CN112993293A - Metal bipolar plate of fuel cell and preparation method thereof - Google Patents
Metal bipolar plate of fuel cell and preparation method thereof Download PDFInfo
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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
- H01M8/0206—Metals or alloys
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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
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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
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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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- 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
- H01M8/0258—Collectors; Separators, e.g. bipolar separators; Interconnectors characterised by the configuration of channels, e.g. by the flow field of the reactant or coolant
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- 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
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Abstract
The invention belongs to the field of fuel cells, and particularly relates to a metal bipolar plate of a fuel cell and a preparation method thereof. Comprises a metal substrate, wherein a niobium carbide and amorphous carbon coating is co-deposited on the metal substrate. The bipolar plate has high corrosion resistance, conductivity, wear resistance and membrane-substrate binding force, and can meet the use requirements of fuel cells. The amorphous carbon increases the compactness of the coating and can effectively prevent corrosive media from permeating inwards; the mixing of niobium carbide and amorphous carbon increases the hardness and conductivity of the coating, thereby improving the wear resistance and reducing the contact resistance; in addition, the good interaction of niobium carbide with the substrate increases the coating bonding force.
Description
Technical Field
The invention belongs to the field of fuel cells, and particularly relates to a metal bipolar plate of a fuel cell and a preparation method thereof.
Background
With the shortage of fossil energy and the increasing environmental pollution, it is urgent to optimize the utilization of traditional energy and develop new clean energy with high efficiency. Fuel cell can be through the electrochemical mode chemical energy conversion electric energy in with active material to a clean efficient power generation facility, and the electricity generation process does not receive carnot circulation restriction and only result for water, has characteristics such as energy conversion efficiency height, environment friendly, noise are little, has wide application prospect in fields such as electric automobile, unmanned aerial vehicle.
The bipolar plate is one of the key components of the fuel cell, and plays roles in electrically conducting connection between adjacent single cells, preventing mixing of cathode and anode gases, transmitting reaction gases, conducting out excessive heat and water, providing mechanical support and the like. Currently, fuel cell bipolar plates mainly include three major categories, namely graphite bipolar plates, composite bipolar plates and metal bipolar plates. Among them, the metal bipolar plate is considered as the main trend of the development of the bipolar plate in the future due to its advantages of high strength, good toughness, suitability for mass production, etc. However, under PEM fuel cell conditions, SO4 2-、F-The high temperature acidic environment can cause corrosion and passivation of the metal plate material, which in turn causes performance loss of the fuel cell. Therefore, the surface modification of the metal bipolar plate to improve its conductive corrosion resistance in the fuel cell is the main direction of the metal bipolar plate research.
Chinese patent CN 109037723A discloses a graphite microcrystalline carbon modified layer prepared on the surface of a metal plate by magnetron sputtering, which changes the energy of deposited particles by changing the sputtering power supply of a target material, the intensity of the sputtering magnetic field, the deposition temperature of a coating and the like, and further changes the structure of a carbon coating. However, the carbon coating is deposited with a lower efficiency by magnetron sputtering, which increases the production cost of the material. Chinese patent CN 102623715 a discloses a modified layer of niobium carbide prepared by physical vapor deposition on stainless steel bipolar plates, which has good electrical conductivity, but its corrosion resistance under simulated fuel cell environment is unknown. Therefore, the search for more stable coating systems and the optimization of coating preparation techniques remains a great need.
Disclosure of Invention
In order to solve the technical problems, the invention provides a fuel cell metal bipolar plate and a surface modification method thereof, which can reduce the interface contact resistance of the metal bipolar plate and improve the corrosion resistance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a fuel cell metal bipolar plate comprises a metal substrate on which a niobium carbide and amorphous carbon coating is co-deposited.
In the above technical solution, further, the carbon atom ratio of the niobium carbide and the amorphous carbon coating is 33% to 99%, and the niobium atom ratio is 1% to 67%.
In the above technical solution, further, the thickness of the co-deposited coating of niobium carbide and amorphous carbon is 50nm to 3000 nm.
In the above technical solution, further, the metal substrate is made of stainless steel, titanium or titanium alloy.
A method for preparing a metal bipolar plate for a fuel cell, the method comprising: firstly, ultrasonically cleaning and drying a metal substrate in deionized water, ethanol and acetone in sequence, and then depositing a niobium carbide and amorphous carbon codeposition coating on the surface of the metal substrate.
In the above technical solution, further, the preparation method of the niobium carbide and amorphous carbon co-deposition coating is magnetron sputtering or arc ion plating.
In the above technical solution, further, the source of the carbon in the preparation of the niobium carbide and amorphous carbon co-deposition coating is one of graphite target, methane, ethane, ethylene and acetylene. The carbon in the niobium carbide and chromium carbide codeposition layer is mainly in the form of carbide, but the existence of partial simple carbon is not excluded.
In the above technical solution, further, the method comprises: sequentially ultrasonically cleaning and drying a metal substrate in deionized water, ethanol and acetone; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then to vacuumIntroducing 15-30 sccm acetylene gas into the chamber, controlling the target current to be 50-100A, controlling the substrate bias voltage to be-100-300V, and depositing a niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the metal bipolar plate.
The invention has the beneficial effects that: the bipolar plate has high corrosion resistance, conductivity, wear resistance and membrane-substrate binding force, and can meet the use requirements of fuel cells. The amorphous carbon in the coating avoids the generation of crystal material grain boundaries, enhances the compactness of the coating, effectively prevents corrosive media from permeating into the substrate, and ensures that the bipolar plate has better corrosion resistance; niobium carbide is a transition metal ceramic material and has extremely high hardness and metalloid conductivity, so that the wear resistance of the coating can be effectively improved, and the contact resistance between the coating and carbon paper is reduced; in addition, the niobium transition layer and the niobium carbide are well combined, and the co-deposition of the niobium carbide and the amorphous carbon can effectively improve the binding force between the coating and the substrate.
Drawings
Fig. 1 is a schematic structural diagram of a bipolar plate according to the present invention, in which 1, a metal plate substrate, 2, amorphous carbon, 3, niobium carbide;
FIG. 2 is a scanning electron microscope cross-sectional view of the coating prepared in example 5;
FIG. 3 is a graph showing the ratios of niobium and carbon in the coatings prepared in the examples;
FIG. 4 is a graph showing the variation of contact resistance between the metal bipolar plate and the carbon paper according to pressure, which is prepared in each example;
fig. 5 is a graph showing the results of accelerated corrosion tests of the metal bipolar plates prepared in the examples under simulated fuel cell cathode conditions.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
Comparative example 1
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece frame of an arc ion plating machine, and vacuumizing to below 3 x 10 < -3 > Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then 15sccm of acetylene gas is introduced into the vacuum chamber, the target current is controlled to be 100A, the substrate is biased to be minus 200V, and the niobium carbide coating is deposited for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 0.97m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4After 10h of constant potential 0.6V (vs. SCE) corrosion under the condition of +5ppm F-air introduction, the corrosion current is 1.92 mu A/cm 2.
Example 1
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then introducing 18sccm of acetylene gas into the vacuum chamber, controlling the target current to be 100A, biasing the substrate to be-150V, and depositing the niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 7.7m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.38 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
Example 2
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; using niobium target as evaporation source, controlling target current 60ABottom bias voltage is-600V, and sputtering and cleaning are carried out for 5 min; then 18sccm of acetylene gas is introduced into the vacuum chamber, the target current is controlled to be 100A, the substrate bias voltage is-200V, and the niobium carbide and amorphous carbon codeposition layer is deposited for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 2.1m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.60 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
Example 3
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then introducing 18sccm acetylene gas into the vacuum chamber, controlling the target current to be 100A, biasing the substrate to be-250V, and depositing the niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 3.1m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.59 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
Example 4
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; using niobium target as evaporation source, controlling target current at 60A, substrate bias at-600V, sputteringCleaning for 5 min; then introducing acetylene gas of 21sccm into the vacuum chamber, controlling the target current to be 100A, biasing the substrate to be-200V, and depositing the niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 6.9m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.45 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
Example 5
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then introducing acetylene gas of 21sccm into the vacuum chamber, controlling the target current to be 80A, biasing the substrate to be-200V, and depositing the niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the surface modified metal plate.
As shown in the figure, the thickness of the obtained coating is about 600nm, and the contact resistance between the bipolar plate and the carbon paper is 1.7m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.52 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
Example 6
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then to vacuumIntroducing 27sccm acetylene gas into the chamber, controlling the target current to be 60A, biasing the substrate to be-200V, and depositing the niobium carbide and amorphous carbon codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 7.5m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.29 mu A/cm2Compared with a TA1 type pure titanium substrate, the conductivity and the corrosion resistance are both obviously improved.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (8)
1. A fuel cell metal bipolar plate comprises a metal substrate, and is characterized in that a niobium carbide and amorphous carbon coating is co-deposited on the metal substrate.
2. A fuel cell metallic bipolar plate as in claim 1, wherein said niobium carbide, amorphous carbon coating has a carbon atom ratio of 33% to 99%, and a niobium atom ratio of 1% to 67%.
3. The fuel cell metallic bipolar plate of claim 1, wherein said co-deposited coating of niobium carbide and amorphous carbon has a thickness of 50nm to 3000 nm.
4. A fuel cell metallic bipolar plate as in claim 1, wherein said metal substrate is made of stainless steel, titanium or titanium alloy.
5. The method of manufacturing a metal bipolar plate for a fuel cell according to claim 1, wherein the method comprises: firstly, ultrasonically cleaning and drying a metal substrate in deionized water, ethanol and acetone in sequence, and then depositing a niobium carbide and amorphous carbon codeposition coating on the surface of the metal substrate.
6. The method for preparing a metallic bipolar plate for a fuel cell as claimed in claim 5, wherein the method for preparing the niobium carbide and amorphous carbon co-deposition coating is magnetron sputtering or arc ion plating.
7. The method for preparing a metallic bipolar plate for a fuel cell as claimed in claim 6, wherein the carbon source in the preparation of the niobium carbide and amorphous carbon co-deposition coating is one of graphite target, methane, ethane, ethylene and acetylene.
8. The method for preparing a metal bipolar plate for a fuel cell according to claim 5, wherein the method comprises:
sequentially ultrasonically cleaning and drying a metal substrate in deionized water, ethanol and acetone; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; then 15-30 sccm of acetylene gas is introduced into the vacuum chamber, the target current is controlled to be 50-100A, the substrate bias voltage is controlled to be-100-300V, and the niobium carbide and amorphous carbon codeposition layer is deposited for 30 min; and cooling and taking out to obtain the metal bipolar plate.
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Cited By (2)
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| CN114231925A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Fuel cell metal bipolar plate composite coating and preparation method thereof |
| CN115911437A (en) * | 2022-11-11 | 2023-04-04 | 西部金属材料股份有限公司 | Metal fiber felt composite material and preparation method and application thereof |
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| CN115911437A (en) * | 2022-11-11 | 2023-04-04 | 西部金属材料股份有限公司 | Metal fiber felt composite material and preparation method and application thereof |
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