CN111740120A - Membrane electrode, preparation method thereof and fuel cell - Google Patents

Membrane electrode, preparation method thereof and fuel cell Download PDF

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CN111740120A
CN111740120A CN202010625308.0A CN202010625308A CN111740120A CN 111740120 A CN111740120 A CN 111740120A CN 202010625308 A CN202010625308 A CN 202010625308A CN 111740120 A CN111740120 A CN 111740120A
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transfer
catalyst
membrane electrode
film
catalyst layer
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段奔
潘牧
宛朝辉
刘素芬
郑伟倩
陈�峰
钟青
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Wuhan Technique New Sources Of Energy Co ltd
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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
    • H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
    • 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
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • 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
    • H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
    • 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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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Inert Electrodes (AREA)
  • Fuel Cell (AREA)

Abstract

The application provides a membrane electrode, a preparation method thereof and a fuel cell, and belongs to the technical field of membrane electrode preparation. The preparation method of the membrane electrode comprises the following steps: coating catalyst slurry on the transfer printing film, and drying to form a catalyst layer; wherein, the transfer printing film is a release film. Transferring the catalyst layer to the surface of the proton exchange membrane; wherein the transfer temperature is 20-80 deg.C, and the transfer pressure is 5-50kgf/cm2. The release film with low peeling force is used as the transfer film, transfer printing under low temperature and low pressure can be realized, and the transfer printing effect is better. The membrane electrode and the fuel cell prepared by the membrane electrode have better performance.

Description

Membrane electrode, preparation method thereof and fuel cell
Technical Field
The application relates to the technical field of membrane electrode preparation, in particular to a membrane electrode, a preparation method thereof and a fuel cell.
Background
The key components of a proton exchange membrane fuel cell include a proton exchange membrane, a catalytic layer, a gas diffusion layer, and a bipolar plate. Membrane Electrode Assemblies (MEAs) are the main parts of proton exchange Membrane fuel cell systems, and the structural design and preparation process technology of the MEA is one of the key points of fuel cell research, and determines the working performance of the fuel cell.
Among them, CCM type membrane electrodes are produced by a direct coating method and a transfer method. The transfer printing method is that the slurry is sprayed/printed on a transfer printing film and then transferred to a proton exchange membrane to form a catalyst layer; the direct spray coating method is to mix and prepare a catalyst and ion exchange resin to form slurry, and coat the slurry on a proton exchange membrane to form a catalytic layer. Compared with a direct spraying method, the transfer printing method has high efficiency and stable product performance, and is the current mainstream process.
In the prior art, in the process of preparing the CCM type membrane electrode by a transfer printing method, a commonly used transfer printing film is a polytetrafluoroethylene film or an aluminum foil film, the temperature and the pressure required by transfer printing are high, the transfer printing temperature is generally 140-.
Disclosure of Invention
A first object of the present application is to provide a method for preparing a membrane electrode, in which the transfer effect of the catalyst layer is good.
The second objective of the present application is to provide a membrane electrode prepared by the above preparation method and a fuel cell prepared by the membrane electrode, which have better electrical properties.
In a first aspect, the present application provides a method for preparing a membrane electrode, comprising the steps of: coating catalyst slurry on the transfer printing film, and drying to form a catalyst layer; wherein, the transfer printing film is a release film. Transferring the catalyst layer to the surface of the proton exchange membrane; wherein the transfer temperature is 20-80 deg.C, and the transfer pressure is 5-50kgf/cm2。
In one possible embodiment, the rotorPrinting temperature is 50-70 deg.C, and transfer pressure is 10-40kgf/cm2。
In one possible embodiment, the transfer film is selected from one of a fluoroplastic release film, a silicon-containing release film and a silicon-free release film.
In one possible embodiment, the solvent in the catalyst slurry comprises one or more of ethylene glycol, propylene glycol, butylene glycol, t-butanol, pentylene glycol.
In one possible embodiment, the catalyst slurry further comprises a catalyst and an ion exchange resin; the catalyst is a carbon-supported platinum catalyst or a carbon-supported platinum alloy catalyst, and the ion exchange resin is perfluorinated sulfonic acid resin.
In one possible embodiment, the drying temperature of the catalyst layer is 80 to 200 ℃.
In one possible embodiment, the mode of transferring the catalyst layer is flat transfer, and the transfer time is 10-60 s.
In one possible embodiment, the mode of transferring the catalyst layer is continuous roll transfer at a transfer speed of 5 to 10 m/min.
In a second aspect, the present application provides a membrane electrode prepared by the above preparation method.
In a third aspect, the present application provides a fuel cell comprising the membrane electrode described above.
The membrane electrode, the preparation method thereof and the fuel cell provided by the embodiment of the application have the beneficial effects that:
the transfer printing film with low peeling force is used as the transfer printing film, transfer printing under low temperature and low pressure can be realized, the transfer printing condition is easier to achieve, the catalyst on the transfer printing film is completely transferred, the proton exchange film cannot be damaged, and the transfer printing effect is better. The obtained membrane electrode has better electrical property, and the performance of the cell is better when the membrane electrode is used for preparing a fuel cell.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive efforts and also belong to the protection scope of the present application.
FIG. 1 is a flow chart of a method of making a membrane electrode provided by an embodiment of the present application;
FIG. 2 is a photograph of a membrane electrode provided in example 1 of the present application;
FIG. 3 is a photograph of a membrane electrode provided in comparative example 1 of the present application;
FIG. 4 is a photograph of a membrane electrode provided in comparative example 2 of the present application;
fig. 5 is a graph of the electrical performance of the membrane electrode provided herein.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.
Fig. 1 is a flowchart of a method for manufacturing a membrane electrode according to an embodiment of the present disclosure. Referring to fig. 1, the preparation method includes the following steps:
s10, coating catalyst slurry on the transfer printing film, and drying to form a catalyst layer; wherein, the transfer printing film is a release film.
The release film has lower peeling force, so that the catalyst layer can be more easily peeled on the transfer film.
Optionally, the transfer film is selected from one of a fluoroplastic release film, a silicon-containing release film and a silicon-free release film. For example: the transfer printing film is a fluoroplastic release film, or a silicon-containing release film or a silicon-free release film, and the transfer printing films are low-peeling-force release films. In other embodiments, the transfer film may also be other release films with low peel force, which are all within the protection scope of the present application.
However, if the peel force of the transfer film is low, the catalyst paste cannot be coated on the transfer film. The inventor researches and discovers that if the solvent in the catalyst slurry comprises one or more of ethylene glycol, propylene glycol, butanediol, tert-butyl alcohol and pentanediol, the surface tension of the catalyst slurry can be smaller, and the coating effect of the catalyst slurry on the release film can be good. The catalyst layer obtained by drying can be easily peeled off from the release film, and the catalyst slurry can form a more uniform catalyst layer on the release film, so that the preparation effect of the membrane electrode is better, and the performance of the membrane electrode is improved. Furthermore, the solvent is used as the solvent of the catalyst slurry, and other surfactants, thickeners and the like do not need to be added, so that the performance of the catalyst is not affected.
The catalyst slurry also includes a catalyst and an ion exchange resin. Wherein the catalyst is a conventional catalyst (for example, a carbon-supported platinum catalyst or a carbon-supported platinum alloy catalyst), and the ion exchange resin is a conventional ion exchange resin (for example, a perfluorosulfonic acid resin), which is not limited in the present application.
In the embodiment of the present application, if the solvent in the catalyst slurry includes one or more of ethylene glycol, propylene glycol, butylene glycol, t-butyl alcohol, and pentylene glycol, the drying temperature of the resulting catalyst layer is 80 to 200 ℃. The solvent is used for drying at the temperature, the release film cannot be damaged, the drying of the catalyst layer can be realized, and the obtained catalyst layer is more uniform. In some possible embodiments, the drying temperature of the catalyst layer is 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃ or 200 ℃.
S20, transferring the catalyst layer to the surface of the proton exchange membrane; wherein the transfer temperature is 20-80 deg.C, and the transfer pressure is 5-50kgf/cm2。
In the prior art, the transfer temperature of the catalyst layer is usually above 100 ℃, and the inventor researches and discovers that the temperature can damage the proton exchange membrane to a certain extent, residual or adsorbed liquid water in the catalyst layer and the proton exchange membrane can quickly form a gaseous state, and the discharge of the gaseous water can cause the problems of damage of the proton exchange membrane, incomplete transfer and the like.
Therefore, in the present application, since the release film is selected as the transfer film, the transfer temperature of the catalyst layer can be lowered to 20 to 80 ℃ (below 100 ℃) and the transfer pressure can be lowered to 5 to 50kgf/cm2. The transfer temperature can be keptAvoid high temperature to proton exchange membrane's damage, can not produce gaseous state water, avoid the formation of rendition in-process gaseous state water to strike proton exchange membrane, avoid proton exchange membrane's mechanical damage, the rendition temperature is more even, has promoted the rendition quality, improves membrane electrode's performance.
Alternatively, the transfer temperature of the catalyst layer is 50-70 ℃. In some possible embodiments, the transfer temperature of the catalyst layer is 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ or 80 ℃. Alternatively, the transfer pressure of the catalyst layer is 10 to 40kgf/cm2. In some possible embodiments, the transfer pressure of the catalyst layer is 5kgf/cm2、10kgf/cm2、20kgf/cm2、30kgf/cm2、40kgf/cm2Or 50kgf/cm2。
Further, in the present application, not only the transfer temperature and the transfer pressure can be reduced, but also the transfer time can be shortened. Alternatively, the manner of transferring the catalyst layer is flat press transfer, and the transfer time of the catalyst layer is 10 to 60 seconds. In some possible embodiments, the transfer time of the catalyst layer is 10s, 20s, 30s, 40s, 50s, or 60 s.
The transfer condition is easy to reach, and the transfer efficiency can be improved. The catalyst layer is transferred by continuous roll transfer, and the transfer speed of the catalyst layer can be 5-10 m/min. In some possible embodiments, the transfer speed of the catalyst layer may be 5m/min, 6m/min, 7m/min, 8m/min, 9m/min, or 10 m/min.
Therefore, the release film with low peeling force is used as the transfer film and matched with the solvent of the catalyst slurry, so that the transfer temperature can be reduced, the transfer pressure can be reduced, the transfer time can be shortened, the transfer speed is higher, the transfer condition can be easily achieved, and the transfer efficiency can be improved.
In the transfer printing process, the catalyst is completely transferred, the proton exchange membrane is not damaged, and the electrical property of the obtained membrane electrode is better. The performance of the fuel cell is better when the fuel cell is prepared by using the catalyst.
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: mixing 8 mass percent of carbon-supported platinum catalyst, 2 mass percent of perfluorinated sulfonic acid resin and 90 mass percent of ethylene glycol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of the fluoroplastic release film, and drying at 120 ℃ to form a catalyst layer.
(3) Attaching release films covered with catalyst layers on two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and performing flat-pressing transfer at a transfer temperature of 20 deg.C and a transfer pressure of 5kgf/cm2Is heated and pressed for 10s, and then taken out, and then the release film is removed to complete the transfer printing.
Example 2
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorosulfonic acid resin and 90 mass percent of tertiary butanol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of the silicon-containing release film, and drying at 80 ℃ to form a catalyst layer.
(3) Attaching release films covered with catalyst layers on two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and performing flat-pressing transfer at 40 deg.C and 20kgf/cm under pressure2Is heated and pressed for 30s, and then taken out, and then the release film is removed to finish the transfer printing.
Example 3
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorosulfonic acid resin and 90 mass percent of pentanediol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of the non-silicon release film, and drying at 200 ℃ to form a catalyst layer.
(3) Attaching release films covered with catalyst layers on two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and continuously rolling and transferring at 80 deg.C and 50kgf/cm under pressure2Is heated and pressed for 60s, and then taken out, and then the release film is removed to complete the transfer printing.
Example 4
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorosulfonic acid resin and 90 mass percent of propylene glycol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of the fluoroplastic release film, and drying at 140 ℃ to form a catalyst layer.
(3) Attaching release films covered with catalyst layers on two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and continuously rolling and transferring at a transfer temperature of 50 deg.C and a transfer pressure of 25kgf/cm2And rolling at a transfer speed of 7m/min, and removing the release film to complete transfer.
Comparative example 1
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorosulfonic acid resin and 90 mass percent of tertiary butanol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of a polytetrafluoroethylene membrane, and drying at 120 ℃ to form a catalyst layer.
(3) Attaching polytetrafluoroethylene films covered with catalyst layers on two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and performing flat-pressing transfer at a transfer temperature of 160 ℃ and a transfer pressure of 80kgf/cm2Is heated and pressed for 120s under the condition of (1), and then taken out, and then the polytetrafluoroethylene film is removed to finish the transfer printing.
Comparative example 2
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorosulfonic acid resin and 90 mass percent of tertiary butanol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of a polytetrafluoroethylene membrane, and drying at 120 ℃ to form a catalyst layer.
(3) Attaching polytetrafluoroethylene films covered with catalyst layers to two surfaces of the proton exchange membrane, contacting the catalyst layers with the proton exchange membrane, and performing flat-pressing transfer at a transfer temperature of 120 ℃ and a transfer pressure of 120kgf/cm2Is heated and pressed for 120s under the condition of (1), and then taken out, and then the polytetrafluoroethylene film is removed to finish the transfer printing.
Comparative example 3
The preparation method of the membrane electrode comprises the following steps:
(1) preparing catalyst slurry: mixing 6 mass percent of carbon-supported platinum catalyst, 4 mass percent of perfluorinated sulfonic acid resin, 2 mass percent of thickening agent, 38 mass percent of deionized water and 50 mass percent of ethanol to obtain catalyst slurry.
(2) And (2) uniformly coating the catalyst slurry obtained in the step (1) on the surface of the single-sided silicon-containing release film, so that a catalyst layer cannot be formed.
Experimental example 1
The peel force of the transfer film was measured and the transfer conditions were matched to obtain table 1.
The detection method of the peeling force of the transfer film comprises the following steps: a Desha 7475 adhesive tape with the width of 25mm is attached to the transfer printing film, the transfer printing film is pressed twice back and forth by a standard press roller with the weight of 2kg at the speed of 10mm/s, after 20min, the stripping angle is adjusted to be 180 degrees, the setting speed is 300mm/min, and the stripping force test is carried out.
TABLE 1 preparation parameters of membrane electrodes
Figure BDA0002563418400000081
Figure BDA0002563418400000091
As can be seen from table 1, the catalyst slurry using the solvent and the transfer film having a low peeling force were combined to make it easier to achieve the transfer conditions of the catalyst layer and to improve the transfer efficiency (examples 1 to 4).
If a transfer film with a high peel force is used, the transfer conditions of the catalyst layer are severe and the transfer efficiency is low (comparative example 1-comparative example 2).
If the surface tension of the catalyst paste is too large, the catalyst layer cannot be formed on the transfer film with low peeling force (comparative example 3).
Experimental example 2
Photographs were taken of the membrane electrodes provided in example 1, comparative example 1 and comparative example 2, respectively, to obtain fig. 2, fig. 3 and fig. 4. As can be seen from fig. 2, the catalyst layer is transferred under the mild transfer condition, so that the performance of the membrane electrode is better, the proton exchange membrane is not deformed at high temperature, and the transfer is complete. As can be seen from fig. 3, the transfer temperature is too high, reaching 160 ℃, which may damage the proton exchange membrane and deform it. As can be seen from fig. 4, the transfer temperature was high, 120 ℃, and the transfer could not be completed.
Fig. 5 was obtained by measuring the electrical properties of the membrane electrode provided in example 1 and the membrane electrode provided in comparative example 1, respectively. As can be seen from fig. 5, the membrane electrode prepared by the membrane electrode preparation method provided in example 1 has better performance.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. 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 application.

Claims (10)

1. A preparation method of a membrane electrode is characterized by comprising the following steps:
coating catalyst slurry on the transfer printing film, and drying to form a catalyst layer; wherein the transfer printing film is a release film;
transferring the catalyst layer to the surface of the proton exchange membrane; wherein the transfer temperature is 20-80 deg.C, and the transfer pressure is 5-50kgf/cm2。
2. The production method according to claim 1, wherein the transfer temperature is 50 to 70 ℃, and the transfer pressure is 10 to 40kgf/cm2。
3. The manufacturing method according to claim 1, wherein the transfer film is selected from one of a fluoroplastic release film, a silicon-containing release film and a silicon-free release film.
4. The method of claim 1, wherein the solvent in the catalyst slurry comprises one or more of ethylene glycol, propylene glycol, butylene glycol, t-butanol, and pentylene glycol.
5. The production method according to claim 4, wherein the catalyst slurry further comprises a catalyst and an ion exchange resin;
the catalyst is a carbon-supported platinum catalyst or a carbon-supported platinum alloy catalyst, and the ion exchange resin is perfluorinated sulfonic acid resin.
6. The production method according to claim 5, wherein the drying temperature of the catalyst layer is 80 to 200 ℃.
7. The production method according to any one of claims 1 to 6, wherein the manner of transferring the catalyst layer is flat-press transfer, and the transfer time is 10 to 60 seconds.
8. The production method according to any one of claims 1 to 6, wherein the manner of transferring the catalyst layer is continuous roll transfer at a transfer speed of 5 to 10 m/min.
9. A membrane electrode produced by the method for producing a membrane electrode according to any one of claims 1 to 8.
10. A fuel cell comprising the membrane electrode of claim 9.
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