CN116219391A - AlN doped diamond-like coating process - Google Patents
AlN doped diamond-like coating process Download PDFInfo
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- CN116219391A CN116219391A CN202310513817.8A CN202310513817A CN116219391A CN 116219391 A CN116219391 A CN 116219391A CN 202310513817 A CN202310513817 A CN 202310513817A CN 116219391 A CN116219391 A CN 116219391A
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- 238000000576 coating method Methods 0.000 title claims abstract description 110
- 239000011248 coating agent Substances 0.000 claims abstract description 80
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 15
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 14
- 230000007704 transition Effects 0.000 claims abstract description 14
- 238000005137 deposition process Methods 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- -1 carbon ions Chemical class 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000035515 penetration Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000007373 indentation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification 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
- 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
- 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
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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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
- C23C14/3464—Sputtering using more than one target
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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
- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C23C16/303—Nitrides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—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 using microwave discharges
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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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
- 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
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Abstract
The invention provides an AlN doped diamond-like carbon coating process, which comprises the following steps: s1: providing a PECVD coating machine, configuring at least two groups of sputtering cathodes, wherein one group is a Cr target, the other group is an Al target, starting the sputtering Cr target, and depositing a Cr bottom layer and a CrC transition layer by a sputtering PVD process; s2: providing a microwave generator as an ion source, ionizing acetylene gas by a microwave plasma auxiliary technology, applying bias voltage on the CrC transition layer by a bias power supply to deposit a DLC coating, simultaneously introducing nitrogen and argon in the deposition process, starting a sputtering Al target, enabling the nitrogen and sputtered Al atoms to react preferentially to generate AlN and dope the AlN into the DLC coating, and enabling the AlN phase to be distributed in the DLC coating in an embedded mode. When the DLC coating obtained by the AlN doped diamond-like coating process is in stripping, an AlN phase in the DLC coating can be dissolved by adopting alkaline stripping liquid, so that the purpose of stripping is achieved.
Description
Technical Field
The invention relates to an AlN doped diamond-like coating process.
Background
In order to obtain more excellent physical properties, it is a common technique to dope certain specific elements or compounds during the deposition of diamond-like coating. Such as doping Cr, ti, si, cu, N, al, WC, moS 2 TiN, crC, and the like. The research on the chemical characteristics of the reinforced DLC coating capable of being de-coated is relatively few, and the condition of reworking and recycling of products is frequently encountered in the actual production process. Because DLC itself is inert, the stripping is achieved by dissolving or etching the underlying bonding layer, and for some DLC coatings over 5 μm thick, the stripping solution cannot penetrate, and the stripping process is difficult to perform. Through practical verification, doping DLC with some elements which are easy to be corroded or dissolved can promote the recoating process, such as Al, cu and the like. However, the doping of these elements seriously weakens the physical strength of DLC coatings, resulting in poor practical application.
In view of this, there is a need for improvements in existing diamond-like coating processes to address the above-described problems.
Disclosure of Invention
The invention aims to provide an AlN doped diamond-like carbon coating process for solving the problems that the existing DLC coating is difficult to decoat or poor in physical strength.
To achieve the above object, the present invention provides an AlN-doped diamond-like coating process comprising the steps of:
s1: providing a PECVD coating machine, wherein the PECVD coating machine is provided with at least two groups of sputtering cathodes, one group is a Cr target, the other group is an Al target, the sputtering Cr target is started, and a Cr bottom layer and a CrC transition layer are deposited by a sputtering PVD process;
s2: providing a microwave generator as an ion source, ionizing acetylene gas by a microwave plasma assisted technology, applying bias voltage on the CrC transition layer by a bias power supply to deposit a DLC coating, introducing nitrogen and argon in the process of deposition, starting a sputtering Al target by using a PECVD coating machine, enabling the nitrogen and sputtered Al atoms to react preferentially to generate AlN and dope the AlN into the DLC coating, and enabling an AlN phase to be distributed in the DLC coating in an embedded mode.
As a further improvement of the invention, in the step S1, the thickness of the Cr bottom layer is 0.2-0.5 μm, and the thickness of the CrC transition layer is 0.2-0.5 μm.
As a further improvement of the invention, in step S2, the argon partial pressure during DLC coating deposition is 0.2 to 0.5Pa.
As a further improvement of the invention, in step S2, the partial pressure of nitrogen during DLC coating deposition is 0.1 to 0.5Pa.
As a further improvement of the invention, in step S2, the partial pressure of acetylene gas during DLC coating is 0.5-2Pa.
As a further improvement of the present invention, in step S2, the molar ratio of N element to Al element is 1:1.
as a further improvement of the invention, the content of Al element in DLC coating is 2at% to 20at%.
As a further improvement of the invention, the Al target adopts a power control mode, 0.5-5KW, and is used for adjusting the proportion of Al elements.
As a further improvement of the invention, in step S2, acetylene gas is ionized, a bias power supply is controlled in a current mode in the DLC deposition process, and the pulse frequency of 40-80KHz and the duty ratio of 50% -90% are adopted.
The beneficial effects of the invention are as follows: according to the AlN doped diamond-like carbon coating process, the physical characteristics of the DLC coating are guaranteed by adding AlN into the DLC coating, and an AlN phase in the DLC coating can be dissolved by adopting alkaline stripping liquid when the DLC coating needs to be stripped, so that a channel penetrated by the stripping liquid in the DLC coating is formed and reaches a bottom layer structure, and chemical reaction is carried out with a Cr substrate layer to achieve the purpose of stripping; the microwave generator is used as an ion source, the generated microwave plasma can enhance ionization effect of argon, nitrogen and Al atoms, accelerate reaction of Al and N to generate AlN phase, avoid excessive Al atoms from depositing into the coating, and simultaneously can use lower bias voltage to reduce strong impact of a large amount of carbon ions and argon ions on the bias voltage power supply in the coating process.
Drawings
Fig. 1 is a flow chart of an AlN-doped diamond-like coating process of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art. In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
As shown in fig. 1, the AlN-doped diamond-like coating process of the present invention includes the steps of:
s1: providing a PECVD coating machine, wherein the PECVD coating machine is provided with at least two groups of sputtering cathodes, one group is a Cr target, the other group is an Al target, the sputtering Cr target is started, and a Cr bottom layer and a CrC transition layer are deposited by a sputtering PVD process; wherein the thickness of the Cr bottom layer is 0.2-0.5 mu m, and the thickness of the CrC transition layer is 0.2-0.5 mu m;
s2: providing a microwave generator as an ion source, ionizing acetylene gas by a microwave plasma assisted technology, applying bias voltage on the CrC transition layer by a bias power supply to deposit a DLC coating, introducing nitrogen and argon in the process of deposition, starting a sputtering Al target by using a PECVD coating machine, enabling the nitrogen and sputtered Al atoms to react preferentially to generate AlN and dope the AlN into the DLC coating, and enabling an AlN phase to be distributed in the DLC coating in an embedded mode.
AlN doped in the DLC coating can be dissolved and lost under the corrosion of alkaline stripping liquid, and a channel is provided for continuous penetration of the stripping liquid, so that the stripping effect is promoted, and the effect is more remarkable especially for DLC coatings with the thickness of more than 5 mu m.
In the step S2, the argon partial pressure in the DLC coating deposition process is 0.2-0.5Pa, the nitrogen partial pressure in the DLC coating deposition process is 0.1-0.5Pa, and the acetylene partial pressure in the DLC coating process is 0.5-2Pa.
In the step S2, the bias power supply is controlled in a current mode in the DLC deposition process, and the pulse frequency of 40-80KHz is adopted, and the duty ratio is 50% -90%. The microwave plasma generated by the PECVD coating machine can enhance ionization effect of argon, nitrogen and Al atoms, quicken reaction of Al and N to generate AlN phase, and avoid excessive Al atoms from depositing in the coating.
The microwave generator belongs to an external ion source, so that a lower bias voltage can be used in the process to reduce the strong impact of a large amount of carbon ions and argon ions on a bias voltage power supply in the coating process, for example, a process of enhancing by using pulse glow ions can generate high voltage and high current to damage the power supply. In this embodiment, the bias power supply applies a bias voltage of 100-200V.
In the step S2, the molar ratio of N element to Al element is 1:1, al can be converted into AlN as much as possible, the influence of Al element on conversion from sp3 bond to sp2 bond is reduced, and the DLC coating can keep higher hardness and elastic modulus. The content of Al element in the DLC coating is 2at% to 20at%.
The Al target of the PECVD coating machine adopts a power control mode, and 0.5-5KW is used for adjusting the proportion of Al elements.
In the DLC coating doped with AlN, the nitriding ratio of Al atoms can be controlled by adjusting the power of an Al target and the partial pressure of nitrogen, and a small amount of Al atoms can be reserved in the DLC layer to prepare the coating with the thickness of more than 50 mu m, and the bonding strength is not higher than the HF3 level. The hardness of the doped DLC layer is 1500-2800HV, and the elastic modulus is more than 100 GPa.
The internal stress of the coating can be reduced by doping AlN, the coating with high thickness can be obtained, and the technical effect that the thick DLC coating can be effectively de-coated is achieved.
In the process of the back coating, the thickened AlN doped DLC coating can adopt a process of reinforcing an oxidant by sodium hydroxide, and in order to improve the back coating efficiency, ultrasonic wave auxiliary back coating is preferred to improve the dissolution rate of an AlN phase.
The present invention provides the following three embodiments:
example 1
The PECVD coater is configured with a set of Cr targets and a set of Al targets. At the coating stage, a sputtering Cr target is firstly started, a 0.2 mu mCr bottom layer is sputtered and deposited, and a certain amount of acetylene is introduced to deposit a 0.2 mu mCrC transition layer. Then introducing acetylene with the partial pressure of 0.6Pa, nitrogen with the partial pressure of 0.1Pa and argon with the partial pressure of 0.3Pa, providing a microwave generator as an ion source, ionizing mixed gas by a microwave plasma auxiliary technology, starting a bias power supply, setting the pulse frequency to be 50KHz, setting the duty ratio to be 50%, and simultaneously starting the sputtering Al target power to be 2kw in an 8A constant current mode. The DLC deposition process is jointly affected by a microwave ion source and a sputtered Al cathode, and the bias voltage is maintained between 120 and 130V. The AlN doped DLC layer was finally deposited to a thickness of 5 μm. The AlN doped DLC coating obtained by the process has the hardness of 1800+/-100 HV, the elastic modulus of 160GPa (the measurement standard is ISO 14577-1-2015, the nanometer hardness meter can directly display the hardness and the elastic modulus) and the binding force of HF1 level (the cone-shaped diamond pressure head with the cone angle of 120 ℃ and the tip sphere radius of 0.2mm is utilized, the pressure head is vertically pressed into the surface of the coating under the force of 150Kg, the binding force grade is evaluated according to the damage state of the coating around the indentation according to the VDI 3198 standard), the doping amount of Al element is 12at%, and the molar ratio of N element to Al element is about 1:1, a step of; alN doped in the DLC coating can be dissolved and lost under the corrosion of alkaline stripping liquid, a channel is provided for continuous penetration of the stripping liquid, the stripping effect is promoted, and the coating is completely stripped after being soaked for 10 hours.
Example 2
The PECVD coater is configured with a set of Cr targets and a set of Al targets. At the coating stage, a sputtering Cr target is firstly started, a 0.3 mu mCr bottom layer is sputtered and deposited, and a certain amount of acetylene is introduced to deposit a 0.2 mu mCrC transition layer. Then introducing acetylene with the partial pressure of 1.2Pa, nitrogen with the partial pressure of 0.2Pa and argon with the partial pressure of 0.35Pa, providing a microwave generator as an ion source, ionizing mixed gas by a microwave plasma auxiliary technology, starting a bias power supply, setting the pulse frequency to 60KHz, setting the duty ratio to 60%, and simultaneously starting the sputtering Al target power to 1kw in a 9A constant current mode. The DLC deposition process is jointly affected by a microwave ion source and a sputtered Al cathode, and the bias voltage is maintained between 150 and 160V. The AlN doped DLC layer was finally deposited to a thickness of 10 μm. The AlN doped DLC coating obtained by the process has the hardness of 1900+/-100 HV, the elastic modulus of 170GPa (the measurement standard is ISO 14577-1-2015, the nanometer hardness meter can directly display the hardness and the elastic modulus) and the binding force of HF1 level (the cone-shaped diamond pressure head with the cone angle of 120 ℃ and the top sphere radius of 0.2mm is utilized, the pressure head is vertically pressed into the surface of the coating under the force of 150Kg, the binding force grade is evaluated according to the damage state of the coating around the indentation according to the VDI 3198 standard), the doping amount of Al element is 8at%, and the molar ratio of N element and Al element is about 1:1, a step of; alN doped in the DLC coating can be dissolved and lost under the condition of alkaline stripping liquid matched with ultrasonic waves, a channel is provided for continuous penetration of the stripping liquid, the stripping effect is promoted, and the coating is completely stripped after ultrasonic soaking for 2 hours.
Example 3
The PECVD coater is configured with a set of Cr targets and a set of Al targets. At the coating stage, a sputtering Cr target is firstly started, a 0.3 mu mCr bottom layer is sputtered and deposited, and a certain amount of acetylene is introduced to deposit a 0.2 mu mCrC transition layer. Then introducing acetylene with the partial pressure of 1.2Pa, nitrogen with the partial pressure of 0.2Pa and argon with the partial pressure of 0.3Pa, providing a microwave generator as an ion source, ionizing mixed gas by a microwave plasma auxiliary technology, starting a bias power supply, setting the pulse frequency to be 60KHz, the duty ratio to be 70%, and starting the sputtering Al target power to be 4kw in a 10A constant current mode. The DLC deposition process is jointly affected by a microwave ion source and a sputtered Al cathode, and the bias voltage is maintained between 100 and 105V. The AlN doped DLC layer was finally deposited to a thickness of 50. Mu.m. The AlN doped DLC coating obtained by the process has the hardness of 1500+/-100 HV, the elastic modulus of 105GPa (the measurement standard is ISO 14577-1-2015, the nanometer hardness meter can directly display the hardness and the elastic modulus) and the binding force of HF2 level (the cone-shaped diamond pressure head with the cone angle of 120 ℃ and the top sphere radius of 0.2mm is utilized, the pressure head is vertically pressed into the surface of the coating under 150Kg force, the binding force grade is evaluated according to the damage state of the coating around the indentation according to the VDI 3198 standard), the doping amount of the Al element is 18at%, and the molar ratio of the N element to the Al element is about 1:1, a step of; alN doped in the DLC coating can be dissolved and lost under the condition of alkaline stripping liquid matched with ultrasonic waves, a channel is provided for continuous penetration of the stripping liquid, the stripping effect is promoted, and the coating is completely stripped after ultrasonic soaking for 5 hours.
According to the AlN doped diamond-like carbon coating process, the AlN is added into the DLC coating to ensure the physical characteristics of the DLC coating, and the AlN phase in the DLC coating can be dissolved by adopting alkaline stripping liquid when the stripping is required, so that a channel penetrated by the stripping liquid in the DLC coating is formed and reaches a bottom structure, and the chemical reaction is carried out with the Cr substrate layer to achieve the purpose of stripping. The microwave generator is used as an ion source, the generated microwave plasma can enhance ionization effect of argon, nitrogen and Al atoms, accelerate reaction of Al and N to generate AlN phase, avoid excessive Al atoms from depositing into the coating, and simultaneously can use lower bias voltage to reduce strong impact of a large amount of carbon ions and argon ions on the bias voltage power supply in the coating process.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. An AlN doped diamond-like coating process, which is characterized in that: the AlN doped diamond-like coating process comprises the following steps:
s1: providing a PECVD coating machine, wherein the PECVD coating machine is provided with at least two groups of sputtering cathodes, one group is a Cr target, the other group is an Al target, the sputtering Cr target is started, and a Cr bottom layer and a CrC transition layer are deposited by a sputtering PVD process;
s2: providing a microwave generator as an ion source, ionizing acetylene gas by a microwave plasma assisted technology, applying bias voltage on the CrC transition layer by a bias power supply to deposit a DLC coating, introducing nitrogen and argon in the process of deposition, starting a sputtering Al target by using a PECVD coating machine, enabling the nitrogen and sputtered Al atoms to react preferentially to generate AlN and dope the AlN into the DLC coating, and enabling an AlN phase to be distributed in the DLC coating in an embedded mode.
2. An AlN-doped diamond-like coating process according to claim 1, wherein: in the step S1, the thickness of the Cr bottom layer is 0.2-0.5 mu m, and the thickness of the CrC transition layer is 0.2-0.5 mu m.
3. An AlN-doped diamond-like coating process according to claim 1, wherein: in step S2, the argon partial pressure in the DLC coating deposition process is 0.2Pa to 0.5Pa.
4. An AlN-doped diamond-like coating process according to claim 1, wherein: in step S2, the partial pressure of nitrogen in the DLC coating deposition process is 0.1Pa to 0.5Pa.
5. An AlN-doped diamond-like coating process according to claim 1, wherein: in the step S2, the partial pressure of acetylene gas in the DLC coating process is 0.5Pa to 2Pa.
6. An AlN-doped diamond-like coating process according to claim 1, wherein: in the step S2, the molar ratio of N element to Al element is 1:1.
7. an AlN-doped diamond-like coating process according to claim 1, wherein: the content of Al element in the DLC coating is 2at% to 20at%.
8. An AlN-doped diamond-like coating process according to claim 1, wherein: the Al target adopts a power control mode, 0.5-5KW, and is used for adjusting the proportion of Al elements.
9. An AlN-doped diamond-like coating process according to claim 1, wherein: the bias power supply is controlled in a current mode in the DLC deposition process, and the pulse frequency of 40-80KHz is adopted, and the duty ratio is 50% -90%.
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