CN113529048A - An ultra-high-speed deposition method of high-bonding ultra-thick DLC coating on the surface of piston rings - Google Patents
An ultra-high-speed deposition method of high-bonding ultra-thick DLC coating on the surface of piston rings Download PDFInfo
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- 238000000151 deposition Methods 0.000 title claims abstract description 93
- 238000000576 coating method Methods 0.000 title claims abstract description 55
- 239000011248 coating agent Substances 0.000 title claims abstract description 51
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 102
- 230000008021 deposition Effects 0.000 claims abstract description 57
- 229910052786 argon Inorganic materials 0.000 claims abstract description 51
- 239000007789 gas Substances 0.000 claims abstract description 41
- 239000010410 layer Substances 0.000 claims abstract description 38
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910000077 silane Inorganic materials 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 36
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000004140 cleaning Methods 0.000 claims abstract description 29
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 230000007704 transition Effects 0.000 claims abstract description 17
- 239000002346 layers by function Substances 0.000 claims abstract description 14
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 238000007654 immersion Methods 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 229910001018 Cast iron Inorganic materials 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000005121 nitriding Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 21
- 238000001816 cooling Methods 0.000 abstract description 7
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- 230000000694 effects Effects 0.000 description 7
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- 238000004381 surface treatment Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- VNTLIPZTSJSULJ-UHFFFAOYSA-N chromium molybdenum Chemical compound [Cr].[Mo] VNTLIPZTSJSULJ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910001141 Ductile iron Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 238000005137 deposition process Methods 0.000 description 1
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- 238000000635 electron micrograph Methods 0.000 description 1
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- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
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- 239000010687 lubricating oil Substances 0.000 description 1
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- 229910000734 martensite Inorganic materials 0.000 description 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
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- 238000007747 plating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 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
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- 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
- C23C16/24—Deposition of silicon 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
- C23C16/458—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 characterised by the method used for supporting substrates in the reaction chamber
- C23C16/4582—Rigid and flat substrates, e.g. plates or discs
- C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
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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
- C23C16/515—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 pulsed discharges
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
本发明涉及一种活塞环表面高结合力超厚DLC涂层的超高速沉积方法，该方法包括以下步骤：⑴将活塞环经脱脂、清洗后进行活塞环夹装；将夹好的活塞环放入样品台上，在夹好的活塞环的外围且样品台上放置一个同轴的辅助阴极，密闭抽真空；⑵通入氩气，然后对辅助阴极施加负脉冲偏压，对活塞环表面进行去氧化物清洗和活化；⑶通入氩气和硅烷的混合气体，采用等离子体浸没注入方式进行沉积，得到梯度硅支撑层；⑷通过逐步增加乙炔气流量进行沉积，得到梯度硅掺杂DLC过渡层；⑸通过周期交替调节乙炔的气流量在活塞环表面进行周期交替沉积，得到多层硅掺杂DLC功能层，经自然降温，去真空，取出所述活塞环即可。本发明工艺简单、稳定易于工业化生产。
The invention relates to an ultra-high-speed deposition method for a high-bonding and ultra-thick DLC coating on the surface of a piston ring. The method comprises the following steps: (1) degreasing and cleaning the piston ring, and then clamping the piston ring; Put a coaxial auxiliary cathode on the periphery of the clamped piston ring and on the sample stage, and seal the vacuum; De-oxidation cleaning and activation; (3) A mixed gas of argon and silane is introduced, and the plasma immersion injection method is used for deposition to obtain a gradient silicon support layer; (4) For deposition by gradually increasing the flow rate of acetylene gas, a gradient silicon-doped DLC transition is obtained. (5) Periodically alternate deposition on the surface of the piston ring by adjusting the gas flow of acetylene alternately to obtain a multi-layer silicon-doped DLC functional layer. After natural cooling, the vacuum is removed, and the piston ring can be taken out. The process of the invention is simple, stable and easy for industrial production.
Description
Technical Field
The invention relates to the field of surface treatment, in particular to an ultra-high-speed deposition method of a high-bonding-force ultra-thick DLC coating on the surface of a piston ring.
Background
With the upgrading of emission standards, the popularization of engine types of the national V and the national VI, and the current surface treatment processes such as nitriding, chromium plating and the like can not meet increasingly strict environmental protection requirements gradually. Generally, the main approaches for energy saving and emission reduction of engines are: the engine lightweight technology, the new energy automobile technology and the part low friction technology. However, the traditional surface treatment technology (such as nitriding, electroplating, etc.) of the parts does not pay attention to the lubricating property of the system; and the single surface treatment technology of the parts is difficult to ensure the effective lubrication and the stable service of the parts in the all-working-condition environment. Therefore, the friction pair loss on the surfaces of the parts is reduced, the lubricating performance is improved, and the essence is to develop a composite surface treatment (coating) technology with good friction reduction and wear resistance under all working conditions. Therefore, the wear-resistant carbon-based solid lubricating film technology represented by diamond-like carbon is an indispensable key new technology for meeting the requirement of engine emission reduction.
Generally, the film layer applied to the commercial automobile is used under special working conditions of heavy load or super-long time high load operation and the like, the coating is thin, the wearing risk exists, the required film layer can reach 10-50 mu m, and some film layers are even thicker. Moreover, experiments prove that the thicker the diamond-like carbon film is, the more excellent the performances such as wear resistance and the like are. And also increases the difficulty of the object penetrating thick coatings and reduces the chance of crack propagation to the film-substrate interface during frictional wear. However, the diamond-like thin film has high in-film stress due to high disorder of its own structure, and in continuous growth, due to the surface physical properties of the thin film: such as surface binding energy, surface conductivity and the like, so that the deposition process of the thin film is changed, and the ultra-thick film is difficult to deposit. Moreover, the DLC coating has large difference with the substrate in thermal expansion coefficient and other properties, which results in poor film-substrate adhesion.
In addition, the existing technology for depositing the DLC thick film on the surface of the piston ring mostly uses Cr as a transition layer, or firstly performs low-temperature plasma nitridation treatment on a substrate and then combines a physical vapor deposition technology to deposit the DLC thick film, but the bonding force between the coating and the substrate of a sample prepared by the method is generally low, the phenomenon of coating falling off can occur in the long-term service process, and the deposition rate of the existing ultra-thick DLC coating technology is relatively slow. The method disclosed by the Chinese patent CN 108359938 has the defect that the whole furnace time for depositing the ultra-thick DLC coating with the thickness of about 20-30 mu m needs more than 30 hours, the large-batch preparation cannot be realized at one time, and the rapid industrialization is difficult to realize.
In conclusion, the diamond-like carbon film has high internal stress due to the highly disordered structure and is difficult to deposit an ultra-thick film; the DLC coating and the piston ring have different properties such as thermal expansion coefficient and the like, so that the bonding force between the coating and the piston ring is poor; the bonding force between the DLC thick film deposited by the traditional physical vapor deposition technology and a piston ring is generally low; in addition, the deposition rate of the existing piston ring ultra-thick DLC coating technology is relatively slow, and the one-time large-batch preparation cannot be realized, so that the rapid industrialization is difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing the ultrahigh-speed deposition method of the high-bonding-force and ultra-thick DLC coating on the surface of the piston ring, which has simple process, stability and easy industrial production.
In order to solve the problems, the ultrahigh-speed deposition method of the high-bonding-force super-thick DLC coating on the surface of the piston ring, disclosed by the invention, comprises the following steps of:
the method comprises the steps of performing piston ring clamping after degreasing and cleaning of a piston ring; placing the clamped piston ring on a sample table in a vacuum chamber of a plasma enhanced chemical vapor deposition device, then placing a coaxial auxiliary cathode on the periphery of the clamped piston ring and the sample table, connecting the auxiliary cathode with the negative electrode of a direct current pulse power supply, and hermetically vacuumizing to 1.5 multiplied by 10-3 Pa；
Argon is introduced between the auxiliary cathode and the piston ring through an air inlet on the sample table, then negative pulse bias is applied to the auxiliary cathode, and oxide removal cleaning and activation are carried out on the surface of the piston ring;
thirdly, introducing mixed gas of argon and silane, and depositing by adopting a plasma immersion injection mode to obtain a gradient silicon supporting layer with the thickness of 50-1000 nm;
fourthly, keeping the flow velocity same as that of the argon and the silane in the step three, and gradually increasing the flow of acetylene gas to deposit to obtain a gradient silicon-doped DLC transition layer with the thickness of 1-4 mu m;
fifthly, keeping the flow velocity same as that of argon and silane in the step three, periodically and alternately depositing on the surface of the piston ring by periodically and alternately adjusting the flow of acetylene to obtain a multilayer silicon-doped DLC functional layer with the total thickness of 8-35 mu m, naturally cooling, removing vacuum, and taking out the piston ring.
The piston ring is made of one of cast iron, stainless steel and nitrided stainless steel.
The distance between a piston ring and the auxiliary cathode in the step is 60-200 mm.
The piston rings in the step are one group or a plurality of groups.
The method is characterized in that the cleaning conditions in the step II include that argon flow is 100-400 sccm, vacuum degree is 1-3 Pa, negative bias is 5-10 kV, pulse frequency is 1-2 kHz, and continuous cleaning time is 20-60 min.
The deposition condition of the gradient silicon support layer in the step three is that argon gas flow is 100-400 sccm, silane gas flow is 10-100 sccm, vacuum degree is 10-20 Pa, negative bias variation range is 10-20 kV, pulse frequency is 1-2 kHz, negative bias is changed every 2-10 min, and deposition time is 20-60 min.
The deposition condition of the gradient silicon-doped DLC transition layer in the step four is that the flow of argon is 100-400 sccm, the flow of silane is 10-100 sccm, the flow of acetylene is 0-300 sccm, the vacuum degree is 2-6 Pa, the negative bias is 0.5-1.2 kV, the pulse frequency is 0.1-2 kHz, the flow of acetylene is changed once every 5-20 min, and the deposition time is 30-120 min.
The deposition conditions of the multilayer silicon-doped DLC functional layer in the step are that the flow of argon is 100-400 sccm, the flow of silane is 10-100 sccm, the flow of acetylene is 0-300 sccm, the vacuum degree is 2-6 Pa, the negative bias is 0.5-1.5 kV, the pulse frequency is 0.1-2 kHz, the flow of acetylene is changed once every 1.5-20 min, and the total deposition time is 60-480 min.
The deposition rate in the step three-step fifthly is 70-120 nm/min.
Compared with the prior art, the invention has the following advantages:
1. the invention adds a coaxial auxiliary cathode at the periphery of the piston ring, introduces precursor gas and applies negative bias to form hollow cathode effect between the piston ring and the auxiliary cathode, thereby generating high-density plasma to realize ultra-high-speed deposition of DLC coating.
2. The invention is introduced with argon gas, applies negative pulse bias voltage to the auxiliary cathode, and utilizes the generated argon plasma to remove oxide on the surface of the piston ring for cleaning and activating so as to improve the interface state of the piston ring and enhance the bonding force between the diamond-like coating and the surface of the piston ring.
3. According to the invention, mixed gas of argon and silane is introduced, a high-voltage direct-current pulse power supply is used for applying negative pulse bias to the auxiliary cathode to generate high-energy plasma, the bonding strength of the DLC coating and the interface of a piston ring is improved by changing the silicon supporting layer with negative bias deposition gradient hardness, and the film-substrate bonding force is improved.
4. The invention realizes the transition from the pure silicon supporting layer to the silicon-doped DLC functional layer by keeping the flow rates of argon and silane constant and gradually increasing the flow rate of acetylene gas so as to enhance the combination.
5. The method adopts the hollow cathode effect, adopts a low-voltage and low-current plasma discharge mode, directly ionizes the precursor gas at a lower temperature, and deposits the precursor gas on the surface of a piston ring at an ultrahigh speed, the furnace finishing time of depositing the ultra-thick DLC coating with the thickness of more than 30 mu m only needs about 6.5 hours, and the deposition efficiency is improved by more than 4 times on the original basis; in addition, a plurality of groups of piston ring samples can be clamped at one time, so that the one-time large-batch preparation of the ultra-thick DLC coating on the surface of the piston ring is realized, and the method is suitable for batch production.
6. The piston ring with the super-thick DLC coating coated on the surface, which is prepared by the invention, has the thickness of more than 30 mu m, uniform and compact alternative multilayer structure of the coating section, smooth surface and no microscopic defect.
7. The piston ring coated with the ultra-thick DLC coating on the surface has excellent film-substrate binding force, and the Lc1 is about 45-55N, and the Lc2 is about more than 60N. The bonding force of the Si transition layer is higher than that of the Cr transition layer (20-35N) and the nitriding treatment (35-40) by about 10N (Chinese patent CN 108359938).
8. The super-thick DLC coating deposited by the method has excellent mechanical properties, the microhardness of the super-thick DLC coating is about 11-17 GPa, and the elastic modulus of the super-thick DLC coating is about 200-240 GPa. Also has ultrahigh toughness. Meanwhile, the wear-resistant lubricating oil has high film-substrate bonding strength, has excellent wear-resistant and lubricating effects under dry friction conditions and actual working conditions, effectively prolongs the service life of a piston ring, and ensures the stable operation of an engine.
When the load is 10N, the dry friction coefficient is about 0.10-0.11, the surface is almost not abraded, and the dual GCr15 steel ball is seriously abraded. The dry friction coefficient is lower than that of the nitriding/titanium-doped DLC composite coating (0.13-0.15) on the surface of the piston ring. When the actual working condition of a piston ring and the boron cast iron matched pair of the cylinder sleeve material are simulated for opposite grinding, the friction coefficient is unstable and is about 0.18 when the piston ring is preloaded at 50N, the friction coefficient is reduced to about 0.15 when the piston ring is loaded to 100N, the edge of a coating is not peeled off and almost has no abrasion when the piston ring is subjected to opposite grinding, and the abrasion of the matched pair is obvious, so that the coating is high in hardness and good in abrasion resistance.
9. The preparation method provided by the invention is simple and feasible in preparation process, green and environment-friendly, does not cause pollution to the environment, and is suitable for industrial production.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a top view of an apparatus for obtaining ultra-thick DLC coatings on a set of piston ring surfaces in accordance with the present invention.
Fig. 2 is a front view of a device for obtaining ultra-thick DLC coatings on a set of piston ring surfaces according to the invention.
FIG. 3 is a top view of the apparatus for obtaining ultra-thick DLC coatings on multiple piston ring surfaces in accordance with the present invention.
FIG. 4 is a schematic cross-sectional structure of an ultra-thick DLC coating on the surface of a piston ring according to the present invention.
FIG. 5 is an electron micrograph and a partial enlarged view of a cross section of an ultra-thick DLC coating on a functional surface of a cast iron piston ring in example 1 of the present invention.
FIG. 6 is an electron microscope photograph of the surface of the cross section of the ultra-thick DLC coating on the functional surface of the cast iron piston ring in example 1 of the present invention.
In the figure: 1-a vacuum chamber; 2-an auxiliary cathode; 3-a piston ring; 4-sample stage; 5-an air inlet; 6-DC pulse power supply.
Detailed Description
An ultra-high speed deposition method of a high-bonding-force ultra-thick DLC coating on the surface of a piston ring comprises the following steps:
as shown in fig. 1 to 3, a piston ring 3 is degreased and cleaned and then clamped; placing the clamped piston ring 3 on a sample table 4 in a vacuum chamber 1 of a plasma enhanced chemical vapor deposition device, then placing a coaxial auxiliary cathode 2 on the periphery of the clamped piston ring 3 and the sample table 4, connecting the auxiliary cathode 2 with the negative electrode of a direct current pulse power supply 6, sealing and vacuumizing to 1.5 multiplied by 10-3 Pa。
Wherein: the material of the piston ring 3 is one of cast iron, stainless steel, and nitrided stainless steel.
The distance between the piston ring 3 and the auxiliary cathode 2 is 60-200 mm.
The piston rings 3 are one or more groups.
Secondly, argon is introduced between the auxiliary cathode 2 and the piston ring 3 through an air inlet 5 on the sample table 4, then negative pulse bias voltage is applied to the auxiliary cathode 2, and the surface of the piston ring 3 is subjected to oxide removal cleaning and activation by utilizing the generated argon plasma. The cleaning conditions include argon flow of 100-400 sccm, vacuum degree of 1-3 Pa, negative bias of 5-10 kV, pulse frequency of 1-2 kHz, and continuous cleaning time of 20-60 min.
Thirdly, introducing mixed gas of argon and silane, and depositing by adopting a plasma immersion injection mode. The deposition conditions include argon flow of 100-400 sccm, silane flow of 10-100 sccm, vacuum degree of 10-20 Pa, negative bias variation range of 10-20 kV, pulse frequency of 1-2 kHz, negative bias variation every 2-10 min, and deposition time of 20-60 min. The gradient silicon supporting layer with the hardness range of 6-13 GPa and the thickness of 50-1000 nm is obtained by changing the deposition negative bias.
And fourthly, maintaining the same flow rate of argon and silane in the step three, and performing deposition by gradually increasing the flow of acetylene. The deposition conditions include 100-400 sccm of argon gas flow, 10-100 sccm of silane gas flow, 0-300 sccm of acetylene gas flow, 2-6 Pa of vacuum degree, 0.5-1.2 kV of negative bias voltage, 0.1-2 kHz of pulse frequency, once acetylene gas flow change every 5-20 min, and deposition time of 30-120 min. Thereby realizing the transition from the pure silicon supporting layer to the silicon-doped DLC layer and obtaining the gradient silicon-doped DLC transition layer with the thickness of 1-4 mu m.
And fifthly, keeping the flow velocity same as that of argon and silane in the step three, periodically and alternately adjusting the flow rate of acetylene, and periodically and alternately depositing high-density plasma generated by utilizing the hollow cathode effect on the surface of the piston ring 3. The deposition conditions include 100-400 sccm of argon gas flow, 10-100 sccm of silane gas flow, 0-300 sccm of acetylene gas flow, 2-6 Pa of vacuum degree, 0.5-1.5 kV of negative bias voltage, 0.1-2 kHz of pulse frequency, change of the acetylene gas flow once every 1.5-20 min, and total deposition time of 60-480 min. And after the deposition is finished, obtaining a multi-layer silicon-doped DLC functional layer with the total thickness of 8-35 mu m, naturally cooling, removing vacuum, and taking out the piston ring 3.
Step three, the deposition rate in the step five is 70-120 nm/min.
As shown in FIG. 4, the invention deposits a gradient silicon supporting layer a, a gradient silicon-doped DLC transition layer b and a plurality of periodically alternating silicon-doped DLC functional layers c on a piston ring 3 substrate in sequence, wherein the plurality of functional layers of silicon-doped DLC are formed by alternately arranging silicon-doped DLC with high silicon content (c 1) and low silicon content (c 2) for a plurality of times of repeated generation. Wherein: the support layer and the transition layer can be flexibly selected according to the mechanical property difference between the piston ring 3 substrate and the DLC functional layer.
Example 1
Piston ring made of chromium molybdenum nodular cast ironThe main parameters are as follows: a sheet opening ring-shaped part with the diameter of 140 mm, the diameter width of 4 mm and the thickness of 2.5 mm. The chemical components (mass fraction%) of which are 3.0-3.5C, 2.6-2.9 Si, 0.6-0.8 Mn,<0.1 P、<0.03S, 0.1-0.45 Cr, 0.1-0.45 Mo, typical MgDisabled person0.021, typical Re 0.032 and Fe for the rest. Mechanical properties: hardness is 105-112 HRB, bending strength is 940-1600 MPa, and elastic modulus is 150-180 GPa. The diameter of the auxiliary cathode 2 is 300 mm. The specific operation steps are as follows:
the method comprises the steps of degreasing and cleaning the piston ring 3, and then clamping the piston ring; placing the clamped sample in a vacuum chamber 1 of a plasma enhanced chemical vapor deposition device, coaxially placing an auxiliary cathode 2 connected with a power supply cathode as shown in figures 1-2, and then hermetically vacuumizing to obtain a local vacuum degree of 1.5 × 10-3 Pa, special disposable gloves must be worn in the whole clamping process to ensure the surface cleaning of the piston ring 3.
The cleaning process is as follows: introducing 150 sccm argon gas between the piston ring 3 and the auxiliary cathode 2, maintaining the required vacuum degree in the glow discharge process to be stable at 1.5 Pa, applying negative pulse bias voltage (bias voltage is 6 kV, pulse frequency is 1.5 kHz) to the piston ring 3, and cleaning and activating the argon plasma generated by the hollow cathode effect for 60 min.
Depositing a gradient silicon support layer: the flow rates of the introduced argon and silane are respectively 150 sccm and 50 sccm, the required vacuum degree in the glow discharge process is kept stable at 15 Pa, the initial negative bias voltage is 10 kV, the deposition voltage is changed every 6 min, each time, the deposition voltage is changed by 2 kV, and the duration is 30 min.
Fourthly, depositing a gradient silicon-doped DLC transition layer: keeping the flow of argon and silane as same as the step three, stabilizing the vacuum degree at 3.1 Pa, applying negative bias of 0.85 kV, pulse frequency of 1.5 kHz, introducing acetylene with initial flow of 30 sccm, changing the deposition voltage every 8 min, changing 30 sccm each time, and lasting for 40 min.
Fifthly, depositing silicon doped functional layers with alternate periods: the flow rates of silane and argon are respectively 50 sccm and 150 sccm and are constant, the bias voltage is 0.85 kV, the pulse frequency is 1.5 kHz, the flow rates of silane and acetylene (150 sccm and 50 sccm) are alternately adjusted, the vacuum degrees are respectively corresponding to 3.1 Pa and 2.3 Pa, the deposition time is 16 min and 4 min, and the total deposition time is 400 min after 20 cycles of repeated deposition; and after the coating is finished, naturally cooling, removing vacuum, and taking out the piston ring 3.
An electron microscope photograph and a partial enlarged view of a cross section of the super-thick DLC coating on the functional surface of the cast iron piston ring, as shown in FIG. 5, and an electron microscope photograph of the surface of the super-thick DLC coating on the functional surface of the cast iron piston ring, as shown in FIG. 6, were obtained using a field emission scanning electron microscope (FESEM, JSM-6701F, Japan). As can be seen from the figure, the coating has a uniform and dense multilayer structure, the bonding between layers is tight, the micro-crack propagation and extension are avoided, and the total thickness is about 31 μm; the surface appearance is uniform and compact, and no microscopic defects exist.
Example 2
Taking a tempered martensitic stainless steel (according with ISO 6621-3 fine grade MC 65) piston ring, wherein the main parameters are as follows: a sheet opening ring-shaped part with the diameter of 120 mm, the diameter width of 4 mm and the thickness of 2.5 mm. The chemical composition (mass fraction,%) is 0.50-0.75C, <1.00 Si, <1.00 Mn, < 0.045P, < 0.04S, 11.00-15.00 Cr, <0.6 Mo, and the rest is Fe. The hardness is about 300-400 HV, the typical elastic modulus is 200 GPa, and the transverse rupture strength is about 1128 MPa. The diameter of the auxiliary cathode 2 is 300 mm. The specific operation steps are as follows:
the method comprises the steps of degreasing and cleaning the piston ring 3, and then clamping the piston ring; placing the clamped sample in a vacuum chamber 1 of a plasma enhanced chemical vapor deposition device, coaxially placing an auxiliary cathode 2 connected with a power supply cathode as shown in figures 1-2, and then hermetically vacuumizing to obtain a local vacuum degree of 1.5 × 10-3 Pa, special disposable gloves must be worn in the whole clamping process to ensure the surface cleaning of the piston ring 3.
The cleaning process is as follows: introducing argon gas of 200 sccm between the piston ring 3 and the auxiliary cathode 2, keeping the required vacuum degree in the glow discharge process stable at 1.5 Pa, applying negative pulse bias voltage (bias voltage is 6 kV, pulse frequency is 1.5 kHz) to the piston ring 3, and cleaning and activating by using argon plasma generated by the hollow cathode effect, wherein the whole process lasts for 60 min.
Depositing a gradient silicon support layer: the flow rates of the introduced argon and silane are respectively 150 sccm and 50 sccm, the required vacuum degree in the glow discharge process is kept stable at 15 Pa, the initial negative bias voltage is 10 kV, the deposition voltage is changed every 10 min, each time, the deposition voltage is changed by 1 kV, and the duration is 50 min.
Fourthly, depositing a gradient silicon-doped DLC transition layer: keeping the flow of argon and silane as same as the step three, stabilizing the vacuum degree at 6.0 Pa, applying negative bias of 0.65 kV, pulse frequency of 1.5 kHz, introducing acetylene with initial flow of 20 sccm, changing the deposition voltage every 5 min, changing 20 sccm each time, and keeping the duration of 30 min.
Fifthly, depositing silicon doped functional layers with alternate periods: the flow rates of silane and argon are respectively 50 sccm and 150 sccm and are constant, the bias voltage is 0.65 kV, the pulse frequency is 1.5 kHz, the flow rates of silane and acetylene (120 sccm and 50 sccm) are alternately adjusted, the vacuum degrees are respectively corresponding to 6.0 Pa and 4.2 Pa, the deposition time is 12 min and 4 min, and the total deposition time is 480 min after 30 repeated deposition cycles; and after the coating is finished, naturally cooling, removing vacuum, and taking out the piston ring 3.
Example 3
Taking a nitrided hot martensite stainless steel piston ring, wherein the main parameters are as follows: a sheet opening ring-shaped part with the diameter of 120 mm, the diameter width of 4 mm and the thickness of 2.5 mm. The hardness is about 700-800 HV. The auxiliary cathode 2 has a diameter of 320 mm. The specific operation steps are as follows:
the method comprises the steps of degreasing and cleaning the piston ring 3, and then clamping the piston ring; placing the clamped sample in a vacuum chamber 1 of a plasma enhanced chemical vapor deposition device, coaxially placing an auxiliary cathode 2 connected with a power supply cathode as shown in figures 1-2, and then hermetically vacuumizing to obtain a local vacuum degree of 1.5 × 10-3 Pa, special disposable gloves must be worn in the whole clamping process to ensure the surface cleaning of the piston ring 3.
The cleaning process is as follows: introducing 100 sccm argon gas between the piston ring 3 and the auxiliary cathode 2, maintaining the required vacuum degree in the glow discharge process to be stable at 3.0 Pa, applying negative pulse bias voltage (bias voltage is 6 kV, pulse frequency is 1.5 kHz) to the piston ring 3, and cleaning and activating the argon plasma generated by the hollow cathode effect for 20 min.
Depositing a gradient silicon support layer: the flow rates of the introduced argon and silane are respectively 100 sccm and 50 sccm, the required vacuum degree in the glow discharge process is kept to be stable at 10 Pa, the initial negative bias voltage is 15 kV, the deposition voltage is changed every 10 min, each time, the deposition voltage is changed by 1 kV, and the duration is 50 min.
Fourthly, depositing a gradient silicon-doped DLC transition layer: keeping the flow of argon and silane as same as the step three, stabilizing the vacuum degree at 3.1 Pa, applying negative bias of 1.0 kV, pulse frequency of 1.5 kHz, introducing acetylene with initial flow of 25 sccm, changing the deposition voltage every 5 min, changing 25 sccm each time, and keeping the duration of 30 min.
Fifthly, depositing silicon doped functional layers with alternate periods: the flow rates of silane and argon are respectively 50 sccm and 100 sccm and are constant, the bias voltage is 1.0 kV, the pulse frequency is 1.0 kHz, the flow rates of silane and acetylene (150 sccm and 50 sccm) are alternately adjusted, the vacuum degrees are respectively corresponding to 3.1 Pa and 2.7 Pa, the deposition time is 20 min and 5 min, and the total deposition time is 500 min after 20 cycles of repeated deposition; and after the coating is finished, naturally cooling, removing vacuum, and taking out the piston ring 3.
Example 4
Different from the embodiments 1 to 3, the embodiment describes a one-time large-batch preparation method of an ultra-thick DLC coating with high bonding force, wear resistance and low friction characteristics on the surface of a piston ring, and multiple groups of piston ring samples can be clamped at one time.
Taking a chromium-molybdenum nodular cast iron piston ring, wherein the main parameters are as follows: a thin plate opening ring-shaped part with the diameter of 100 mm, the diameter width of 4 mm and the thickness of 2.5 mm. The diameter of the auxiliary cathode 2 is 200 mm. The specific operation steps are as follows:
the method comprises the steps of degreasing and cleaning the piston ring 3, and then clamping the piston ring; placing the clamped sample in a vacuum chamber of a plasma enhanced chemical vapor deposition device1, coaxially placing an auxiliary cathode 2, placing 4 sets of piston rings (as shown in figure 3) on a sample table 4 according to the method, connecting with a power supply cathode, and then sealing and vacuumizing, wherein the required local vacuum degree is 1.5 × 10-3 Pa, special disposable gloves must be worn in the whole clamping process to ensure the surface cleaning of the piston ring 3.
The cleaning process is as follows: introducing argon gas of 300 sccm between the piston ring 3 and the auxiliary cathode 2, keeping the required vacuum degree in the glow discharge process stable at 1.5 Pa, applying negative pulse bias voltage (the bias voltage is 6 kV, the pulse frequency is 1.5 kHz) to the piston ring, and cleaning and activating the argon plasma generated by the hollow cathode effect for 60 min.
Depositing a gradient silicon support layer: the flow rates of the introduced argon and silane are respectively 300 sccm and 80 sccm, the required vacuum degree in the glow discharge process is kept to be stable at 10 Pa, the initial negative bias voltage is 10 kV, the deposition voltage is changed every 6 min, 2 kV is changed every time, and the duration is 30 min.
Fourthly, depositing a gradient silicon-doped DLC transition layer: keeping the flow of argon and silane as same as the step three, stabilizing the vacuum degree at 3.1 Pa, applying negative bias of 0.85 kV, pulse frequency of 1.5 kHz, introducing acetylene with initial flow of 40 sccm, changing the deposition voltage once every 10 min, changing 40 sccm each time, and keeping the duration of 60 min.
Fifthly, depositing silicon doped functional layers with alternate periods: the flow rates of silane and argon are respectively 80 sccm and 300 sccm and are constant, the bias voltage is 0.85 kV, the pulse frequency is 1.5 kHz, the flow rates of silane and acetylene (240 sccm and 80 sccm) are alternately adjusted, the vacuum degrees are respectively corresponding to 3.1 Pa and 2.3 Pa, the deposition time is 16 min and 4 min, and the total deposition time is 400 min after 20 cycles of repeated deposition; and after the coating is finished, naturally cooling, removing vacuum, and taking out the piston ring 3.
Claims (9)
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