CN114686829A - Wear-resistant, fatigue-resistant and repeated impact-resistant coating and production process thereof - Google Patents
Wear-resistant, fatigue-resistant and repeated impact-resistant coating and production process thereof Download PDFInfo
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- CN114686829A CN114686829A CN202011586336.2A CN202011586336A CN114686829A CN 114686829 A CN114686829 A CN 114686829A CN 202011586336 A CN202011586336 A CN 202011586336A CN 114686829 A CN114686829 A CN 114686829A
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- 238000000576 coating method Methods 0.000 title claims abstract description 74
- 239000011248 coating agent Substances 0.000 title claims abstract description 73
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000010410 layer Substances 0.000 claims abstract description 129
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000002344 surface layer Substances 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 19
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 230000009194 climbing Effects 0.000 claims description 9
- 239000011159 matrix material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 230000003252 repetitive effect Effects 0.000 claims 6
- 238000000137 annealing Methods 0.000 abstract description 4
- 238000009991 scouring Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 3
- 238000005496 tempering Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005406 washing Methods 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
- C23C14/22—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
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- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
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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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- 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
- C23C14/0635—Carbides
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- 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
- C23C14/0641—Nitrides
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- 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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- 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
- C23C14/50—Substrate holders
- C23C14/505—Substrate holders for rotation of the substrates
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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
- 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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- 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
- 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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- 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
- C23C28/32—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
- C23C28/341—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 with at least one carbide layer
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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
- C23C28/343—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 with at least one DLC or an amorphous carbon based layer, the layer being doped or not
Abstract
The invention discloses a wear-resistant, fatigue-resistant and repeated impact-resistant coating and a production process thereof, wherein the coating comprises a Cr substrate layer, a CrN + Cr repeating layer and a surface layer made of a CrC and DLC mixed material, which are sequentially generated on a substrate, and the CrN + Cr repeating layer is formed by alternately arranging a CrN layer and a Cr layer and repeating the layers for multiple times. According to the production process, the temperature is strictly controlled below 160 ℃ in the whole process, the performance of a substrate of a workpiece can be guaranteed not to be affected by annealing, meanwhile, the hardness of a Cr substrate layer in the generated coating is improved in a stepped manner, so that the coating has better impact resistance, and the generated coating can effectively resist high-frequency fatigue impact resistance and high-pressure scouring by adopting a structure that CrN and Cr are alternately repeated for multiple times; the surface layer adopts a mixed layer of CrC + DLC, which not only can ensure the hardness required by the coating, but also can ensure that the coating has very high toughness, and the combination with the CrN + Cr repeated layer can greatly improve the performances of wear resistance, fatigue resistance and high pressure impact resistance of the generated coating.
Description
Technical Field
The invention relates to the technical field of coating materials and coating production processes, in particular to a wear-resistant, fatigue-resistant and repeated impact-resistant coating and a production process thereof.
Background
In many mechanical devices, particularly some high-end precision devices, it is often desirable to enhance the performance of the device with a high performance coating. For example, in a high-pressure common rail system, an oil nozzle control valve is the core of the whole system, and at present, China can achieve high-pressure oil supply, but the service life of the domestic oil nozzle control valve is far shorter than that of the domestic oil nozzle control valve. In the prior art, the coating commonly adopted for coating the oil nozzle control valve comprises a common DLC coating (also called a diamond-like coating) and a CrN coating, the two coatings have respective advantages and disadvantages, the DLC coating has small friction coefficient, high hardness and large brittleness, the applicability is wide below national standard 4, the CrN coating has good binding force and certain impact resistance, but the friction coefficient is low, the wear resistance is deficient, and the service life is short.
The coating of the fuel injector control valve should have the comprehensive properties of friction resistance, high-frequency impact resistance, high pressure resistance, low coating temperature and the like. While the friction resistance requires a coating layer having a high hardness and a low friction coefficient, and DLC generally has such properties, the DLC coating layer having a high hardness is not resistant to high frequency impact, and the coating layer is easily broken and fails when the hardness is high. The high pressure resistance is mainly high pressure washing resistance of high pressure fuel oil, and the surface granularity of the coating is required to be small. In order to ensure the hardness of the material of the high-pressure common rail control valve, the tempering temperature is generally within 180 degrees, and the low coating temperature can ensure that a plurality of workpieces with low tempering temperature can also be coated. The prior coating can not ensure the comprehensive performance, so the prior coating material and the production process of the coating need to be improved to meet the performance requirements.
Disclosure of Invention
Aiming at the problem that the coating prepared by the existing coating material and the coating production process in the background technology can not meet the performance requirements of friction resistance, high-frequency impact resistance, high-pressure resistance, low coating temperature and the like at the same time, the invention provides a wear-resistant fatigue-resistant and repeated impact-resistant coating which can solve the problems.
The technical scheme adopted for solving the technical problems is as follows: the Cr + Cr composite material comprises a Cr substrate layer, a CrN + Cr repeating layer and a surface layer made of a CrC and DLC mixed material, wherein the Cr + Cr repeating layer is formed by alternately arranging a CrN layer and a Cr layer and repeating the CrN + Cr layers for multiple times.
In a further proposal, the thickness of the Cr substrate layer is 0.4 to 0.8 micron.
The further scheme is that the CrN + Cr repeated layer comprises a plurality of CrN layers and a plurality of Cr layers, the thickness of each CrN layer is 0.2-0.3 micron, the thickness of the outermost Cr layer is 0.25-0.35 micron, the thickness of the rest Cr layers is 0.02-0.08 micron, and the surface layer made of the mixed material of CrC and DLC is generated on the outer layer of the outermost Cr layer.
In a further proposal, the thickness of the surface layer made of the CrC and DLC mixed material is 0.8 to 1.5 microns.
Another object of the present invention is to provide a process for producing a wear-resistant, fatigue-resistant and repeated impact-resistant coating, comprising the following production steps:
s1, cleaning the workpiece needing to generate the coating by a nine-tank cleaning production line;
s2, fixing the cleaned workpiece on a rotating frame, and putting the whole rotating frame into coating equipment;
s3, vacuumizing the coating equipment until the internal air pressure of the coating equipment is 1 x 10-5 mbar, heating the coating equipment to 140-;
S4 H+ion cleaning; h is introduced into the coating equipment2And Ar gas, pure ion cleaning at 2.0 x 10-4 mbar-9.0 x 10-3mbar, ionization of H2 and Ar by upper filament in furnaceAr gas is used for generating glow, the auxiliary anode at the lower part is electrified simultaneously, electrons flow to the auxiliary anode, the workpiece is connected with a bias voltage of minus 10V to minus 30V, and the whole furnace cavity is filled with H+And Ar+， H+The ion energy and the oxide or organic matter which cannot be cleaned on the surface of the workpiece generate chemical reaction, and the workpiece is fully cleaned deep on the surface of the workpiece; ar (Ar)+The ions play a role in auxiliary ionization;
S5 Ar+ion cleaning; close H2Ar gas is continuously input, the workpiece is connected with a bias voltage of minus 200V to minus 300V, and Ar generated by the filament and the auxiliary anode+Bombarding the surface of the workpiece by ion high energy, removing surface microscopic particles and activating the surface of the matrix, and providing a better and cleaner matrix for the gradient Cr layer;
s6 stopping heating by the heater, adjusting the rotating speed of the rotating frame to 2-4 r/min, adjusting the air pressure to 1.0-9.0 x 10-3mbar by inputting Ar gas, carrying out magnetron sputtering on a gradient Cr substrate layer on the surface of the workpiece, applying a climbing bias voltage on the workpiece, connecting the workpiece with a negative 20V bias voltage to a negative 200V bias voltage, gradually climbing the workpiece from the negative 20V bias voltage to the negative 200V bias voltage, wherein the climbing time is 3000 plus 4000 seconds, and the hardness gradient of the generated gradient Cr substrate layer is improved;
s7 magnetron sputtering to generate a CrN + Cr repeated layer; maintaining the rotating speed of the rotating frame and the pressure in the furnace chamber unchanged, generating a CrN + Cr repeating layer by a magnetron sputtering process, wherein the CrN layer is generated on the Cr substrate layer generated in S6, then Cr is generated, and multiple layers are repeated to form the CrN + Cr repeating layer, when the Cr layer is generated, only Ar gas is introduced, the workpiece is connected with a bias voltage of negative 20V to negative 200V, the time for generating the Cr layer is 300-plus-600 seconds, when the CrN layer is generated, in addition to the Ar gas, N gas is introduced2Gas 100-;
s8 generating a CrC + DLC layer; regulating the rotating speed of the rotating frame to 2-4 rpm, and introducing C2H2And (3) gas and Ar gas, wherein the gas pressure is maintained at 1.0-9.0 x 10-3mbar, a magnetron sputtering method and a plasma enhanced chemical vapor deposition method are simultaneously carried out, a mixed layer of CrC + DLC is generated, the workpiece is connected with a bias voltage of 200V to 900V in the process, the power is 2-18kw, and the highest temperature is set to be 160 ℃.
In a further scheme, in step S7, the generated CrN + Cr repeating layers have an alternating structure of 9 CrN layers and 9 Cr layers, each CrN layer has a thickness of 0.2 to 0.3 micron, the outermost Cr layer has a thickness of 0.25 to 0.35 micron, and the remaining Cr layers have a thickness of 0.02 to 0.08 micron.
Further, in step S8, because the bias voltage of the workpiece is large, the temperature in the furnace easily exceeds the maximum temperature of 160 ℃, when the temperature in the furnace exceeds 160 ℃, the controller automatically controls the suspension process and the cooling furnace temperature, and when the temperature in the furnace is lower than 160 ℃, the process is continued until the required CrC + DLC layer is formed, wherein the CrC + DLC layer is of a mixed structure, and the thickness of the CrC + DLC layer is 0.8-1.5 microns.
The bias voltage of the above process means a negative voltage applied to the substrate during the plating process. The positive pole of the bias power supply is connected to the vacuum chamber, the vacuum chamber is grounded, and the negative pole of the bias is connected to the workpiece.
The invention has the beneficial effects that: 1) the wear-resistant, fatigue-resistant and repeated impact-resistant coating provided by the invention adopts a nine-groove cleaning production line and H+Ions and Ar+The ion three-step cleaning can clean pollutants, oxide layers and other foreign matters on the surface of the workpiece, and the foreign matters penetrate into the surface layer to remove micro particles on the surface and activate the surface of the matrix, so that a better and cleaner matrix is provided for the subsequent gradient Cr layer, and the previous step H is just the reason that+The step of cleaning ions does not need particularly high negative bias, so that the surface of a high-precision substrate can be effectively protected, annealing caused by overhigh local temperature due to high-energy bombardment is avoided, and the performance of the part substrate is ensured; 2) when the Cr substrate layer in the coating is generated, the hardness of the generated Cr layer is improved in a gradient manner through the process of improving the bias voltage in a gradient manner; 3) the CrN + Cr repeating layer in the coating adopts a structure that CrN and Cr are alternately repeated for multiple times, so that the generated coating can effectively resist high-frequency fatigue impact resistance and high-pressure scouring; 4) the CrC + DLC layer in the coating can ensure the hardness required by the coating, can ensure that the coating has high toughness, and can greatly improve the wear resistance, fatigue resistance and high-pressure impact resistance of the generated coating by combining with the CrN + Cr repeated layerPerformance of the hammer; 5) in the invention, in the coating generation process, the temperature in the furnace chamber is strictly controlled below 160 ℃, so that the workpiece can be effectively prevented from annealing, and the stability of the substrate performance of the workpiece is ensured.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a schematic structural view of a wear-resistant, fatigue-resistant and repeated impact-resistant coating of the present invention.
In the figure: workpiece 1, Cr substrate layer 2, CrN + Cr repeating layer 3, CrN layer 31, Cr layer 32, surface layer 4.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings. The drawings are simplified schematic diagrams illustrating the basic structure of the present invention only in a schematic manner, and thus show only the constitution related to the present invention, and directions and references (e.g., upper, lower, left, right, etc.) may be used only to help the description of the features in the drawings. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the claimed subject matter is defined only by the appended claims and equivalents thereof.
As shown in FIG. 1, the wear-resistant, fatigue-resistant and repeated impact-resistant coating of the present invention comprises a Cr substrate layer 2, a CrN + Cr repeating layer 3 and a surface layer 4 made of a mixed material of CrC and DLC sequentially formed on a substrate 1. The overall thickness of the coating is 2.5-6 microns.
The Cr substrate layer 2 is formed on the surface of the workpiece where the coating needs to be formed, and the thickness of the Cr substrate layer 2 is 0.4-0.8 microns. The Cr base layer 2 is a Cr base layer whose hardness is increased stepwise from the inside to the outside.
The CrN + Cr repeating layer 3 is a CrN + Cr repeating layer formed by alternately arranging CrN layers and Cr layers and repeating the layers for multiple times. The CrN + Cr repeating layer 3 is formed on the surface of the Cr base layer. The thickness of each CrN layer is 0.2-0.3 micron, the thickness of the outermost Cr layer is 0.25-0.35 micron, and the thickness of the rest Cr layers is 0.02-0.08 micron.
The surface layer 4 made of a mixed material of CrC and DLC is formed on the surface of the CrN + Cr repeating layer 3. The thickness is 0.8-1.5 microns.
The invention relates to a production process of a wear-resistant, fatigue-resistant and repeated impact-resistant coating, which comprises the following production steps:
s1, cleaning the workpiece needing to generate the coating by a nine-tank cleaning production line;
s2, fixing the cleaned workpiece on a rotating frame, and putting the whole rotating frame into coating equipment;
s3, vacuumizing the coating equipment until the internal air pressure of the coating equipment is 1 x 10-5 mbar, heating the coating equipment to 140-;
S4 H+ion cleaning; h is introduced into the coating equipment2And Ar gas, the gas pressure is 2.0-9.0 x 10-4 mbar pure ion cleaning, H2 and Ar gas are ionized by utilizing a filament at the upper part in the furnace to generate glow, meanwhile, the auxiliary anode at the lower part is electrified to enable electrons to flow to the auxiliary anode, the workpiece is connected with a bias voltage of minus 10V to minus 30V, and the whole furnace cavity is filled with H+And Ar+， H+The ion energy and the oxide or organic matter which cannot be cleaned off from the surface of the workpiece generate chemical reaction, and the chemical reaction penetrates into the surface of the workpiece to fully clean the workpiece deeply;
S5 Ar+ion cleaning; close H2Ar gas is continuously input, the workpiece is connected with a bias voltage of minus 200V to minus 300V, and Ar generated by the filament and the auxiliary anode+Bombarding the surface of the workpiece by ion high energy, removing surface microscopic particles and activating the surface of the matrix, and providing a better and cleaner matrix for the gradient Cr layer;
s6 stopping heating by the heater, adjusting the rotating speed of the rotating frame to 2-4 r/min, adjusting the air pressure to 1.0-9.0 x 10-3mbar by inputting Ar gas, carrying out magnetron sputtering on a gradient Cr substrate layer on the surface of the workpiece, applying a climbing bias voltage on the workpiece, connecting the workpiece with a negative 20V bias voltage to a negative 200V bias voltage, gradually climbing the workpiece from the negative 20V bias voltage to the negative 200V bias voltage, wherein the climbing time is 3000 plus 4000 seconds, and the hardness gradient of the generated gradient Cr substrate layer is improved;
s7 magnetron sputtering to generate a CrN + Cr repeated layer; maintaining the rotating speed of the rotating frame and the air pressure in the furnace chamber unchanged, generating a CrN + Cr repeated layer by a magnetron sputtering process, wherein the CrN layer is generated on the Cr substrate layer generated in S6, then Cr is generated, and multiple layers are repeated to form the CrN + Cr repeated layer, and only Ar gas is introduced when the Cr layer is generatedThe time for generating Cr layer is 300-600 seconds after the element is connected with a bias voltage of minus 20V to minus 200V, and when the CrN layer is generated, in addition to the Ar gas, N is also introduced2Gas 100-;
s8 generating a CrC + DLC layer; regulating the rotating speed of the rotating frame to 2-4 rpm, and introducing C2H2And (3) gas and Ar gas, wherein the gas pressure is maintained at 1.0-9.0 x 10-3mbar, a magnetron sputtering method and a plasma enhanced chemical vapor deposition method are simultaneously carried out, a mixed layer of CrC + DLC is generated, the workpiece is connected with a bias voltage of 200V to 900V in the process, the power is 2-18kw, and the highest temperature is set to be 160 ℃.
In step S7, the CrN + Cr repeating layers are formed in an alternating structure of 9 CrN and 9 Cr layers, each of which has a thickness of 0.2 to 0.3. mu.m, the outermost Cr layer has a thickness of 0.25 to 0.35. mu.m, and the remaining Cr layers have a thickness of 0.02 to 0.08. mu.m.
In order to avoid annealing the workpiece due to overhigh temperature, in step S8, because the bias voltage of the workpiece is large, the temperature in the furnace easily exceeds the maximum temperature of 160 ℃, when the temperature in the furnace exceeds 160 ℃, the controller automatically controls the suspension process and the cooling furnace temperature, and the process is continued until the temperature in the furnace is lower than 160 ℃ until the required CrC + DLC layer is generated, wherein the CrC + DLC layer has a mixed structure, and the thickness of the CrC + DLC layer is 0.8-1.5 microns.
In light of the foregoing description of preferred embodiments in accordance with the invention, it is intended that the appended claims be interpreted as including all such alterations and modifications as fall within the true spirit and scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A wear-resistant, fatigue-resistant and repetitive impact-resistant coating, characterized in that: the Cr + Cr composite material comprises a Cr substrate layer, a CrN + Cr repeating layer and a surface layer made of a CrC and DLC mixed material, wherein the Cr + Cr repeating layer is formed by alternately arranging a CrN layer and a Cr layer and repeating the CrN + Cr layers for multiple times.
2. The wear-resistant, fatigue-resistant and repetitive impact-resistant coating of claim 1, wherein: the thickness of the Cr substrate layer is 0.4-0.8 micrometer.
3. The wear-resistant, fatigue-resistant and repetitive impact-resistant coating of claim 1, wherein: the CrN + Cr repeated layer comprises a plurality of CrN layers and a plurality of Cr layers, the thickness of each CrN layer is 0.2-0.3 micron, the thickness of the outermost Cr layer is 0.25-0.35 micron, the thickness of the rest Cr layers is 0.02-0.08 micron, and the surface layer made of the CrC and DLC mixed material is generated on the outer layer of the outermost Cr layer.
4. The wear-resistant, fatigue-resistant and repetitive impact-resistant coating of claim 3, wherein: the thickness of the surface layer made of the CrC and DLC mixed material is 0.8-1.5 microns.
5. A production process of a wear-resistant, fatigue-resistant and repeated impact-resistant coating is characterized by comprising the following steps: the method comprises the following production steps:
s1, cleaning the workpiece needing to generate the coating by a nine-tank cleaning production line;
s2, fixing the cleaned workpiece on a rotating frame, and putting the whole rotating frame into coating equipment;
s3, vacuumizing the coating equipment until the internal air pressure of the coating equipment is below 1 x 10-5 mbar, heating the coating equipment to 100-;
S4 H+ion cleaning; h is introduced into the coating equipment2And Ar gas with the air pressure of 2.0 x 10-4 mbar-9.0 x 10-3mbar, carrying out pure ion cleaning, ionizing H2 and Ar gas by using a filament at the upper part in the furnace to generate glow, electrifying the auxiliary anode at the lower part at the same time, allowing electrons to flow to the auxiliary anode, connecting the workpiece with the bias voltage of minus 10V to minus 30V, and filling H into the whole furnace cavity+And Ar+， H+The ion energy and the oxide or organic matter which can not be cleaned on the surface of the workpiece generate chemical reaction and go deep into the surface of the workpieceFully cleaning the workpieces in layers; ar (Ar)+The ions play a role in auxiliary ionization;
S5 Ar+ion cleaning; close H2Ar gas is continuously input, the workpiece is connected with a bias voltage of minus 200V to minus 300V, and Ar generated by the filament and the auxiliary anode+Bombarding the surface of the workpiece by ion high energy, removing surface microscopic particles and activating the surface of the matrix, and providing a better and cleaner matrix for the gradient Cr layer;
s6 stopping heating by the heater, adjusting the rotating speed of the rotating frame to 2-4 r/min, adjusting the air pressure to 1.0-9.0 x 10-3mbar by inputting Ar gas, carrying out magnetron sputtering on a gradient Cr substrate layer on the surface of the workpiece, applying a climbing bias voltage on the workpiece, connecting the workpiece with a negative 20V bias voltage to a negative 200V bias voltage, gradually climbing the workpiece from the negative 20V bias voltage to the negative 200V bias voltage, wherein the climbing time is 3000 plus 4000 seconds, and the hardness gradient of the generated gradient Cr substrate layer is improved;
s7 magnetron sputtering to generate a CrN + Cr repeated layer; maintaining the rotating speed of the rotating frame and the pressure in the furnace chamber unchanged, generating a CrN + Cr repeating layer by a magnetron sputtering process, wherein the CrN layer is generated on the Cr substrate layer generated in S6, then Cr is generated, and multiple layers are repeated to form the CrN + Cr repeating layer, when the Cr layer is generated, only Ar gas is introduced, the workpiece is connected with a bias voltage of negative 20V to negative 200V, the time for generating the Cr layer is 300-plus-600 seconds, when the CrN layer is generated, in addition to the Ar gas, N gas is introduced2Gas 100-;
s8 generating a CrC + DLC layer; regulating the rotating speed of the rotating frame to 2-4 rpm, and introducing C2H2And (3) gas and Ar gas, wherein the gas pressure is maintained at 1.0-9.0 x 10-3mbar, a magnetron sputtering method and a plasma enhanced chemical vapor deposition method are simultaneously carried out, a mixed layer of CrC + DLC is generated, the workpiece is connected with a bias voltage of 200V to 900V in the process, the power is 2-18kw, and the highest temperature is set to be 160 ℃.
6. The wear-resistant, fatigue-resistant and repetitive impact-resistant coating of claim 5, wherein: in step S7, the CrN + Cr repeating layers are formed as an alternating structure of 9 CrN and 9 Cr layers, each of which has a thickness of 0.2 to 0.3 μm, the outermost Cr layer has a thickness of 0.25 to 0.35 μm, and the remaining Cr layers have a thickness of 0.02 to 0.08. mu.m.
7. The wear-resistant, fatigue-resistant and repetitive impact-resistant coating of claim 5, wherein: in step S8, because the bias voltage of the workpiece is large, the temperature in the furnace is easy to exceed the maximum temperature of 160 ℃, when the temperature in the furnace exceeds 160 ℃, the controller automatically controls the suspension process and the cooling furnace temperature, and when the temperature in the furnace is lower than 160 ℃, the process is continued until the required CrC + DLC layer is generated, wherein the CrC + DLC layer is of a mixed structure, and the thickness of the CrC + DLC layer is 0.8-1.5 microns.
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