CN114976050B - Preparation process of gas diffusion layer for fuel cell - Google Patents
Preparation process of gas diffusion layer for fuel cell Download PDFInfo
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- CN114976050B CN114976050B CN202210523587.9A CN202210523587A CN114976050B CN 114976050 B CN114976050 B CN 114976050B CN 202210523587 A CN202210523587 A CN 202210523587A CN 114976050 B CN114976050 B CN 114976050B
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- 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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- 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
- H01M4/8605—Porous electrodes
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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
- H01M4/8817—Treatment of supports before application of the catalytic active composition
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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
- H01M8/023—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
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0241—Composites
- H01M8/0245—Composites in the form of layered or coated products
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- 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
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Abstract
The invention discloses a gas diffusion layer for a fuel cell, which belongs to the technical field of fuel cells, wherein a microporous layer consists of a plurality of conductive carbon layers and a plurality of hydrophobic agent layers, and the hydrophobic agent layers are arranged between the two conductive carbon layers. The preparation method comprises the following steps: coating conductive carbon slurry on carbon paper or carbon cloth to form a conductive carbon layer, performing heating treatment, coating a hydrophobizing agent slurry on the conductive carbon layer to form a hydrophobizing agent layer, and performing heating treatment; then coating conductive carbon slurry on the hydrophobizing agent layer to form a conductive carbon layer, and performing heating treatment, wherein the conductive carbon slurry forms a snake-shaped coating path II which is staggered with the snake-shaped slurry path I under the action of a spray head group II of coating equipment; repeating the steps to form a microporous layer of the gas diffusion layer with a plurality of conductive carbon layers and a plurality of hydrophobic agent layers. The invention realizes the lamination and construction of the conductive carbon layer and the water repellent layer, can balance the air permeability and the electric conductivity, enhances the mechanical property of the gas diffusion layer and improves the overall battery performance of the gas diffusion layer.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a preparation process of a gas diffusion layer for a fuel cell.
Background
The proton exchange membrane fuel cell is a high-efficiency and environment-friendly power generation device, and the three-in-one core component membrane electrode is generally prepared from a gas diffusion layer, a catalyst layer and a proton exchange membrane through a hot pressing process.
The gas diffusion is composed of conductive porous materials, plays multiple roles of supporting a catalytic layer, collecting current, conducting gas, discharging water and the like, realizes redistribution of reaction gas and product water between a flow field and the catalytic layer, is one of key components affecting electrode performance, and an ideal gas diffusion layer meets 3 conditions: good drainage, good breathability and good electrical conductivity. The microporous layer is a carbon powder layer which is manufactured on the surface of the microporous layer for improving the pore structure of the substrate layer, the thickness of the microporous layer is about 10-100 mu m, the microporous layer is generally manufactured on the surface of the microporous layer through processes such as screen printing, knife coating, sputtering and the like after the substrate layer is subjected to flattening treatment, and the microporous layer has the main effects of reducing the contact resistance between the catalytic layer and the substrate layer, redistributing gas and water, preventing the electrode catalytic layer from being flooded, and preventing the catalytic layer from leaking to the substrate layer in the manufacturing process.
Chinese patent (CN 113241448) discloses a gradient microporous layer and a method for preparing the same, which describes a gas diffusion layer prepared by using different conductive carbon slurries (including different carbon blacks and concentrations) and its performance characteristics, which can reduce the "flooding probability" of GDL due to the gradient microporous structure with gradual changes. Chinese patent (CN 111900417A) discloses a preparation method of a gas diffusion layer with high carbon content, which is to immerse a carbon fiber paper substrate in three conductive inks respectively, and then carry out steps of solidification, heat treatment and the like, wherein the prepared GDL has high mechanical strength, high porosity and stable chemical property.
Disclosure of Invention
The invention aims at solving the existing problems and provides a preparation process of a gas diffusion layer for a fuel cell.
The invention is realized by the following technical scheme:
a preparation process of a gas diffusion layer for a fuel cell comprises the following steps:
(1) Hydrophobic treatment:
Immersing carbon paper or carbon cloth into a hydrophobizing agent solution, and then placing the carbon paper or carbon cloth into an oven for high-temperature treatment;
(2) Preparing a first conductive carbon layer:
coating conductive carbon slurry on the carbon paper or the carbon cloth treated in the step (1) to form a conductive carbon layer and performing heating treatment, wherein the conductive carbon slurry forms a snakelike coating path I along the width range of the carbon paper or the carbon cloth under the action of a first spray head group of coating equipment, and the first spray head group is perpendicular to the conveying direction of the carbon paper or the carbon cloth;
(3) Coating a first hydrophobizing agent layer:
coating a hydrophobizing agent solution on the conductive carbon layer obtained by the treatment in the step (2) along the coating path in the step (1), forming a hydrophobizing agent layer and performing heating treatment;
(4) Coating a second conductive carbon layer:
Coating conductive carbon slurry on the hydrophobic agent layer obtained by the treatment in the step (3) to form a conductive carbon layer, and performing heating treatment, wherein the conductive carbon slurry forms a second serpentine coating path which is staggered with the first serpentine slurry path under the action of a second spray head group of coating equipment, and the second spray head group is parallel to the conveying direction of carbon paper or carbon cloth;
(5) Coating a second hydrophobizing agent layer:
coating a hydrophobizing agent solution on the conductive carbon layer obtained by the treatment in the step (4) along the coating path in the step (4), forming a hydrophobizing agent layer and performing heating treatment;
(6) Repeating the steps (2) - (4):
repeating the steps (2) - (4) to form a gas diffusion layer microporous layer with a plurality of conductive carbon layers and a plurality of hydrophobic agent layers;
(7) And (3) heat treatment:
And (3) putting the products obtained through the treatments in the steps (1) - (6) into an oven for heat treatment to form a gas diffusion layer with a plurality of conductive carbon layers and a plurality of hydrophobic agent layers.
Further, the thickness of the microporous layer is 10-120 μm.
Further, the hydrophobic treatment step is completed by dipping the hydrophobizing agent solution, wherein the concentration of the hydrophobizing agent solution is 2-15%, and the dipping time is 5-40 min; the hydrophobizing agent layer is prepared by coating a hydrophobizing agent solution, and the hydrophobizing agent is one or more of polytetrafluoroethylene emulsion, vinylidene fluoride emulsion and fluorinated ethylene propylene.
Further, the coating method is characterized in that the coating method is one of an ultrasonic spraying method and an electrostatic spraying method.
Further, the conductive carbon paste is: mixing acetylene black with a hydrophobizing agent solution, or mixing one or more of carbon black, graphite, carbon nano tubes and graphene with the hydrophobizing agent solution, wherein the hydrophobizing agent solution accounts for 0.01-20% of the total volume fraction.
Further, the thickness of each conductive carbon layer is 5-20 mu m; the thickness of each layer of the hydrophobizing agent layer is 0.5-5 mu m.
Further, the heat treatment conditions are as follows: the heat treatment temperature is 300-450 ℃, and the heat treatment time is 60-120 min.
Compared with the prior art, the invention has the following advantages:
In view of the above, the present invention is directed to providing a gas diffusion layer having a multi-layered microporous layer structure in which a plurality of sets of repeating structural units of conductive carbon layer-hydrophobizing agent layer-conductive carbon layer are formed, and a method for manufacturing the same, which can balance air permeability and conductivity while realizing lamination of the conductive carbon layer and the hydrophobizing agent layer, enhance the mechanical properties of the gas diffusion layer, and improve the overall battery performance of the gas diffusion layer.
1. The microporous layer structure of the gas diffusion layer adopts a sandwich structure of a conductive carbon layer, a hydrophobic agent layer and a conductive carbon layer, so that the distribution of the hydrophobic agent and the conductive carbon is more hierarchical, and the overall hydrophobic property and the electrical conductivity of the gas diffusion layer are greatly improved;
2. Compared with the traditional printing or coating process, the coated microporous layer is more uniform and loose, and the gas diffusion layer has stronger gas permeability;
3. The conductive carbon layer and the water repellent layer are prepared in a serpentine staggered mode, so that the consistency of the integral distribution of the microporous layer is ensured;
4. the microporous layer is prepared by adopting a coating mode, so that the direct contact between a spray head and a base material is avoided, the yield in the production process of the diffusion layer is improved, and the continuous production of the diffusion layer can be realized.
Drawings
FIG. 1 is a schematic view of a gas diffusion layer structure of a multi-layer microporous layer according to the present application;
FIG. 2 is an example of a process for preparing a gas diffusion layer of a multi-layer microporous layer according to the present application;
FIG. 3 is a flow chart of the steps performed in the gas diffusion layer of the multi-layered microporous layer according to the present application.
In the figure: 1. a conductive carbon layer; 1a, a first conductive carbon layer; 1b, a second conductive carbon layer; 1c, a third conductive carbon layer; 2. a water repellent layer; 2a, a first hydrophobizing agent layer; 2b, a second hydrophobizing agent layer; 3. longitudinally coating a conductive carbon layer; 4. longitudinally coating a hydrophobic agent layer; 5. transversely coating a conductive carbon layer; 6. a hydrophobic agent layer is applied laterally.
Detailed Description
For a further explanation of the invention, reference is made to the accompanying drawings and specific embodiments.
Examples
A gas diffusion layer for fuel cell has a microporous layer as shown in FIG. 1, and is formed by overlapping a plurality of conductive carbon layers 1 and a plurality of water repellent layers 2.
The preparation process of the gas diffusion layer for the fuel cell is shown in fig. 3, and comprises the following steps:
(1) Hydrophobic treatment of carbon paper:
Cutting a piece of carbon paper with the thickness of 190 mu m, keeping the size of 300 x 200 for later use, preparing a hydrophobic agent PTFE solution with the concentration of 5%, carrying out ultrasonic stirring uniformly, immersing the carbon paper in the PTFE solution for 1min, taking out, drying at 100 ℃ for 10min, placing the carbon paper after heat treatment in a high-temperature furnace for high-temperature treatment for 60min, and taking out after the time is up to 350 ℃ to obtain a carbon paper sample subjected to hydrophobic treatment;
(2) Preparing a microporous layer:
coating a first conductive agent layer and a first hydrophobic agent layer:
uniformly mixing acetylene black carbon powder, deionized water, ethanol solution and PTFE solution with the volume fraction of 0.01% until the slurry is sticky, placing the processed carbon paper sample on a table top of a coating group, setting the temperature of the table to 80 ℃, uniformly coating the conductive carbon slurry on the surface of the carbon paper by adopting a longitudinal coating mode to form a first conductive carbon layer (1 a), setting the coating thickness to be 20 mu m, longitudinally coating PTFE solution with the concentration of 0.01% on the surface of the first conductive carbon layer (1 a) immediately after the coating is finished to form a first hydrophobe layer (2 a), and putting the coated sample into a tunnel oven for heat treatment for 5min;
coating a second conductive agent layer and a second hydrophobic agent layer: uniformly coating conductive carbon slurry on the surface of a sample treated by the first coating group on a second coating group platform by adopting a transverse coating mode to form a second conductive carbon layer (1 b), wherein the coating thickness is set to be 20 mu m, and after the coating is finished, a PTFE solution with the concentration of 0.01% is randomly coated on the surface of the second conductive carbon layer (1 b) transversely to form a second hydrophobic agent layer (2 b), and after the coating is finished, the second hydrophobic agent layer enters a tunnel oven to be subjected to heat treatment;
Repeating the coating operation:
repeating the coating step for 2 times, placing the sample into a high temperature furnace for high temperature treatment at 380 ℃ for 80min, and taking out after the high temperature treatment is finished to prepare a gas diffusion layer with a microporous layer having a multi-layer conductive carbon layer and multi-layer hydrophobic agent layer structure;
to further illustrate the technical effects of embodiments of the present invention, fuel cell gas diffusion layers of different numbers of layers implemented using the present invention were tested, and the test characterization results are shown in table 1 below.
TABLE 1 technical parameters of gas diffusion layers prepared by different implementation layers
| N value | Number of implementation layers | Microporous layer thickness (μm) | Air permeability (s/100 cc) | Contact angle (°) | Surface resistor (mΩ cm 2) | Tensile Strength (MPa) |
| 1 | 3 | 42 | 162 | 136 | 5.8 | 36 |
| 2 | 5 | 63 | 200 | 138 | 7.0 | 40 |
| 3 | 7 | 85 | 283 | 137 | 8.6 | 48 |
As can be seen from table 1, the multi-layer micropore structure of the present invention has a plurality of groups of repeating structural units of conductive carbon layer-hydrophobic agent layer-conductive carbon layer, and can balance air permeability and conductivity, enhance mechanical properties of the gas diffusion layer, and improve overall battery performance of the gas diffusion layer while realizing lamination and construction of the conductive carbon layer and the hydrophobic agent layer.
The present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (5)
1. A process for preparing a gas diffusion layer for a fuel cell, comprising the steps of:
(1) Hydrophobic treatment:
Immersing carbon paper or carbon cloth into a hydrophobizing agent solution, and then placing the carbon paper or carbon cloth into an oven for high-temperature treatment;
(2) Preparing a first conductive carbon layer:
coating conductive carbon slurry on the carbon paper or the carbon cloth treated in the step (1) to form a conductive carbon layer and performing heating treatment, wherein the conductive carbon slurry forms a snakelike coating path I along the width range of the carbon paper or the carbon cloth under the action of a first spray head group of coating equipment, and the first spray head group is perpendicular to the conveying direction of the carbon paper or the carbon cloth;
(3) Coating a first hydrophobizing agent layer:
Coating a hydrophobizing agent solution on the conductive carbon layer obtained by the treatment in the step (2) along the coating path in the step (2), forming a hydrophobizing agent layer and performing heating treatment;
(4) Coating a second conductive carbon layer:
Coating conductive carbon slurry on the hydrophobic agent layer obtained by the treatment in the step (3) to form a conductive carbon layer, and performing heating treatment, wherein the conductive carbon slurry forms a second serpentine coating path which is staggered with the first serpentine slurry path under the action of a second spray head group of coating equipment, and the second spray head group is parallel to the conveying direction of carbon paper or carbon cloth;
(5) Coating a second hydrophobizing agent layer:
coating a hydrophobizing agent solution on the conductive carbon layer obtained by the treatment in the step (4) along the coating path in the step (4), forming a hydrophobizing agent layer and performing heating treatment;
(6) Repeating the steps (2) - (4):
repeating the steps (2) - (4) to form a gas diffusion layer microporous layer with a plurality of conductive carbon layers and a plurality of hydrophobic agent layers;
(7) And (3) heat treatment:
And (3) putting the products obtained through the treatments in the steps (1) - (6) into an oven for heat treatment to form a gas diffusion layer with a plurality of conductive carbon layers and a plurality of hydrophobic agent layers.
2. The gas diffusion layer for a fuel cell according to claim 1, wherein the thickness of the microporous layer is 10 to 120 μm.
3. The process for preparing a gas diffusion layer for a fuel cell according to claim 1, wherein the hydrophobic treatment step is performed by impregnating a hydrophobic agent solution, the concentration of the hydrophobic agent solution is 2-15%, and the impregnation time is 5-40 min; the hydrophobizing agent layer is prepared by coating a hydrophobizing agent solution, and the hydrophobizing agent is one or more of polytetrafluoroethylene emulsion, vinylidene fluoride emulsion and fluorinated ethylene propylene.
4. The process for preparing a gas diffusion layer for a fuel cell according to claim 1, wherein the coating method is one of an ultrasonic spraying method and an electrostatic spraying method.
5. The process for preparing a gas diffusion layer for a fuel cell according to claim 1, wherein the conductive carbon paste is: mixing acetylene black with a hydrophobizing agent solution, or mixing one or more of carbon black, graphite, carbon nano tubes and graphene with the hydrophobizing agent solution, wherein the hydrophobizing agent solution accounts for 0.01-20% of the total volume fraction.
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| CN107123822A (en) * | 2017-05-08 | 2017-09-01 | 黄河科技学院 | A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers |
| CN111926309A (en) * | 2020-07-14 | 2020-11-13 | 广东省稀有金属研究所 | Titanium-based passivation prevention coating for metal oxide electrode and preparation method thereof |
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Application publication date: 20220830 Assignee: Carbon International New Materials (Suzhou) Co.,Ltd. Assignor: Shanghai Tanji Industrial Group Co.,Ltd. Contract record no.: X2024980015568 Denomination of invention: Preparation process of gas diffusion layer for fuel cell Granted publication date: 20240625 License type: Common License Record date: 20240920 |
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