CN113793962B - Fuel cell adhesive and preparation method and application thereof - Google Patents
Fuel cell adhesive and preparation method and application thereof Download PDFInfo
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- CN113793962B CN113793962B CN202110919845.0A CN202110919845A CN113793962B CN 113793962 B CN113793962 B CN 113793962B CN 202110919845 A CN202110919845 A CN 202110919845A CN 113793962 B CN113793962 B CN 113793962B
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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
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1041—Polymer electrolyte composites, mixtures or blends
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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
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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
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
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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
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
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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
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
- H01M8/1081—Polymeric electrolyte materials characterised by the manufacturing processes starting from solutions, dispersions or slurries exclusively of polymers
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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
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Abstract
The invention belongs to the technical field of fuel cells, and particularly relates to a fuel cell adhesive, which is prepared by mixing perfluoro sulfonic resin with a short side chain and polytetrafluoroethylene PTFE emulsion to be used as an adhesive matrix, mixing the perfluoro sulfonic resin with the PTFE emulsion with a surfactant to form micelles, and mixing the micelles with a Pt/C catalyst to prepare slurry with uniform dispersion. The fuel cell adhesive has excellent proton conductivity, good water transmission performance and good dispersibility, wherein the perfluorinated sulfonic acid resin and PTFE emulsion exist in the form of micelle under the action of a surfactant, and the dispersion effect is good; in addition, the perfluorinated sulfonic acid resin with a short side chain can increase the binding site of water in the catalytic layer, so that a rich proton transmission network is constructed, and the proton transmission capacity of the catalytic layer is improved; the proper amount of hydrophobic PTFE emulsion can improve the hydrophobic channel and microstructure of the catalytic layer and improve the water transmission performance of the catalytic layer.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a fuel cell adhesive and a preparation method and application thereof.
Background
Polymer electrolyte membrane fuel cells are widely studied for their current and potential use in the electronics market, including the automotive industry and stationary and portable power generation equipment. Proton exchange membrane fuel cells have proven to be a competitive power source due to their high power density, fast start-up, reliability and portability. The presence of the catalyst coating CCM (catalys coated membrane) provides a guarantee in terms of fuel cell performance improvement and cost reduction. The binder in CCM is an important component connecting the catalyst and the proton exchange membrane, and the composition and performance of the binder are critical. The proton conductivity of the catalytic layer is improved by adding the adhesive Nafion into the catalytic layer, and although the proton conductivity of the catalytic layer is improved by adding the hydrophilic Nafion, the Nafion is an insulator and cannot conduct electrons, and the utilization rate of the catalyst is negatively affected by the excessive Nafion content or agglomeration. In addition, nafion is hydrophilic resin, has no hydrophobic network and gas phase channels, is difficult to transmit reaction gas in a high current density area and is very easy to block an output channel for generating water to cause flooding of an electrode, and simultaneously can cause catalyst to fall off, thereby influencing the performance and service life of the electrode.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a fuel cell binder, a preparation method thereof and application as catalyst ink aiming at the defects existing in the prior art.
The invention adopts the technical proposal for solving the problems that:
a kind of fuel cell adhesive, adopt short side chain perfluorosulfonic acid resin solution and Polytetrafluoroethylene (PTFE) emulsion to mix as the adhesive matrix, then add surfactant and deionized water to mix the adhesive matrix and form micelle, then mix with Pt/C catalyst and prepare into sizing agent of uniform composition, namely the fuel cell adhesive; wherein the short side chain perfluorinated sulfonic acid resin solution is a perfluorinated sulfonic acid resin solution with short side chain and low EW value, the EW value is between 700 and 800, and the side chain structure is-O-CF 2- CF 2 -SO 3 H。
According to the scheme, the concentration of the polytetrafluoroethylene emulsion is 50-70wt%.
According to the scheme, the surfactant is one or more of sodium fatty alcohol polyoxyethylene ether sulfate, sodium dodecyl sulfate, alkyl alcohol amide, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and the like.
According to the scheme, the concentration of the short-side-chain perfluorinated sulfonic acid resin solution is 1% -10%.
According to the scheme, the mass ratio of the short side chain perfluorinated sulfonic acid resin solution, the surfactant, the polytetrafluoroethylene emulsion, the deionized water and the Pt/C catalyst is 1:0.04: (0.2-1): 30:3.
the preparation method of the fuel cell adhesive comprises the steps of uniformly mixing a short side chain perfluorinated sulfonic acid resin solution, polytetrafluoroethylene emulsion, a surfactant and deionized water; and then adding a Pt/C catalyst, and obtaining the fuel cell adhesive after ultrasonic and stirring of the obtained mixed solution.
The fuel cell binder of the present invention can be directly applied as a catalyst ink in a catalyst coated film. The specific application method is as follows:
1) Transferring the binder serving as the catalyst ink to a perfluorosulfonic acid proton exchange membrane to obtain a catalyst coating membrane primary product; wherein the thickness of the anode catalytic coating film is controlled to be 3-5 micrometers, and the Pt loading is 0.1mg/cm 2 Left and right (deviation not more than + -0.05 mg/cm) 2 ) The method comprises the steps of carrying out a first treatment on the surface of the The thickness of the cathode catalyst coating film is controlled to be 8-12 microns, and the Pt loading is 0.4mg/cm 2 Left and right (deviation not more than + -0.05 mg/cm) 2 );
2) Sodium treatment and heat treatment are carried out on the catalyst coating film primary product obtained in the step 1) to obtain a catalyst coating film product; wherein the sodium treatment is carried out in sodium hydroxide solution; the heat treatment temperature is 300-350 deg.c and the heat treatment time is 20-40 min.
Compared with the prior art, the invention has the following advantages and beneficial effects:
unlike common adhesive with adhesive effect, the fuel cell adhesive of the present invention is prepared with hydrophobic PTFE emulsion and short side chain perfluorinated sulfonic acid resin as the matrix of the adhesive, pt/C catalyst, surfactant and deionized water as supplementary material, and has excellent proton conductivity, high water transmission performance and high dispersivity, and may be used as catalyst ink for directly applying in catalyst coating film. Wherein, the perfluorinated sulfonic acid resin and PTFE emulsion exist in micelle under the action of the surfactant, and the dispersion effect is good; in addition, the perfluorinated sulfonic acid resin with a short side chain can increase the binding site of water in the catalytic layer, so that a rich proton transmission network is constructed, and the proton transmission capacity of the catalytic layer is improved; the proper amount of hydrophobic PTFE emulsion can improve the hydrophobic channel and microstructure of the catalytic layer and improve the water transmission performance of the catalytic layer.
Drawings
Fig. 1 is an SEM electron microscope image of the fuel cell binder prepared in example 1.
FIG. 2 is a graph showing the voltage and power density test results for the CCM product of example 1 under two test conditions. The test condition I is that the anode humidity is 20% RH, the cathode humidity is 100% RH, and the test condition II is that the anode humidity is 100% RH, and the cathode humidity is 100% RH.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the invention further, but are not to be construed as limiting the invention.
In the following examples, the short-side-chain perfluorosulfonic acid resin solution was specifically perfluorosulfonic acid Aquivion D79-25BS from Suwei corporation, USA, and the perfluorosulfonic acid resin concentration was 5% and the EW value was 790.
In the examples below, the concentration of the PTFE emulsion was 60% by weight, obtained from Miao, chemie, inc.; pt/C is JM catalyst, platinum content is about 20%, chloride is less than 300ppm, and particle size is less than 3.5nm.
In the examples below, the proton exchange membrane was a perfluorosulfonic acid proton exchange membrane having an EW of about 1000, and is specifically a commercial dupont Nafion115 membrane.
Example 1
A preparation method of a fuel cell adhesive comprises the following steps:
(1) The mass ratio of Pt/C is that the short side chain perfluorinated sulfonic acid resin solution comprises sodium dodecyl sulfate: PTFE emulsion, deionized water=3:1:0.04:1:30, is prepared for standby;
(2) Uniformly mixing the short side chain perfluorinated sulfonic acid resin solution, PTFE emulsion, surfactant and deionized water, adding Pt/C catalyst, and carrying out ultrasonic treatment for 8 minutes, high-speed stirring for 2 hours (the rotating speed is 5000 rpm) and ultrasonic treatment for 5 minutes to obtain the fuel cell adhesive.
As can be seen from fig. 1, the fuel cell adhesive prepared in example 1 can be observed under SEM electron microscope to form uniform spheroids of sample micelles, and the micelles are about 200nm, which indicates that the perfluorinated sulfonic acid resin with short side chains and polytetrafluoroethylene PTFE initially form micelle forms in the sample, so that better dispersibility is achieved.
The above-described fuel cell binder can be directly applied as a catalyst ink in a catalyst coated film. The specific application method is as follows:
1) Transferring the binder as a catalyst ink to a Nafion film, controlling the thickness of the anode catalytic layer to be about 4 microns, and controlling the Pt loading to be about 0.1mg/cm 2 The cathode catalyst layer thickness was controlled to be about 10 microns and the Pt loading was about 0.4mg/cm 2 Obtaining a catalyst coating film primary product;
2) And (2) placing the catalyst coating film initial product obtained in the step (1) in a 1mol/L NaOH solution for 12 hours for sodium treatment, and then performing heat treatment at the temperature of about 330 ℃ for 30 minutes to enable PTFE in the catalytic layer to be melted and fibrillated at a high temperature, so as to obtain a catalyst coating film (CCM) product.
As can be seen from FIG. 2, the CCM sample was tested in the low current density region (less than 1000mA/cm 2 ) The power density under both test conditions was almost the same, in the high current density region (greater than 1000mA/cm 2 ) The anode is tested at 100% RH and the anode is tested at slightly higher than 20% RH. The test condition I is that the anode humidity is 20% RH, the cathode humidity is 100% RH, the test condition II is that the anode humidity is 100% RH, and the cathode humidity is 100% RH, and the existence of a water concentration gradient in a membrane when the fuel cell floods is simulated by changing the water content of the anode side under the two conditions. According to analysis of test results, the CCM sample prepared by the binder has strong water balance capacity, strong water transmission capacity and good proton conductivity, and can transfer protons better through excellent water concentration gradient difference in the water transmission balance membrane to a certain extent, so that good electrochemical performance is obtained.
Example 2
A preparation method of a fuel cell adhesive comprises the following steps:
(1) The mass ratio of Pt/C is that the short side chain perfluorinated sulfonic acid resin solution comprises sodium dodecyl sulfate: PTFE emulsion, deionized water=3:1:0.04:0.2:30, and each raw material is prepared for standby;
(2) Uniformly mixing the short side chain perfluorinated sulfonic acid resin solution, PTFE emulsion, surfactant and deionized water, adding Pt/C catalyst, and carrying out ultrasonic treatment for 8 minutes, high-speed stirring for 2 hours (the rotating speed is 5000 rpm) and ultrasonic treatment for 5 minutes to obtain the fuel cell adhesive.
The above-described fuel cell binder can be directly applied as a catalyst ink in a catalyst coated film. The specific application method is as follows:
1) Transferring the binder as a catalyst ink to a Nafion film, controlling the thickness of the anode catalytic layer to be about 4 microns, and controlling the Pt loading to be about 0.1mg/cm 2 The cathode catalyst layer thickness was controlled to be about 10 microns and the Pt loading was about 0.4mg/cm 2 Obtaining a catalyst coating film primary product;
2) And (2) placing the catalyst coating film initial product obtained in the step (1) in a 1mol/L NaOH solution for 12 hours for sodium treatment, and then performing heat treatment at the temperature of about 330 ℃ for 30 minutes to enable PTFE in the catalytic layer to be melted and fibrillated at a high temperature, so as to obtain a catalyst coating film (CCM) product.
Example 3
A preparation method of a fuel cell adhesive comprises the following steps:
(1) The mass ratio of Pt/C is that the short side chain perfluorinated sulfonic acid resin solution comprises sodium dodecyl sulfate: PTFE emulsion, deionized water=3:1:0.04:0.5:30, and each raw material is prepared for standby;
(2) Uniformly mixing the short side chain perfluorinated sulfonic acid resin solution, PTFE emulsion, surfactant and deionized water, adding Pt/C catalyst, and carrying out ultrasonic treatment for 8 minutes, high-speed stirring for 2 hours (the rotating speed is 5000 rpm) and ultrasonic treatment for 5 minutes to obtain the fuel cell adhesive.
The above-described fuel cell binder can be directly applied as a catalyst ink in a catalyst coated film. The specific application method is as follows:
1) Transferring the binder as a catalyst ink to a Nafion film, controlling the thickness of the anode catalytic layer to be about 4 microns, and controlling the Pt loading to be about 0.1mg/cm 2 The cathode catalyst layer thickness was controlled to be about 10 microns and the Pt loading was about 0.4mg/cm 2 Obtaining a catalyst coating film primary product;
2) And (2) placing the catalyst coating film initial product obtained in the step (1) in a 1mol/L NaOH solution for 12 hours for sodium treatment, and then performing heat treatment at the temperature of about 330 ℃ for 30 minutes to enable PTFE in the catalytic layer to be melted and fibrillated at a high temperature, so as to obtain a catalyst coating film (CCM) product.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and changes can be made by those skilled in the art without departing from the inventive concept and remain within the scope of the invention.
Claims (5)
1. A kind of fuel cell adhesive, characterized by that adopt short side chain perfluorosulfonic acid resin solution and polytetrafluoroethylene emulsion mix as the adhesive matrix, then add surfactant and deionized water to mix the adhesive matrix and form the micelle, mix with Pt/C catalyst and prepare and disperse the homogeneous sizing agent, namely the fuel cell adhesive;
the short side chain perfluorinated sulfonic acid resin solution is a perfluorinated sulfonic acid resin solution with short side chain and low EW value, the EW value is between 700 and 800, and the side chain structure is-O-CF 2 -CF 2 -SO 3 H;
The mass ratio of the short side chain perfluorinated sulfonic acid resin solution to the surfactant to the polytetrafluoroethylene emulsion to the deionized water to the Pt/C catalyst is 1:0.04: (0.2-1): 30:3, a step of; the concentration of the polytetrafluoroethylene emulsion is 50-70wt%; the mass concentration of the short side chain perfluorinated sulfonic acid resin solution is 1% -10%;
the surfactant is one or more of fatty alcohol polyoxyethylene ether sodium sulfate, sodium dodecyl sulfate, alkyl alcohol amide, fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene.
2. The method for preparing a fuel cell adhesive according to claim 1, wherein the short-side-chain perfluorosulfonic acid resin solution is uniformly mixed with polytetrafluoroethylene emulsion, a surfactant and deionized water; and then adding a Pt/C catalyst, and obtaining the fuel cell adhesive after ultrasonic and stirring of the obtained mixed solution.
3. Use of the binder of claim 1 as a catalyst ink in a catalyst coated film.
4. Use according to claim 3, characterized in that the specific application method is as follows:
1) Transferring the binder serving as the catalyst ink to a perfluorosulfonic acid proton exchange membrane to obtain a catalyst coating membrane primary product;
2) And (3) carrying out sodium treatment and heat treatment on the catalyst coating film primary product obtained in the step (1) to obtain a catalyst coating film product.
5. The process according to claim 4, wherein in step 1), the anode catalyst coating film thickness is controlled to 3-5 μm, and the Pt loading is 0.1.+ -. 0.05mg/cm 2 The film thickness of the cathode catalyst coating layer is controlled to be 8-12 microns, and the Pt loading is 0.4+/-0.05 mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the In step 2), the sodium treatment is carried out in sodium hydroxide solution; the heat treatment temperature is 300-350 deg.c and the heat treatment time is 20-40 min.
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