CN116607130A - Method for increasing lubricity of plasma carbonized rubber surface - Google Patents
Method for increasing lubricity of plasma carbonized rubber surface Download PDFInfo
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- CN116607130A CN116607130A CN202310562516.4A CN202310562516A CN116607130A CN 116607130 A CN116607130 A CN 116607130A CN 202310562516 A CN202310562516 A CN 202310562516A CN 116607130 A CN116607130 A CN 116607130A
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- rubber
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- acetylene
- plasma
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000007704 transition Effects 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims description 100
- 239000000758 substrate Substances 0.000 claims description 76
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 60
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 23
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000010849 ion bombardment Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 9
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- 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
Abstract
The invention discloses a method for increasing lubricity of a plasma carbonized rubber surface, and relates to a method for increasing lubricity of a plasma carbonized rubber surface. The invention aims to solve the problems of large friction coefficient and poor wear resistance of the surface of a rubber matrix in the prior art. And C injection is carried out on the rubber surface, so that the film base binding force is improved, a transition layer containing Si is deposited, and finally a DLC film layer is deposited. The coefficient of friction of the rubber of the deposited diamond-like film was only 0.22. The invention is applied to the technical field of wear-resistant and antifriction treatment of rubber surfaces.
Description
Technical Field
The invention relates to a method for increasing lubricity of a plasma carbonized rubber surface.
Background
Rubber is widely used in the practical industry as a material with high elasticity. Rubber has been widely used in various engineering sealing systems, particularly in oil seals and O-rings, due to its good elasticity and insulation. However, the rubber has the characteristics of high elasticity and poor deformation capability against external force, and is easy to wear when working under high-speed and high-load conditions, so that the sealing system is invalid. Therefore, it is important to reduce friction and abrasion of rubber. The existing rubber surface treatment methods mainly comprise the technical methods of soaking, heat treatment, physical and chemical deposition, physical filling, chemical blending and the like. Wherein the physical chemical deposition technology is a modification method for the rubber surface by adopting a plasma enhanced chemical vapor deposition technology, and has wider application range.
However, the film deposited by the prior art has the following problems that 1) the film and the rubber substrate are not connected by chemical bonds, the film and the rubber substrate have poor binding force, and the film is easy to fall off. 2) The difference of physical properties between the rubber and the film layer is large, the deformation of the rubber under the stress is large, the hardness of the film layer is high, the deformation is small, and the film layer is easy to fall off under the stress. 3) The use is affected by the denaturation of the rubber surface caused by high temperature generated in the film deposition process. Therefore, the film deposited on the rubber must have a strong bond with the rubber matrix, sufficient elasticity to accommodate the large strains of the rubber under applied loads, low coefficient of friction and good abrasion resistance.
Disclosure of Invention
The invention aims to solve the problems of large friction coefficient and poor wear resistance of the surface of a rubber matrix in the prior art, and provides a method for increasing the lubricity of the surface of plasma carbonized rubber.
The invention relates to a method for increasing lubricity of a plasma carbonized rubber surface, which comprises the following steps:
1. placing the cleaned rubber substrate sample in a hollow cathode of a cage net of a vacuum chamber, wherein the vacuum chamber is taken as an anode and connected with an anode of a pulse power supply, and the cage net is connected with a cathode of the pulse power supply;
2. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 1-50 Pa, starting a pulse power supply, performing cage net hollow cathode discharge, and performing Ar ion bombardment cleaning on the cleaned rubber substrate sample for 10-200 min;
3. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and injecting carbon on the surface of rubber for 10-100min;
4. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage mesh hollow cathode discharge, and performing transition layer deposition on the surface of rubber for 10-100min;
5. and (3) introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and depositing a diamond-like carbon coating on the transition layer for 10-100min.
The invention adopts the plasma technology to carbonize the rubber surface and inject C, and deposits DLC film layer to reduce the friction coefficient of the rubber surface and increase the wear resistance of the rubber. Firstly, treating the rubber surface by adopting plasma, bombarding H element on the rubber surface, and forming a carbonized layer on the rubber surface. And then C injection is carried out on the rubber surface, so that the film base binding force is improved. And finally, depositing a DLC film layer.
The technical scheme of the invention has the following advantages:
1. under the action of the bombardment of plasma and high temperature, the functional groups on the rubber surface are changed, a large number of H atoms are sputtered off, so that the rubber surface is carbonized, the rubber surface is hardened, the hardness is improved, the diamond-like carbon film layer with higher hardness is supported, and the binding force between the film layer and a matrix is increased;
2. and C is injected on the surface of the rubber by plasma bombardment, and the injected C and the C on the surface of the substrate form a C-C bond, so that the binding force of the film layer and the matrix is improved.
3. The transitional layer is doped with Si, so that the DLC hardness is reduced, the problem of large hardness difference between the diamond-like carbon film layer and the rubber matrix is further solved, and the combination of the film layer and the matrix is enhanced.
4. According to the invention, the diamond-like carbon film layer with more graphite phase content is deposited on the surface of the rubber by a plasma enhanced chemical vapor deposition PECVD technology, on one hand, the low hardness can be better matched with the hardness of the rubber, and on the other hand, the graphite phase in the film layer can provide the function of a lubricant in the friction process between the rubber and a workpiece, so that the abrasion of the rubber is reduced.
In summary, the invention reduces the problem of large hardness difference between the diamond-like film and the rubber matrix by carbonizing and depositing the transition layer containing Si and depositing the diamond-like film with more graphite phase content on the rubber surface, improves the binding force between the film and the matrix, successfully deposits the diamond-like film on the rubber surface, increases the lubricity of the rubber surface, reduces the abrasion of the rubber, and ensures that the rubber friction coefficient of the deposited diamond-like film is only 0.22.
Drawings
FIG. 1 is a schematic view of a rubber plasma carbonized coating;
FIG. 2 is an uncarbonized coated rubber surface;
FIG. 3 is a view after carbonization coating of the rubber surface;
FIG. 4 is the coefficient of friction of an uncarbonized coated rubber film rubber ring; wherein a is the friction coefficient and b is the friction force;
FIG. 5 shows the friction coefficient after the rubber is carbonized and coated in example 1; where a is the coefficient of friction and b is the friction.
Detailed Description
The first embodiment is as follows: the method for increasing the lubricity of the surface of the plasma carbonized rubber according to the embodiment comprises the following steps:
1. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
2. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 1-50 Pa, starting a pulse power supply, performing cage net hollow cathode discharge, and performing Ar ion bombardment cleaning on the cleaned rubber substrate sample for 10-200 min;
3. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and injecting carbon on the surface of rubber for 10-100min;
4. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage mesh hollow cathode discharge, and performing transition layer deposition on the surface of rubber for 10-100min;
5. and (3) introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and depositing a diamond-like carbon coating on the transition layer for 10-100min.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the cleaning method of the rubber substrate sample in the first step comprises the following steps: and (3) flushing the surface of the rubber substrate sample by flowing ionized water, then placing the rubber substrate sample into an organic solvent for ultrasonic cleaning, flushing the rubber substrate sample by deionized water, and then drying the rubber substrate sample by high-purity nitrogen. The other features are the same as those of the first embodiment. Wherein the organic solvent selected should not react with the rubber.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: in the first step, the vacuum chamber is pumped to a vacuum degree of 1.0X10 -5 ～1.0×10 -1 Pa. The other embodiments are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: and the air pressure of the vacuum chamber in the second step and the third step is 5Pa to 15Pa. The other is the same as in one of the first to third embodiments.
Fifth embodiment: this embodiment differs from one to four embodiments in that: the pulse voltages of the second step, the third step, the fourth step and the fifth step are 100-10000V, the frequency is 100Hz-1000KHz, and the pulse width is 5-500us. The others are the same as in one to one fourth embodiments.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that: in the third step and the fifth step, the flow ratio of Ar to acetylene is 0.1-5:1. the other is the same as in one of the first to fifth embodiments.
Seventh embodiment: this embodiment differs from one of the first to sixth embodiments in that: in the third step and the fifth step, the flow ratio of Ar to acetylene is 1-3:1. the others are the same as in one of the first to sixth embodiments.
Eighth embodiment: this embodiment differs from one of the first to seventh embodiments in that: in the fourth step, the working gas is mixed gas of Ar, tetramethylsilane gas and acetylene; wherein the flow ratio of Ar, tetramethylsilane gas and acetylene is 5-40:1-5:5-100. The other is the same as in one of the first to seventh embodiments.
Detailed description nine: this embodiment differs from one to eight of the embodiments in that: flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20. the others are the same as in one to eight embodiments.
Detailed description ten: this embodiment differs from one of the embodiments one to nine in that: flow ratio of Ar, tetramethylsilane gas to acetylene 5:1:5. the other is the same as in one of the embodiments one to nine.
The following experiments were performed to verify the beneficial effects of the present invention:
example 1,
The method for increasing lubricity of the surface of the plasma carbonized rubber comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
5. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
6. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Example 2
The method for increasing lubricity of the surface of the plasma carbonized rubber comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 40min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
5. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
6. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Example 3
The method for increasing lubricity of the surface of the plasma carbonized rubber comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 -3 Pa; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon into the rubber at a pulse voltage of 8000V, a frequency of 800KHz, a pulse width of 100us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
5. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
6. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Example 4
The method for increasing lubricity of the surface of the plasma carbonized rubber comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
5. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 5:1:5, a step of;
6. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Example 5
The method for increasing lubricity of the surface of the plasma carbonized rubber comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
5. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
6. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 9Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, wherein the pulse voltage is 20000V, the frequency is 900KHz, the pulse width is 200us, and the time is 30min; wherein the flow ratio of Ar to acetylene is 1:2.
Comparative example 1
The method of the embodiment comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with a power supply anode, and the cage net is connected with a power supply cathode;
3. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1;
4. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
5. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Comparative example 2
The method of the embodiment comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with a power supply anode, and the cage net is connected with a power supply cathode;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 5Pa, then performing cage net hollow cathode discharge, performing transition layer deposition on the rubber surface, and performing pulse voltage 7000V, frequency 800KHz, pulse width 100us and time 10min; wherein the working gas is a mixed gas of Ar, tetramethylsilane gas and acetylene; flow ratio of Ar, tetramethylsilane gas to acetylene 20:1:20, a step of;
5. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 6Pa, then performing cage mesh hollow cathode discharge, depositing a diamond-like coating on the transition layer, and applying a pulse voltage of 10000V, a frequency of 900KHz, a pulse width of 200us and a time of 30min; wherein the flow ratio of Ar to acetylene is 1:1.
Comparative example 3
The method of the embodiment comprises the following steps:
1. washing the surface dirt of the rubber substrate sample by flowing ionized water, then putting the rubber substrate sample into absolute ethyl alcohol for ultrasonic cleaning, then washing the rubber substrate sample cleanly by deionized water, and drying the rubber substrate sample by high-purity nitrogen to obtain a cleaned rubber substrate sample;
2. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber, and vacuumizing to 1.0X10 - 3 Pa; wherein the vacuum chamber is used as an anode and connected with a power supply anode, and the cage net is connected with a power supply cathode;
3. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 10Pa, starting a pulse power supply, performing cage net hollow cathode discharge, performing Ar ion bombardment cleaning on the cleaned rubber substrate sample, wherein the pulse voltage is 1000V, the frequency is 200KHz, the pulse width is 50us, and the time is 20min;
4. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 10Pa, then performing cage mesh hollow cathode discharge, injecting carbon on the surface of rubber, and injecting carbon with a pulse voltage of 6000V, a frequency of 600KHz, a pulse width of 50us and a time of 10min; wherein the flow ratio of Ar to acetylene is 2:1.
FIG. 1 is a schematic view of a carbonized film layer on a rubber surface. Fig. 2 shows the surface of the rubber without the carbonized coating film, fig. 3 shows the morphology of the carbonized coating film of the rubber obtained in example 1, and fig. 3 shows that the surface of the rubber has a film layer deposited thereon, and it is observed under a microscope that the surface of the rubber has a film layer deposited on the protrusions and depressions.
In summary, the plated samples of examples 1-5 and comparative examples 1-3 were tested and the results showed that a DLC film layer with better properties was prepared on the rubber. The wear resistance of the film layer is tested by adopting a group standard T/CI 003-2023 and a friction and wear testing machine (MS-T3001), a 304 stainless steel ball with the diameter of 5mm is selected as a counter-grinding pair, the load is 10N, the rotating speed is 36r/min, and the testing time is 1200min. The test results are shown in Table 1.
Table 1 example film friction coefficient
| Examples | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Coefficient of friction | 0.21 | 0.22 | 0.22 | 0.23 | 0.22 | 0.33 | 0.31 | 0.62 |
As is clear from Table 1, the coefficient of friction of the rubber after coating was substantially about 0.22, the coefficients of friction of comparative example 1 and comparative example 2 were 0.33 and 0.31, respectively, and the coefficient of friction of comparative example 3 was 0.62, indicating that the film layer acted to reduce the abrasion of the rubber surface. FIG. 4 shows the friction coefficient of rubber rings of rubber film without carbonized coating, and FIG. 4 shows that the friction coefficient of rubber rings without carbonized coating is about 1.0; FIG. 5 shows the friction coefficient after the rubber is carbonized and coated in example 1; as shown in fig. 5, the friction coefficient of the film layer stabilized around 0.2 after a wear test for a long time and a large load of 20 hours.
TABLE 2 film adhesion test results
Method for determining adhesion by ASTM D3359-02 tape test-X method, as shown in Table 2, the test results of sample adhesion in the examples show that the adhesion of the film is between 5A and 4A, indicating that the film and the substrate can be firmly bonded, and the injection of C enhances the bonding strength between the substrate and the film.
Claims (10)
1. A method for increasing lubricity of a plasma carbonized rubber surface is characterized by comprising the following steps:
1. placing the cleaned rubber substrate sample in a cage net of a vacuum chamber; wherein the vacuum chamber is used as an anode and connected with the positive electrode of the pulse power supply, and the cage net is connected with the negative electrode of the pulse power supply;
2. introducing Ar gas into the vacuum chamber until the air pressure of the vacuum chamber is 1-50 Pa, starting a pulse power supply, performing cage net hollow cathode discharge, and performing Ar ion bombardment cleaning on the cleaned rubber substrate sample for 10-200 min;
3. introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and injecting carbon on the surface of rubber for 10-100min;
4. introducing working gas into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage mesh hollow cathode discharge, and performing transition layer deposition on the surface of rubber for 10-100min;
5. and (3) introducing mixed gas of Ar gas and acetylene into a vacuum chamber, wherein the air pressure of the vacuum chamber is 1-50 Pa, then performing cage net hollow cathode discharge, and depositing a diamond-like carbon coating on the transition layer for 10-100min.
2. The method for increasing lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the cleaning method of the rubber substrate sample in the step one is: and (3) flushing the surface of the rubber substrate sample by flowing ionized water, then placing the rubber substrate sample into an organic solvent for ultrasonic cleaning, flushing the rubber substrate sample by deionized water, and then drying the rubber substrate sample by high-purity nitrogen.
3. A method for increasing lubricity of a plasma carbonized rubber surface as described in claim 1The method is characterized in that in the first step, the vacuum chamber is pumped to a vacuum degree of 1.0X10 -5 ～1.0×10 -1 Pa。
4. The method for increasing lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the air pressure of the vacuum chamber in the second and third steps is 5 to 15Pa.
5. The method for increasing the lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the pulse voltages of the second, third, fourth and fifth steps are 100 to 10000V, the frequency is 100Hz to 1000KHz, and the pulse width is 5 to 500us.
6. The method for increasing lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the flow ratio of Ar to acetylene in the third and fifth steps is 0.1 to 5:1.
7. the method for increasing lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the flow ratio of Ar to acetylene in step three and step five is 1-3:1.
8. the method for increasing lubricity of a surface of a plasma carbonized rubber according to claim 1, wherein the working gas in the fourth step is a mixed gas of Ar, tetramethylsilane gas and acetylene; wherein the flow ratio of Ar, tetramethylsilane gas and acetylene is 5-40:1-5:5-100.
9. The method for increasing the lubricity of a plasma carbonized rubber surface according to claim 8, wherein the flow ratio of Ar, tetramethylsilane gas to acetylene is 20:1:20.
10. the method for increasing the lubricity of a plasma carbonized rubber surface according to claim 8, wherein the flow ratio of Ar, tetramethylsilane gas to acetylene is 5:1:5.
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| CN115627457B (en) * | 2022-08-22 | 2024-04-23 | 哈尔滨工业大学 | Preparation method of DLC film layer on copper surface |
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