CN110875482A - Method for preparing carbon film on surface of stainless steel bipolar plate by using graphite as carbon source - Google Patents
Method for preparing carbon film on surface of stainless steel bipolar plate by using graphite as carbon source Download PDFInfo
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- CN110875482A CN110875482A CN201810996009.0A CN201810996009A CN110875482A CN 110875482 A CN110875482 A CN 110875482A CN 201810996009 A CN201810996009 A CN 201810996009A CN 110875482 A CN110875482 A CN 110875482A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 74
- 239000010935 stainless steel Substances 0.000 title claims abstract description 73
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 64
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 41
- 239000010439 graphite Substances 0.000 title claims abstract description 40
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000004070 electrodeposition Methods 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000007770 graphite material Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims 1
- 239000000446 fuel Substances 0.000 abstract description 25
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 10
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- 235000010333 potassium nitrate Nutrition 0.000 abstract description 7
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- 239000012528 membrane Substances 0.000 abstract description 5
- 239000003792 electrolyte Substances 0.000 abstract description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 abstract 2
- 235000010344 sodium nitrate Nutrition 0.000 abstract 1
- 239000004317 sodium nitrate Substances 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 description 14
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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Classifications
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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
- H01M8/0213—Gas-impermeable carbon-containing materials
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
- C25D9/10—Electrolytic coating other than with metals with inorganic materials by cathodic processes on iron or steel
-
- 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
- H01M8/0206—Metals or alloys
- H01M8/0208—Alloys
- H01M8/021—Alloys based on iron
-
- 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
-
- 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
-
- 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
The invention relates to a method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source, which belongs to the technical field of fuel cells and is used for Proton Exchange Membrane Fuel Cells (PEMFCs). The method is characterized in that: 1. polishing commercial stainless steel to remove an oxide layer on the surface, removing oil, cleaning with deionized water, and drying for later use; 2. preparing nitrate (such as potassium nitrate, sodium nitrate, etc.) solution with certain concentration. 3. A two-electrode system is used for electrochemical deposition of the carbon film, wherein stainless steel is used as a cathode, graphite is used as an anode, and the solution temperature, the treatment current density and the treatment time are strictly controlled in the experimental process. And cleaning the treated stainless steel sample by using deionized water to remove residual electrolyte, and then drying. 4. The dried stainless steel sample carrying the carbon film was subjected to vacuum heat treatment. The performance of the stainless steel metal bipolar plate loaded with the carbon film prepared by the steps is obviously improved, and the manufacturing cost of the fuel cell is expected to be reduced.
Description
Technical Field
The invention belongs to the technical field of fuel cells, relates to a manufacturing method of a PEMFC stainless steel bipolar plate with low contact resistance and low corrosion current, and particularly relates to a method for modifying the surface of the PEMFC stainless steel bipolar plate by performing constant-current electrochemical deposition of a carbon film in a nitrate solution by using graphite as a carbon source.
Background
The energy structure directly determines the track and the speed of the development of human civilization, and the modern industrial civilization is established on the basis of fossil energy such as coal, petroleum and the like. Fossil energy is characterized by being non-renewable and limited worldwide reserves. In addition, combustion of fossil energy generates a large amount of greenhouse gases such as CO and nitrogen oxides. More urgently, serious environmental pollution problems are generated in the current fossil energy utilization process, and people are forced to start researching a clean energy utilization mode. The human society must find a way to utilize energy sources different from the current way of directly burning fossil energy sources.
A Proton Exchange Membrane Fuel Cell (PEMFC) is a power generation device that directly converts chemical energy in fuel into electrical energy using an electrochemical reaction process. The energy conversion efficiency is up to more than 80 percent without the limit of Carnot cycle because the combustion process of the traditional internal combustion engine is not carried out, and the emission of polluting gases is not generated. If hydrogen and oxygen are used as reaction substances, only water is generated, and no pollution problem is caused. In particular, in recent years there has been a great breakthrough in fuel cell technology. The basic principle of fuel cells determines that it is also an environmentally friendly energy conversion device with fast start-up at room temperature and low noise. It generates little noise because there is no moving part like other energy machines. Due to the outstanding physical and chemical properties, research and development of fuel cell technology are paid much attention by governments and major companies of various countries, especially in the field of electric vehicles, and the fuel cell technology is likely to be widely used in the fields of mobile power supplies, standby power supplies, power supplies and the like in the future, is considered to be a first-choice clean and efficient power generation technology in the 21 st century, and has great development potential.
The current commercialization of fuel cells still has many problems, especially the high manufacturing cost and long life in service. These have severely limited the development and application of fuel cell technology. Without overcoming these fatal problems, short-term fuel cells cannot compete with internal combustion engines. The bipolar plate is a key component in the fuel cell, and the manufacturing cost and service life directly determine the large-scale commercial application of the fuel cell. Bipolar Plates (also called collector Plates, flow field Plates or barrier Plates) are stacked and assembled with membrane Modules (MEAs) to form a cell stack, which is one of the key components of PEMFC stacks. The mass of the bipolar plate accounts for 60-80% of the total cell stack, the processing cost accounts for 45% of the total cell cost, and the bipolar plate is one of important factors for restricting the commercial production of the PEMFC, so that the development and research of the bipolar plate with low cost and excellent performance have important significance. At present, the PEMFC bipolar plate is mainly made of graphite and composite materials or metal materials thereof. Depending on the function and service characteristics of bipolar plates in fuel cells, the choice of materials must be made with a view to a combination of problems, in particular electrical conductivity, corrosion resistance, heat transfer properties, mechanical strength, weight, and processability.
The metal material is a potential material for manufacturing the fuel cell bipolar plate due to the advantages of excellent toughness, conductivity, heat conductivity, compactness, processability and the like. At present, metal bipolar plates, particularly stainless steel and the like, are receiving wide attention from the international society. In order to select a suitable metal material, the fuel cell operating environment must be well understood. Especially, PEMFCs operate in acidic, high-temperature and high-humidity environments, water formed by humidification and chemical reactions usually contains fluoride ions which easily cause stainless steel pitting corrosion, and the voltage difference between the cathode and the anode can reach up to 1.0V at the start-up, under such harsh working environments, common metal materials can suffer serious corrosion problems, stainless steel bipolar plates can also suffer electrochemical corrosion, the service life of the metal bipolar plates is reduced, and finally, the fuel cell cost cannot be reduced. In addition, the poor-conductivity oxide film formed on the surface of the stainless steel in an acidic oxygen-rich environment can increase the internal resistance of the battery and reduce the output power of the battery. Therefore, the main problems faced by the application of metallic bipolar plates are to solve the problem of corrosion phenomena in the range of the operating potential on the anode side of the cell and the problem of increased contact resistance due to oxidation during operation on the cathode side. The metal corrosion process not only damages the bipolar plate structure, but also reduces the performance of the battery because metal ions generated by corrosion pollute the electrolyte membrane. One of the key technologies for using metallic materials as PEMFC bipolar plates is surface modification of metals. The corrosion-resistant coating with good conductivity is formed on the surface to reduce the contact resistance and improve the corrosion resistance of the anode metal. A number of surface modification techniques have been used to improve the corrosion resistance and electrical conductivity of stainless steels.
The current methods for preparing the coatings on the surface of the stainless steel mainly comprise: high temperature Physical Vapor Deposition (PVD), nitrogen ion implantation, and gas nitriding, among others. The modified stainless steel by the surface treatment methods can form metal and metal compound coatings with excellent conductivity and corrosion resistance on the surface, and the surface treatment process cost of the stainless steel is high, the cost reduction space is not large compared with the current bipolar plate manufacturing process, and the modified bipolar plate material also finds that the damage phenomena such as pitting corrosion and the like are generated after the bipolar plate material runs for a long time. Therefore, the development of a simple, efficient and low-cost stainless steel surface treatment method instead of the traditional stainless steel modification process is forced.
Graphite materials are widely applied to the manufacture of fuel cell bipolar plates due to various good physical and chemical properties, and the excellent processability and good electrical and thermal conductivity of metal materials attract the attention of people, so that the graphite materials can be combined to exert good properties so as to be applied to the fuel cell bipolar plates. According to research, the graphite material is stripped in the electrochemical process and enters a solution, and under the action of an electric field, the graphite material migrates to a cathode to be precipitated to form a film layer, so that a carbon film is formed on the surface of the cathode after deposition for a certain time. After subsequent vacuum heat treatment, the binding force is obviously increased. By regulating and controlling electrochemical preparation parameters, the carbon film meeting the requirements can be obtained. Through the electrochemical process, the deposition of the carbon film on the surface of the stainless steel is realized. As an electrochemical modification of stainless steel surface processes, electrodeposition of carbon films promises to reduce the cost of stainless steel bipolar plate manufacture, driving the development of fuel cell technology.
Disclosure of Invention
The invention discloses a method for electrochemically depositing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source to be applied to a PEMFC (proton exchange membrane fuel cell), aiming at solving the outstanding problems that metal ions are formed by corrosion of the stainless steel bipolar plate in the using process of the PEMFC, the surface contact resistance is increased, and the like, and simultaneously improving the corrosion resistance and the conductivity of the stainless steel. The preparation method can prepare the modified stainless steel bipolar plate with excellent performance at low cost, is easy to realize low-cost mass production of the metal bipolar plate and deduces the commercial application of the fuel cell.
In order to achieve the purpose, the invention adopts the following technical scheme, which comprises the following specific steps:
(1) pretreatment of commercial stainless steel:
in order to remove oxide films and oil stains formed on the surface of the stainless steel, the stainless steel is polished and degreased.
(2) Preparing an electrochemical deposition carbon film solution:
the solution of the carbon film formed by electrochemical deposition of the stainless steel bipolar plate consists of nitrate and additives, and the pH value of the solution is controlled to be proper.
(3) Preparing a carbon film on the surface of the stainless steel:
and (3) placing the stainless steel obtained in the step (1) in the nitrate solution prepared in the step (2), and maintaining the process temperature to be higher than room temperature (25 ℃). The carbon film is formed by constant-current electrochemical treatment for a certain time, wherein a stainless steel electrode is used as a cathode, graphite is used as an anode, and the solution is stirred electromagnetically. And cleaning and drying the treated product by deionized water.
(4) Heat treatment of the carbon film stainless steel bipolar plate:
and carrying out vacuum heat treatment on the dried carbon film stainless steel bipolar plate.
Further, the stainless steel must be polished in step (1) to remove an oxide film and remove grease. The polishing means is one of mechanical polishing, chemical polishing and electrochemical polishing.
Further, in the step (2), the pH value of the solution is controlled to be 1-14, the concentration of the nitrate is 0.5-1.0M, and the pH value of the solution is adjusted by nitric acid or potassium hydroxide, which is determined according to the experimental design requirements.
Furthermore, the additive in the step (2) is methanol, and the concentration is 0.5 mL-5 mL/L.
Further, the temperature of the solution in the step (3) is maintained to be higher than room temperature, the operation temperature is selected to be 30-50 ℃ in order to prevent the moisture in the solution from evaporating, and the temperature is controlled by a constant-temperature water bath heater.
Further, the anode graphite material in the step (3) is graphite plate, graphite paper or the like. The graphite plate (rod) is operated in a large current interval corresponding to the pH value of the solution, and the graphite electrode has long service life when the graphite paper is operated in a small current interval corresponding to the pH value of the solution, but the preparation of the carbon film is not influenced. I.e. pH<At 3 hours, the recommended current density of the graphite plate (rod) is 40-50 mA/cm2The current density of the graphite paper is 20-25 mA/cm2；pH>The recommended current density of the graphite plate (rod) is 10-15 mA/cm when the graphite plate (rod) is 12 hours2The current density of the graphite paper is 1-5 mA/cm2。
Further, in the step (3), the pH of the nitrate solution<The current density is 20-50 mA/cm at 3 DEG C2To (c) to (d); pH of the solution>The current density is 1-20 mA/cm at 12 DEG C2The time is 0.5 h-8 h;
further, in the step (4), the stainless steel sample loaded with the carbon film is subjected to heat treatment at the temperature of 100-250 ℃ for 0.5-5 hours in an inert atmosphere.
And cleaning the treated stainless steel sample by using deionized water, and then carrying out tests such as electrochemistry and the like by blow drying.
The innovation of the invention is that: and (3) stripping the graphite flake by using electrochemistry to enable the graphite flake to enter a solution, and transferring the graphite flake to the surface of the cathode stainless steel under the action of an electric field to deposit and form a carbon film. By controlling the current, the processing time and the solution composition, a carbon film meeting the design requirements of the fuel cell bipolar plate can be obtained. After the stainless steel loaded with the carbon film is further subjected to vacuum heat treatment, the binding force is increased. The method for preparing the carbon film combines the advantages of the carbon material and the stainless steel substrate by depositing the carbon film on the surface of the stainless steel through electrochemistry, provides a simple method for preparing the carbon film, and provides an idea for modifying the surface of the stainless steel.
Drawings
FIG. 1 is a schematic view of the experimental setup of examples 1 and 2;
FIG. 2 is an XPS survey of example 1;
FIG. 3 is an XPS survey of example 2;
FIG. 4 is a potentiodynamic polarization plot for examples 1 and 2;
FIG. 5 is a surface SEM image of 316L stainless steel of electrochemically deposited carbon film of example 1;
FIG. 6 is a surface SEM image of 316L stainless steel of electrochemically deposited carbon film of example 2;
table 1 surface element content of example 1;
table 2 surface element content of example 2.
Detailed Description
The technical scheme of the invention is further explained by the concrete example and the attached drawings:
example one:
polishing commercial stainless steel to remove an oxide film on the surface, removing grease on the surface by ultrasonic treatment of 30Min in an alcohol solution, cleaning with deionized water, and drying and storing with a blower.
The stainless steel electrochemical deposition carbon film solution is composed of potassium nitrate solution, the pH is adjusted to 12 +/-0.5 by potassium hydroxide, and the concentration of potassium nitrate is 0.5M. To the solution was added dropwise 1mL of methanol. The solution temperature was maintained at 40. + -. 2 ℃. A constant current source was used as a power source for electrochemically depositing a carbon film, in which stainless steel was used as a cathode and a graphite rod was used as an anode. The electrodes are connected with a power supply correctly and then immersed in a potassium nitrate solution to form an experimental device. Then selecting the current density to be 15mA/cm2The carbon film deposition was carried out for a treatment time of 4 h. And cleaning the surface residual electrolyte of the treated stainless steel sample by using deionized water, drying, and then carrying out vacuum heat treatment for 2 hours at the temperature of 120 ℃. After the steps, the carbon film with good binding force is prepared on the surface of the stainless steel.
Example two:
polishing commercial stainless steel to remove an oxide film on the surface, removing grease on the surface by ultrasonic treatment of 30Min in an alcohol solution, cleaning with deionized water, and drying and storing with a blower.
The stainless steel electrochemical deposition carbon film solution is composed of potassium nitrate solution, the pH value is adjusted to 1 +/-0.5 by nitric acid, and the concentration of potassium nitrate is 1.0M. 5.0mL of methanol was added dropwise to the above solution. The solution temperature was maintained at 50. + -. 2 ℃. A constant current source was used as a power source for electrochemically depositing a carbon film, in which stainless steel was used as a cathode and a graphite rod was used as an anode. The electrodes were connected to a power supply and immersed in a potassium nitrate solution as an experimental apparatus. Then the current density was selected to be 40mA/cm2The carbon film deposition was carried out for a process time of 2 h. And cleaning the surface residual electrolyte of the treated stainless steel sample by using deionized water, drying, and then carrying out vacuum heat treatment for 1 hour at the temperature of 150 ℃. After the steps, the carbon film with good binding force is prepared on the surface of the stainless steel.
TABLE 1
TABLE 2
The above examples are merely illustrative of several embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (8)
1. A method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source is characterized by comprising the following specific steps:
(1) pretreatment of commercial stainless steel:
in order to remove oxide films and oil stains formed on the surface of the stainless steel, polishing and degreasing treatment are carried out on the stainless steel;
(2) preparing an electrochemical deposition carbon film solution:
the solution of the electrochemical deposition carbon film of the stainless steel bipolar plate consists of nitrate and additives, and the proper pH value of the solution is controlled;
(3) preparing a carbon film on the surface of the stainless steel:
placing the stainless steel obtained in the step (1) in the nitrate solution prepared in the step (2), maintaining the process temperature at 25 ℃ higher than room temperature, and forming a carbon film by adopting constant-current electrochemical treatment, wherein a stainless steel electrode is a cathode, graphite is an anode, the solution is electromagnetically stirred, and the solution is washed and dried by deionized water after treatment;
(4) heat treatment of the carbon film stainless steel bipolar plate:
and in order to improve the bonding force of the carbon film, carrying out vacuum heat treatment on the dried carbon film stainless steel bipolar plate.
2. The method for preparing a carbon film on the surface of a stainless steel bipolar plate using graphite as a carbon source according to claim 1, wherein the stainless steel must be polished to remove the oxide film in step (1); the polishing means is one of mechanical polishing, chemical polishing and electrochemical polishing.
3. The method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source according to claim 1, wherein the pH of the solution in the step (2) is controlled to be 1-14, the concentration of nitrate is 0.5-1.0M, and the pH of the solution is adjusted by nitric acid and potassium hydroxide.
4. The method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source according to claim 1, wherein the additive in the step (2) is methanol at a concentration of 0.5 mL-5 mL/L.
5. The method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source according to claim 1, wherein the solution operation temperature in the step (3) is selected to be 30-50 ℃.
6. The method for preparing a carbon film on the surface of a stainless steel bipolar plate by using graphite as a carbon source according to claim 1, wherein the anode graphite material in the step (3) is graphite plate or graphite paper; wherein, the graphite and the rod are operated under large current, and the graphite paper is operated under small current; i.e. pH<At 3 hours, the recommended current density of the graphite plate (rod) is 40-50 mA/cm2The current density of the graphite paper is 20-25 mA/cm2；pH>The recommended current density of the graphite plate (rod) is 10-15 mA/cm when the graphite plate (rod) is 12 hours2The current density of the graphite paper is 1-5 mA/cm2。
7. The method for preparing a carbon film on the surface of a stainless steel bipolar plate using graphite as a carbon source according to claim 1, wherein in the step (3), the pH of the nitrate solution is set to<The current density is 20-50 mA/cm at 3 DEG C2To (c) to (d); pH of the solution>The current density is 1-15 mA/cm at 12 DEG C2The time is 0.5 h-8 h.
8. The method for preparing the carbon film on the surface of the stainless steel bipolar plate by using graphite as a carbon source according to claim 1, wherein in the heat treatment in the step (4), the treatment temperature is 100-250 ℃, the treatment time is 0.5-5 hours, and the atmosphere is an inert atmosphere.
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| CN112760688A (en) * | 2021-03-08 | 2021-05-07 | 浙江大学 | Electrolyte solution for carbon plating and preparation and use methods thereof |
| CN116154204A (en) * | 2023-02-23 | 2023-05-23 | 浙江菲尔特过滤科技股份有限公司 | Carbon film coating process for fuel cell plate |
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| CN112760688A (en) * | 2021-03-08 | 2021-05-07 | 浙江大学 | Electrolyte solution for carbon plating and preparation and use methods thereof |
| CN112760688B (en) * | 2021-03-08 | 2022-05-24 | 浙江大学 | Electrolyte solution for carbon plating and preparation and use methods thereof |
| CN116154204A (en) * | 2023-02-23 | 2023-05-23 | 浙江菲尔特过滤科技股份有限公司 | Carbon film coating process for fuel cell plate |
| CN116154204B (en) * | 2023-02-23 | 2023-07-25 | 浙江菲尔特过滤科技股份有限公司 | Carbon film coating process for fuel cell plate |
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