CN113463062A - Deposition method of diamond-like carbon-based coating on inner wall of bent pipe - Google Patents
Deposition method of diamond-like carbon-based coating on inner wall of bent pipe Download PDFInfo
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- CN113463062A CN113463062A CN202110820226.6A CN202110820226A CN113463062A CN 113463062 A CN113463062 A CN 113463062A CN 202110820226 A CN202110820226 A CN 202110820226A CN 113463062 A CN113463062 A CN 113463062A
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- 238000000576 coating method Methods 0.000 title claims abstract description 51
- 239000011248 coating agent Substances 0.000 title claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 238000000151 deposition Methods 0.000 title claims abstract description 37
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052786 argon Inorganic materials 0.000 claims abstract description 32
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000077 silane Inorganic materials 0.000 claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 238000007654 immersion Methods 0.000 claims abstract description 5
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 21
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 210000002381 plasma Anatomy 0.000 description 14
- 239000010963 304 stainless steel Substances 0.000 description 6
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- -1 chemical engineering Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
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- 238000005086 pumping Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 238000004381 surface treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a method for depositing a diamond-like carbon-based coating on the inner wall of a bent pipe, which comprises the following steps: the method comprises the steps of loading a bent pipe workpiece into a vacuum cavity of a plasma chemical vapor deposition chamber after polishing and cleaning; argon is introduced, and argon plasma bombardment cleaning and preheating are carried out on the inner wall of the bent pipe; introducing silane, performing in-situ plasma immersion on the inner wall of the bent pipe, and injecting silicon element, and depositing to obtain a silicon middle layer with the thickness of 50-1000 nm; and fourthly, taking the bent pipe as a cathode, applying negative pulse bias voltage on the pipe, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene with different flow rates, and finally obtaining the silicon-doped diamond-like carbon-based coating with the thickness of 10-20 mu m on the inner wall of the bent pipe. The method is simple and has stable process.
Description
Technical Field
The invention relates to the field of surface modification of inner walls of pipe workpieces, in particular to a method for depositing a diamond-like carbon-based coating on the inner wall of a bent pipe.
Background
The elbow pipe series pipeline fitting product is widely applied to the construction and inspection requirements of industries such as petroleum, chemical engineering, medicine, electric power, aerospace, fire fighting, military industry, metallurgy, shipbuilding, gas, nuclear power, urban construction, water heating, environmental protection and the like. The quality of the elbow directly affects the structural rationality, safety and reliability of the products of these industries. Generally, in the process of machining the bent pipe, the bent pipe has various defects in different degrees due to process conditions, operation and the like, and the bent pipe is usually used in a working condition environment with high strength and coexistence of corrosion and friction, and the defects often become initial failure points and diffuse around, so that the safety of the product is directly influenced, and the service life of the bent pipe is also reduced.
Surface treatment techniques are an effective means of reducing the impact of these defects on the performance of the bend. Such as thermal spraying, electroplating, and build-up welding. However, the technology for spraying the inner wall coating has requirements on the inner diameter of the pipeline, for example, an inner hole spray gun of advanced plasma spraying equipment is adopted to spray a wear-resistant coating on the inner wall of the pipeline, and the technology is suitable for the pipeline with the length less than 600mm and the inner diameter more than 160 mm. In addition, the plasma spraying coating has low bonding strength and is not suitable for the condition of assembling and welding short pipelines into long pipelines, and the local high-temperature coating is easy to fall off during welding. Both supersonic flame spraying and electric arc spraying are only suitable for larger diameter pipes. The method for preparing the coating on the large-size bent pipe workpiece by thermal spraying disclosed by the Chinese patent CN104611665A needs to adopt a specially designed bent pipe spraying tool for clamping and fixing, and has poor universality and complex process; in addition, it is only applicable to elbow members having a radius of curvature of 2m or more, and the elbow is usually 0.5 m or less. A decrease in the radius of the bend means a decrease in its radius of curvature and also indicates an increase in bending stress in the radial direction; in addition, the thinner the pipe diameter is, the smaller the axial curvature radius which can be achieved in the bending process is, and the bending stress is increased, so that the deposition difficulty of the diamond-like carbon film is greatly increased.
Diamond-like carbon based coatings are often used for surface protection materials due to their high mechanical strength, high chemical inertness, low coefficient of friction and wear rate, and excellent corrosion resistance. The diamond-like carbon based coating on the inner wall of the straight pipe is reported to have high hardness and excellent corrosion resistance and tribological properties, and the service life of the pipeline is effectively prolonged. The technical difficulty of the deposition of the diamond-like carbon-based coating on the inner wall of the bent pipe is as follows: firstly, the bent pipe has double stress (axial and radial) so that the growth difficulty of the diamond-like carbon-based coating is greatly increased; secondly, the flow direction of the introduced argon, silane and acetylene gas mixture changes by 180 degrees from the gas inlet to the gas outlet along the pipeline, and the flow velocity of the gas is gradually reduced due to the resistance of the outer pipe wall, so that the density of the generated plasma is not uniformly distributed in the pipe, and the uniform deposition of the diamond-like carbon-based coating is difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for depositing the diamond-like carbon-based coating on the inner wall of the bent pipe, which is simple and stable in process.
In order to solve the problems, the invention provides a method for depositing a diamond-like carbon-based coating on the inner wall of a bent pipe, which comprises the following steps:
the method comprises the steps of loading a bent pipe workpiece into a vacuum cavity of a plasma chemical vapor deposition chamber after polishing and cleaning;
argon is introduced, and argon plasma bombardment cleaning and preheating are carried out on the inner wall of the bent pipe;
introducing silane, performing in-situ plasma immersion on the inner wall of the bent pipe, and injecting silicon element, and depositing to obtain a silicon middle layer with the thickness of 50-1000 nm;
and fourthly, taking the bent pipe as a cathode, applying negative pulse bias voltage on the pipe, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene with different flow rates, and finally obtaining the silicon-doped diamond-like carbon-based coating with the thickness of 10-20 mu m on the inner wall of the bent pipe.
The shape of the elbow pipe in the step includes a right-angle pipe and a U-shaped pipe, and the diameter of the elbow pipe is 10-100 mm.
The method comprises the following steps that in the step two, the cleaning condition is that 5-10 kV negative pulse bias voltage is applied to the bent pipe, the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the glow discharge vacuum pressure is 4-8 Pa, and the cleaning time is 10-120 min.
And the deposition condition of the silicon intermediate layer in the step three is that 10-20 kV negative pulse bias voltage is applied to the inner wall of the bent pipe, the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the silane flow is 50-150 sccm, the glow discharge vacuum pressure is 10-20 Pa, and the silicon element injection time is 10-60 min.
The deposition conditions of the silicon-doped diamond-like carbon-based coating in the fourth step include that negative pulse bias voltage is applied to the pipe fitting and is 500-1500V, the pulse frequency is 100-1500 Hz, the argon gas flow is 100-500 sccm, the silane gas flow is 50-150 sccm, the acetylene gas flow is 50-500 sccm, the glow discharge vacuum pressure is 12-20 Pa, and the deposition time is 30-300 min.
Compared with the prior art, the invention has the following advantages:
1. the invention utilizes the high-voltage direct-current pulse power supply to remove impurities, oil stain molecules, an oxidation layer and activate Ar plasmas on the inner wall of the tube, thereby improving the interface state and being beneficial to enhancing the film-substrate binding force.
2. The invention utilizes the high-energy ion implantation and hollow cathode high-density plasma chemical vapor deposition integrated technology to deposit a Si intermediate layer between the substrate and the coating starting from the structure of the deposited coating; the multilayer structure is used for relieving interface mismatch and reducing the internal stress of the coating by changing the component deposition compressive stress and tensile stress of the introduced gas precursor; the deposition rate of the coating is reduced through process optimization, so that the deposition of the diamond-like carbon-based coating on the inner wall of the bent pipe is realized. On the other hand, the uniform filling of the gas in the U-shaped pipe is realized by increasing the flow rate of the precursor gas and the pumping speed of the dry pump.
3. The invention can form uniform and stable glow plasma with high density in the tube, and uniformly deposit the diamond-like carbon-based coating with high mechanical strength, low friction coefficient, excellent wear resistance and excellent corrosion resistance under lower vacuum degree, thereby solving the technical problem that the service life of the bent tube is greatly shortened due to cracks and defects generated by bending in the processing process. Meanwhile, the problem that the diamond-like carbon-based coating is difficult to deposit due to double stress of the bent pipe is solved by designing a multilayer structure with alternating compressive stress and tensile stress and optimizing the process.
4. By adopting the method, the diamond-like carbon-based coating with high strength, low friction, high wear resistance and high corrosion resistance is successfully deposited on the inner wall of the bent pipe, and the problem of deposition of the diamond-like carbon-based coating with small curvature radius on the inner wall of the bent pipe is solved.
5. The method is simple, flexible in operation, stable in process and good in repeatability. And no special fixing device is needed, the parts are convenient to replace, the processing cost is low, and the popularization and the application are easy.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows an ultra-thick diamond-like carbon-based coating with an inner diameter of 30 mm, a tube wall thickness of 1.5mm, a curvature radius of 80 mm and a tube height of 130 mm on the inner wall of a 304 stainless steel U-shaped tube obtained by the invention.
FIG. 2 shows a diamond-like carbon-based coating with an inner diameter of 45 mm, a tube wall thickness of 1.5mm, a curvature radius of 85 mm and a tube height of 150 mm on the inner wall of a 304 stainless steel U-shaped tube obtained by the method.
FIG. 3 shows a diamond-like carbon-based coating with an inner diameter of 15 mm and a tube wall thickness of 1.5mm, which is obtained by the invention, on the inner wall of a 304 stainless steel right-angle tube.
FIG. 4 shows a diamond-like carbon-based coating on the inner wall of a cast iron U-shaped pipe, which is obtained by the invention, and has the inner diameter of 15 mm, the pipe wall thickness of 1.5mm, the curvature radius of 65 mm and the pipe height of 200 mm.
Detailed Description
A method for depositing a diamond-like carbon-based coating on the inner wall of a bent pipe comprises the following steps:
the method comprises the steps of polishing and cleaning a bent pipe workpiece, and then loading the bent pipe workpiece into a vacuum cavity of a plasma chemical vapor deposition chamber. The deposition chamber has the technical functions of plasma immersion injection, hollow cathode plasma chemical vapor deposition and the like.
The shape of return bend includes right angle pipe and U type pipe, and its diameter is 10~100 mm. The elbow pipe is made of stainless steel, cast iron, aluminum and other common metals.
And introducing argon, and performing argon plasma bombardment cleaning and preheating on the inner wall of the bent pipe. Namely: and applying a negative pulse bias voltage of 5-10 kV to the bent pipe, wherein the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the glow discharge vacuum pressure is 4-8 Pa, and the cleaning time is 10-120 min. The operator can select the cleaning time and the process parameters according to the elbow material and the surface state.
Introducing silane, performing in-situ plasma immersion on the inner wall of the bent pipe, and injecting silicon element, and depositing to obtain a silicon middle layer with the thickness of 50-1000 nm.
Wherein: the deposition condition of the silicon intermediate layer is that a negative pulse bias voltage of 10-20 kV is applied to the inner wall of the bent pipe, the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the silane flow is 50-150 sccm, the glow discharge vacuum pressure is 10-20 Pa, and the silicon element injection time is 10-60 min. The material of the bent pipe is properly selected according to the difference of the interface between the material of the bent pipe and the diamond-like carbon-based coating.
The key technology of high-voltage direct-current pulse power supply for injecting silicon element into the inner wall of the tube and high-energy ion injection can obviously improve the bonding strength of the subsequent diamond-like carbon-based coating and the substrate on the inner wall of the tube.
And fourthly, taking the bent pipe as a cathode, applying negative pulse bias voltage on the pipe, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene with different flow rates, and finally obtaining the silicon-doped diamond-like carbon-based coating with the thickness of 10-20 mu m on the inner wall of the bent pipe.
Wherein: the deposition conditions of the silicon-doped diamond-like carbon-based coating include that negative pulse bias voltage is applied to the pipe fitting and is 500-1500V, the pulse frequency is 100-1500 Hz, the argon flow is 100-500 sccm, the silane flow is 50-150 sccm, the acetylene flow is 50-500 sccm, the glow discharge vacuum pressure is 12-20 Pa, and the deposition time is 30-300 min.
Step two ~ the introduction of precursor gas must increase gas flow and gas extraction speed and keep pressure invariable in the return bend.
Example 1
The U-shaped pipe fitting is a 304 stainless steel pipe with the inner diameter of 30 mm, the pipe wall thickness of 1.5mm, the curvature radius of 80 mm and the pipe height of 130 mm.
The method comprises the steps of ultrasonically cleaning a U-shaped pipe by using acetone and absolute ethyl alcohol, placing the cleaned U-shaped pipe into a vacuum cavity of a plasma chemical vapor deposition chamber, and vacuumizing the vacuum cavity to 3 x 10-3Pa。
And introducing argon gas of 300 sccm, applying negative pulse bias voltage of 6 kV on the tube wall by using a high-voltage direct-current pulse power supply, keeping the pressure of a vacuum cavity at 5 Pa, and performing argon plasma cleaning on the inner wall of the tube for 40 min and preheating the inner wall of the tube.
Thirdly, introducing argon of 300 sccm and silane of 100 sccm, adjusting the negative pulse bias voltage to 15 kV, adjusting the high-voltage direct current pulse frequency to 1.5 kHz, keeping the pressure of the vacuum cavity to 15 Pa, and injecting silicon element into the inner wall of the tube for 30 min.
Fourthly, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene of 300 sccm and 100 sccm, applying a negative bias voltage of 650V on the pipe fitting by using a low-voltage direct-current pulse power supply, keeping the pulse frequency at 500Hz and the vacuum cavity pressure at 20 Pa and 13 Pa, and finally obtaining a diamond-like carbon-based coating with the thickness of about 10 microns on the inner wall of the pipe after deposition for 180 min, as shown in FIG. 1.
Example 2
The pipe fitting is a 304 stainless steel pipe with the inner diameter of 45 mm, the pipe wall thickness of 1.5mm, the curvature radius of 85 mm and the pipe height of 150 mm.
The steps are the same as those of embodiment 1.
Thirdly, introducing 200 sccm argon gas and 50 sccm silane, adjusting the negative pulse bias voltage to 15 kV, adjusting the high-voltage direct current pulse frequency to 1.5 kHz, keeping the vacuum cavity pressure to be 20 Pa, and injecting silicon element into the inner wall of the tube for 20 min.
Fourthly, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene of 150 sccm and 50 sccm, applying a negative bias voltage of 800V on the pipe by using a low-voltage direct-current pulse power supply, keeping the pulse frequency at 1000 Hz and the vacuum cavity pressure at 20 Pa and 13 Pa, and finally obtaining a diamond-like carbon-based coating with the thickness of about 15 mu m on the inner wall of the pipe after 240 min of deposition, as shown in FIG. 2.
Example 3
The pipe fitting is a 304 stainless steel right-angle pipe with the inner diameter of 15 mm and the pipe wall thickness of 1.5 mm.
The steps are the same as those of embodiment 1.
Thirdly, introducing argon gas of 400 sccm and silane of 150 sccm, adjusting the negative pulse bias voltage to 15 kV, adjusting the high-voltage direct current pulse frequency to 1.5 kHz, keeping the pressure of the vacuum cavity to 10 Pa, and injecting silicon element into the inner wall of the tube for 30 min.
Fourthly, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene of 450 sccm and 150 sccm, applying a negative bias voltage of 650V on the pipe fitting by using a low-voltage direct-current pulse power supply, keeping the pulse frequency at 100 Hz and the vacuum cavity pressure at 20 Pa and 13 Pa, and finally obtaining a diamond-like carbon-based coating with the thickness of about 6 microns on the inner wall of the pipe after deposition for 120 min, as shown in FIG. 3.
Example 4
The pipe fitting is a cast iron pipe with the inner diameter of 15 mm, the pipe wall thickness of 1.5mm, the curvature radius of 65 mm and the pipe height of 200 mm.
The steps are the same as those of embodiment 1.
Thirdly, introducing argon gas of 400 sccm and silane of 150 sccm, adjusting the negative pulse bias voltage to 15 kV, adjusting the high-voltage direct current pulse frequency to 1.5 kHz, keeping the pressure of the vacuum cavity to 10 Pa, and injecting silicon element into the inner wall of the tube for 30 min.
Fourthly, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene of 450 sccm and 150 sccm, applying a negative bias voltage of 650V on the pipe fitting by using a low-voltage direct-current pulse power supply, keeping the pulse frequency at 100 Hz and the vacuum cavity pressure at 20 Pa and 13 Pa, and finally obtaining a diamond-like carbon-based coating with the thickness of about 6 microns on the inner wall of the pipe after deposition for 120 min, as shown in FIG. 4.
A friction wear testing machine is adopted to evaluate the performance of the ultra-thick diamond-like carbon-based coating on the inner wall of the bent pipe obtained in the embodiment 1-4, the friction condition adopts a ball-disk reciprocating mode, the reciprocating sliding stroke is 5mm, the reciprocating frequency is 5Hz, the normal load is 5N, the friction couple is a GCr15 steel ball with phi 6 mm, and the testing environment is atmosphere.
And (4) evaluating the mechanical property of the diamond-like carbon-based coating on the inner wall of the bent pipe by adopting a nano-indenter.
And (3) evaluating the electrochemical corrosion behavior of the inner wall of the elbow in 3.5 wt% NaCl solution by using an electrochemical workstation, wherein the sweep speed of the polarization test is 10 mV/s, and the amplitude of the impedance is 10 mV.
The test results are shown in Table 1.
TABLE 1 test results
As can be seen from table 1: inner wall of elbowThe friction coefficient of the diamond-like carbon-based coating is stabilized at 0.06-0.04, and the wear rate is as low as 2.5 multiplied by 10-7The hardness is above 12 GPa, and the corrosion current density is reduced by two orders of magnitude compared with that of a bare substrate.
Claims (5)
1. A method for depositing a diamond-like carbon-based coating on the inner wall of a bent pipe comprises the following steps:
the method comprises the steps of loading a bent pipe workpiece into a vacuum cavity of a plasma chemical vapor deposition chamber after polishing and cleaning;
argon is introduced, and argon plasma bombardment cleaning and preheating are carried out on the inner wall of the bent pipe;
introducing silane, performing in-situ plasma immersion on the inner wall of the bent pipe, and injecting silicon element, and depositing to obtain a silicon middle layer with the thickness of 50-1000 nm;
and fourthly, taking the bent pipe as a cathode, applying negative pulse bias voltage on the pipe, keeping the flow rates of argon and silane unchanged, alternately introducing acetylene with different flow rates, and finally obtaining the silicon-doped diamond-like carbon-based coating with the thickness of 10-20 mu m on the inner wall of the bent pipe.
2. The method for depositing a diamond-like carbon-based coating on the inner wall of an elbow pipe according to claim 1, wherein the method comprises the following steps: the shape of the elbow pipe in the step includes a right-angle pipe and a U-shaped pipe, and the diameter of the elbow pipe is 10-100 mm.
3. The method for depositing a diamond-like carbon-based coating on the inner wall of an elbow pipe according to claim 1, wherein the method comprises the following steps: the method comprises the following steps that in the step two, the cleaning condition is that 5-10 kV negative pulse bias voltage is applied to the bent pipe, the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the glow discharge vacuum pressure is 4-8 Pa, and the cleaning time is 10-120 min.
4. The method for depositing a diamond-like carbon-based coating on the inner wall of an elbow pipe according to claim 1, wherein the method comprises the following steps: and the deposition condition of the silicon intermediate layer in the step three is that 10-20 kV negative pulse bias voltage is applied to the inner wall of the bent pipe, the pulse frequency is 1-2 kHz, the argon flow is 100-500 sccm, the silane flow is 50-150 sccm, the glow discharge vacuum pressure is 10-20 Pa, and the silicon element injection time is 10-60 min.
5. The method for depositing a diamond-like carbon-based coating on the inner wall of an elbow pipe according to claim 1, wherein the method comprises the following steps: the deposition conditions of the silicon-doped diamond-like carbon-based coating in the fourth step include that negative pulse bias voltage is applied to the pipe fitting and is 500-1500V, the pulse frequency is 100-1500 Hz, the argon gas flow is 100-500 sccm, the silane gas flow is 50-150 sccm, the acetylene gas flow is 50-500 sccm, the glow discharge vacuum pressure is 12-20 Pa, and the deposition time is 30-300 min.
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