CN113078326B - Preparation method of fuel cell gas diffusion layer - Google Patents
Preparation method of fuel cell gas diffusion layer Download PDFInfo
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- CN113078326B CN113078326B CN202110320469.3A CN202110320469A CN113078326B CN 113078326 B CN113078326 B CN 113078326B CN 202110320469 A CN202110320469 A CN 202110320469A CN 113078326 B CN113078326 B CN 113078326B
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a preparation method of a gas diffusion layer of a fuel cell, which comprises the following steps: step 1, carrying out hydrophobic treatment on a supporting layer: dipping the support layer in a water repellent solution, taking out and drying the support layer, and then carrying out sectional heat treatment; step 2, preparing microporous layer slurry: uniformly mixing a conductive material, a two-dimensional MXene sheet layer material, a water repellent and an organic solvent to prepare microporous layer slurry; step 3, preparing a gas diffusion layer: and repeatedly spraying the microporous layer slurry on the support layer after the hydrophobic treatment until the microporous layer slurry on the support layer reaches a preset loading amount, and then carrying out heat treatment to prepare the gas diffusion layer. In the preparation method of the gas diffusion layer of the fuel cell, a sectional heating mode is adopted during the hydrophobic treatment of the supporting layer, so that the hydrophobic treatment effect of the supporting layer is better; in addition, when the microporous layer is prepared, the conductivity of the diffusion layer is improved by adding the two-dimensional MXene sheet layer material.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a preparation method of a gas diffusion layer of a fuel cell.
Background
The fuel cell has the advantages of high starting speed, high running power, high reliability and the like, draws great attention worldwide, and becomes clean energy with great development prospect. The fuel cell takes a proton exchange membrane as electrolyte, directly converts the chemical energy of oxyhydrogen into electric energy, and does not need to compress gas or heat. A typical fuel cell mainly includes the following parts: proton exchange membrane, catalyst layer, gas diffusion layer and bipolar plate.
The gas diffusion layer is a channel for the flow of reactant gas and product water, can provide an electronic channel for electrochemical reaction, can collect current and support a catalytic layer, and is an important component of a fuel cell. The gas diffusion layer is composed of two parts, a support layer (substrate layer) and a microporous layer. The main function of the supporting layer is to realize 'water-gas' double-phase flow and flow collection; the microporous layer not only has a certain 'water management' function, but also can reduce the contact resistance between the catalytic layer and the supporting layer. At present, porous carbon paper with high porosity is mostly used as a support layer, and a microporous layer is a high-conductivity carbon powder layer with the thickness of 10-100m and covered on the support layer, but the control of the microstructure of the scale is not easy, and the problems of poor hydrophobicity and conductivity of a gas diffusion layer exist.
Disclosure of Invention
In view of the above problems, the present invention discloses a method for preparing a gas diffusion layer for a fuel cell to overcome or at least partially solve the above problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a preparation method of a gas diffusion layer of a fuel cell, which comprises the following steps:
Further, in the step 1, the step of performing the segmented heat treatment specifically includes:
and raising the temperature to 240-250 ℃ for heat treatment of the support layer for 15-45min, and then continuing raising the temperature to 340-350 ℃ for heat treatment of the support layer for 15-45 min.
Further, the two-dimensional MXene sheet layer material is composed of a single layer or few layers of at least one of transition metal nitride, metal carbide and metal carbonitride.
Further, in the step 2, the mass ratio of the conductive material, the two-dimensional MXene lamellar material, the water repellent and the organic solvent is 10 (0.1-5): 1-50): 100-1000);
and uniformly mixing the conductive material, the two-dimensional MXene sheet layer material, the water repellent and the organic solvent in an ultrasonic dispersion mode.
Further, the support layer is a carbon material, preferably carbon paper or carbon cloth, and the specification of the carbon material is 20-100g/m2。
Further, in the step 1 and the step 2, the water repellent is one or two of polytetrafluoroethylene and polyvinylidene fluoride-hexafluoropropylene; (ii) a
In the step 2, the conductive material comprises carbon nano tubes, graphite powder and carbon black powder; the organic solvent comprises one or more of methanol, isopropanol, ethanol and N-methyl pyrrolidone.
Further, in the step 1, the mass fraction of the water repellent solution is 1-10 wt%;
and repeatedly dipping and drying the supporting layer to ensure that the content of the water repellent on the supporting layer is 10-30 wt%.
Further, in the step 1, the impregnated support layer is dried in a low-temperature slow drying mode, wherein the drying temperature is 25-35 ℃.
Further, in the step 3, the spraying mode of the microporous layer slurry is ultrasonic spraying; and (3) placing the support layer subjected to the hydrophobic treatment at a temperature of 70-85 ℃ for spraying operation.
Further, in the step 3, the preset loading capacity is 2-4mg/cm2(ii) a The heat treatment specifically comprises the following steps: heat treatment at 345 ℃ and 355 ℃ for 25-35 min.
The invention has the advantages and beneficial effects that:
in the preparation method of the gas diffusion layer of the fuel cell, a sectional heating mode is adopted during the hydrophobic treatment of the supporting layer, so that the hydrophobic treatment effect of the supporting layer is better; in addition, when the microporous layer is prepared, the conductivity of the diffusion layer is improved by adding the two-dimensional MXene sheet layer material.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a diagram illustrating steps in a method for fabricating a gas diffusion layer according to an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of a carbon paper (support layer) before hydrophobic treatment, after hydrophobic treatment and after spraying a microporous layer slurry according to an embodiment of the present invention;
FIG. 3 is a graph of carbon paper hydrophobicity (contact angle) as a function of dip times and PTFE (water repellent) concentration for one embodiment of the invention;
FIG. 4 is a graph of the results of a carbon paper hydrophobicity (contact angle) test in an example of the present invention;
fig. 5 is a stress-strain test graph of gas diffusion layers prepared by different preparation methods.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and fully with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solutions provided by the embodiments of the present invention are described in detail below with reference to the accompanying drawings.
In one embodiment of the present invention, a method for preparing a gas diffusion layer of a fuel cell is disclosed, as shown in fig. 1, the method comprising the steps of:
The present example improves the preparation method of the gas diffusion layer, aiming at the problems of poor hydrophobicity and poor electrical conductivity of the existing gas diffusion layer. Specifically, compared with the existing gas diffusion layer preparation method in which the support layer is subjected to the hydrophobic treatment only once, the present embodiment adopts a segmented thermal treatment manner, which can effectively improve the hydrophobic treatment effect of the support layer and improve the hydrophobic performance of the diffusion layer. In addition, when the microporous layer is prepared, the high-conductivity MXene material is added, so that the conductivity of the diffusion layer is greatly improved. Fig. 2 shows the change of the surface of the carbon paper after the hydrophobic treatment and the spraying treatment in the preparation method of the present invention when the carbon paper is used as a support layer, and it can be seen that the diffusion layer prepared by the preparation method has a more uniform surface.
The MXene material is a metal carbide and metal nitride material with a two-dimensional layered structure, and near-free electrons of the MXene material are positioned near a Fermi level, so that an ideal transmission channel is provided for rapid carrier transmission, and the MXene material has excellent conductivity. The material composition may be represented as Mn+1XnTx(wherein M represents a transition metal element, X is carbon and/or nitrogen, TxRepresenting that MXene material generates functional groups such as-OH, -O, -F and the like attached to the surface of MXene material by chemically etching a precursor MAX phase), and M-X is a mixed bond of covalent bond-ionic bond-metal bond compared with a single carbon atom bonding structure of a carbon material such as grapheneThe valence bond, so MXene material possess than graphite alkene abundant tunable performance. As shown in fig. 5, the tensile property of the carbon paper after the hydrophobic treatment is improved to a certain extent, and the tensile property of the microporous layer (example 2) to which the MXene material is added is further improved compared with that of the microporous layer (comparative example 1) to which the MXene material is not added.
In one embodiment, the step 1 of the step-wise heat treatment specifically comprises:
firstly, the temperature is raised to 240-250 ℃, the supporting layer is thermally treated for 15-45min, preferably for 30min, and the surfactant in the water repellent solution can be removed through the thermal treatment at the lower temperature; and then the temperature is continuously increased to 340-350 ℃ for heat treatment of the support layer for 15-45min, preferably for 30min, the heating can melt the water repellent agent, and a film is formed to cover the surface of the support layer, so that the hydrophobic property is realized. The water repellent used in the embodiment of the patent is Polytetrafluoroethylene (PTFE) emulsion, a nonionic surfactant is usually added into the PTFE emulsion, and the temperature is raised to be more than 200 ℃ for a period of time, so that the nonionic surfactant can be decomposed or evaporated. The polytetrafluoroethylene is almost completely melted at 327 ℃, so that the polytetrafluoroethylene can be completely melted on the surface of the support layer to form a hydrophobic layer by heating the polytetrafluoroethylene at 340-350 ℃. This application utilizes different temperatures through sectional heating methods for the hydrophobic agent melts better and forms the hydrophobic layer on supporting layer surface, has improved gas diffusion layer's hydrophobic performance.
In one embodiment, the two-dimensional MXene sheet material is comprised of a single or few layers of at least one of a transition metal nitride, a metal carbide, and a metal carbonitride.
Preferably, in the step 2, the mass ratio of the conductive material, the two-dimensional MXene lamellar material, the water repellent and the organic solvent is 10 (0.1-5) to (1-50) to (100-1000), and the mixing mass ratio of the raw materials is adjusted within the range according to the requirement. Although MXene has good conductivity, transition metal oxide-like performance and other properties, the MXene is easy to collapse and stack, so that the properties are difficult to exert. Through continuous research on material compositions, the applicant finally selects a two-dimensional MXene sheet layer material as a dopant, and mixes the conductive material, the two-dimensional MXene sheet layer material, the water repellent and the organic solvent in the specific proportion, and the microporous layer slurry prepared by the proportion can effectively embody the comprehensive performances of conductivity, transition metal oxide-like performance, polyfunctional group and the like of the MXene material, so that the conductivity and mechanical properties of the gas diffusion layer of the fuel cell are improved, and the double-phase flow, "water management" capability and conductivity of the gas diffusion layer are better exerted.
In one embodiment of the application, the uniform mixing of the conductive material, the two-dimensional MXene lamellar material, the water repellent and the organic solvent is realized by means of ultrasonic dispersion, for example, ultrasonic dispersion is carried out by an ultrasonic cleaning machine, so that the raw materials can be rapidly mixed, and the mixing is more uniform.
Preferably, the support layer is a carbon material, the carbon material is preferably carbon paper or carbon cloth, and the specification of the carbon material is 20-100g/m2。
In one embodiment, the water repellent in step 1 and step 2 is one or both of polytetrafluoroethylene and polyvinylidene fluoride-hexafluoropropylene.
The conductive material in the step 2 comprises carbon nano tubes, graphite powder and carbon black powder, wherein the carbon black powder comprises one or more of acetylene black, VulcanXC-72 carbon black powder, black pearls, Ketjen black and hydrophobic carbon black; the organic solvent comprises one or more of methanol, isopropanol, ethanol and N-methylpyrrolidone.
In one embodiment, in step 1, the mass fraction of the water repellent solution is 1-10 wt%.
In order to uniformly and massively load the water repellent on the supporting layer, the water repellent content on the supporting layer is 10-30 wt% by repeatedly dipping and drying the supporting layer. As can be seen from fig. 3, as the number of times of impregnating and drying the support layer and the concentration of the water repellent are increased, the hydrophobic effect of the support layer is better and better.
Preferably, in step 1, in order to make the distribution of the water repellent on the support layer more uniform, the impregnated support layer is dried by slow drying at a low temperature, wherein the drying temperature is 25-35 ℃.
In one embodiment, the microporous layer slurry in step 3 is sprayed by ultrasonic spraying; the ultrasonic spraying is to atomize the slurry of the microporous layer into fine particles by an ultrasonic atomizing device, and then to uniformly coat the fine particles on the surface of the supporting layer by a certain amount of current-carrying gas, thereby forming a coating or a film. By adjusting the height of the spray head of the ultrasonic spraying machine, the moving speed of the spray head and the flow rate of liquid, the uniformity and the thickness of spraying are controllable, a coating with high uniformity can be obtained, and the performance of the gas diffusion layer is improved.
In order to further make the spraying more uniform, the support layer subjected to the hydrophobic treatment is subjected to a spraying operation at a temperature of 70 to 85 ℃, so that the slurry of the microporous layer sprayed on the support layer is rapidly dried, the non-uniformity of the spraying caused by the aggregation of the slurry of the microporous layer is prevented, the microporous layer on the diffusion layer is made flat and crack-free, and the microporous layer and the support layer are tightly bonded. For example, the support layer subjected to the hydrophobic treatment may be placed on a heating plate, the temperature of the heating plate is maintained at 70 to 85 ℃, and then ultrasonic spraying is performed.
Preferably, in step 3, the microporous layer slurry is repeatedly sprayed on the support layer after the hydrophobic treatment until the microporous layer slurry on the support layer reaches the preset loading amount of 2-4mg/cm2(ii) a The heat treatment specifically comprises the following steps: heat treatment at 345 ℃ and 355 ℃ for 25-35min, preferably 30 min.
Example 1
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE (polytetrafluoroethylene) emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 10 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 30min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 30min to enable PTFE to be melted to form a PTFE film to cover the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed, and the test result is shown in fig. 4, and the test contact angle is 131.4 ° (122 ° before treatment). The larger the contact angle, the more hydrophobic the film.
Preparing microporous layer slurry: XC Vulcan700mg of-72 carbon black powder, 3g of 10 wt% PTFE emulsion and two-dimensional MXene lamellar material (Ti)2CTx)70mg was put into 70ml of absolute ethanol, and ultrasonic dispersion was carried out using an ultrasonic cleaner to prepare a microporous layer slurry.
Preparing a gas diffusion layer: the carbon paper containing 10 wt% of PTFE and subjected to the hydrophobic treatment was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. And finally, putting the sprayed carbon paper into a muffle furnace, and carrying out heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
Example 2
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 20 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 30min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 30min to enable PTFE to be melted to form a PTFE film to cover the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed and the test result is shown in fig. 4, with a test contact angle of 136.7 ° (122 ° before treatment).
Preparing microporous layer slurry: 700mg of Vulcan XC-72 carbon black powder, 3g of 10 wt% PTFE emulsion and two-dimensional MXene lamellar material (Ti)2CTx)70mg was put into 70ml of absolute ethanol, and ultrasonic dispersion was carried out using an ultrasonic cleaner to prepare a microporous layer slurry.
Preparing a gas diffusion layer: the carbon paper containing 20 wt% PTFE and subjected to the hydrophobic treatment was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. And finally, putting the sprayed carbon paper into a muffle furnace, and carrying out heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
Example 3
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 30 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 30min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 30min to enable PTFE to be melted to form a PTFE film to cover the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed and the test result is shown in fig. 4, with a tested contact angle of 139.2 ° (122 ° before treatment).
Preparing microporous layer slurry: 700mg of Vulcan XC-72 carbon black powder, 3g of 10 wt% PTFE emulsion and two-dimensional MXene lamellar material (Ti)2CTx)70mg was put into 70ml of absolute ethanol, and ultrasonic dispersion was carried out using an ultrasonic cleaner to prepare a microporous layer slurry.
Preparing a gas diffusion layer: the hydrophobic treated PTFE carbon paper containing 30 wt% PTFE was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. And finally, putting the sprayed carbon paper into a muffle furnace, and carrying out heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
Example 4
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 20 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 15min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 15min to melt PTFE to form a PTFE film on the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed and the test result is shown in fig. 4, with a test contact angle of 133.5 ° (122 ° before treatment).
Preparing microporous layer slurry: 700mg of Vulcan XC-72 carbon black powder, 3g of 10 wt% PTFE emulsion and two-dimensional MXene lamellar material (Ti)2CTx)70mg was put into 70ml of absolute ethanol, and ultrasonic dispersion was carried out using an ultrasonic cleaner to prepare a microporous layer slurry.
Preparing a gas diffusion layer: the carbon paper containing 20 wt% PTFE and subjected to the hydrophobic treatment was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. And finally, putting the sprayed carbon paper into a muffle furnace, and carrying out heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
Example 5
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 20 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 45min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 45min to melt PTFE to form a PTFE film on the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed and the test result is shown in fig. 4, with a test contact angle of 137.2 ° (122 ° before treatment).
Preparing microporous layer slurry: 700mg of Vulcan XC-72 carbon black powder, 3g of 10 wt% PTFE emulsion and two-dimensional MXene lamellar material (Ti)2CTx)70mg was put into 70ml of absolute ethanol, and ultrasonic dispersion was carried out using an ultrasonic cleaner to prepare a microporous layer slurry.
Preparing a gas diffusion layer: the carbon paper containing 20 wt% PTFE and subjected to the hydrophobic treatment was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. Finally, the sprayed carbon paper is put into a muffle furnaceAnd performing heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
Comparative example 1
Carrying out hydrophobic treatment on the support layer: soaking the carbon paper (supporting layer) in 5 wt% PTFE emulsion (water repellent solution) for 1-2min, taking out, drying in an oven at 30 deg.C, and repeating the soaking-drying treatment to obtain carbon paper with PTFE content of 20 wt%. Placing the dried carbon paper into a roasting furnace, heating to 250 ℃, roasting for 30min, and removing the surfactant in the PTFE emulsion; and then, raising the temperature of the furnace to 350 ℃, and continuing to bake for 30min to enable PTFE to be melted to form a PTFE film to cover the surface of the carbon fiber of the carbon paper, so as to realize hydrophobization of the carbon paper. The hydrophobicity test was performed and the test result is shown in fig. 4, with a test contact angle of 136.7 ° (122 ° before treatment).
Preparing microporous layer slurry: 700mg of Vulcan XC-72 carbon black powder and 3g of 10 wt% PTFE emulsion are put into 70ml of absolute ethyl alcohol, and ultrasonic dispersion is carried out by using an ultrasonic cleaner to prepare microporous layer slurry.
Preparing a gas diffusion layer: the carbon paper containing 20 wt% PTFE and subjected to the hydrophobic treatment was placed on a heating plate, and the temperature of the heating plate was maintained at 80 ℃. Spraying the dispersed microporous layer slurry onto the carbon paper after hydrophobic treatment by using an ultrasonic spraying machine, and repeatedly spraying to make Vulcan XC-72 carbon black powder on the carbon paper reach 2mg/cm2. And finally, putting the sprayed carbon paper into a muffle furnace, and carrying out heat treatment at 350 ℃ for 30min to prepare the gas diffusion layer.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, extension, etc. made within the spirit and principle of the present invention are included in the protection scope of the present invention.
Claims (9)
1. A method of preparing a gas diffusion layer for a fuel cell, the method comprising the steps of:
step 1, carrying out hydrophobic treatment on a supporting layer: dipping the support layer in a water repellent solution, taking out and drying the support layer, and then carrying out sectional heat treatment;
step 2, preparing microporous layer slurry: uniformly mixing a conductive material, a two-dimensional MXene sheet layer material, a water repellent and an organic solvent to prepare microporous layer slurry;
step 3, preparing a gas diffusion layer: repeatedly spraying the microporous layer slurry on the support layer after the hydrophobic treatment until the microporous layer slurry on the support layer reaches a preset loading amount, and then carrying out heat treatment to obtain the gas diffusion layer;
in the step 1, the step heat treatment specifically comprises:
heating the supporting layer to 240-250 ℃ for heat treatment for 15-45min, and then continuing heating to 340-350 ℃ for heat treatment for 15-45 min;
the two-dimensional MXene sheet layer material consists of a single layer or few layers of at least one of transition metal nitride, metal carbide and metal carbonitride.
2. The preparation method of claim 1, wherein in the step 2, the mass ratio of the conductive material, the two-dimensional MXene lamellar material, the water repellent and the organic solvent is 10 (0.1-5): 1-50): 100- > 1000;
and uniformly mixing the conductive material, the two-dimensional MXene sheet layer material, the water repellent and the organic solvent in an ultrasonic dispersion mode.
3. The method according to claim 1, wherein the support layer is a carbon material having a size of 20 to 100g/m2。
4. The method of claim 3, wherein the support layer is a carbon paper or a carbon cloth.
5. The preparation method according to claim 1, wherein in the step 1 and the step 2, the water repellent is one or both of polytetrafluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
in the step 2, the conductive material comprises carbon nano tubes, graphite powder and carbon black powder; the organic solvent comprises one or more of methanol, isopropanol, ethanol and N-methyl pyrrolidone.
6. The preparation method of claim 1, wherein in the step 1, the mass fraction of the water repellent solution is 1-10 wt%;
and repeatedly dipping and drying the supporting layer to ensure that the content of the water repellent on the supporting layer is 10-30 wt%.
7. The preparation method according to claim 1, wherein in the step 1, the impregnated support layer is dried by slow drying at a low temperature, wherein the drying temperature is 25-35 ℃.
8. The method according to claim 1, wherein in the step 3, the microporous layer slurry is sprayed by ultrasonic spraying; and (3) placing the support layer subjected to the hydrophobic treatment at a temperature of 70-85 ℃ for spraying operation.
9. The method according to any one of claims 1 to 8, wherein the predetermined loading amount in the step 3 is 2 to 4mg/cm2(ii) a The heat treatment specifically comprises the following steps: heat treatment at 345 ℃ and 355 ℃ for 25-35 min.
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| CN113707892B (en) * | 2021-08-27 | 2022-12-27 | 广州市香港科大霍英东研究院 | Gas diffusion layer for fuel cell and method for preparing the same |
| CN113991129A (en) * | 2021-10-28 | 2022-01-28 | 无锡威孚高科技集团股份有限公司 | Microporous layer of gas diffusion layer of proton exchange membrane fuel cell and preparation method thereof |
| CN114023974A (en) * | 2021-11-08 | 2022-02-08 | 重庆大学 | Preparation method of multipurpose gas diffusion electrode with controllable performance, product and application thereof |
| CN114430050B (en) * | 2022-01-18 | 2023-10-24 | 山东仁丰特种材料股份有限公司 | Gas diffusion layer for high-performance hydrogen fuel cell and preparation method thereof |
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| CN110518259A (en) * | 2019-08-26 | 2019-11-29 | 浙江锋源氢能科技有限公司 | A kind of gas diffusion layers and preparation method thereof and fuel cell |
| CN111584887A (en) * | 2020-05-27 | 2020-08-25 | 无锡威孚高科技集团股份有限公司 | Preparation method of gas diffusion layer for proton exchange membrane fuel cell |
| CN111628182A (en) * | 2020-05-25 | 2020-09-04 | 常熟氢能源研究院有限公司 | Membrane electrode for fuel cell and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101038970A (en) * | 2007-03-29 | 2007-09-19 | 武汉理工大学 | Method for preparing water-keeping diffusion layer of high temperature proton exchange film fuel cell |
| CN110518259A (en) * | 2019-08-26 | 2019-11-29 | 浙江锋源氢能科技有限公司 | A kind of gas diffusion layers and preparation method thereof and fuel cell |
| CN111628182A (en) * | 2020-05-25 | 2020-09-04 | 常熟氢能源研究院有限公司 | Membrane electrode for fuel cell and preparation method thereof |
| CN111584887A (en) * | 2020-05-27 | 2020-08-25 | 无锡威孚高科技集团股份有限公司 | Preparation method of gas diffusion layer for proton exchange membrane fuel cell |
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