.5-2.0 μm, wherein the thickness of the CrN/Cr soft-hard alternating transition layer is 0.3-0.5 μm, and the thickness of the fullerene-like carbon film is 1.2-1.5 μm. Meanwhile, the CrN/Cr soft-hard alternating transition layer is obtained by magnetron sputtering deposition, and the fullerene-like carbon layer is obtained by PECVD technology deposition.
Example two
Based on the above embodiments, the present embodiment provides a method for preparing a high-hardness wear-resistant fullerene-like carbon film, including the following steps:
the method comprises the following steps that a radio frequency power supply ionizes methane into a plurality of different plasmas, and the plasmas with positive charges are mutually reacted and then attracted by a lower polar plate connected with negative bias voltage, so that a fullerene-like carbon film is deposited on a CrN/Cr soft-hard alternating transition layer; the argon is used for colliding with ions after the methane ionization so as to improve the activity of the ions, meanwhile, the radio frequency power supply of the upper polar plate influences the density of the plasma, and the direct current pulse power supply of the lower polar plate influences the energy of the plasma;
and 7, stopping coating until the temperature in the coating vacuum chamber is reduced to be below 80 ℃ to obtain the metal substrate coated with the fullerene-like carbon layer and the CrN/Cr soft-hard alternating transition layer.
EXAMPLE III
Based on the above embodiments, this embodiment further illustrates a method for preparing a high-hardness wear-resistant fullerene-like carbon film, which specifically includes the following steps:
(1) the method comprises the steps of taking a 9Cr18 stainless steel material as a substrate, grinding and mechanically polishing the substrate material before experiment, sequentially placing the substrate material in acetone and alcohol solution for ultrasonic cleaning for 5min, drying the substrate material by a blower, placing the substrate material into a vacuum chamber, vacuumizing until the vacuum degree is lower than 3 multiplied by 10-3Pa。
(2) Introducing argon gas of 0.5Pa into the vacuum chamber, applying-600V pulse bias voltage on the substrate, etching and cleaning the substrate surface for 20min by using anode layer ion beam source to ionize argon ions, and setting the anode layer ion beam source voltage to be 1000V.
(3) Introducing nitrogen and argon into the coating chamber, wherein the flow of the nitrogen is 8SCCM, the flow of the argon is 30SCCM, the air pressure is kept at 0.5Pa, and the substrate is applied with a direct current bias of-50V. Preparing a CrN layer by adopting a reactive magnetron sputtering technology, wherein the current of a Cr target is 2.0A, the purity of the Cr target is 99.99 percent, and the thickness of the deposited CrN layer is 15 nm;
(4) introducing 45SCCM argon into the coating chamber, wherein the pressure of the argon is 0.5Pa, applying-50V direct current bias on the substrate, and preparing a Cr layer by adopting a magnetron sputtering technology, wherein the current of a Cr target 3 is 2.0A, and the thickness of the deposited Cr layer is 10 nm;
(5) sequentially repeating the step (3) and the step (4) for 12 periods to prepare a soft-hard alternating transition layer with the thickness of 300 nm;
(6) preparing fullerene-like carbon film, introducing methane (CH) into the film coating chamber4) And argon (Ar), the flow ratio of methane and argon being 1:1, the gas pressure being 10 Pa. The upper polar plate 2 is connected with a radio frequency power supply 1, and the radio frequency power is 0.8 kW. The lower polar plate 5 is connected with a direct current pulse power supply 6, the bias voltage is-600V, the duty ratio is 0.4, and the frequency is 20 kHz. Class IThe fullerene carbon film thickness was controlled at 1200 nm.
(7) Stopping coating until the temperature in the coating chamber is reduced to below 80 ℃, and taking out the metal substrate.
The structure of the film was characterized using a Jobin Yvon LabRam HR800 Raman spectrometer, indicating that five-membered and seven-membered rings were formed in the film, indicating that a fullerene-like microstructure was formed in the film.
The hardness and elastic recovery of the nanoindenter film from CSM instruments Switzerland were 28.5GPa and 84.6%, respectively.
The friction coefficient and the wear rate of the film were measured by a friction wear tester from CSM instruments of Switzerland, respectively, 0.08 and 8.1X 10-17m3/m.N。
Example four
Based on the above embodiments, this embodiment further illustrates a method for preparing another high-hardness wear-resistant fullerene-like carbon film, which specifically includes the following steps:
(1) adopting GCr15 stainless steel material as matrix, grinding the matrix material with sand paper and mechanically polishing before experiment, sequentially placing in acetone and alcohol solution, ultrasonic cleaning for 5min, blowing dry with blower, placing into vacuum chamber, and vacuumizing to vacuum degree lower than 3 × 10-3Pa。
(2) Introducing argon gas of 1.0Pa into the vacuum chamber, applying-1000V pulse bias voltage on the substrate, etching and cleaning the substrate surface for 30min by using anode layer ion beam source to ionize argon ions, and setting the anode layer ion beam source voltage to be 1200V.
(3) Introducing nitrogen and argon into the coating chamber, wherein the flow of the nitrogen is 12SCCM, the flow of the argon is 40SCCM, the air pressure is kept at 0.8Pa, and the substrate is applied with a direct current bias of-100V. Preparing a CrN layer by adopting a reactive magnetron sputtering technology, wherein the current of a Cr target is 2.5A, the purity of the Cr target is 99.99 percent, and the thickness of the deposited CrN layer is 20 nm;
(4) introducing 50SCCM argon into the coating chamber, wherein the pressure of the argon is 0.8Pa, applying-100V direct current bias on the substrate, and preparing a Cr layer by adopting a magnetron sputtering technology, wherein the current of a Cr target is 2.5A, and the thickness of the deposited Cr layer is 15 nm;
(5) sequentially repeating the step (3) and the step (4) for 14 periods to prepare a soft-hard alternating transition layer with the thickness of 490 nm;
(6) preparing fullerene-like carbon film, introducing methane (CH) into the film coating chamber4) And argon (Ar), the flow ratio of methane and argon being 1:1, the gas pressure being 15 Pa. The upper polar plate is connected with a radio frequency power supply, and the radio frequency power is 1.0 kW. The lower polar plate is connected with a direct current pulse power supply, the bias voltage is-1000V, the duty ratio is 0.7, and the frequency is 40 kHz. The thickness of the fullerene-like carbon film is controlled to be 1500 nm.
(7) Stopping coating until the temperature in the coating chamber is reduced to below 80 ℃, and taking out the metal substrate.
The structure of the film was characterized using a Jobin Yvon LabRam HR800 Raman spectrometer, indicating that five-membered and seven-membered rings were formed in the film, indicating that a fullerene-like microstructure was formed in the film.
The hardness and elastic recovery of the nanoindenter film from Swiss CSM Instrument company were 32.3GPa and 85.9%, respectively.
The friction coefficient and the wear rate of the film were measured by a friction wear tester from CSM instruments of Switzerland, respectively, 0.07 and 6.3X 10-17m3/m.N。
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it will be understood by those skilled in the art that various changes and modifications may be made herein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. The high-hardness wear-resistant fullerene-like carbon film is characterized by sequentially comprising a fullerene-like carbon layer, a CrN/Cr soft-hard alternating transition layer and a metal substrate from top to bottom.
2. The high-hardness abrasion-resistant fullerene-like carbon film according to claim 1, wherein the metal matrix is 9Cr18 stainless steel material or GCr15 stainless steel material.
3. The high-hardness wear-resistant fullerene-like carbon film according to claim 1, wherein the CrN/Cr soft-hard alternating transition layer is deposited by magnetron sputtering, and the fullerene-like carbon layer is deposited by PECVD technique.
4. The highly hard wear-resistant fullerene-like carbon film as claimed in claim 1, wherein the CrN/Cr soft-hard alternating transition layer has a thickness of 0.3 μm to 0.5 μm, and the fullerene-like carbon film has a thickness of 1.2 μm to 1.5 μm.
5. A preparation method of a high-hardness wear-resistant fullerene-like carbon film is characterized by comprising the following steps:
step 1, introducing argon into a coating vacuum chamber to enable the air pressure in the coating vacuum chamber to be 0.3-1.0 Pa, and etching and cleaning the surface of a metal matrix for 20-30 min by using argon ions obtained by ionizing argon by an anode layer ion beam source;
step 2, introducing nitrogen into the coating vacuum chamber, wherein the nitrogen flow is 10SCCM, the argon flow is 40SCCM, so that the air pressure in the coating vacuum chamber is 0.5 Pa-0.8 Pa, simultaneously, applying a direct current bias of-50V to-100V to the metal substrate, preparing a CrN layer by adopting a reactive magnetron sputtering method, and setting the current of a Cr target to be 2.0A-2.5A;
step 3, stopping introducing nitrogen, adjusting the flow of the argon to ensure that the air pressure in the coating vacuum chamber is 0.5 Pa-0.8 Pa, applying a direct current bias voltage of-50V to-100V to the metal substrate, preparing a Cr layer by adopting a magnetron sputtering method, and setting the current of a Cr target to be 2.0A-2.5A;
step 4, repeating the step 2 and the step 3 in sequence until the thickness of the CrN/Cr soft-hard alternating transition layer is 300-500 nm;
step 5, introducing methane and argon into the coating vacuum chamber at a flow ratio of 1:1 to ensure that the air pressure in the coating vacuum chamber is 10-15 Pa;
step 6, connecting an upper polar plate in a coating vacuum chamber to a radio frequency power supply, connecting a lower polar plate to a direct current pulse power supply with bias voltage of-600V to-1000V, ionizing methane under the action of the radio frequency power supply to obtain different ions, and depositing the different ions on a metal substrate placed on the lower polar plate under the attraction of the lower polar plate with negative bias voltage after chemical reaction to obtain a fullerene-like carbon layer with the thickness of 1.2-1.5 mu m;
and 7, stopping coating until the temperature in the coating vacuum chamber is reduced to be below 80 ℃ to obtain the metal substrate coated with the fullerene-like carbon layer and the CrN/Cr soft-hard alternating transition layer.
6. The method for preparing a highly hard and wear-resistant fullerene-like carbon film as claimed in claim 5, wherein the anode layer ion beam source voltage in step 1 is 1000V-1200V, and a pulse bias of-600V-1000V is applied to the metal substrate.
7. The method of claim 5, wherein the purity of the Cr target is 99.99%.
8. The method according to claim 5, wherein the duty ratio of the DC pulse power supply in step 5 is 0.4-0.7, and the frequency is 20 kHz-40 kHz.
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