CN110311144B - Anode gas diffusion layer for prolonging service life of metal bipolar plate and preparation method thereof - Google Patents
Anode gas diffusion layer for prolonging service life of metal bipolar plate and preparation method thereof Download PDFInfo
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- 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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- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
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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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- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
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Abstract
The invention belongs to the technical field of fuel cells, and particularly relates to an anode gas diffusion layer capable of prolonging the service life of a metal bipolar plate and a preparation method thereof. The anode gas diffusion layer comprises a gas diffusion layer and a metal corrosion inhibitor layer based on the gas diffusion layer. The gas diffusion layer consists of a support layer and a microporous layer attached to one side of the support layer; the supporting layer is porous carbon paper and carbon cloth; the microporous layer is prepared by mixing a conductive carbon material, a water repellent, water and/or a dispersing agent and then coating the mixture on the surface of the supporting layer. According to the preparation method, the metal corrosion inhibitor is coated on the contact side of the gas diffusion layer and the anode metal bipolar plate, when the metal substrate is exposed due to failure of the anode metal bipolar plate coating, the metal corrosion inhibitor on the gas diffusion layer and the metal substrate are subjected to chemical adsorption, the anode metal bipolar plate is protected, the service life of the anode metal bipolar plate is prolonged, the service life of a fuel cell stack is further prolonged, and the defects of the conventional fuel cell are overcome.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to an anode gas diffusion layer for prolonging the service life of a metal bipolar plate and a preparation method thereof.
Background
A Proton Exchange Membrane Fuel Cell (PEMFC) is a fuel cell, and its main constituent components are a gas diffusion layer, a catalyst layer, a proton exchange membrane, a bipolar plate, an end plate, and the like. The bipolar plate is also called as a current collecting plate, the bipolar plate widely used at present comprises three types of graphite plates, metal plates and composite plates, and the metal bipolar plate occupies more and more market share due to the advantages of volume specific power density, electric and heat conducting performance, mass production cost and the like. The metal bipolar plate has poor corrosion resistance, so the surface of the metal bipolar plate is mostly modified, and the service life of the metal bipolar plate is prolonged by the surface modification technology. The surface modified coating can expose the metal substrate of the metal bipolar plate to generate corrosion due to the problems of micro defects, coating stripping in the battery operation process and the like. Corrosion not only damages the bipolar plate itself, but also reduces cell performance. The reason why the corrosion causes the performance reduction of the battery is that metal ions generated by the corrosion are absorbed by a proton exchange membrane, and the proton conduction capability of the membrane is reduced; meanwhile, metal ions generated by corrosion enter the catalyst layer, so that the activity of the catalyst is changed, and the durability of the battery is reduced. Therefore, it is necessary to develop a new method for secondarily protecting the metal substrate of the metal bipolar plate to prolong the service life of the metal bipolar plate and further prolong the service life of the fuel cell in case of failure of the coating of the metal bipolar plate.
Disclosure of Invention
The invention provides an anode gas diffusion layer for prolonging the service life of a metal bipolar plate and a preparation method thereof.
The technical scheme of the invention is described as follows by combining the attached drawings:
an anode gas diffusion layer for prolonging the service life of a metal bipolar plate comprises a gas diffusion layer and a metal corrosion inhibitor layer based on the gas diffusion layer.
The gas diffusion layer consists of a support layer and a microporous layer attached to one side of the support layer; the supporting layer is porous carbon paper and carbon cloth; the microporous layer is prepared by mixing a conductive carbon material, a water repellent, water and/or a dispersing agent and then coating the mixture on the surface of the supporting layer.
The conductive carbon material is one or a mixture of more than two of conductive carbon black, activated carbon, carbon nanotubes, carbon nanofibers, carbon fibers, carbon microspheres or graphite powder; the carrying amount of the conductive carbon material is 0.1-6 mg of the conductive carbon material contained in each square centimeter of the supporting layer.
The water repellent is one or a mixture of more than two of polytetrafluoroethylene, polychlorotrifluoroethylene, polyvinylidene fluoride, a copolymer of tetrafluoroethylene and hexafluoropropylene, and a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether; the loading amount of the water repellent is 5-60% of the total mass of the water repellent and the conductive carbon material.
The dispersing agent is one or a mixture of more than two of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene ether, polyvinylpyrrolidone, polyoxyethylene-polyoxypropylene-polyoxyethylene block copolymer, hexadecyl trimethyl ammonium bromide, lauryl sodium sulfate, linear alkylbenzene sulfonate and lauryl succinic acid.
The coating mode is one or more than two modes of blade coating, spraying, brushing, printing, silk-screen printing or suction filtration.
The metal corrosion inhibitor layer consists of a metal corrosion inhibitor attached to the other side of the supporting layer of the gas diffusion layer; the metal corrosion inhibitor is one or a mixture of more than two of C4-C12 monobasic fatty acid salt, C4-C12 dibasic fatty acid salt, C6-C21 ternary fatty acid salt, aromatic acid salt, amino acid salt and siloxane; the loading amount of the metal corrosion inhibitor is 0.1 mg-3 mg of the metal corrosion inhibitor contained in each square centimeter of the supporting layer.
A method for preparing an anode gas diffusion layer for prolonging the service life of a metal bipolar plate comprises the following steps:
step one, adding a dispersing agent into deionized water or distilled water, and forming a uniform dispersing agent water solution with the concentration of 0.1-2 wt% of the dispersing agent through one or two dispersing modes;
step two, adding a conductive carbon material into the aqueous solution of the dispersant prepared in the step one, and forming a uniform conductive carbon material suspension by one or two dispersion modes;
step three, adding water repellent emulsion into the conductive carbon material suspension prepared in the step two, and forming microporous layer slurry containing 1-60 wt% of water repellent by one or two dispersion modes;
step four, coating the microporous layer slurry prepared in the step three to one side of the support layer subjected to hydrophobic treatment in one or more than two coating modes, and performing heat treatment to obtain a gas diffusion layer;
step five, adding the metal corrosion inhibitor into deionized water or distilled water, and simultaneously heating at room temperature to 100 ℃ in one or two dispersion modes to form a uniform metal corrosion inhibitor aqueous solution;
and step six, coating the aqueous solution of the metal corrosion inhibitor prepared in the step five to the other side of the support layer subjected to hydrophobic treatment in one or more coating modes, and performing heat treatment to obtain the metal corrosion inhibitor layer based on the gas diffusion layer.
The dispersion mode is one or two of mechanical stirring for 1 minute to 10 hours and ultrasonic dispersion for 1 minute to 2 hours.
The heat treatment mode is that the heat treatment temperature is 50-400 ℃, the treatment time is 30 minutes-5 hours, and the treatment atmosphere is air, nitrogen or argon.
The beneficial effects of the invention are as follows:
according to the invention, the metal corrosion inhibitor is coated on the contact side of the gas diffusion layer and the anode metal bipolar plate, and when the coating of the anode metal bipolar plate fails and the metal matrix is exposed, the metal corrosion inhibitor on the gas diffusion layer and the metal matrix carry out chemical adsorption, so that the anode metal bipolar plate is protected, the service life of the anode metal bipolar plate is prolonged, and the service life of a fuel cell stack is further prolonged.
Drawings
FIG. 1 is a schematic structural diagram of a PEM fuel cell unit cell including an anode gas diffusion layer for extending the life of a metallic bipolar plate according to an embodiment of the present invention;
fig. 2 is a graph comparing the results of the durability test conducted on two assembled unit cells of example one and comparative example.
In the figure: 1. an anode gas diffusion layer; 2. a microporous layer; 3. a support layer; 4. a metal corrosion inhibitor layer.
Detailed Description
Referring to fig. 1, an anode gas diffusion layer 1 for extending the life of a metal bipolar plate includes a gas diffusion layer and a metal corrosion inhibitor layer 4 based on the gas diffusion layer.
The gas diffusion layer consists of a support layer 3 and a microporous layer 2 attached to one side of the support layer; the supporting layer 3 is porous carbon paper and carbon cloth; the microporous layer 2 is prepared by mixing a conductive carbon material, a water repellent, water and/or a dispersing agent and then coating the mixture on the surface of the support layer.
The conductive carbon material is one or a mixture of more than two of conductive carbon black, activated carbon, carbon nanotubes, carbon nanofibers, carbon fibers, carbon microspheres or graphite powder; the carrying amount of the conductive carbon material is 0.1-6 mg of the conductive carbon material contained in each square centimeter of the supporting layer.
The water repellent is one or a mixture of more than two of polytetrafluoroethylene, polychlorotrifluoroethylene, polyvinylidene fluoride, a copolymer of tetrafluoroethylene and hexafluoropropylene, and a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether; the loading amount of the water repellent is 5-60% of the total mass of the water repellent and the conductive carbon material.
The dispersing agent is one or a mixture of more than two of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene, polyvinylpyrrolidone, polyoxyethylene-polyoxypropylene-polyoxyethylene block copolymer, cetyl trimethyl ammonium bromide, sodium dodecyl sulfate, linear alkyl benzene sulfonate and dodecyl succinic acid.
The coating mode is one or more than two modes of blade coating, spraying, brushing, printing, silk screen printing or suction filtration.
The metal corrosion inhibitor layer consists of a metal corrosion inhibitor attached to the other side of the supporting layer of the gas diffusion layer; the metal corrosion inhibitor is one or a mixture of more than two of C4-C12 monobasic fatty acid salt, C4-C12 dibasic fatty acid salt, C6-C21 ternary fatty acid salt, aromatic acid salt, amino acid salt and siloxane; the loading amount of the metal corrosion inhibitor is 0.1 mg-3 mg of the metal corrosion inhibitor contained in each square centimeter of the supporting layer.
A method for preparing an anode gas diffusion layer for prolonging the service life of a metal bipolar plate comprises the following steps:
step one, adding a dispersing agent into deionized water or distilled water, and forming a uniform dispersing agent water solution with the concentration of 0.1-2 wt% of the dispersing agent by one or two dispersing modes;
step two, adding a conductive carbon material into the aqueous solution of the dispersant prepared in the step one, and forming a uniform conductive carbon material suspension by one or two dispersion modes;
step three, adding water repellent emulsion into the conductive carbon material suspension prepared in the step two, and forming microporous layer slurry containing 1-60 wt% of water repellent by one or two dispersion modes;
step four, coating the microporous layer slurry prepared in the step three to one side of the support layer subjected to hydrophobic treatment in one or more than two coating modes, and performing heat treatment to obtain a gas diffusion layer;
step five, adding the metal corrosion inhibitor into deionized water or distilled water, and simultaneously heating at room temperature to 100 ℃ in one or two dispersion modes to form a uniform metal corrosion inhibitor aqueous solution;
and step six, coating the aqueous solution of the metal corrosion inhibitor prepared in the step five to the other side of the support layer subjected to hydrophobic treatment in one or more coating modes, and performing heat treatment to obtain the metal corrosion inhibitor layer based on the gas diffusion layer.
The dispersion mode is one or two of mechanical stirring for 1 minute to 10 hours and ultrasonic dispersion for 1 minute to 2 hours.
The heat treatment mode is that the heat treatment temperature is 50-400 ℃, the treatment time is 30 minutes-5 hours, and the treatment atmosphere is air, nitrogen or argon.
Example one
Adding sodium dodecyl sulfate and isooctanol polyoxyethylene ether sodium phosphate into distilled water, and mechanically stirring for 2 hours to form a uniform dispersant aqueous solution with the dispersant concentration of 0.5 wt%; adding activated carbon and carbon nanotubes into the dispersant aqueous solution, and mechanically stirring for 20 minutes to form uniform conductive carbon material suspension; adding polytetrafluoroethylene emulsion into the conductive carbon material suspension, and performing ultrasonic dispersion for 1 minute to form microporous layer slurry with the water repellent concentration of 20 wt%; and (2) coating the microporous layer slurry on one side of the support layer subjected to hydrophobic treatment in a mode of combining blade coating and spraying, heating and weighing in a 105 ℃ oven, repeating the steps until the loading amount of the conductive carbon material reaches 1.5mg/cm2 and the loading amount of the water repellent reaches 40% of the total mass of the water repellent and the conductive carbon material, placing in a nitrogen-filled oven, and sintering at the temperature of 400 ℃ for 2 hours to obtain the gas diffusion layer.
Adding sodium butyrate, sodium benzoate and triazine triaminocaproate into distilled water, and mechanically stirring for 6 hours at 100 ℃ to form a uniform metal corrosion inhibitor aqueous solution; and (2) brushing the metal corrosion inhibitor aqueous solution to the other side of the support layer subjected to hydrophobic treatment, heating and weighing in an oven at 80 ℃, and repeating the step until the loading amount of the metal corrosion inhibitor is 0.5mg of the metal corrosion inhibitor contained in each square centimeter of the support layer, thereby obtaining the metal corrosion inhibitor layer based on the gas diffusion layer.
Example two
Adding polyvinylpyrrolidone into deionized water, and mechanically stirring for 1 hour to form a uniform dispersant aqueous solution with the dispersant concentration of 0.1 wt%; adding conductive carbon black into the dispersant aqueous solution, and mechanically stirring for 10 minutes to form uniform conductive carbon material suspension; adding polychlorotrifluoroethylene and polyvinylidene fluoride emulsion into the conductive carbon material suspension, mechanically stirring for 1 minute, and ultrasonically dispersing for 30 minutes to form microporous layer slurry with the water repellent concentration of 1 wt%; and (2) pumping and filtering the microporous layer slurry to one side of the support layer subjected to hydrophobic treatment, heating and weighing the microporous layer slurry in a 100 ℃ oven, repeating the steps until the loading capacity of the conductive carbon material reaches 0.1mg/cm2 and the loading capacity of the water repellent reaches 60% of the total mass of the water repellent and the conductive carbon material, placing the microporous layer slurry in a nitrogen-filled oven, and sintering the microporous layer slurry at the temperature of 350 ℃ for 4 hours to obtain the gas diffusion layer.
Adding sodium glutamate, sodium neodecanoate and sodium succinate into deionized water, and mechanically stirring at room temperature for 10 hours to form a uniform metal corrosion inhibitor aqueous solution; and spraying the metal corrosion inhibitor aqueous solution to the other side of the support layer subjected to hydrophobic treatment, then placing the support layer in a 50 ℃ oven for heating and weighing, and repeating the steps until the loading amount of the metal corrosion inhibitor is 0.1mg of the metal corrosion inhibitor contained in each square centimeter of the support layer, thereby obtaining the metal corrosion inhibitor layer based on the gas diffusion layer.
EXAMPLE III
Adding polyoxyethylene-polyoxypropylene-polyoxyethylene block copolymer and hexadecyl trimethyl ammonium bromide into distilled water, and performing ultrasonic dispersion for 30 minutes to form a uniform dispersant aqueous solution with the dispersant concentration of 1.44 wt%; adding carbon nanofibers and graphite powder into the dispersant aqueous solution, and performing ultrasonic dispersion for 20 minutes to form a uniform conductive carbon material suspension; adding copolymer emulsion of tetrafluoroethylene and hexafluoropropylene into the conductive carbon material suspension, and performing ultrasonic dispersion for 1 hour to form microporous layer slurry with the water repellent concentration of 42 wt%; and (2) printing the microporous layer slurry to one side of the support layer subjected to hydrophobic treatment in a screen printing mode, heating and weighing in a 95 ℃ oven, repeating the steps until the loading capacity of the conductive carbon material reaches 3mg/cm2 and the loading capacity of the water repellent reaches 10% of the total mass of the water repellent and the conductive carbon material, placing in a nitrogen-filled oven, and sintering at 330 ℃ for 5 hours to obtain the gas diffusion layer.
Adding potassium dodecadicarboxylate and potassium citrate into distilled water, and mechanically stirring for 5 hours at 50 ℃ to form a uniform metal corrosion inhibitor aqueous solution; and spraying the metal corrosion inhibitor aqueous solution to the other side of the hydrophobic support layer, heating and weighing in a 110 ℃ oven, and repeating the steps until the loading amount of the metal corrosion inhibitor is 1.5mg per square centimeter of the support layer, thereby obtaining the metal corrosion inhibitor layer based on the gas diffusion layer.
Example four
Adding octyl phenol polyoxyethylene ether, dodecyl benzene sulfonate and dodecyl succinic acid into distilled water, and performing ultrasonic dispersion for 1 hour and 30 minutes to form a uniform dispersant aqueous solution with the dispersant concentration of 2 wt%; adding carbon fibers and carbon microspheres into the dispersant aqueous solution, and performing ultrasonic dispersion for 10 minutes to form uniform conductive carbon material suspension; adding copolymer emulsion of tetrafluoroethylene and perfluoroalkyl vinyl ether into the conductive carbon material suspension, and mechanically stirring for 2 hours to form microporous layer slurry with the water repellent concentration of 60 wt%; and (2) coating the microporous layer slurry on one side of the support layer subjected to hydrophobic treatment in a mode of combining brush coating and print coating, heating and weighing in a 100 ℃ oven, repeating the steps until the loading amount of the conductive carbon material reaches 6mg/cm2 and the loading amount of the water repellent reaches 5% of the total mass of the water repellent and the conductive carbon material, placing in a nitrogen-filled oven, and sintering at the temperature of 370 ℃ for 3 hours to obtain the gas diffusion layer.
Adding sulfonic siloxane into distilled water, and performing ultrasonic dispersion for 2 hours at 88 ℃ to form a uniform metal corrosion inhibitor aqueous solution; and (2) brushing the metal corrosion inhibitor aqueous solution to the other side of the hydrophobic support layer, heating and weighing in a 100 ℃ oven, and repeating the step until the loading amount of the metal corrosion inhibitor is 3mg per square centimeter of the support layer, thereby obtaining the metal corrosion inhibitor layer based on the gas diffusion layer.
Comparative example 1
The same as the first embodiment: adding sodium dodecyl sulfate and isooctanol polyoxyethylene ether sodium phosphate into distilled water, and mechanically stirring for 2 hours to form a uniform dispersant water solution with the dispersant concentration of 0.5 wt%; adding activated carbon and carbon nanotubes into the dispersant aqueous solution, and mechanically stirring for 20 minutes to form a uniform conductive carbon material suspension; adding polytetrafluoroethylene emulsion into the conductive carbon material suspension, and performing ultrasonic dispersion for 1 minute to form microporous layer slurry with the water repellent concentration of 20 wt%; and (2) coating the microporous layer slurry on one side of the support layer subjected to hydrophobic treatment in a mode of combining blade coating and spraying, heating and weighing in a 105 ℃ oven, repeating the steps until the loading amount of the conductive carbon material reaches 1.5mg/cm2 and the loading amount of the water repellent reaches 40% of the total mass of the water repellent and the conductive carbon material, placing in a nitrogen-filled oven, and sintering at the temperature of 400 ℃ for 2 hours to obtain the gas diffusion layer.
Two single cells were assembled to perform a durability test using the gas diffusion layers obtained in the above example one and comparative example one as anode gas diffusion layers, respectively, and the other components were the same. The test results are shown in fig. 2, and the battery durability test of example one is superior to that of comparative example one.
Claims (2)
1. An anode gas diffusion layer for prolonging the service life of a metal bipolar plate is characterized by comprising a gas diffusion layer and a metal corrosion inhibitor layer based on the gas diffusion layer;
the gas diffusion layer consists of a support layer and a microporous layer attached to one side of the support layer; the supporting layer is porous carbon paper and carbon cloth; the microporous layer is prepared by mixing a conductive carbon material, a water repellent, water and/or a dispersing agent and then coating the mixture on the surface of the supporting layer;
the conductive carbon material is one or a mixture of more than two of conductive carbon black, activated carbon, carbon nanotubes, carbon nanofibers, carbon fibers, carbon microspheres or graphite powder; the carrying amount of the conductive carbon material is 0.1-6 mg of the conductive carbon material contained in each square centimeter of the supporting layer;
the water repellent is one or a mixture of more than two of polytetrafluoroethylene, polychlorotrifluoroethylene, polyvinylidene fluoride, a copolymer of tetrafluoroethylene and hexafluoropropylene, and a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether; the loading amount of the water repellent is 5-60% of the total mass of the water repellent and the conductive carbon material;
the dispersing agent is one or a mixture of more than two of alkylphenol polyoxyethylene, fatty alcohol polyoxyethylene, polyvinylpyrrolidone, polyoxyethylene-polyoxypropylene-polyoxyethylene block copolymer, cetyl trimethyl ammonium bromide, sodium dodecyl sulfate, linear alkyl benzene sulfonate and dodecyl succinic acid;
the coating mode is one or more than two modes of blade coating, spraying, brushing, printing, silk-screen printing or suction filtration;
the metal corrosion inhibitor layer consists of a metal corrosion inhibitor attached to the other side of the supporting layer of the gas diffusion layer; the metal corrosion inhibitor is one or a mixture of more than two of C4-C12 monobasic fatty acid salt, C4-C12 dibasic fatty acid salt, C6-C21 ternary fatty acid salt, aromatic acid salt, amino acid salt and siloxane; the carrying amount of the metal corrosion inhibitor is 0.1 mg-3 mg of the metal corrosion inhibitor contained in each square centimeter of the supporting layer.
2. The method of claim 1, wherein the method comprises the steps of:
step one, adding a dispersing agent into deionized water or distilled water, and forming a uniform dispersing agent water solution with the concentration of 0.1-2 wt% of the dispersing agent through one or two dispersing modes;
step two, adding a conductive carbon material into the aqueous solution of the dispersant prepared in the step one, and forming a uniform conductive carbon material suspension by one or two dispersion modes;
step three, adding water repellent emulsion into the conductive carbon material suspension prepared in the step two, and forming microporous layer slurry containing 1-60 wt% of water repellent in one or two dispersion modes;
step four, coating the microporous layer slurry prepared in the step three to one side of the support layer subjected to hydrophobic treatment in one or more than two coating modes, and performing heat treatment to obtain a gas diffusion layer;
step five, adding the metal corrosion inhibitor into deionized water or distilled water, and simultaneously heating at room temperature to 100 ℃ in one or two dispersion modes to form a uniform metal corrosion inhibitor aqueous solution;
step six, coating the aqueous solution of the metal corrosion inhibitor prepared in the step five to the other side of the support layer subjected to hydrophobic treatment in one or more coating modes, and performing heat treatment to obtain a metal corrosion inhibitor layer based on the gas diffusion layer;
the dispersion mode is one or two of mechanical stirring for 1 minute to 10 hours and ultrasonic dispersion for 1 minute to 2 hours;
the heat treatment mode is that the heat treatment temperature is 50-400 ℃, the treatment time is 30 minutes-5 hours, and the treatment atmosphere is air, nitrogen or argon.
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| CN112701299A (en) * | 2020-12-29 | 2021-04-23 | 一汽解放汽车有限公司 | Gas diffusion layer of fuel cell and preparation method and application thereof |
| CN112993280B (en) * | 2021-03-11 | 2023-11-14 | 大连交通大学 | Preparation method of microporous layer of gas diffusion layer of lithium air battery |
| CN113140768B (en) * | 2021-04-12 | 2022-03-18 | 上海交通大学 | Cathode side structure of integrated reversible fuel cell membrane electrode |
| CN115011211B (en) * | 2022-07-25 | 2023-08-25 | 浙江万畅科技有限公司 | Self-repairing anticorrosive paint and preparation method thereof |
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| CN109193004A (en) * | 2018-08-09 | 2019-01-11 | 成都新柯力化工科技有限公司 | A kind of metal base fuel battery gas diffusion layer material and preparation method |
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