CN108598497B - Nano metal layer for fuel cell metal polar plate and preparation method - Google Patents
Nano metal layer for fuel cell metal polar plate and preparation method Download PDFInfo
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8867—Vapour deposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
-
- 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
Abstract
The invention provides a nano metal coating for a metal polar plate of a fuel cell, which comprises a substrate layer formed by a metal polar plate, wherein at least one non-noble metal layer is deposited on the substrate layer, a mixed layer formed by alternating non-noble metal and noble metal is deposited on the non-noble metal layer, the noble metal is positioned at the outermost side of the nano metal coating, the thickness of the non-noble metal layer is 1-500 nm, and the mass ratio of the non-noble metal to the noble metal in the mixed layer formed by the non-noble metal and the noble metal is 1-90:100, the thickness of the mixed layer coating is 1-100 nm. The invention also provides a preparation method of the nano metal coating for the fuel cell metal polar plate. Compared with the existing coating, the invention can obviously reduce the consumption of noble metal, obviously enhance the surface conductivity and corrosion resistance of the metal polar plate and improve the durability of the fuel cell polar plate.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a metal polar plate of a fuel cell, in particular to a nano metal layer for the metal polar plate of the fuel cell and a preparation method thereof.
Background
The proton exchange membrane fuel cell is a novel energy device, has the characteristics of quick start, no pollution, high efficiency, quick load change response and the like, and has wide application prospects in the aspects of automobiles, fixed power stations, portable power sources and the like. A typical proton exchange membrane fuel cell mainly comprises a membrane electrode assembly, a polar plate, a sealing ring, an end plate and the like. The polar plate is one of key components in the fuel cell and mainly plays a main role in supporting a membrane electrode, distributing reaction gas, collecting current, discharging water generated by reaction and the like. The polar plate accounts for 80% of the total weight of the fuel cell, and the cost is 30% -40%. The traditional graphite polar plate is gradually replaced by a metal polar plate due to the difficult processing and poor vibration resistance. However, the metal polar plate has passivation on the running surface in the acidic environment of the fuel cell, so that the contact resistance is increased, and meanwhile, the precipitated metal ions pollute the catalyst and reduce the conductivity of the proton exchange membrane. Therefore, the preparation of a conductive and corrosion-resistant coating on the surface of a metal is an important research direction for improving the performance of a metal polar plate and promoting the commercialization of a fuel cell.
The surface coatings of the metal polar plates which are mature at present are mainly divided into noble metal coatings and carbon-based coatings. The graphite-like carbon-based coating has good conductivity and corrosion resistance, and has been widely studied in recent years. Patent publication No. CN102800871A discloses that a chromium bottom layer is deposited on the surface of stainless steel by adopting a closed field unbalanced magnetron sputtering technology, then a chromium carbon doped layer is deposited, and finally an amorphous carbon layer is deposited, and the structural components of the coating are regulated by regulating the technological parameters such as chromium target current, carbon target current, argon flow, substrate bias voltage and the like, so that the contact resistance and corrosion resistance of a metal polar plate are greatly reduced. The main problem of carbon coating is poor durability, graphite-like coating is an amorphous structure, and there are many defects, and the oxidation of amorphous carbon surface is caused by long-time corrosion in the acid environment of fuel cell, so that the contact resistance is increased remarkably. Noble metals such as platinum and gold have good stability and conductivity, and can be used in fuel cell environment. The surface electro-gold plating is a common preparation process, but due to poor compactness of an electro-gold coating, the thickness of a required gold film is at least more than 100nm, the cost is too high, and the method is not suitable for the commercialization requirement of a metal polar plate. Therefore, it is important to prepare a metal polar plate coating with low cost and high durability.
Disclosure of Invention
The invention provides a nano metal layer for a fuel cell metal plate and a preparation method thereof, aiming at solving the technical problems of poor conductivity and corrosion resistance of the fuel cell metal plate and poor durability of a coating in an acidic environment of a fuel cell in the prior art.
The invention provides a nano metal coating for a metal polar plate of a fuel cell, which comprises a substrate layer formed by a metal polar plate, wherein at least one layer of non-noble metal or non-noble metal oxide or non-noble metal suboxide layer is deposited on the substrate layer, a mixed layer formed by non-noble metal or non-noble metal oxide or non-noble metal suboxide and noble metal alternately is deposited on the non-noble metal or non-noble metal oxide or non-noble metal suboxide layer, the noble metal is positioned at the outermost side of the nano metal coating, the non-noble metal layer elements are Cr element, ni element, ti element, nb element, ta element, W element and Zr element, the non-noble metal oxide or non-noble metal suboxide is an oxide or suboxide of Cr element, an oxide or suboxide of Ni element, an oxide or suboxide of Ti element, an oxide or suboxide of Nb element, an oxide or suboxide of Ta element, an oxide or suboxide of W element or an oxide or suboxide of Zr element, the thickness of the non-noble metal or non-noble metal oxide or non-noble metal suboxide layer is 1-500 nm, the noble metal is Pt element, au element, Y element or Ru element, and the mass ratio of the non-noble metal or non-noble metal oxide or non-noble metal suboxide layer to the noble metal is 1-90 in the mixed layer formed by the non-noble metal or non-noble metal oxide or non-noble metal suboxide layer and the noble metal: 100, wherein the thickness of the mixed layer coating is 1-100 nm.
Further, the noble metal layer is in a dot structure.
Further, the mixed layer is formed by alternately compounding non-noble metal and noble metal, and the mixed layer is alternately compounded at least twice.
The invention also provides a preparation method of the nano metal coating for the fuel cell metal polar plate, which comprises the following steps:
1) Depositing at least one non-noble metal or non-noble metal oxide or non-noble metal suboxide layer on the surface of the metal polar plate by utilizing a vacuum vapor deposition method; the non-noble metal layer element is Cr element, ni element, ti element, nb element, ta element, W element and Zr element, the non-noble metal oxide or non-noble metal suboxide is Cr element oxide or suboxide, ni element oxide or suboxide, ti element oxide or suboxide, nb element oxide or suboxide, ta element oxide or suboxide, W element oxide or suboxide or Zr element oxide or suboxide, and the thickness of the non-noble metal or non-noble metal oxide or non-noble metal suboxide layer is 1-500 nm; in the deposition process, the deposition temperature is lower than 200 ℃, and the deposition air pressure is lower than 0.1 and Pa;
2) A step of depositing a mixed layer of a non-noble metal or a non-noble metal oxide or a non-noble metal suboxide and a noble metal; the noble metal is Pt element, au element, Y element or Ru element, and in the mixed layer formed by non-noble metal or non-noble metal oxide or non-noble metal suboxide and noble metal, the mass ratio of the non-noble metal or non-noble metal oxide or non-noble metal suboxide to the noble metal is 1-90:100, wherein the thickness of the mixed layer coating is 1-100 nm; in the deposition process, the deposition temperature is 200-800 ℃, the deposition air pressure is 0.1-Pa-1 Pa,
3) A step of etching a mixed layer formed by non-noble metal or non-noble metal oxide or non-noble metal suboxide and noble metal by adopting plasma, wherein reaction gas is introduced into a vacuum cavity, the etching time is between 1 and 100 and s, and the non-noble metal layer on the surface is removed;
4) A step of vacuum annealing treatment; the temperature is controlled between 200 ℃ and 1000 ℃, the treatment time is between 0.1 ℃ and 2 h, the vacuum degree is more than 1Pa, and the cavity defect left by etching treatment is eliminated.
Specifically, the reaction gas is hydrogen.
The invention is characterized in thatThe first step of depositing metal layer material is Cr, ni, ti, nb, ta, W or Zr, or Cr, ni, ti, nb, ta, W or Zr oxide or suboxide, so that on one hand, the binding force between the nano metal layer and the matrix can be improved, on the other hand, the deposited metal material has strong corrosion resistance, and the corrosion resistance of the matrix is enhanced. And thirdly, removing the surface non-noble metal layer by plasma etching, wherein gas which reacts with the surface non-noble metal element is introduced into a vacuum chamber, and the etching depth is 1-100 nm. In nano-metal layers such as titanium and gold, it is necessary to place the metal plate in the CF 4 The etching time is controlled to ensure the etching depth. And fourthly, carrying out vacuum annealing treatment to eliminate cavity defects left by etching treatment and improve the bonding strength of the outer noble metal layer. And simultaneously, the non-noble metal layer exposed by etching is subjected to oxidation treatment so as to achieve the purpose of enhancing the corrosion resistance.
When the non-noble metal bottom layer is prepared in the first step, the deposition temperature is lower than 200 ℃, the deposition air pressure is lower than 0.1 and Pa, and a compact bottom layer structure is deposited; and a second step of depositing a non-noble metal and noble metal mixed coating, wherein the deposition air pressure is 0.1-1 Pa, and the deposition temperature is 200-1000 ℃ to form a stable columnar structure. And thirdly, carrying out plasma etching treatment on the surface non-noble metal layer, wherein the etching depth is 1-100nm, and removing the surface non-noble metal layer. . Fourth, vacuum annealing treatment is carried out at 200-1000 ℃ for 0.1-2 h, and the vacuum degree is 1Pa, so that coating defects are eliminated, and the bonding strength of outer noble metal is improved.
The inner layer of the nano metal coating can be a multi-layer periodic structure with alternating non-noble metal layers and non-noble metal and noble metal composite layers, the periodic thickness is 1-100nm, and the corrosion resistance of the coating is enhanced. The outermost layer is a punctiform noble metal layer subjected to plasma etching and vacuum heat treatment, so that the conductivity of the coating is ensured, the thickness of the coating is between 1 and 100nm, and the corrosion resistance of the coating is enhanced. The outmost layer is a punctiform noble metal layer which is subjected to plasma etching and vacuum heat treatment, so that the conductivity of the coating is ensured.
The preparation method of the invention can be prepared by physical vapor deposition methods such as multi-arc ion plating, magnetron sputtering, pulse laser deposition and the like.
The invention adopts a quick evaluation method of constant potential polarization, and the corrosion solution is simulated pH 3H of the acidic environment of the fuel cell 2 SO 4 +0.1 ppm HF+80℃with an applied potential of 0.84V SHE And 1.6. 1.6V SHE The contact resistance test pressure was 1.4 MPa.
In the preferred embodiment of the invention, the contact resistance of the nano metal composite coating is between 1 and 1.5mΩ cm < 2 > after the potentiostatic 1.6-V h and 0.84V-200 h polarization experiments, the ion concentration detection result of the solution after corrosion shows that the ion concentration is far lower than that of other coating processes. Therefore, the nano metal coating provided by the invention can effectively improve the durability of the metal polar plate.
The nano metal layer for the metal polar plate of the fuel cell has higher conductivity and durability in an acidic environment, and is suitable for various load-changing working conditions; meanwhile, the coating has good binding force and low internal stress, the problem that the coating falls off in the long-time operation process can not occur, and the durability of the metal polar plate can be obviously enhanced. Compared with the traditional electroplating process or physical sputtering deposition of the noble metal film, the coating structure and the preparation process provided by the invention can greatly reduce the use amount of the noble metal, reduce the production cost and are suitable for batch production.
Compared with the prior art, the invention has obvious technical progress. Compared with the existing coating, the process can obviously reduce the consumption of noble metal, can obviously enhance the surface conductivity and corrosion resistance of the metal polar plate, and the durability of the coating in the acidic environment of the fuel cell, thereby meeting the durability requirement of the fuel cell on the metal polar plate. Meanwhile, the manufacturing efficiency of the metal polar plate coating is improved, and the production cost is reduced. The invention is particularly applied to the field of fuel cells, reduces the consumption of noble metal, reduces the contact resistance between a metal polar plate and a gas diffusion layer, and improves the durability of the metal polar plate of the fuel cell.
Drawings
FIG. 1 is a nano-metal composite coating, wherein 11 is a metal substrate, 12 is a non-noble metal layer, and 13 is a mixed layer of non-noble metal and noble metal;
FIG. 2 is a nano-metal composite coating, wherein 21 is a metal substrate, 22 is a non-metal layer, and 23 is a punctiform noble metal layer;
FIG. 3 is a multilayer alternating nano-metal composite coating wherein 31 metal matrix, 32 non-noble metal layer, 33 non-noble metal and noble metal composite layer;
FIG. 4 is a multilayer alternating nano-metal composite coating, wherein 41 metal matrix, 42 is a non-noble metal layer, 43 is a non-noble metal and noble metal composite layer, 44 noble metal layers;
fig. 5 is a schematic diagram of a process for preparing a nano metal coating for a metal plate of a fuel cell, wherein the nano metal coating is prepared by the steps of pre-coating a nano metal composite coating, performing plasma treatment in a vacuum environment, and performing post-coating treatment to obtain the nano metal coating. The same treatment process is also applicable to the treatment of the multilayer periodic structure coating.
Fig. 6 is a schematic structural view of a nano-metal coating for a fuel cell metal plate according to the present invention.
FIG. 7 is a graph of corrosion curve (A) and contact resistance before and after corrosion (B) obtained in example 7 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. Some embodiments will assist those skilled in the art in further understanding the invention, but do not limit the invention in any way. Several variations and modifications may be made by those skilled in the art without departing from the spirit of the invention.
Example 1
A nano-metal layer for a metal electrode plate of a fuel cell is shown in figure 1, wherein the nano-metal layer is formed by firstly depositing a bottom metal 12 on an electrode plate 11, and then depositing a non-noble metal and noble metal mixed coating 13, and the mixing ratio of the non-noble metal and the noble metal is 1% -90%.
Example 2
The nano metal layer for the metal polar plate of the fuel cell has the structure shown in figure 2, wherein the nano metal layer is formed by firstly depositing a bottom layer 22 on the polar plate 21, then depositing a non-noble metal and noble metal mixed coating, wherein the mixing ratio of the non-noble metal and the noble metal is between 0% and 90%, and finally carrying out plasma treatment and post treatment to obtain the dot-shaped noble metal conductive layer 23.
Example 3
The nano metal coating for the metal electrode plate of the fuel cell has a structure shown in fig. 3, wherein a bottom non-noble metal layer 32 is firstly deposited on the electrode plate 31, a non-noble metal layer and a noble metal composite layer 33 are periodically and alternately deposited, and then plasma etching and vacuum annealing treatment are carried out to obtain a nano multi-layer structure.
Example 4
The nano metal coating for the metal electrode plate of the fuel cell has a structure as shown in fig. 4, wherein the nano metal layer is formed by depositing a bottom non-noble metal layer 42 on an electrode plate 41, periodically and alternately depositing a non-noble metal layer and a noble metal composite layer 43, and finally performing plasma treatment and post-treatment to obtain a punctiform noble metal conducting layer 44.
Example 5
As shown in fig. 5 and 6, a nano metal layer for a metal plate of a fuel cell may be prepared by the following specific process:
the first step: the metal polar plate 1 is put into a deionized water ultrasonic cleaning device in turn in advance, so that pollutants such as greasy dirt, impurities and the like on the surface of a product are removed, the surface cleanliness of a sample is improved, and then the sample is dried and is ready to be put into a furnace chamber.
And a second step of: and placing the cleaned metal polar plate 1 product into a vacuum coating cavity for plasma cleaning, removing an oxide layer on the surface of a sample and adsorbing gas, and enhancing the binding force of the coating.
And a third step of: depositing a metal Cr layer 2 on the surface of the cleaned metal polar plate 1, wherein the thickness of the Cr layer is 50 nm;
fourth step: and (3) depositing a Cr and Au doped layer 3 on the surface of the deposited bottom layer 2, wherein Cr: the Au atomic ratio is 1:1, the deposition air pressure is 0.2. 0.2 Pa, and the thickness of the deposited coating is 30 nm.
Example 6
As shown in fig. 5 and 6, a nano metal layer for a metal plate of a fuel cell may be prepared by the following specific process:
the first step: the metal polar plate 1 is put into a deionized water ultrasonic cleaning device in turn in advance, so that pollutants such as greasy dirt, impurities and the like on the surface of a product are removed, the surface cleanliness of a sample is improved, and then the sample is dried and is ready to be put into a furnace chamber.
And a second step of: and placing the cleaned metal polar plate 1 product into a vacuum coating cavity for plasma cleaning, removing an oxide layer on the surface of a sample and adsorbing gas, and enhancing the binding force of the coating.
And a third step of: depositing a metal Cr layer 2 on the surface of the cleaned metal polar plate 1, wherein the thickness of the Cr layer is 50 nm;
fourth step: depositing Cr and Y doped layers 3 on the deposited bottom layer surface 2, wherein Cr: the atomic ratio of Y is 1:1, the deposition temperature is 300 ℃, the deposition air pressure is 0.2 Pa, and the thickness of the deposited coating is 30 nm;
fifth step: placing the deposited metal polar plate into a plasma etching cavity, and introducing Cl at a radio frequency source 2 And O 2 Mixing the reaction gas to remove non-noble metal Cr element on the surface of the metal polar plate; in the mixed reaction gas, cl 2 And O 2 The volume ratio of (1): 1, a step of;
sixth step: and placing the etched metal polar plate into a vacuum oven, vacuumizing to 1Pa, heating to 300 ℃, preserving heat for 1h, and then introducing shielding gas argon to cool to room temperature to eliminate coating defects.
Example 7
The nano metal layer for the fuel cell metal polar plate can be prepared by adopting the following specific process:
the first step: the metal polar plate 1 is put into a deionized water ultrasonic cleaning device in turn in advance, so that pollutants such as greasy dirt, impurities and the like on the surface of a product are removed, the surface cleanliness of a sample is improved, and then the sample is dried and is ready to be put into a furnace chamber.
And a second step of: and placing the cleaned metal polar plate 1 product into a vacuum coating cavity for plasma cleaning, removing an oxide layer on the surface of a sample and adsorbing gas, and enhancing the binding force of the coating.
And a third step of: depositing a metal Ta layer 2 on the surface of the cleaned metal polar plate 1, wherein the thickness of the Ta layer is 30 nm;
fourth step: sputtering Ta by using magnetron sputtering method 2 O 5 Target material, deposit Ta on the surface of the deposited bottom layer 2 O 5 A layer, oxide layer thickness of 20nm;
fifth step: continuing to deposit Ta on the surface of the metal polar plate 1 on which the oxide layer is deposited 2 O 5 And a mixed layer of Pt 3, ta and Pt atomic ratio of 7:3, a step of;
sixth step: putting the metal polar plate with the deposited coating into a vacuum cavity for plasma etching removal, and introducing H from a radio frequency source 2 Removing oxide on the surface of the coating;
seventh step: and (3) placing the prepared metal polar plate into a vacuum oven, vacuumizing to 1Pa, heating to 400 ℃, preserving heat by 0.5 h, and then introducing protective gas argon to cool to room temperature to eliminate coating defects.
Eighth step: and carrying out contact resistance measurement and electrochemical corrosion performance evaluation on the prepared metal polar plate in a fuel cell simulation environment. While using a conventional metal plate coating as a comparison. From the test results, the initial contact resistance of the nano metal coating prepared by the invention is 3-4 m Ω cm of the traditional coating under the assembly pressure of 1.4 MPa 2 Reduced to 1mΩ cm 2 The internal ohmic resistance of the fuel cell can be significantly reduced. Meanwhile, the corrosion performance of the prepared nano metal coating is obviously improved, the current density is obviously reduced compared with the traditional coating, and after long-time acceleration test (pH 3H 2 SO 4 Solution +80℃, potentiostatic polarization 1.6V SHE 1 h) The appearance of the coating is complete, and no corrosion trace exists. Comparison of sample resistances after test corrosion, the contact resistance after conventional coating corrosion increased significantly, whereas the sample contact resistance of inventive example 7 was substantially unchanged after accelerated corrosion (fig. 7).
Claims (1)
1. A nano-metal coating for the metallic polar plate of fuel cell is composed of a metallic polar plate as the substrate layer, and features thatIn the following steps: sequentially depositing at least one metal Ta layer and one Ta layer on the substrate layer 2 O 5 A layer; the Ta is 2 O 5 A layer of Ta is deposited on the upper surface of the layer 2 O 5 A mixed layer with noble metal Pt, wherein the atomic ratio of Ta to Pt is 7:3; the thickness of the mixed layer coating is 1-100 nm; removing Ta on the surface of the mixed layer by adopting plasma etching 2 O 5 Obtaining a Pt layer with a punctiform structure;
the nano metal coating for the fuel cell metal polar plate is prepared by the following steps: 1) Sequentially depositing at least one metal Ta layer and one Ta layer on the surface of the metal polar plate 2 O 5 A layer of metal Ta having a thickness of 30nm, the Ta 2 O 5 The thickness of the layer is 20nm, and the total thickness is not more than 500 nm; the metal Ta layer is deposited by adopting a vacuum vapor deposition method, and Ta is deposited by adopting a magnetron sputtering method 2 O 5 A layer, wherein in the deposition process, the deposition temperature is lower than 200 ℃ and the deposition air pressure is lower than 0.1Pa;
2) Continuing to deposit Ta 2 O 5 A mixed layer with noble metal Pt; in the deposition process, the deposition temperature is 200-800 ℃, and the deposition air pressure is 0.1-1 Pa;
3) Putting the metal polar plate with the deposited coating into a vacuum cavity for plasma etching to remove Ta on the surface of the mixed layer 2 O 5 Etching time is 1-100 s;
4) And (3) carrying out vacuum annealing treatment on the etched metal polar plate, controlling the temperature between 200 and 1000 ℃, controlling the vacuum degree to be more than or equal to 1Pa, controlling the treatment time to be between 0.1 and 2 h, and then introducing protective gas to cool to room temperature.
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| CN109346743B (en) * | 2018-08-31 | 2022-07-12 | 上海交通大学 | Conductive corrosion-resistant coating for metal bipolar plate of fuel cell |
| CN114457293B (en) * | 2021-12-29 | 2023-03-31 | 常州翊迈新材料科技有限公司 | Conductive hydrophobic coating and preparation method thereof |
| CN115312798B (en) * | 2022-09-16 | 2023-12-05 | 广东省科学院新材料研究所 | Metal polar plate surface protective coating, preparation method and application thereof, and metal polar plate |
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