CN114107899B - Carbon-based composite coating on surface of aluminum alloy and preparation method thereof - Google Patents
Carbon-based composite coating on surface of aluminum alloy and preparation method thereof Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 61
- 238000000576 coating method Methods 0.000 title claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 49
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 63
- 230000003197 catalytic effect Effects 0.000 claims abstract description 45
- 238000005516 engineering process Methods 0.000 claims abstract description 25
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 22
- 238000007737 ion beam deposition Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 238000001020 plasma etching Methods 0.000 claims description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 7
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000010884 ion-beam technique Methods 0.000 claims description 2
- 239000013077 target material Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 147
- 230000000052 comparative effect Effects 0.000 description 23
- 239000002346 layers by function Substances 0.000 description 21
- 230000008021 deposition Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 10
- 239000002344 surface layer Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000005728 strengthening Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 238000005087 graphitization Methods 0.000 description 4
- 238000007373 indentation Methods 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910001234 light alloy Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000011253 protective coating Substances 0.000 description 2
- 229910001008 7075 aluminium alloy Inorganic materials 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
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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
- C23C14/22—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
-
- 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
-
- 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
- C23C14/0611—Diamond
-
- 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
-
- 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
- C23C14/221—Ion beam deposition
Abstract
The invention discloses a carbon-based composite coating on the surface of an aluminum alloy, which consists of three elements of Ti, si and C, wherein the carbon-based composite coating has a multi-layer structure, and a combined Ti layer, a Si layer, a catalytic Ti layer and a DLC layer are sequentially arranged from the surface of the aluminum alloy to the surface of the carbon-based composite coating. The carbon-based composite coating has good surface binding force and high bearing capacity. The invention also discloses a preparation method of the carbon-based composite coating on the surface of the aluminum alloy, which comprises the steps of sequentially depositing and combining a Ti layer, a Si layer, a catalytic Ti layer and a DLC layer on the surface of the aluminum alloy by a high-power pulse magnetron sputtering technology, a direct-current magnetron sputtering technology and an ion beam deposition technology to obtain the carbon-based composite coating on the surface of the aluminum alloy. The preparation method is simple and efficient.
Description
Technical Field
The invention belongs to the technical field of surface protection, and particularly relates to a carbon-based composite coating on an aluminum alloy surface and a preparation method thereof.
Background
The aluminum alloy has the advantages of small density, high specific strength, good plasticity and the like, and has good application prospect in the high-tech fields of aerospace, military, transportation and the like as an important lightweight material. In recent years, with the high-speed development of the fields, the service condition of the aluminum alloy tends to be bad, but the aluminum alloy has the key problems of low hardness, poor wear resistance and the like, and the long-life reliable operation of key equipment is restricted. The surface of the mechanical moving part is coated with the hard coating by the material surface strengthening technology, so that the performances of the aluminum alloy such as surface strength, hardness, wear resistance, corrosion resistance and the like can be effectively enhanced, the working efficiency is improved, the service life is prolonged, and the method is an ideal way for breaking through the use limit and widening the application field.
The surface strengthening treatment of aluminum alloy has many methods, such as thermal spraying, electroplating, chemical plating, electric spark deposition, micro-arc oxidation, laser shock strengthening, plasma deposition and the like. Compared with other technologies, the physical vapor deposition (Physics vapor deposition, PVD) technology has the advantages of low deposition temperature (generally below room temperature-600 ℃), small matrix deformation (suitable for precision parts), good uniformity, high purity, multiple coating systems, fine and controllable coating structure, environmental protection and the like, and can meet the strengthening requirement of the surface of the precision material in the high technical field.
A Diamond-like carbon (DLC) film has many excellent properties similar to or close to Diamond, hardness inferior to Diamond, and can be used as an excellent wear-resistant protective coating; compared with a CVD diamond coating, DLC is amorphous and has no grain boundary, which means that the coating is quite smooth and compact, has no grain boundary defect, has high abrasion resistance, high heat conductivity, stable chemical property and the like, and can be used as a good corrosion-resistant coating. Meanwhile, the material has unique tribological properties, and is a very promising material. The diamond-like carbon-based coating material is an amorphous material with the characteristics of graphite and diamond, has the comprehensive properties of high hardness, wear resistance, corrosion resistance and the like, and is an ideal protective material for solving the problem of poor wear resistance and corrosion resistance of an aluminum alloy material.
However, due to the obvious physical and chemical property differences between the light alloy and the carbon-based coating, the light alloy matrix-coating system bears complex load action under the service conditions of sliding, vibration, friction and the like, various forms of surface/interface failures of the film-based structure are easily caused, and the service life of the coating is influenced. The former has reported the structural design of DLC film deposited on the surface of aluminum alloy. Chinese patent CN109082647 discloses that by depositing a mixed transition layer of SiC and Si-DLC on 7075 aluminum alloy, and then directly depositing a DLC layer containing H on the transition layer, the method adopts the mixed transition layer deposition of SiC and Si-DLC, while SiC and Al have a large difference in modulus and thermal expansion coefficient, etc., as a transition layer, there is a problem of bonding during service.
Therefore, it is needed to solve the technical problem that the binding force of the Al matrix to the DLC layer is poor and the bearing capacity is poor.
Disclosure of Invention
The invention provides an aluminum alloy surface carbon-based composite coating with good surface binding force and high bearing capacity.
The carbon-based composite coating on the surface of the aluminum alloy consists of three elements of Ti, si and C, wherein the carbon-based composite coating has a multi-layer structure, and a bonding layer of Ti, a Si layer, a catalytic layer of Ti and a DLC layer are sequentially arranged from the surface of the aluminum alloy to the surface of the carbon-based composite coating.
The aluminum alloy and Ti have better interface bonding capability, and the strain energy can be absorbed through microcracks under the action of external force through the thickness regulation of the bonding layer Ti, so that the aluminum alloy has better deformation resistance and the carbon-based composite coating on the surface of the aluminum alloy has stronger bearing capability.
Because the Si layer has better physical and chemical property matching with the surface DLC, the mechanical property, the thermal expansion coefficient and the like are similar, the chemical affinity of Si and C elements is stronger, and the structure of the Si layer is a composite structure of extremely small nanocrystalline dispersed in an amorphous structure, the plastic deformation resistance can be improved remarkably.
The Ti valence electron layer structure of the catalytic layer has an empty d track, and is easy to bond with C. The alignment principle exists between the DLC layer and atoms on a diamond-like structure on a certain surface, carbon atoms tend to be in a plane, so that the carbon atoms are converted into graphite, the DLC layer is graphitized, meanwhile, the thickness and the grain size of the catalytic Ti layer are regulated and controlled, the morphology of the DLC layer can be changed, on one hand, the internal stress of the DLC layer is reduced, and the bearing capacity is improved; on the other hand, the friction coefficient of the DLC layer surface is reduced, and the wear resistance is improved.
The thickness of the bonding layer Ti is 800-1000nm, the thickness of the Si layer is 1500-2000nm, the thickness of the catalytic layer Ti is 100-200nm, and the thickness of the DLC layer is 1000-1500nm.
The bonding layer Ti is thicker, the bearing capacity can be improved by absorbing strain energy through microcracks, the mechanical property of the Si layer is good, as the middle layer, the physical and chemical property difference between the bottom layer and the surface layer can be coordinated through thickness change, meanwhile, the plastic deformation resistance of the coating is improved, the thickness of the catalytic layer Ti is thinner, the graphitization degree and the morphology of the surface layer DLC are mainly influenced to a certain extent, if thicker, the thicker layer can cause the surface layer DLC to present a certain loose structure along the thick columnar structure when the surface layer DLC grows, and the mechanical property of the DLC is influenced. The thickness of the DLC layer is a thickness control that determines the next few layers. Because DLC is a wear resistant protective coating, the overall coating thickness is typically controlled to 3-5 μm for precision transmission components, so the overall coating thickness design is optimized as above.
The nano grain size of the bonding layer Ti is 5-20nm, and the nano grain size of the catalytic layer Ti is 50-200nm.
The grain size of the bonding layer is small, so that the compactness of the bonding layer can be ensured, and the bonding performance is improved. The grain size of the catalytic layer is controlled to be 50-150nm, on one hand, the DLC structure of the surface layer is influenced by a certain grain size of the catalytic layer, and the internal stress of the DLC of the surface layer is reduced and the wear resistance is increased by influencing the DLC structure of the surface layer and the like; on the other hand, too large grain size can cause too loose of the DLC coating structure on the surface layer, and reduce the mechanical property of DLC, thereby affecting the exertion of wear resistance.
The invention also provides a preparation method of the carbon-based composite coating on the surface of the aluminum alloy, which comprises the following steps:
(1) Etching the surface of the aluminum alloy matrix by using plasma, opening a Ti target material by adopting a high-power pulse magnetron sputtering technology, and depositing a combined Ti layer on the etched aluminum alloy surface;
(2) Closing a Ti target, opening a Si target, depositing a Si layer on the Ti surface of the bonding layer by adopting a direct current magnetron sputtering technology, closing the Si target, opening the Ti target, depositing a catalytic layer Ti on the Ti surface of the Si layer, closing the Ti target, introducing acetylene gas, and depositing a DLC layer on the Ti surface of the catalytic layer by adopting an ion beam technology to obtain the aluminum alloy surface carbon-based composite coating.
The bonding layer adopts a high-power pulse technology, so that the ionization rate of Ti can be increased, fine Ti grains are formed, the compactness of the bonding layer Ti is improved, and the bonding between Ti and an aluminum alloy matrix is enhanced. The direct current magnetron sputtering technology for the catalytic layer is easy to control the grain size of the Ti layer, and promotes the performance of the surface DLC (reducing internal stress and improving wear resistance).
The parameters of the plasma etching are as follows: under the argon atmosphere, the power is 300-500W, and the air pressure is 3-10mTorr.
The parameters of the high-power pulse magnetron sputtering technology are as follows: the pulse voltage is 400-1000V, and the argon pressure is 2-10mTorr.
The magnetron sputtering technological parameters of depositing the Si layer on the Ti surface of the bonding layer are as follows: the power is 0.5-2.5KW, and the air pressure is 1.5-6.0mTorr.
The magnetron sputtering technical parameters of depositing the catalytic layer Ti on the surface of the Si layer are as follows: the power is 1.5-3KW, and the argon pressure is 3-5mTorr.
The ion beam deposition technical parameters of the DLC layer deposited on the Ti surface of the catalytic layer are as follows: acetylene environment with power of 200-400W and air pressure of 3-5mTorr.
Compared with the prior art, the invention has the beneficial effects that:
(1) The bonding layer Ti with optimized thickness and grain size is deposited, so that the bonding layer Ti has good interface bonding with an aluminum alloy matrix and can coordinate deformation; on the other hand, under the action of load, strain energy can be absorbed in the form of microcracks through fine grain strengthening, the deformation resistance capacity is remarkably improved, and the bearing capacity of the aluminum alloy/carbon-based coating is improved.
(2) Through the deposition of the Si supporting layer with optimized thickness, the DLC film has better performance matching with the DLC film functional layer, can obviously improve the plastic deformation resistance of the aluminum alloy/carbon-based coating and improve the film-based binding force.
(3) Through the construction of the Ti catalytic layer, the thickness and the grain size of the Ti catalytic layer are optimized, and the mechanical property of the coating is not influenced, so that on one hand, the DLC catalytic layer on the surface layer can be graphitized to a certain extent, the friction coefficient of the coating is reduced, and the wear resistance is improved; on the other hand, the thickness and the grain size of the catalytic layer can be controlled to regulate the surface morphology of the surface DLC layer, release the internal stress to a certain extent and improve the high stress of DLC.
Drawings
FIG. 1 is a schematic diagram of a carbon-based composite coating on an aluminum alloy surface according to an embodiment of the present invention;
FIG. 2 is a cross-sectional profile of comparative example 1, comparative example 2, comparative example 3 after indentation testing;
FIG. 3 is a DLC carbon bond structure diagram of example 1, comparative example 4, comparative example 5;
FIG. 4 is a graph showing the results of binding force test of example 1, comparative example 4, and comparative example 5;
FIG. 5 is a graph of DLC friction coefficients for example 1, comparative example 4, comparative example 5;
FIG. 6 is a graph of DLC wear rates for example 1, comparative example 4, and comparative example 5;
FIG. 7 is a graph showing the surface topography of example 1, comparative example 2, and comparative example 3.
Detailed Description
The invention provides a high-bonding low-friction carbon-based coating on the surface of an aluminum alloy and a preparation method thereof, wherein the carbon-based coating has the structure shown in figure 1 that: (1) the bonding layer is a Ti layer; (2) the supporting layer is a Si layer; (3) the catalytic layer is a Ti layer; the functional layer (4) is a DLC layer. The thickness of the bonding layer is 800-1000nm; the thickness of the supporting layer is 1500-2000nm; the thickness of the catalytic layer is 100-200nm; the thickness of the functional layer is 1000-1500nm; the Ti nanocrystalline size of the bonding layer is 5-20nm; the Ti nanocrystalline size of the catalytic layer is 50-150nm.
The technical scheme of the present invention is further described in detail below with reference to the preferred embodiments and the accompanying drawings, and the embodiments are implemented on the premise of the technical scheme of the present invention, and detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples described below, unless otherwise specified, were all commercially available from conventional biochemicals.
Example 1
The carbon-based coating structure is as follows:
(1) Depositing a bonding layer Ti, wherein the thickness is 800nm, and the grain size is 5-10nm;
(2) Depositing a supporting layer Si with the thickness of 1500nm;
(3) Depositing a catalytic layer Ti, wherein the thickness is 100nm, and the grain size is 100-120nm;
(4) The DLC functional layer is deposited with a thickness of 1000nm.
The preparation process comprises the following steps: (1) Placing the cleaned aluminum alloy substrate into a vacuum chamber for plasma etching, wherein the plasma etching conditions are as follows: under the argon environment, the power is 300W, and the air pressure is 3mTorr; depositing a bonding layer on the surface of the substrate, wherein the bonding layer is a Ti layer, and the deposition conditions of the bonding layer are as follows: adopting a high-power pulse magnetron sputtering technology, wherein the pulse voltage is 400V, and the argon pressure is 3mTorr; (2) And depositing a supporting layer on the bonding layer obtained in the last step, wherein the supporting layer is a Si layer, and the depositing conditions of the supporting layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 1.5KW, and the air pressure is 2.5mTorr; (3) Depositing a catalytic layer on the support layer obtained in the last step, wherein the catalytic layer is a Ti layer, and the deposition conditions of the catalytic layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 3KW, and the argon pressure is 3mTorr; (4) Depositing a functional layer on the catalytic layer obtained in the last step, wherein the functional layer is a DLC layer, and the deposition conditions of the functional layer are as follows: acetylene environment, power 200W, air pressure 3.5mTorr.
The bonding strength of the carbon-based coating obtained on the surface of the aluminum alloy is 35N, the friction coefficient is 0.11 under the test conditions of 20N load and 30min friction time, and the wear rate is 5.0x10 -17 mm 3 /N m. As shown in FIG. 7, the surface topography of the indentations (enlarged 800 times) of comparative examples 1 to 3 had more cracks, and the surface topography of the indentations (enlarged 1200 times) of example 1 had fewer cracks and the entire resistance to deformation was strong.
Example 2
The carbon-based coating structure is as follows:
(1) Depositing a bonding layer Ti, wherein the thickness is 950nm, and the grain size is 10-15nm;
(2) Depositing a supporting layer Si with the thickness of 1800nm;
(3) Depositing a catalytic layer Ti, wherein the thickness is 120nm, and the grain size is 120-150nm;
(4) And depositing a functional layer DLC with the thickness of 1200nm.
The preparation process comprises the following steps: (1) Placing the cleaned aluminum alloy substrate into a vacuum chamber for plasma etching, wherein the plasma etching conditions are as follows: under the argon environment, the power is 400W, and the air pressure is 8mTorr; depositing a bonding layer on the surface of the substrate, wherein the bonding layer is a Ti layer, and the deposition conditions of the bonding layer are as follows: adopting a high-power pulse magnetron sputtering technology, wherein the pulse voltage is 700V, and the argon pressure is 6mTorr; (2) And depositing a supporting layer on the bonding layer obtained in the last step, wherein the supporting layer is a Si layer, and the depositing conditions of the supporting layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 0.5KW, and the air pressure is 1.5mTorr; (3) Depositing a catalytic layer on the support layer obtained in the last step, wherein the catalytic layer is a Ti layer, and the deposition conditions of the catalytic layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 1.5KW, and the argon pressure is 3.5mTorr; (4) Depositing a functional layer on the catalytic layer obtained in the last step, wherein the functional layer is a DLC layer, and the deposition conditions of the functional layer are as follows: acetylene environment, power 350W, air pressure 3mTorr.
The bonding strength of the carbon-based coating obtained on the surface of the aluminum alloy is 32N, the friction coefficient is 0.11 under the test conditions of 20N load and 30min friction time, and the wear rate is 6.9X10 -17 mm 3 /N m。
Example 3
The carbon-based coating structure is as follows:
(1) Depositing a bonding layer Ti with the thickness of 1000nm and the grain size of 15-20nm;
(2) Depositing a supporting layer Si with the thickness of 2000nm;
(3) Depositing a catalytic layer Ti, wherein the thickness is 200nm, and the grain size is 120-200nm;
(4) And depositing a functional layer DLC with the thickness of 1500nm.
The preparation process comprises the following steps: (1) Placing the cleaned aluminum alloy substrate into a vacuum chamber for plasma etching, wherein the plasma etching conditions are as follows: under the argon environment, the power is 500W, and the air pressure is 10mTorr; depositing a bonding layer on the surface of the substrate, wherein the bonding layer is a Ti layer, and the deposition conditions of the bonding layer are as follows: adopting a high-power pulse magnetron sputtering technology, wherein the pulse voltage is 1000V, and the argon pressure is 10mTorr; (2) And depositing a supporting layer on the bonding layer obtained in the last step, wherein the supporting layer is a Si layer, and the depositing conditions of the supporting layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 2.5KW, and the air pressure is 6mTorr; (3) Depositing a catalytic layer on the support layer obtained in the last step, wherein the catalytic layer is a Ti layer, and the deposition conditions of the catalytic layer are as follows: adopting a direct current magnetron sputtering technology, wherein the power is 2KW, and the argon pressure is 5mTorr; (4) Depositing a functional layer on the catalytic layer obtained in the last step, wherein the functional layer is a DLC layer, and the deposition conditions of the functional layer are as follows: acetylene environment, power 400W, air pressure 5mTorr.
The bonding strength of the carbon-based coating obtained on the surface of the aluminum alloy is 30N, the friction coefficient is 0.12 under the test conditions of 20N load and 30min friction time, and the wear rate is 6.5X10 -17 mm 3 /N m。
Comparative example 1
(1) Depositing a bonding layer Ti with the thickness of 200nm and the grain size of 5-10nm;
(2) The DLC functional layer is deposited with a thickness of 1000nm.
The preparation parameters were the same as in example 1.
Comparative example 2
(1) Depositing a bonding layer Ti, wherein the thickness is 800nm, and the grain size is 5-10nm;
(2) The DLC functional layer is deposited with a thickness of 1000nm.
The preparation parameters were the same as in example 1.
Comparative example 3
(1) Depositing a bonding layer Ti with the thickness of 1100nm and the grain size of 5-10nm;
(2) The DLC functional layer is deposited with a thickness of 1000nm.
The preparation parameters were the same as in example 1.
The indentation morphology test of comparative examples 1-3 shows that the thickness of the bonding layer Ti seriously affects the crack propagation resistance of the coating, and the Ti layer can absorb strain energy through microcracks when the thickness is 800nm, thus showing better plastic deformation resistance as shown in figure 2.
Comparative example 4
(1) The DLC functional layer is directly deposited with the thickness of 1000nm.
The preparation parameters were the same as in example 1.
Comparative example 5
(1) Depositing a bonding layer Si with the thickness of 200nm;
(2) The DLC functional layer is deposited with a thickness of 1000nm.
The preparation parameters were the same as in example 1.
The raman carbon bond structure test was performed on example 1, comparative example 4 and comparative example 5, and the results are shown in fig. 3, wherein the left column represents the graphitization degree, the larger the value is, the larger the graphitization degree is, the right represents the disorder degree of the coating structure, the smaller the value is, the more ordered the structure is, and the smaller the internal stress is, so that the strong bonding can be promoted. The Ti layer was found to catalyze the graphitization of the surface carbon-based coating (I D /I G Increased) such that the coating structure order increases (peak G half width decreases). Through a binding force test (figure 4), the Ti layer can improve the cohesive binding force of the coating, and the Si layer can improve the interfacial binding force of the coating; further through friction testing (5 n,5 hz) (fig. 5 and 6), the friction coefficient and wear rate of the carbon-based coating were significantly improved by the Ti layer catalysis, with example 1 achieving the strongest binding force, the lowest friction coefficient and wear rate.
Comparative example 6
(1) Depositing a bonding layer Ti with the thickness of 200nm and the grain size of 100-120nm;
(2) Depositing a supporting layer Si with the thickness of 1500nm;
(3) Depositing a catalytic layer Ti, wherein the thickness is 100nm, and the grain size is 100-120nm;
(4) The DLC functional layer is deposited with a thickness of 1000nm.
The bonding strength of the carbon-based coating obtained on the surface of the aluminum alloy is 18.6N, the friction coefficient is 0.15 under the test conditions of 20N load and 30min friction time, and the wear rate is 20.1 multiplied by 10 -17 mm 3 /N m。
Claims (7)
1. The carbon-based composite coating is characterized by comprising three elements of Ti, si and C, wherein the carbon-based composite coating has a multi-layer structure, and a bonding layer Ti, a Si layer, a catalytic layer Ti and a DLC layer are sequentially arranged from the surface of the aluminum alloy to the surface of the carbon-based composite coating;
the thickness of the bonding layer Ti is 800-1000nm, the thickness of the Si layer is 1500-2000nm, the thickness of the catalytic layer Ti is 100-200nm, and the thickness of the DLC layer is 1000-1500nm;
the nano grain size of the bonding layer Ti is 5-20nm, and the nano grain size of the catalytic layer Ti is 50-200nm.
2. A method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 1, comprising the steps of:
(1) Etching the surface of the aluminum alloy matrix by using plasma, opening a Ti target material by adopting a high-power pulse magnetron sputtering technology, and depositing a bonding layer Ti on the etched aluminum alloy surface;
(2) Closing a Ti target, opening a Si target, depositing a Si layer on the Ti surface of the bonding layer by adopting a direct current magnetron sputtering technology, closing the Si target, opening the Ti target, depositing a catalytic layer Ti on the Ti surface of the Si layer, closing the Ti target, introducing acetylene gas, and depositing a DLC layer on the Ti surface of the catalytic layer by adopting an ion beam technology to obtain the aluminum alloy surface carbon-based composite coating.
3. The method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 2, wherein the parameters of the plasma etching are as follows: under the argon atmosphere, the power is 300-500W, and the air pressure is 3-10mTorr.
4. The method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 2, wherein the parameters of the high-power pulse magnetron sputtering technology are as follows: pulse voltage 400-1000V, pulse duty ratio 2-5%, argon pressure 2-10mTorr.
5. The method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 2, wherein the magnetron sputtering technical parameters of depositing the Si layer on the Ti surface of the bonding layer are as follows: the power is 0.5-2.5kW, and the air pressure is 1.5-6.0mTorr.
6. The method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 2, wherein the magnetron sputtering technical parameters for depositing the catalytic layer Ti on the surface of the Si layer are as follows: the power is 1.5-3kW, and the argon pressure is 3-5mTorr.
7. The method for preparing the carbon-based composite coating on the surface of the aluminum alloy according to claim 2, wherein the ion beam deposition technical parameters for depositing the DLC layer on the Ti surface of the catalytic layer are as follows:
the acetylene environment has the power of 200-400W and the air pressure of 3-5mTorr.
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| JP2002372029A (en) * | 2001-06-12 | 2002-12-26 | Tdk Corp | Connecting rod coated with dlc |
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| JP2002372029A (en) * | 2001-06-12 | 2002-12-26 | Tdk Corp | Connecting rod coated with dlc |
| JP2004169137A (en) * | 2002-11-21 | 2004-06-17 | Hitachi Ltd | Sliding member |
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