CN106784915A - A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating - Google Patents
A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating Download PDFInfo
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- CN106784915A CN106784915A CN201611082741.4A CN201611082741A CN106784915A CN 106784915 A CN106784915 A CN 106784915A CN 201611082741 A CN201611082741 A CN 201611082741A CN 106784915 A CN106784915 A CN 106784915A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/505—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 radio frequency discharges
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating, it is related to the preparation method of stainless steel surfaces anticorrosive coat.The invention solves the problems that existing stainless steel material is not corrosion-resistant in the sour environment of fuel cell, the problem in life-span more long cannot be possessed in high-temperature fuel cell.Method：First, stainless steel surfaces pretreatment；2nd, graphene oxide solution is prepared；3rd, the preset graphene oxide layer of stainless steel surfaces；4th, the graphene oxide layer to stainless steel surfaces is processed；5th, stainless steel surfaces vertical-growth original position Graphene, that is, complete the preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.The present invention is used for a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.
Description
Technical field
The present invention relates to the preparation method of stainless steel surfaces anticorrosive coat.
Background technology
Today's society, environment and energy problem have become the focus of research, and exploitation uses renewable, clean environment firendly new
The key that the energy even more wherein develops.Therefore, fuel cell technology is increasingly widely applied in the world, fuel
Battery is a kind of TRT that fuel and oxidant efficiently can be converted into electric energy by electrode reaction.This dress
Put energy density high, toggle speed is fast, cleanliness without any pollution.Bipolar plates are important functional units in fuel cell, it is necessary to have
Reacting gas, afflux are conductive, membrane electrode are supported, for reacting gas provides the functions such as passage.Stainless steel material is inexpensive due to it,
High intensity, easy processing shaping, thermal conductivity is good etc., and advantage turns into one of bipolar plate material that current fuel cell is commonly used.
But, stainless steel material is not corrosion-resistant in the sour environment of fuel cell, cannot possess more long in high-temperature fuel cell
Life-span.If it is possible to by relatively simple method, be surface-treated to metal, anticorrosion, the antioxygen of material are improved
Change ability, then have significant help to stainless steel material further application in a fuel cell.
The content of the invention
The invention solves the problems that existing stainless steel material is not corrosion-resistant in the sour environment of fuel cell, in high-temperature fuel electricity
The problem in life-span more long cannot be possessed in pond, and a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating is provided.
A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating is followed the steps below：
First, stainless steel surfaces pretreatment：
Stainless steel is polished with the abrasive paper for metallograph of 600 mesh, 1000 mesh and 1500 mesh successively, then by the stainless steel after polishing
It is cleaned by ultrasonic 20min respectively with acetone, absolute ethyl alcohol and deionized water successively, obtains pretreated stainless steel；
2nd, graphene oxide solution is prepared：
Graphene oxide is dissolved in deionized water, the graphene oxide that concentration is 1mg/mL~10mg/mL is obtained molten
Liquid；
3rd, the preset graphene oxide layer of stainless steel surfaces：
1. it is, drop coating face with the one side of pretreated stainless steel, with 5 μ L/cm2~20 μ L/cm2Consumption, use spin coating
Machine drops on the drop coating face of pretreated stainless steel the graphene oxide water solution that concentration is 1mg/mL~10mg/mL, so
The rotating speed of regulation spin coater is 1000rpm~3000rpm afterwards, and spin-coating time is 5s~30s, then puts the stainless steel after spin coating
In the baking oven that temperature is 100 DEG C, 10min~30min is toasted, obtain to surface and be covered with the stainless steel of film；
1. the stainless steel that 2., surface is covered with film is repeated 1 times~5 times by step 3, is obtained to surface and is covered with graphite oxide
The stainless steel of alkene layer；
4th, the graphene oxide layer to stainless steel surfaces is processed：
The stainless steel that surface is covered with graphene oxide layer is placed in plasma activated chemical vapour deposition vacuum plant, takes out true
Empty is 5Pa to pressure, is passed through hydrogen, and regulation hydrogen gas flow is 40sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 200Pa~500Pa in chemical vapor deposition vacuum plant, and under conditions of pressure is 200Pa~500Pa,
Temperature is increased to 600 DEG C, then radio-frequency power be 200W~600W, pressure be 200Pa~500Pa, hydrogen gas flow
It is that 40sccm and temperature are to be processed under conditions of 600 DEG C, process time is 30min；
5th, stainless steel surfaces vertical-growth original position Graphene：
Radio frequency is closed, and under conditions of pressure is 200Pa~500Pa, by temperature by 600 DEG C of regulations to 600 DEG C~800
DEG C, methane gas and argon gas are passed through, regulation methane gas gas flow is 1sccm~100sccm, and regulation argon gas flow is
1sccm~100sccm, regulation hydrogen gas flow is 1sccm~100sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 100Pa~1000Pa in chemical vapor deposition vacuum plant, is then 20W~800W, pressure in radio-frequency power
For 100Pa~1000Pa, methane gas gas flow be 1sccm~100sccm, argon gas flow be 1sccm~
100sccm, hydrogen gas flow are 1sccm~100sccm and temperature is deposition, sedimentation time under conditions of 600 DEG C~800 DEG C
It is 1min~120min, after deposition terminates, closes power supply, stopping is passed through methane gas, is cooled under argon gas and hydrogen atmosphere
Room temperature, that is, complete the preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.
Beneficial effects of the present invention：
1st, the present invention prepares super-hydrophobic antisepsis erosion layer by PECVD in metal substrate surface original position vertical-growth Graphene,
Graphenic surface prepared by this method is pure, does not have oxygen-containing functional group, and stable performance, hydrophobicity is prepared compared with oxidation-reduction method
Graphene will get well；
2nd, before PECVD vertical-growth Graphenes, preset one layer of graphene oxide, can help vertical graphite in substrate
Alkene forming core, forms finer and close graphene layer, and monolithic graphite alkene size is bigger, and corrosion resistance is more notable；
3rd, by stainless steel surfaces original position vertical-growth Graphene, changing the wellability of metal material, make it have
Stable performance is well combined significantly hydrophobicity, and grapheme material with substrate in itself, therefore with substantially increasing material anti-corruption
Corrosion energy；
4th, the inventive method is simply efficient, and cleaning thing pollutant is produced, and the surface that can be used for noncorroding metal material is modified.
The present invention is used for a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the stainless steel that surface prepared by embodiment one is covered with Graphene corrosion-inhibiting coating；
Fig. 2 is that surface prepared by embodiment one is covered with the stainless steel of Graphene corrosion-inhibiting coating as dis-eff in weight percent
Number is 10% H2SO4Tafel polarization curves in solution.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also including each specific embodiment it
Between any combination.
Specific embodiment one：A kind of preparation method of the stainless steel surfaces Graphene corrosion-inhibiting coating described in present embodiment
Follow the steps below：
First, stainless steel surfaces pretreatment：
Stainless steel is polished with the abrasive paper for metallograph of 600 mesh, 1000 mesh and 1500 mesh successively, then by the stainless steel after polishing
It is cleaned by ultrasonic 20min respectively with acetone, absolute ethyl alcohol and deionized water successively, obtains pretreated stainless steel；
2nd, graphene oxide solution is prepared：
Graphene oxide is dissolved in deionized water, the graphene oxide that concentration is 1mg/mL~10mg/mL is obtained molten
Liquid；
3rd, the preset graphene oxide layer of stainless steel surfaces：
1. it is, drop coating face with the one side of pretreated stainless steel, with 5 μ L/cm2~20 μ L/cm2Consumption, use spin coating
Machine drops on the drop coating face of pretreated stainless steel the graphene oxide water solution that concentration is 1mg/mL~10mg/mL, so
The rotating speed of regulation spin coater is 1000rpm~3000rpm afterwards, and spin-coating time is 5s~30s, then puts the stainless steel after spin coating
In the baking oven that temperature is 100 DEG C, 10min~30min is toasted, obtain to surface and be covered with the stainless steel of film；
1. the stainless steel that 2., surface is covered with film is repeated 1 times~5 times by step 3, is obtained to surface and is covered with graphite oxide
The stainless steel of alkene layer；
4th, the graphene oxide layer to stainless steel surfaces is processed：
The stainless steel that surface is covered with graphene oxide layer is placed in plasma activated chemical vapour deposition vacuum plant, takes out true
Empty is 5Pa to pressure, is passed through hydrogen, and regulation hydrogen gas flow is 40sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 200Pa~500Pa in chemical vapor deposition vacuum plant, and under conditions of pressure is 200Pa~500Pa,
Temperature is increased to 600 DEG C, then radio-frequency power be 200W~600W, pressure be 200Pa~500Pa, hydrogen gas flow
It is that 40sccm and temperature are to be processed under conditions of 600 DEG C, process time is 30min；
5th, stainless steel surfaces vertical-growth original position Graphene：
Radio frequency is closed, and under conditions of pressure is 200Pa~500Pa, by temperature by 600 DEG C of regulations to 600 DEG C~800
DEG C, methane gas and argon gas are passed through, regulation methane gas gas flow is 1sccm~100sccm, and regulation argon gas flow is
1sccm~100sccm, regulation hydrogen gas flow is 1sccm~100sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 100Pa~1000Pa in chemical vapor deposition vacuum plant, is then 20W~800W, pressure in radio-frequency power
For 100Pa~1000Pa, methane gas gas flow be 1sccm~100sccm, argon gas flow be 1sccm~
100sccm, hydrogen gas flow are 1sccm~100sccm and temperature is deposition, sedimentation time under conditions of 600 DEG C~800 DEG C
It is 1min~120min, after deposition terminates, closes power supply, stopping is passed through methane gas, is cooled under argon gas and hydrogen atmosphere
Room temperature, that is, complete the preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.
Graphene is a kind of new carbon of two-dimentional conjugated structure, and its hexagonal structure makes it have electronic structure stabilization
Characteristic, electrical and thermal conductivity is good, and carbon material stable chemical performance.This specific embodiment is by situ vertical in substrate surface
Growing straight Graphene long can directly obtain the graphene layer of three-dimensional structure on metal, and surface is pure, stable performance, with substrate knot
Close good, make material surface that there is good corrosion resistance.In general, vertical-growth Graphene in situ include forming core and from
Two processes of growth, in the preset one layer of graphene oxide of metal substrate surface, can help forming core therefore can cause what is prepared
Graphene sheet layer is bigger, makes its distribution more even compact, increases its corrosion resistance.And the method is simply efficient, safety and environmental protection,
There is no unnecessary accessory substance, be adapted to large-scale industrial production, be a kind of preferable vertical Graphene of stainless steel surfaces growth in situ
The method for preparing etch resistant layer.
The beneficial effect of this specific embodiment：
1st, this specific embodiment is prepared super-hydrophobic anti-by PECVD in metal substrate surface original position vertical-growth Graphene
Corrosion layer, graphenic surface prepared by this method is pure, does not have an oxygen-containing functional group, stable performance, and hydrophobicity is compared with redox
Graphene prepared by method will get well；
2nd, before PECVD vertical-growth Graphenes, preset one layer of graphene oxide, can help vertical graphite in substrate
Alkene forming core, forms finer and close graphene layer, and monolithic graphite alkene size is bigger, and corrosion resistance is more notable；
3rd, by stainless steel surfaces original position vertical-growth Graphene, changing the wellability of metal material, make it have
Stable performance is well combined significantly hydrophobicity, and grapheme material with substrate in itself, therefore with substantially increasing material anti-corruption
Corrosion energy；
4th, this specific embodiment method is simply efficient, and cleaning thing pollutant is produced, and can be used for noncorroding metal material
Surface is modified.
Specific embodiment two：Present embodiment from unlike specific embodiment one：It is stainless described in step one
Steel is 304 stainless steels, 316 stainless steels, 316L stainless steels or 321 stainless steels.Other are identical with specific embodiment one.
Specific embodiment three：Unlike one of present embodiment and specific embodiment one or two：Will in step 2
Graphene oxide is dissolved in deionized water, obtains the graphene oxide solution that concentration is 1mg/mL.Other and specific embodiment party
Formula one or two is identical.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Step 3 1. in
Then the rotating speed of regulation spin coater is 1000rpm, and spin-coating time is 15s.Other are identical with specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Lead in step 4
Enter hydrogen, regulation hydrogen gas flow is 40sccm.Other are identical with specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Adjusted in step 4
Pressure in plasma enhanced chemical vapor deposition vacuum plant is controlled to 500Pa by section vacuum pumping rate.Other and specific reality
Apply mode one to five identical.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：In step 4
Pressure be 500Pa under conditions of, temperature is increased to 600 DEG C, then radio-frequency power be 600W, pressure be 500Pa, hydrogen gas
Body flow is that 40sccm and temperature are to be processed under conditions of 600 DEG C, and process time is 30min.Other and specific embodiment party
Formula one to six is identical.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Pressed in step 5
It is by force under conditions of 500Pa, temperature to be adjusted to 800 DEG C by 600 DEG C.Other are identical with specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Adjusted in step 5
Section methane gas gas flow is 50sccm, and regulation argon gas flow is 10sccm, and regulation hydrogen gas flow is 10sccm,
Pressure in plasma enhanced chemical vapor deposition vacuum plant is controlled to 1000Pa by regulation vacuum pumping rate.Other with it is specific
Implementation method one to eight is identical.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：In step 5 so
It is afterwards that 400W, pressure are that 1000Pa, methane gas gas flow are that 50sccm, argon gas flow are in radio-frequency power
10sccm, hydrogen gas flow are 10sccm and temperature is deposition under conditions of 800 DEG C, and sedimentation time is 20min.Other and tool
Body implementation method one to nine is identical.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment one to ten：In step 4
Then it is 200W, the bar that pressure is 200Pa~500Pa, hydrogen gas flow is 40sccm and temperature is 600 DEG C in radio-frequency power
Processed under part, process time is 30min.Other are identical with specific embodiment one to ten.
Specific embodiment 12：Present embodiment from unlike specific embodiment one to one of 11：Step 4
In then in radio-frequency power be that 400W, pressure are that 200Pa~500Pa, hydrogen gas flow are that 40sccm and temperature are 600 DEG C
Under the conditions of processed, process time is 30min.Other are identical with specific embodiment one to 11.
Specific embodiment 13：Present embodiment from unlike specific embodiment one to one of 12：Step 5
Middle regulation methane gas gas flow is 5sccm~10sccm.Other are identical with specific embodiment one to 12.
Specific embodiment 14：Present embodiment from unlike specific embodiment one to one of 13：Step 5
Middle regulation argon gas flow is 80sccm~90sccm.Other are identical with specific embodiment one to 13.
Specific embodiment 15：Present embodiment from unlike specific embodiment one to one of 14：Step 5
Pressure in plasma enhanced chemical vapor deposition vacuum plant is controlled to 500Pa~600Pa by middle regulation vacuum pumping rate.Its
It is identical with specific embodiment one to 14.
Specific embodiment 16：Present embodiment from unlike specific embodiment one to one of 15：Step 2
It is middle that graphene oxide is dissolved in deionized water, obtain the graphene oxide solution that concentration is 3mg/mL.Other and specific reality
Apply mode one to 15 identical.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
A kind of preparation method of the stainless steel surfaces Graphene corrosion-inhibiting coating described in the present embodiment is entered according to following steps
Capable：
First, stainless steel surfaces pretreatment：
Stainless steel is polished with the abrasive paper for metallograph of 600 mesh, 1000 mesh and 1500 mesh successively, then by the stainless steel after polishing
It is cleaned by ultrasonic 20min respectively with acetone, absolute ethyl alcohol and deionized water successively, obtains pretreated stainless steel；
2nd, graphene oxide solution is prepared：
Graphene oxide is dissolved in deionized water, the graphene oxide solution that concentration is 1mg/mL is obtained；
3rd, the preset graphene oxide layer of stainless steel surfaces：
1. it is, drop coating face with the one side of pretreated stainless steel, with 10 μ L/cm2Consumption, using spin coater by concentration
For the graphene oxide water solution of 1mg/mL is dropped on the drop coating face of pretreated stainless steel, the rotating speed of spin coater is then adjusted
It is 1000rpm, spin-coating time is 15s, then the stainless steel after spin coating is placed in the baking oven that temperature is 100 DEG C, toasts
10min, obtains to surface and is covered with the stainless steel of film；
2., 1. the stainless steel that surface is covered with film is repeated 3 times by step 3, is obtained to surface and is covered with graphene oxide layer
Stainless steel；
4th, the graphene oxide layer to stainless steel surfaces is processed：
The stainless steel that surface is covered with graphene oxide layer is placed in plasma activated chemical vapour deposition vacuum plant, takes out true
Empty is 5Pa to pressure, is passed through hydrogen, and regulation hydrogen gas flow is 40sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 500Pa in chemical vapor deposition vacuum plant, and under conditions of pressure is 500Pa, temperature is increased into 600
DEG C, it is then that 600W, pressure are that 500Pa, hydrogen gas flow are under conditions of 40sccm and temperature are 600 DEG C in radio-frequency power
Processed, process time is 30min；
5th, stainless steel surfaces vertical-growth original position Graphene：
Radio frequency is closed, and under conditions of pressure is 500Pa, temperature is passed through methane gas by 600 DEG C of regulations to 800 DEG C
Body and argon gas, regulation methane gas gas flow are 50sccm, and regulation argon gas flow is 10sccm, adjusts hydrogen gas stream
It is 10sccm to measure, and be controlled to for pressure in plasma enhanced chemical vapor deposition vacuum plant by regulation vacuum pumping rate
1000Pa, then radio-frequency power be 400W, pressure be 1000Pa, methane gas gas flow be 50sccm, argon gas stream
Measure as 10sccm, hydrogen gas flow are that 10sccm and temperature are deposition under conditions of 800 DEG C, sedimentation time is 20min, deposition
After end, power supply is closed, stopping is passed through methane gas, room temperature is cooled under argon gas and hydrogen atmosphere, obtains to surface and be covered with stone
The stainless steel of black alkene corrosion-inhibiting coating；
Stainless steel described in step one is 316L stainless steels.
Fig. 1 is the scanning electron microscope (SEM) photograph of the stainless steel that surface prepared by embodiment one is covered with Graphene corrosion-inhibiting coating.Can by figure
Know, the graphene film frame sheet of vertical-growth is larger, reach 200nm~500nm, and even compact is distributed in stainless steel
Material surface.
Fig. 2 is that surface prepared by embodiment one is covered with the stainless steel of Graphene corrosion-inhibiting coating as dis-eff in weight percent
Number is 10% H2SO4Tafel polarization curves in solution, corrosion potential be -0.230V, corrosion current density for -
0.230×10-7A/cm2, polarization resistance is 10.046k Ω/cm2, show by stainless steel surfaces original position vertical-growth graphite
Alkene, changes the wellability of metal material, makes it have significant hydrophobicity, and grapheme material stable performance and substrate in itself
It is well combined, therefore substantially increases material ground corrosion resistance.
Claims (10)
1. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating, it is characterised in that a kind of stainless steel surfaces Graphene is prevented
The preparation method of rotten coating is followed the steps below：
First, stainless steel surfaces pretreatment：
Stainless steel is polished with the abrasive paper for metallograph of 600 mesh, 1000 mesh and 1500 mesh successively, then by the stainless steel after polishing successively
It is cleaned by ultrasonic 20min respectively with acetone, absolute ethyl alcohol and deionized water, obtains pretreated stainless steel；
2nd, graphene oxide solution is prepared：
Graphene oxide is dissolved in deionized water, the graphene oxide solution that concentration is 1mg/mL~10mg/mL is obtained；
3rd, the preset graphene oxide layer of stainless steel surfaces：
1. it is, drop coating face with the one side of pretreated stainless steel, with 5 μ L/cm2~20 μ L/cm2Consumption, use spin coater will
Concentration is dropped on the drop coating face of pretreated stainless steel for the graphene oxide water solution of 1mg/mL~10mg/mL, is then adjusted
The rotating speed for saving spin coater is 1000rpm~3000rpm, and spin-coating time is 5s~30s, and the stainless steel after spin coating then is placed in into temperature
Spend in the baking oven for 100 DEG C, toast 10min~30min, obtain to surface and be covered with the stainless steel of film；
1. the stainless steel that 2., surface is covered with film is repeated 1 times~5 times by step 3, is obtained to surface and is covered with graphene oxide layer
Stainless steel；
4th, the graphene oxide layer to stainless steel surfaces is processed：
The stainless steel that surface is covered with graphene oxide layer is placed in plasma activated chemical vapour deposition vacuum plant, is evacuated to
Pressure is 5Pa, is passed through hydrogen, and regulation hydrogen gas flow is 40sccm, adjusts vacuum pumping rate by plasma enhanced chemical
Pressure is controlled to 200Pa~500Pa in vapour deposition vacuum plant, and under conditions of pressure is 200Pa~500Pa, by temperature
Degree is increased to 600 DEG C, is then that 200W~600W, pressure are that 200Pa~500Pa, hydrogen gas flow are in radio-frequency power
, to be processed under conditions of 600 DEG C, process time is 30min for 40sccm and temperature；
5th, stainless steel surfaces vertical-growth original position Graphene：
Radio frequency is closed, and under conditions of pressure is 200Pa~500Pa, by temperature by 600 DEG C of regulations to 600 DEG C~800 DEG C,
Methane gas and argon gas are passed through, regulation methane gas gas flow is 1sccm~100sccm, and regulation argon gas flow is
1sccm~100sccm, regulation hydrogen gas flow is 1sccm~100sccm, adjusts vacuum pumping rate by plasma enhancing
Pressure is controlled to 100Pa~1000Pa in chemical vapor deposition vacuum plant, is then 20W~800W, pressure in radio-frequency power
For 100Pa~1000Pa, methane gas gas flow be 1sccm~100sccm, argon gas flow be 1sccm~
100sccm, hydrogen gas flow are 1sccm~100sccm and temperature is deposition, sedimentation time under conditions of 600 DEG C~800 DEG C
It is 1min~120min, after deposition terminates, closes power supply, stopping is passed through methane gas, is cooled under argon gas and hydrogen atmosphere
Room temperature, that is, complete the preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating.
2. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Stainless steel described in rapid one is 304 stainless steels, 316 stainless steels, 316L stainless steels or 321 stainless steels.
3. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Graphene oxide is dissolved in deionized water in rapid two, obtains the graphene oxide solution that concentration is 1mg/mL.
4. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Rapid three 1. in then regulation spin coater rotating speed be 1000rpm, spin-coating time is 15s.
5. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Hydrogen is passed through in rapid four, regulation hydrogen gas flow is 40sccm.
6. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Vacuum pumping rate is saved in rapid four pressure in plasma enhanced chemical vapor deposition vacuum plant is controlled to 500Pa.
7. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
In rapid four under conditions of pressure is 500Pa, temperature is increased to 600 DEG C, is then that 600W, pressure are in radio-frequency power
500Pa, hydrogen gas flow are that 40sccm and temperature are to be processed under conditions of 600 DEG C, and process time is 30min.
8. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
Under conditions of pressure is 500Pa in rapid five, temperature is adjusted to 800 DEG C by 600 DEG C.
9. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
It is 50sccm that methane gas gas flow is adjusted in rapid five, and regulation argon gas flow is 10sccm, adjusts hydrogen gas flow
It is 10sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is controlled to 1000Pa by regulation vacuum pumping rate.
10. a kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating according to claim 1, it is characterised in that step
In rapid five then radio-frequency power be 400W, pressure be 1000Pa, methane gas gas flow be 50sccm, argon gas flow
For 10sccm, hydrogen gas flow are that 10sccm and temperature are deposition under conditions of 800 DEG C, sedimentation time is 20min.
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