CN109301258B - Fuel cell gas diffusion layer and preparation method thereof - Google Patents
Fuel cell gas diffusion layer and preparation method thereof Download PDFInfo
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- CN109301258B CN109301258B CN201811056404.7A CN201811056404A CN109301258B CN 109301258 B CN109301258 B CN 109301258B CN 201811056404 A CN201811056404 A CN 201811056404A CN 109301258 B CN109301258 B CN 109301258B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/8803—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 provides a fuel cell gas diffusion layer, which is prepared by coating gas diffusion layer slurry on one surface of carbon paper and then sintering, wherein the gas diffusion layer slurry comprises PTFE (polytetrafluoroethylene), carbon powder and porous nano-fibrous nickel powder, the solid content of the gas diffusion layer slurry is 2.2-3.75%, and the mass ratio of the carbon powder to the porous nano-fibrous nickel powder is (1-5): 1, the mass of the PTFE is 10% -25% of the total mass of the carbon powder and the porous nano fibrous nickel powder, and the solid loading capacity on the carbon paper is 1-3 mg/cm2. The invention also provides a preparation method of the gas diffusion layer of the fuel cell. The gas diffusion layer of the fuel cell has the advantages of small internal resistance, excellent water management performance, long service life, high conductivity and porosity, and simple and feasible preparation method.
Description
Technical Field
The invention relates to a fuel cell gas diffusion layer and a preparation method thereof.
Background
The core component of a Proton Exchange Membrane Fuel Cell (PEMFC) is a Membrane Electrode (MEA), which is composed of a gas diffusion layer, a catalyst layer, and a proton exchange membrane. The Gas Diffusion Layer (GDL) is located between the catalytic layer and the bipolar plate, and mainly functions to support the catalytic layer, collect current, and transmit reaction gas and water generated by the reaction.
A typical gas diffusion layer is generally composed of a support layer, the substrate of which is mainly composed of a porous material such as carbon fiber paper, and a microporous layer composed of carbon powder and hydrophobic Polytetrafluoroethylene (PTFE). One of the main parameters for measuring the quality of the gas diffusion layer is electrical conductivity, which is mainly determined by the material, and the other is water drainage and gas conductivity, which determines the diffusion of reaction gas and the drainage of water generated by the reaction, thereby greatly affecting the performance of the battery.
In order to meet the drainage and electric conduction functions of the gas diffusion layer widely applied at present, PTFE emulsion is adopted for impregnation and carbon paper is used as a matrix for solving the problems. However, the porosity is low, gas channels are not ideal, and the battery performance is reduced under the condition of large-current discharge. And under the long-term operating environment of the fuel cell, the carbon black material is gradually oxidized, so that the microporous layer becomes hydrophilic, the mass transfer polarization is increased, and the service life and the stability of the cell are shortened.
Disclosure of Invention
The invention aims to provide a fuel cell gas diffusion layer with small internal resistance, excellent water management performance and long service life, and also provides a preparation method of the fuel cell gas diffusion layer.
The invention is realized by the following scheme:
the fuel cell gas diffusion layer is prepared by coating gas diffusion layer slurry on one surface of carbon paper and then sintering, wherein the gas diffusion layer slurry comprises PTFE (polytetrafluoroethylene), carbon powder and porous nano-fibrous nickel powder, the solid content of the gas diffusion layer slurry is 2.2% -3.75%, and the mass ratio of the carbon powder to the porous nano-fibrous nickel powder is (1-5): 1, the mass of the PTFE is 10% -25% of the total mass of the carbon powder and the porous nano fibrous nickel powder, and the solid loading capacity on the carbon paper is 1-3 mg/cm2。
The preparation method of the fuel cell gas diffusion layer comprises the following steps:
adding nano fibrous iron-nickel alloy powder into an excessive acid solution, stirring for a certain time, filtering, washing filter residues to be neutral, and drying the filter residues to obtain porous nano fibrous nickel powder; stirring in an acid solution for 0.5-5 h generally, dissolving iron metal in the nano fibrous iron-nickel alloy powder in the acid solution, and washing filter residues with deionized water generally; the drying treatment process generally comprises the following steps: placing the filter residue in an oven at 70-90 ℃ for 3-5 h;
II, adding carbon powder and the porous nano fibrous nickel powder prepared in the step I into an alcohol solution containing a dispersing agent according to a certain mass ratio, uniformly stirring and dispersing to obtain a suspension, wherein the stirring time is generally controlled to be 2-5 h, ultrasonic dispersion is adopted, the dispersing time is generally controlled to be 0.5-2 h, the mass percentage of the dispersing agent in the alcohol solution is 0.1-1%, and the solid content of the suspension is controlled to be 2-3%; the preparation process of the alcohol solution containing the dispersing agent comprises the following specific steps: dissolving a dispersing agent in an alcohol solution with the mass concentration of 50-90% and uniformly stirring;
III, adding a water repellent into the suspension prepared in the step II, and uniformly dispersing to obtain gas diffusion layer slurry, wherein the solid content of the gas diffusion layer slurry is controlled to be 2.2-3.75%; ultrasonic dispersion is adopted, and the dispersion time is generally controlled to be 0.5-2 h;
IV, coating the gas diffusion layer slurry prepared in the step III on one surface of the carbon paper subjected to dipping and sintering treatment at the ambient temperature of 60-90 ℃, finally, placing the carbon paper coated with the gas diffusion layer slurry in a heat treatment device filled with protective gas and at the temperature of 300-450 ℃ for sintering treatment for 3-5 hours, wherein the solid loading capacity on the carbon paper is controlled to be 1-3 mg/cm2The solid loading on the carbon paper is controlled by the spraying flow and the spraying frequency or time of an ultrasonic spraying instrument and the like.
In the step II, the mass ratio of the carbon powder to the porous nano fibrous nickel powder is (1-5): 1.
in the step III, the water repellent is PTFE solution, and the mass of PTFE is 10-25% of the total mass of the carbon powder and the porous nano fibrous nickel powder added in the step II. The concentration of the PTFE solution can be selected according to the needs, and is generally selected to be 10-25%.
In the step I, the acid solution is a hydrochloric acid solution or a sulfuric acid solution; in the step II, the alcoholic solution is one or more of an isopropanol solution, an ethanol solution and an ethylene glycol solution, and the dispersing agent is polyvinylpyrrolidone or alkylphenol polyoxyethylene.
The dipping and sintering treatment process of the carbon paper comprises the following specific steps: the carbon paper is soaked in a water repellent with the mass concentration of 10% -25% and subjected to vacuum pumping treatment for 1-2 hours, and the carbon paper is taken out, dried and then placed in a heat treatment device filled with protective gas and at the temperature of 300-450 ℃ for sintering treatment for 3-5 hours.
The protective gas is one or more of nitrogen and inert gas.
The fuel cell gas diffusion layer has the advantages of small internal resistance, excellent water management performance and long service life, and the porosity and the electric conductivity of the fuel cell gas diffusion layer are high by adding the porous nano fibrous nickel powder into the slurry and controlling the mass ratio of the carbon powder to the porous nano fibrous nickel powder. The preparation method of the fuel cell gas diffusion layer is simple and feasible.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the description of the examples.
Example 1
A preparation method of a gas diffusion layer of a fuel cell comprises the following steps:
i, soaking 5cm multiplied by 5cm carbon paper with the thickness of 200 mu m in a PTFE solution with the mass concentration of 10%, vacuumizing for 1 hour, taking out, drying, and sintering in an oven filled with nitrogen and at the temperature of 300 ℃ for 5 hours;
II, adding the nano fibrous iron-nickel alloy powder into an excessive hydrochloric acid solution, stirring for 2 hours, filtering, washing filter residues to be neutral by using deionized water, and drying the filter residues to obtain porous nano fibrous nickel powder;
III, dissolving polyvinylpyrrolidone (PVP) in an isopropanol solution with the mass concentration of 50% and uniformly stirring, wherein the mass ratio of the PVP is controlled to be 0.5%;
IV, adding 1.5g of carbon powder and 1.5g of the porous nano fibrous nickel powder prepared in the step II into 97g of the isopropanol solution prepared in the step III, stirring at a high speed for 2 hours, and then performing ultrasonic dispersion for 2 hours to obtain a suspension;
v, adding 3g of PTFE solution with the mass concentration of 10% into the suspension prepared in the step IV, and performing ultrasonic dispersion for 1h to obtain gas diffusion layer slurry;
and VI, spraying the gas diffusion layer slurry prepared in the step V on one surface of the carbon paper obtained by the step I by using an ultrasonic spraying instrument under the condition that the ambient temperature is 80 ℃, controlling the spraying flow of the ultrasonic spraying instrument to be 5ml/min and the reciprocating spraying time to be 10min, and finally sintering the carbon paper coated with the gas diffusion layer slurry in an oven which is filled with nitrogen and has the temperature of 350 ℃ for 4h to obtain the gas diffusion layer of the fuel cell.
The fuel cell gas diffusion layer prepared in example 1 was tested and the solid loading on the carbon paper was 2mg/cm2. The gas diffusion layer of the fuel cell prepared in example 1 was fabricated into a membrane electrode, and the internal resistance of the membrane electrode was measured to be 0.00008 ohm/cm2。
Example 2
A preparation method of a gas diffusion layer of a fuel cell comprises the following steps:
i, soaking carbon paper of 5cm multiplied by 5cm and 200 mu m in a PTFE solution with the mass concentration of 20%, vacuumizing for 2 hours, taking out, drying, and sintering in an oven filled with inert gas and at the temperature of 450 ℃ for 3 hours;
II, adding the nano fibrous iron-nickel alloy powder into an excessive sulfuric acid solution, stirring for 3.5 hours, filtering, washing filter residues to be neutral by using deionized water, and drying the filter residues to obtain porous nano fibrous nickel powder;
III, dissolving Alkylphenol Polyoxyethylene Ether (APEO) in an ethanol solution with the mass concentration of 70% and uniformly stirring, wherein the mass ratio of the APEO is controlled to be 0.2%;
IV, adding 3g of carbon powder and 1g of the porous nano fibrous nickel powder prepared in the step II into 156g of the ethanol solution prepared in the step III, stirring at a high speed for 3.5h, and then performing ultrasonic dispersion for 1h to obtain a suspension;
v, adding 10g of PTFE solution with the mass concentration of 10% into the suspension prepared in the step IV, and performing ultrasonic dispersion for 2 hours to obtain gas diffusion layer slurry;
and VI, spraying the gas diffusion layer slurry prepared in the step V on one surface of the carbon paper obtained by the step I by using an ultrasonic spraying instrument at the ambient temperature of 90 ℃, controlling the spraying flow of the ultrasonic spraying instrument to be 5ml/min and the reciprocating spraying time to be 15min, and finally placing the carbon paper coated with the gas diffusion layer slurry in an oven filled with inert gas and at the temperature of 450 ℃ for sintering treatment for 3h to obtain the gas diffusion layer of the fuel cell.
The fuel cell gas diffusion layer prepared in example 2 was testedThe solid loading on the carbon paper was 3mg/cm2. The gas diffusion layer of the fuel cell prepared in example 2 was fabricated into a membrane electrode, and the internal resistance of the membrane electrode was measured to be 0.00012 ohm/cm2。
Example 3
A preparation method of a gas diffusion layer of a fuel cell comprises the following steps:
i, soaking carbon paper of 5cm multiplied by 5cm and 200 mu m in a PTFE solution with the mass concentration of 25%, vacuumizing for 2 hours, taking out, drying, and sintering in an oven filled with nitrogen and inert gas and at the temperature of 350 ℃ for 4 hours;
II, adding the nano fibrous iron-nickel alloy powder into an excessive sulfuric acid solution, stirring for 4 hours, filtering, washing filter residues to be neutral by using deionized water, and drying the filter residues to obtain porous nano fibrous nickel powder;
III, dissolving Alkylphenol Polyoxyethylene Ether (APEO) in 90% glycol solution by mass concentration and uniformly stirring, wherein the mass percentage of the APEO is controlled to be 1%;
IV, adding 4g of carbon powder and 0.8g of the porous nano fibrous nickel powder prepared in the step II into 235g of the ethylene glycol solution prepared in the step III, stirring at a high speed for 5 hours, and then performing ultrasonic dispersion for 0.5 hour to obtain a suspension;
v, adding 7.2g of PTFE solution with the mass concentration of 10% into the suspension prepared in the step IV, and performing ultrasonic dispersion for 0.8h to obtain gas diffusion layer slurry;
and VI, spraying the gas diffusion layer slurry prepared in the step V on one surface of the carbon paper obtained by the step I by using an ultrasonic spraying instrument under the condition that the ambient temperature is 60 ℃, controlling the spraying flow of the ultrasonic spraying instrument to be 5ml/min and the reciprocating spraying time to be 8min, and finally placing the carbon paper coated with the gas diffusion layer slurry in an oven which is filled with nitrogen and has the temperature of 300 ℃ for sintering treatment for 5h to obtain the gas diffusion layer of the fuel cell.
The fuel cell gas diffusion layer prepared in example 3 was tested and the solid loading on carbon paper was 1.5mg/cm2. The gas diffusion layer of the fuel cell prepared in example 3 was fabricated into a membrane electrode, and the internal resistance of the membrane electrode was measured to be 0.0001Ohm/cm2。
Claims (3)
1. A method of preparing a gas diffusion layer for a fuel cell, comprising: the method comprises the following steps:
adding nano fibrous iron-nickel alloy powder into an excessive acid solution, stirring for a certain time, filtering, washing filter residues to be neutral, and drying the filter residues to obtain porous nano fibrous nickel powder;
II, adding carbon powder and the porous nano fibrous nickel powder prepared in the step I into an alcoholic solution containing a dispersing agent according to a certain mass ratio, uniformly stirring and dispersing to obtain a suspension, wherein the mass ratio of the dispersing agent in the alcoholic solution is 0.1-1%, and the solid content of the suspension is controlled to be 2-3%; the mass ratio of the carbon powder to the porous nano fibrous nickel powder is (1-5): 1;
III, adding a water repellent into the suspension prepared in the step II, and uniformly dispersing to obtain gas diffusion layer slurry, wherein the solid content of the gas diffusion layer slurry is controlled to be 2.2-3.75%; the water repellent is PTFE solution, and the mass of PTFE is 10-25% of the total mass of the carbon powder and the porous nano fibrous nickel powder added in the step II;
IV, coating the gas diffusion layer slurry prepared in the step III on one surface of the carbon paper subjected to dipping and sintering treatment at the ambient temperature of 60-90 ℃, finally, placing the carbon paper coated with the gas diffusion layer slurry in a heat treatment device filled with protective gas and at the temperature of 300-450 ℃ for sintering treatment for 3-5 hours, wherein the solid loading capacity on the carbon paper is controlled to be 1-3 mg/cm2。
2. The method of preparing a gas diffusion layer for a fuel cell according to claim 1, wherein: in the step I, the acid solution is a hydrochloric acid solution or a sulfuric acid solution; in the step II, the alcoholic solution is one or more of an isopropanol solution, an ethanol solution and an ethylene glycol solution, and the dispersing agent is polyvinylpyrrolidone or alkylphenol polyoxyethylene.
3. The method of producing a gas diffusion layer for a fuel cell according to claim 1 or 2, wherein: the dipping and sintering treatment process of the carbon paper comprises the following specific steps: the carbon paper is soaked in a water repellent with the mass concentration of 10% -25% and subjected to vacuum pumping treatment for 1-2 hours, and the carbon paper is taken out, dried and then placed in a heat treatment device filled with protective gas and at the temperature of 300-450 ℃ for sintering treatment for 3-5 hours.
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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 |
| CN111628183B (en) * | 2020-05-27 | 2022-12-13 | 先进储能材料国家工程研究中心有限责任公司 | Preparation method of fuel cell catalyst slurry |
| CN111900416A (en) * | 2020-07-31 | 2020-11-06 | 齐鲁工业大学 | Preparation method and application of carbon paper impregnating resin for fuel cell gas diffusion layer |
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| CN101286564A (en) * | 2008-05-28 | 2008-10-15 | 中国科学院上海微***与信息技术研究所 | Composite anode for direct methanol fuel cell and method for making the same |
| JP2011076848A (en) * | 2009-09-30 | 2011-04-14 | Dainippon Printing Co Ltd | Micro porous layer for fuel cell, gas diffusion electrode with micro porous layer, catalyst layer with micro porous layer, gas diffusion electrode with catalyst layer, membrane electrode assembly, and polymer electrolyte fuel cell |
| CN105014064A (en) * | 2015-07-22 | 2015-11-04 | 常州市好利莱光电科技有限公司 | Method for manufacturing nanofiber material by means of iron-nickel alloy pipe |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101286564A (en) * | 2008-05-28 | 2008-10-15 | 中国科学院上海微***与信息技术研究所 | Composite anode for direct methanol fuel cell and method for making the same |
| JP2011076848A (en) * | 2009-09-30 | 2011-04-14 | Dainippon Printing Co Ltd | Micro porous layer for fuel cell, gas diffusion electrode with micro porous layer, catalyst layer with micro porous layer, gas diffusion electrode with catalyst layer, membrane electrode assembly, and polymer electrolyte fuel cell |
| CN105014064A (en) * | 2015-07-22 | 2015-11-04 | 常州市好利莱光电科技有限公司 | Method for manufacturing nanofiber material by means of iron-nickel alloy pipe |
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