CN110578114A - Doped graphite-like composite film, preparation method thereof and part containing doped graphite-like composite film - Google Patents

Doped graphite-like composite film, preparation method thereof and part containing doped graphite-like composite film Download PDF

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Publication number
CN110578114A
CN110578114A CN201910979180.5A CN201910979180A CN110578114A CN 110578114 A CN110578114 A CN 110578114A CN 201910979180 A CN201910979180 A CN 201910979180A CN 110578114 A CN110578114 A CN 110578114A
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graphite
composite film
cerium
doped
aluminum
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蔡海潮
薛玉君
叶军
司东宏
李航
贺江涛
杨芳
刘春阳
马喜强
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Henan University of Science and Technology
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Henan University of Science and Technology
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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
    • 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
    • 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
    • C23C14/0605—Carbon
    • 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
    • C23C14/22—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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

the invention relates to a doped graphite-like composite film, a preparation method thereof and a part containing the doped graphite-like composite film, wherein the doped graphite-like composite film consists of doping elements and graphite-like materials, and the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.21-12.26%, and the balance is graphite-like. The mechanical property of the doped graphite-like composite film is enhanced, and excellent wear resistance is further shown; the cerium and aluminum co-doped graphite-like composite film has high crystallization strength, and the hardness and the elastic modulus are both improved by more than 10%.

Description

Doped graphite-like composite film, preparation method thereof and part containing doped graphite-like composite film
Technical Field
The application relates to the technical field of surface engineering, in particular to a doped graphite-like composite film, a preparation method thereof and a component containing the doped graphite-like composite film.
Background
The graphite-like carbon-based film is SP2The amorphous carbon film mainly containing hybridized carbon bonds and having the hydrogen content of less than 20 percent is also called GLC, the graphite-like film material is widely researched and focused due to the excellent lubricating property of the amorphous carbon film material, the film material has higher oxidation resistance temperature and excellent antifriction and radiation resistance, has the integrated property of wear resistance and self lubrication, and is widely applied to the fields of aerospace, high-end equipment oil-free lubricating systems and the like. However, the graphite-like film has the problems of high internal stress, poor plastic toughness, poor compatibility with a metal matrix and the like, and the graphite-ic graphite composite film prepared by the Teer company regulates the plastic toughness of the graphite-like film by compounding a certain content of Cr element, reduces the internal stress and improves the bearing capacity and the wear resistance of the composite film. However, since the Cr transition layer is columnar crystal, there are voids between grain boundaries, which makes the film easy to peel off, affecting its wear resistance and service life.
The rare earth element has coupling effect and microalloying effect, and the doping of the rare earth element in the graphite-like thin film can improve the comprehensive performance, particularly the thermal stability and the wear resistance of the thin film, so that the rare earth doping is an important research direction of a novel solid lubricating thin film, for example, a graphite-like thin film doped with the rare earth element is disclosed in Chinese patent application with application publication No. CN 101613855A.
However, the doped graphite-like thin film in the prior art has the problems of low hardness, high friction coefficient and high wear rate.
Disclosure of Invention
The invention aims to provide a doped graphite-like composite film to solve the problems of low hardness, high friction coefficient and high wear rate of the graphite-like film in the prior art.
The second purpose of the invention is to provide a preparation method of a doped graphite-like composite film, so as to solve the problems of complicated preparation method and high cost in the prior art.
A third object of the present invention is to provide a component comprising a doped graphite-like composite film, which can improve the service life of the component.
In order to achieve the purpose, the technical scheme of the invention is as follows:
A doped graphite-like composite film is composed of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.19-12.26%, and the balance is graphite-like.
The doped graphite-like composite film consists of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum, and the mass percentages of the doping elements cerium and the doping elements aluminum are controlled; the doped graphite-like composite film with a specific mass percentage effectively inhibits the rapid growth of graphite-like film columnar crystals, eliminates holes formed when film-forming particles are rapidly diffused, enhances the mechanical property of the composite film, and then shows excellent wear resistance; the binary (cerium and aluminum) co-doped graphite-like base composite film has high crystallization strength, and the hardness and the elastic modulus are both improved by more than 10%.
A preparation method of a doped graphite-like composite film comprises the following steps: and depositing a doped graphite-like composite film on the surface of the preheated substrate by adopting a magnetron sputtering method, and cooling to obtain the graphite-like composite film.
According to the preparation method of the doped graphite-like composite film, a substrate is preheated under a protective atmosphere, then the doped graphite-like composite film is deposited on the surface of the substrate by adopting a magnetron sputtering method, and the part containing the doped graphite-like composite film is obtained after cooling. The preparation method has the characteristics of simplicity and low cost. The magnetron sputtering method is that under the protective atmosphere, voltage is applied between a sputtering target and the wall of a coating chamber, and magnetic control type abnormal glow discharge is generated in the coating chamber to ionize the protective atmosphere; the protective atmosphere is accelerated by the sputtering target and bombards the surface of the sputtering target, atoms on the surface of the target material are sputtered to deposit on the surface of the substrate to form a film, and the films of different materials and different thicknesses can be obtained by replacing targets of different materials and controlling different sputtering time.
Preferably, the doped graphite-like composite film consists of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.19-12.26%, and the balance is graphite-like.
Preferably, the substrate is any one of quartz glass, silicon wafer or steel.
Preferably, the pressure of the working gas is 0.4-1.6 Pa; the protective atmosphere is argon; the flow rate of the working gas is 20sccm to 100 sccm.
Preferably, the temperature of the preheating treatment is 300 ℃ and the time of the preheating treatment is 60 to 90 minutes.
Preferably, the substrate is subjected to a pre-heat treatment, followed by the steps of cleaning the substrate and vacuum treating the substrate. The cleaning of the matrix is that the matrix is cleaned by absolute ethyl alcohol ultrasonic for 15 minutes and then cleaned by acetone for 10 minutes. The vacuum treatment of the matrix is to place the matrix in a vacuum environment with the vacuum degree of 5e-4 Pa.
In order to further improve the hardness of the doped graphite-like composite film, preferably, the deposition of the doped graphite-like composite film comprises co-sputtering a graphite target and a doping target; the doped target is a cerium-aluminum alloy target; the co-sputtering time is 100-150 minutes, the sputtering power of the graphite target is 120-250W, and the sputtering power of the cerium-aluminum alloy target is 10-50W; the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target material is (5-50): (50-95).
In order to further increase the hardness of the doped graphite-like composite film, preferably, the co-sputtering time is 150-.
in order to further improve the film-substrate binding force between the doped graphite-like composite film and the substrate, preferably, before the doped graphite-like composite film is deposited, a transition layer is sputtered and deposited, the transition layer is a cerium-aluminum alloy layer, and a cerium-aluminum alloy target is used for the sputtering and deposition of the transition layer.
In order to further improve the film-substrate bonding force between the doped graphite-like composite film and the substrate, preferably, the sputtering power of the sputtering deposition transition layer is 10-50W, and the sputtering time of the sputtering deposition transition layer is 10-20 minutes.
A component containing a doped graphite-like composite film comprises a component substrate and a composite coating plated on the component substrate, wherein the composite coating comprises the doped graphite-like composite film; the doped graphite-like composite film consists of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.19-12.26%, and the balance is sulfide.
the part containing the doped graphite-like composite film effectively inhibits the rapid growth of the graphite-like film columnar crystals, eliminates the holes formed when film-forming particles are rapidly diffused, enhances the mechanical property of the composite film and then shows excellent wear resistance; the binary (cerium and aluminum) co-doped graphite-like composite film has high crystallization strength, and the hardness and the elastic modulus are both improved by more than 10%. The doped graphite-like composite film is matched with the component substrate, so that the film-substrate binding force between the doped graphite-like composite film and the substrate is improved by more than 30%.
Preferably, the component substrate is any one of quartz glass, silicon wafer or steel.
In order to improve the film-substrate binding force between the doped graphite-like matrix composite film and the substrate, preferably, the composite plating layer further comprises a transition layer arranged between the doped graphite-like matrix composite film and the component substrate; the transition layer is a cerium-aluminum alloy layer; the transition layer is obtained by depositing cerium and aluminum on the surface of a component substrate by a magnetron sputtering method; the ratio of cerium atoms to aluminum atoms in the transition layer is (5-50): (50-95).
Detailed Description
the following examples are provided to further illustrate the practice of the invention. In the following examples, the raw materials such as the cerium-aluminum alloy target, the cerium target, the aluminum target, and the graphite target, and the apparatuses such as the ultrasonic cleaner, the vacuum chamber, and the magnetron sputtering method were all available from commercially available conventional sources. The ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target is 50: 50, or the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target is 10: 90, or the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target is 5: 95.
First, embodiment of doped graphite-like composite film
Example 1
The doped graphite-like composite film of the embodiment is composed of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum, the mass percent of the doping element cerium is 12.98%, the mass percent of the doping element aluminum is 2.12%, and the balance is graphite-like.
Examples 2 to 14
The doped graphite-like composite films of examples 2-14 were composed of doping elements cerium and aluminum and graphite-like; the contents of the ingredients are listed in table 1.
TABLE 1 doped sulfides (WS) of examples 2-132) Composition of composite film
second, the following specific examples of the methods for producing the doped graphite-like composite thin films will explain the production of the doped graphite-like composite thin films of examples 1 to 14, respectively.
Example 15
The preparation method of the doped graphite-like composite film of the embodiment is described in the preparation of the doped graphite-like composite film of the embodiment 1, and specifically includes the following steps:
1) Cleaning the surface of the substrate silicon wafer in an ultrasonic cleaning machine for 15 minutes by using absolute ethyl alcohol, and then cleaning the surface of the substrate silicon wafer in the ultrasonic cleaning machine for 10 minutes by using acetone; putting the substrate silicon wafer into a vacuum chamber for vacuum treatment, wherein the vacuum degree is 5e-4 Pa; introducing argon gas, wherein the flow of the argon gas is 40sccm, the pressure of the argon gas in the vacuum chamber is controlled to be 1.2Pa, and preheating the substrate for 60 minutes at the temperature of 300 ℃;
2) Maintaining the flow rate of argon in the vacuum chamber to be 40sccm and the pressure of the argon to be 1.2 Pa; depositing a doped graphite-like composite film on the surface of a substrate silicon wafer by adopting a magnetron sputtering method: opening a baffle plate of a doped target cerium-aluminum alloy target, exciting the cerium-aluminum alloy target by using a 20W direct current power supply, forming stable glow, keeping the power of 20W, sputtering for 20 minutes to form a transition layer, then opening the baffle plate of a graphite target, co-sputtering with the doped target cerium-aluminum alloy target by using the power of 120W for 120 minutes to prepare a graphite-like composite film containing 2.2 mu m cerium-aluminum doping; the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target is 50: 50, the cerium-aluminum alloy target has a purity of 99.99%.
Examples 16 to 18
The doped sulfide composite thin films of examples 16 to 18 were prepared in substantially the same manner as in example 15 except that the operating pressures were 0.4Pa, 0.8Pa and 1.6Pa, respectively.
Examples 19 to 22
the doped sulfide composite thin films of examples 19 to 22 were prepared in substantially the same manner as in example 15, except that the excitation powers of the cerium-aluminum alloy targets were 10W, 30W, 40W, and 50W, respectively.
examples 23 to 26
The doped sulfide composite thin films of examples 23 to 26 were prepared in substantially the same manner as in example 15 except that the flow rates of argon gas were 20sccm, 60sccm, 80sccm, and 100sccm, respectively.
Example 27
The doped sulfide composite thin film of example 27 was prepared in substantially the same manner as in example 15 except that the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target was 10: 90.
Example 28
The doped sulfide composite thin film of example 28 was prepared in substantially the same manner as in example 15, except that the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target was 5: 95.
In other embodiments of the method for preparing a doped graphite-like composite film, a plasma metal layer may be pre-sputtered on the component substrate for 5 minutes before sputtering the transition layer to achieve a better bonding effect.
third, examples of components containing doped graphite-like composite films
The resulting final product, which corresponded to the preparation methods of examples 15-28, respectively, included the component substrate, the transition layer plated on the component, and the doped graphite-like composite film plated on the transition layer.
The component substrate of the embodiment is a silicon wafer, the component substrate can also be quartz glass or steel, and aiming at other implementation situations, the wear-resistant working surface of the component is plated.
Fourth, comparative example
comparative example 1
This comparative example prepared a pure graphite-like thin film, which was substantially the same as the preparation method of example 15 except that only the graphite target was used for sputtering after the cerium-aluminum transition layer was plated, and the specific sputtering parameters were kept the same.
Fifth, test example:
The test example compares the binding force, hardness, friction coefficient and wear rate of the pure graphite-like film and the corresponding composite film. The binding force and the hardness are obtained according to the test of a nano-indenter, the friction coefficient is obtained according to the test of a high-temperature friction wear testing machine (the friction radius is 4mm, the diameter of a grinding ball is 6mm, the rotating speed is 336r/min, and the load is 1N), and the wear rate is obtained by calculation according to a formula W (V/F) L (in the formula, V is the wear volume of a grinding trace, F is the normal load applied by the friction test, and L is the length of a friction stroke).
The film prepared by the process method is subjected to relevant tests by using a nano indenter and a friction and wear testing machine, and the specific test results are shown in table 1:
TABLE 1 comparison of properties of parts containing doped graphite-like based composite films and parts containing graphite-like films
Numbering Film-substrate binding force Hardness of Coefficient of friction Rate of wear
Comparative example 1 20N 9GPa 0.1-0.12 7E-16m3/N*m
Example 15 50N 4.2GPa 0.05-0.075 7E-18m3/N*m
Example 27 38N 1.8GPa 0.095-0.11 6E-17m3/N*m
Example 28 42N 1.9GPa 0.08-0.095 5E-17m3/N*m

Claims (8)

1. A doped graphite-like composite film is characterized by consisting of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.19-12.26%, and the balance is graphite-like.
2. A method for preparing the doped graphite-like composite film according to claim 1, comprising the steps of:
And depositing a doped graphite-like composite film on the surface of the preheated substrate by adopting a magnetron sputtering method, and cooling to obtain the graphite-like composite film.
3. The method of claim 2, wherein depositing the doped graphite-like composite film comprises co-sputtering a graphite target and a doping target; the doped target is a cerium-aluminum alloy target; the co-sputtering time is 100-150 minutes, the sputtering power of the graphite target is 120-250W, and the sputtering power of the cerium-aluminum alloy target is 10-50W; the ratio of cerium atoms to aluminum atoms in the cerium-aluminum alloy target material is (5-50): (50-95).
4. The method for preparing the doped graphite-like composite film as claimed in claim 3, wherein the co-sputtering time is 150-150 minutes, and the sputtering power of the graphite target is 150-250W.
5. The method of claim 2 ~ 3, wherein the doped graphite-like composite film is prepared by sputtering a transition layer, the transition layer is a cerium-aluminum alloy layer, and the transition layer is prepared by sputtering a cerium-aluminum alloy target.
6. The method for preparing the doped graphite-like composite film according to claim 5, wherein the sputtering power for sputtering and depositing the transition layer is 10-50W, and the sputtering time for sputtering and depositing the transition layer is 10 ~ 20 minutes.
7. A component containing a doped graphite-like composite film is characterized by comprising a component substrate and a composite coating plated on the component substrate, wherein the composite coating comprises the doped graphite-like composite film; the doped graphite-like composite film consists of doping elements and graphite-like materials, wherein the doping elements are cerium and aluminum; the mass percent of the doping element cerium is 6.47-13.49%, the mass percent of the doping element aluminum is 1.19-12.26%, and the balance is sulfide.
8. The doped graphite-like composite film-containing component of claim 7, wherein the composite coating further comprises a transition layer disposed between the doped graphite-like composite film and the component substrate; the transition layer is a cerium-aluminum alloy layer; the transition layer is obtained by depositing cerium and aluminum on the surface of a component substrate by a magnetron sputtering method; the ratio of cerium atoms to aluminum atoms in the transition layer is (5-50): (50-95).
CN201910979180.5A 2019-10-15 2019-10-15 Doped graphite-like composite film, preparation method thereof and part containing doped graphite-like composite film Pending CN110578114A (en)

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CN114023561A (en) * 2021-10-29 2022-02-08 华中科技大学 Extrinsic two-dimensional composite magnetic material, preparation method and application

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Publication number Priority date Publication date Assignee Title
CN114023561A (en) * 2021-10-29 2022-02-08 华中科技大学 Extrinsic two-dimensional composite magnetic material, preparation method and application
CN114023561B (en) * 2021-10-29 2022-12-09 华中科技大学 Extrinsic two-dimensional composite magnetic material, preparation method and application

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Application publication date: 20191217