CN111162299A - Method for preparing membrane electrode of low-temperature proton exchange membrane fuel cell - Google Patents

Method for preparing membrane electrode of low-temperature proton exchange membrane fuel cell Download PDF

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CN111162299A
CN111162299A CN201911413174.XA CN201911413174A CN111162299A CN 111162299 A CN111162299 A CN 111162299A CN 201911413174 A CN201911413174 A CN 201911413174A CN 111162299 A CN111162299 A CN 111162299A
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electrode
proton exchange
fuel cell
exchange membrane
gas diffusion
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章俊良
吴爱明
朱凤鹃
夏国锋
罗柳轩
柯长春
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Shanghai Jiaotong University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00Fuel cells; Manufacture thereof
    • H01M8/10Fuel cells with solid electrolytes
    • H01M8/1004Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8825Methods for deposition of the catalytic active composition
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90Selection of catalytic material
    • H01M4/92Metals of platinum group
    • H01M4/925Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a preparation method of a membrane electrode of a low-temperature proton exchange membrane fuel cell; the method comprises the following steps: preparation of microporous layer (MPL) on surface of carbon paper: printing a mixed solution of carbon powder and PTFE on the surface of the carbon paper subjected to hydrophobic treatment, drying, placing the carbon paper in an inert atmosphere for high-temperature treatment, and cooling to obtain a Gas Diffusion Layer (GDL) with an MPL layer on the surface; directly depositing Pt nano particles on the MPL layer by adopting an Atomic Layer Deposition (ALD) technology to form a continuous Gas Diffusion Electrode (GDE); uniformly spraying the ionic resin on the electrode; the membrane electrode is assembled by a cathode gas electrode, a proton exchange membrane and an anode gas diffusion electrode. The catalyst layer prepared by the atomic layer deposition technology is very clean, the thin catalyst layer is favorably prepared, the pore structure is rich, the uniformity is good, the traditional idea that catalyst slurry is prepared firstly and then the electrode catalyst layer is prepared is broken through, and the membrane electrode prepared by the method is favorable for improving the performance of a large-current density area of the fuel cell.

Description

Method for preparing membrane electrode of low-temperature proton exchange membrane fuel cell
Technical Field
The invention relates to the field of proton exchange membrane fuel cells, in particular to a preparation method of a membrane electrode of a low-temperature proton exchange membrane fuel cell.
Background
Hydrogen energy is considered as the ultimate solution for automobile energy, and Proton Exchange Membrane Fuel Cell (PEMFC) is a very important energy source for converting hydrogen energy into electric energy, and its energy conversion efficiency is as high as 60% -70%. The hydrogen fuel cell has the outstanding characteristics of low working temperature (about 80 ℃), long service life, quick response to load change, high energy density, environmental friendliness and the like, and can be widely applied to various modern vehicles and other aspects.
The membrane electrode is a core component of the proton exchange membrane fuel cell and is a place for converting hydrogen energy into electric energy. A typical fuel cell membrane electrode consists of a cathode gas diffusion layer, a cathode catalytic layer, a proton exchange membrane, an anode catalytic layer, and an anode gas diffusion layer, which play a crucial role in the performance of a fuel cell. During operation of the fuel cell, hydrogen is oxidized at the anode to form protons (H)+) Then the water passes through a proton exchange membrane to reach a cathode to react with oxygen and intermediate species thereof to generate water, and the current is connected to an external circuit after being collected. At present, catalysts generally used in the catalyst layer of the fuel cell are mainly carbon-supported nano platinum and platinum alloy catalysts, and the utilization rate of platinum is directly related to the cost of the fuel cell. The preparation of the catalyst layer in the membrane electrode is closely connected with the performance of the membrane electrode, so that the improvement of the preparation mode of the catalyst layer of the membrane electrode is one of important means for improving the performance of the membrane electrode of the fuel cell.
According to the search, in the prior art, a platinum source is mainly deposited on a carrier by using an atomic layer deposition method to prepare a platinum or platinum shell loaded electrocatalyst (such as the chinese patent application with the application number of CN 201710108023.8), and the complicated processes of preparing slurry and manufacturing an electrode are still required to be performed to manufacture the platinum or platinum shell loaded electrocatalyst into a membrane electrode, so that the production efficiency is reduced, and the performance of the final membrane electrode is possibly affected by the occurrence of problems in intermediate links. In the traditional spraying and printing electrode technology, the problem of catalyst sedimentation often occurs in the slurry spraying or printing process, so that not only can the pipeline be blocked, but also the catalyst layer is greatly non-uniform, and the performance of the membrane electrode is influenced.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a preparation method of a membrane electrode of a low-temperature proton exchange membrane fuel cell. In the preparation method, the Pt nano particles are directly deposited on the MPL, the utilization rate of the catalyst is high, the impedance of the membrane electrode is reduced, and the performance of the fuel cell is improved.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a membrane electrode of a low-temperature proton exchange membrane fuel cell, which comprises the following steps:
s1, preparation of microporous layer (MPL) on carbon paper surface: uniformly mixing carbon powder and PTFE emulsion, coating the mixture on the surface of carbon paper subjected to hydrophobic treatment, drying the mixture, then performing high-temperature treatment in an inert atmosphere, and cooling the mixture to obtain carbon paper (or called Gas Diffusion Layer (GDL)) with a microporous layer (MPL) on the surface;
s2, directly depositing Pt nano particles on the microporous layer (MPL) by adopting an Atomic Layer Deposition (ALD) technology to obtain an electrode loaded with the Pt nano particles;
s3, spraying the ionic resin solution on the surface of one side of the electrode on which the Pt nano particles are deposited, and drying to obtain the gas diffusion electrode;
and S4, taking two gas diffusion electrodes, and assembling the two gas diffusion electrodes into the membrane electrode of the proton exchange membrane fuel cell by compression joint according to the sequence of the cathode gas diffusion electrode, the proton exchange membrane and the anode gas diffusion electrode.
In the invention, electrodes with different platinum carrying capacity are prepared to be respectively used as a cathode gas diffusion electrode and an anode gas diffusion electrode. The platinum loading capacity of the cathode gas diffusion electrode is 0.1-0.2mgPt/cm2The size of the Pt nano particles is 2-4.5 nm; the platinum loading capacity of the anode gas diffusion electrode is 0.05-0.1mgPt/cm2The size of the Pt nano-particles is 2-3.5 nm.
Preferably, in step S1, the hydrophobic treatment includes immersing the carbon paper in 2 wt% to 20 wt% of PTFE emulsion for immersion treatment. And taking out and drying after impregnation, and repeating the operation until the content of PTFE in the carbon paper reaches a set value.
Preferably, in step S1, the carbon powder is one or more of XC-72R, Super P, EC300J, EC600J, acetylene black, graphene, carbon nanotubes, BP2000, and treated carbon thereof.
Preferably, in step S1, the treatment temperature of the high-temperature treatment is 300 to 400 ℃.
Preferably, in step S1, the mass ratio of the carbon powder to the PTFE is 10:1 to 2: 1.
Preferably, step S2 specifically includes the following steps:
A. placing the carbon paper with the microporous layer on the surface in an ALD reactor, vacuumizing, and starting to heat the reactor and a platinum source bottle;
B. after the vacuum degree and the temperature reach set values, opening a platinum source bottle, opening a platinum source control valve, enabling a platinum source to enter the microporous layer in a steam mode, then closing the platinum source control valve, opening an oxygen valve, introducing oxygen, and controlling the reaction time;
C. and closing the oxygen valve, opening the nitrogen valve, cooling the reactor to room temperature, and taking out to obtain the electrode loaded with the Pt nanoparticles.
Preferably, in the step A, the heating temperature of the reactor is 200-300 ℃, and the gas pressure (namely the vacuum degree of the reactor) in the reactor is lower than 0.01 atm; the heating temperature of the platinum source is 200-250 ℃.
Preferably, in the step B, the opening time of the platinum source control valve is 0.05-0.5 s; the opening time of the oxygen valve is 5-30 min.
Preferably, in the step C, the loading amount of Pt on the electrode loaded with Pt nano particles is 0.025-1.0 mg/cm2(ii) a The size of the Pt nano-particles is 2-10 nm.
Preferably, in step S3, the concentration of the ionic resin solution is 5 wt% to 20 wt%.
Compared with the prior art, the invention has the following beneficial effects:
1) complicated processes such as slurry preparation, spraying, transfer printing and the like are not involved;
2) the problem of catalyst sedimentation in the process of preparing the slurry to manufacture the electrode is effectively avoided;
3) the ultralow platinum membrane electrode is easier to prepare, and the amount of Pt in the membrane electrode is effectively reduced, so that the cost is reduced.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural diagram of a membrane electrode for a proton exchange membrane fuel cell according to the present invention;
FIG. 2 is a graph comparing CV test results of batteries assembled in examples 1 and 3;
FIG. 3 is a micrograph of an anode gas diffusion electrode prepared in example 1;
FIG. 4 is a micrograph of a cathode gas diffusion electrode prepared in example 3;
wherein, 1 is a proton exchange membrane, 2 is Pt nano particles, 3 is an MPL layer, and 4 is carbon paper.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and the accompanying drawings. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The structural schematic diagram of the membrane electrode of the proton exchange membrane fuel cell of each of the following embodiments is shown in fig. 1, and the basic preparation concept is as follows: firstly, carrying out hydrophobic treatment on carbon paper 1, then preparing an MPL layer 3 (microporous layer) on the surface of carbon paper 4, directly depositing Pt nanoparticles 2 on the MPL layer 3 by an atomic deposition technology to form an integrated gas diffusion electrode, and spraying resin on the gas diffusion electrode; finally, a Membrane Electrode (MEA) is assembled according to the sequence of the cathode gas diffusion electrode, the proton exchange membrane 1 and the anode gas diffusion electrode. The specific application is shown in the following examples:
example 1
1. Immersing carbon paper of 10cm X10 cm in 2% of PTFE emulsion for 5-10 min, taking out, drying, and repeating for several times until the percentage content of PTFE in the carbon paper reaches 5%, thereby obtaining hydrophobic carbon paper;
2. weighing 80mg of XC-72 and 1000mg of 2% PTFE emulsion, adding a proper amount of ethanol, uniformly stirring by ultrasonic, uniformly coating on the surface of hydrophobic carbon paper, drying, treating at 350 ℃ for 60min under the protection of argon atmosphere, and cooling to room temperature to obtain carbon paper with an MPL layer;
3. placing the side of the carbon paper on which the MPL layer grows upwards in an ALD reactor, vacuumizing and heating simultaneously until the temperature in the reactor reaches 240 ℃ and the pressure is lower than 0.01atm, starting to heat a source bottle of a platinum source to 200 ℃, opening a control valve of the platinum source for 0.05s, then closing, opening an oxygen valve, introducing oxygen for 10min, closing the oxygen valve, opening a nitrogen valve, exhausting for 20min, cooling to room temperature, and taking out to obtain an anode gas diffusion electrode; platinum loading on electrode 0.05mgPt/cm2The size of the platinum nanoparticles is 2-3 nm, as shown in FIG. 3. The preparation steps of the cathode gas diffusion electrode are similar to those of the anode, and the cathode gas diffusion electrode is obtained only by adjusting the opening time of a control valve of a platinum source to 0.1 s; platinum loading on the electrode was 0.1mgPt/cm2The size of the platinum nanoparticles is 2-4 nm.
4. Spraying 5% Nafion resin solution on the MPL surface deposited with the catalyst, and drying to obtain an electrode;
5. the membrane electrode of the proton exchange membrane fuel cell is formed by pressing and connecting a cathode gas diffusion electrode, a proton exchange membrane and an anode gas diffusion electrode.
Example 2
1. Immersing carbon paper of 10cm X10 cm in 5% of PTFE emulsion for 5-10 min, taking out, drying, and repeating for several times until the percentage content of PTFE in the carbon paper reaches 10%, thereby obtaining hydrophobic carbon paper;
2. weighing 70mg of BP-2000 and 1500mg of 2% PTFE emulsion, adding a proper amount of ethanol, uniformly stirring by ultrasonic, uniformly coating on the surface of hydrophobic carbon paper, drying, and treating at 350 ℃ for 60min under the protection of argon atmosphere to obtain carbon paper with an MPL layer;
3. placing the side of the carbon paper on which the MPL layer grows upwards in an ALD reactor, vacuumizing and heating simultaneously until the temperature in the reactor reaches 240 ℃ and the pressure is lower than 0.01atm, starting to heat a source bottle of a platinum source to 200 ℃, opening a control valve of the platinum source for 0.1s, then closing, opening an oxygen valve, introducing oxygen for 30min, closing the oxygen valve, opening a nitrogen valve, exhausting for 20min, cooling to room temperature, and taking out to obtain an anode gas diffusion electrode; platinum loading on the electrode was 0.1mgPt/cm2The size of the platinum nanoparticles is 2-3.5 nm. The preparation steps of the cathode gas diffusion electrode are similar to those of the anode, and the cathode gas diffusion electrode is obtained only by adjusting the opening time of a control valve of a platinum source to 0.15 s; platinum loading on the electrode was 0.15mgPt/cm2The size of the platinum nanoparticles is 3-4 nm.
4. Spraying 5% Nafion resin solution on the MPL surface deposited with the catalyst, and drying to obtain an electrode; the prepared electrodes with different platinum loading capacity are respectively used as a cathode gas diffusion electrode and an anode gas diffusion electrode;
5. and (3) pressing and connecting the cathode gas diffusion electrode, the proton exchange membrane and the anode gas diffusion electrode into a membrane electrode of the proton exchange membrane fuel cell.
Example 3
1. Immersing carbon paper of 10cm X10 cm in 2% of PTFE emulsion for 5-10 min, taking out, drying, and repeating for several times until the percentage content of PTFE in the carbon paper reaches 5%, thereby obtaining hydrophobic carbon paper;
2. weighing 80mg of XC-72 and 1000mg of 2% PTFE emulsion, adding a proper amount of ethanol, uniformly stirring by ultrasonic, uniformly coating on the surface of hydrophobic carbon paper, drying, and treating at 400 ℃ for 30min under the protection of argon atmosphere to obtain carbon paper with an MPL layer;
3. the side of the carbon paper on which the MPL layer is grown is placed upwards in an ALD reactor, and vacuum and heating are carried out until the temperature in the reactor reaches 240 ℃ and the pressure is increasedWhen the pressure is lower than 0.01atm, starting to heat a source bottle of the platinum source to 200 ℃, opening a control valve of the platinum source for 0.05s, then closing, opening an oxygen valve, introducing oxygen for 30min, closing the oxygen valve, opening a nitrogen valve, exhausting for 20min, cooling to room temperature, and taking out to obtain an anode gas diffusion electrode; platinum loading on electrode 0.05mgPt/cm2The size of the platinum nanoparticles is 2-3 nm. The preparation steps of the cathode gas diffusion electrode are similar to those of the anode, and the cathode gas diffusion electrode is obtained only by adjusting the opening time of a control valve of a platinum source to 0.2 s; platinum loading on the electrode was 0.2mgPt/cm2The size of the platinum nanoparticles is 3-4.5 nm, as shown in FIG. 4.
4. Spraying a 10% Nafion resin solution on the MPL surface deposited with the catalyst, and drying to obtain an electrode; the prepared electrodes with different platinum loading capacity are respectively used as a cathode gas diffusion electrode and an anode gas diffusion electrode;
5. and (3) pressing and connecting the cathode gas diffusion electrode, the proton exchange membrane and the anode gas diffusion electrode into a membrane electrode of the proton exchange membrane fuel cell.
Example 4
1. Immersing carbon paper of 10cm X10 cm in 2% of PTFE emulsion for 5-10 min, taking out, drying, and repeating for several times until the percentage content of PTFE in the carbon paper reaches 5%, thereby obtaining hydrophobic carbon paper;
2. weighing 80mg of EC-300J and 1000mg of 2% PTFE emulsion, adding a proper amount of ethanol, uniformly stirring by ultrasonic, uniformly coating on the surface of hydrophobic carbon paper, drying, and treating at 350 ℃ for 120min under the protection of argon atmosphere to obtain carbon paper with an MPL layer;
3. placing the side of the carbon paper on which the MPL layer grows upwards in an ALD reactor, vacuumizing and heating simultaneously until the temperature in the reactor reaches 240 ℃ and the pressure is lower than 0.01atm, starting to heat a source bottle of a platinum source to 200 ℃, opening a control valve of the platinum source for 0.05s, then closing, opening an oxygen valve, introducing oxygen for 20min, closing the oxygen valve, opening a nitrogen valve, exhausting for 20min, cooling to room temperature, and taking out to obtain an anode gas diffusion electrode; platinum loading on electrode 0.05mgPt/cm2The size of the platinum nanoparticles is2-3 nm. The preparation steps of the cathode gas diffusion electrode are similar to those of the anode, and the cathode gas diffusion electrode is obtained only by adjusting the opening time of a control valve of a platinum source to 0.2 s; platinum loading on the electrode was 0.2mgPt/cm2The size of the platinum nanoparticles is 3-4.5 nm.
4. Spraying a 20% Nafion resin solution on the MPL surface deposited with the catalyst, and drying to obtain an electrode; (ii) a The prepared electrodes with different platinum loading capacity are respectively used as a cathode gas diffusion electrode and an anode gas diffusion electrode;
5. and (3) pressing and connecting the cathode gas diffusion electrode, the proton exchange membrane and the anode gas diffusion electrode into a membrane electrode of the proton exchange membrane fuel cell.
Membrane electrodes were prepared according to examples 1 and 3, from 2 pieces of 5cm X5cm cut from the above 10cm X10 cm gas diffusion electrode, with a Pt loading of 0.1mg eachPt/cm2And 0.2mgPt/cm2Respectively serving as an anode and a cathode to prepare MEA; the Pt loading was prepared as 0.1mg according to conventional methods using commercial Pt/C catalyst slurriedPt/cm2And 0.2mgPt/cm2Then an MEA is fabricated. CV test results of the cells as shown in fig. 2, the active area of the MEA cell fabricated by ALD is significantly better than that of the conventional process under the same Pt loading, which may be related to the contact state of the electrode structure, catalyst and ionic resin.
In summary, the invention adopts the Atomic Layer Deposition (ALD) technology to directly grow Pt nanoparticles on the microporous carbon layer of the gas diffusion layer close to the proton membrane, does not involve complicated processes such as slurry preparation and spraying, can prepare electrode catalyst layers with different loading amounts by only adjusting the opening time and the deposition period of the platinum source control valve, improves the utilization rate of the ionic resin and the catalyst, has controllable porous layer structure and rich porosity, and improves the performance of the fuel cell.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (10)

1. A preparation method of a membrane electrode of a low-temperature proton exchange membrane fuel cell is characterized by comprising the following steps:
s1, preparing a microporous layer on the surface of the carbon paper: mixing carbon powder and PTFE emulsion, coating the mixture on the surface of carbon paper subjected to hydrophobic treatment, drying the mixture, performing high-temperature treatment in an inert atmosphere, and cooling the mixture to obtain carbon paper with a microporous layer on the surface;
s2, directly depositing Pt nano particles on the microporous layer by adopting an atomic layer deposition technology to obtain an electrode loaded with Pt nano particles;
s3, spraying the ionic resin solution on the surface of one side of the electrode obtained in the step S2, on which the Pt nano particles are deposited, and drying to obtain the gas diffusion electrode;
and S4, taking two gas diffusion electrodes, and assembling the two gas diffusion electrodes into the membrane electrode of the proton exchange membrane fuel cell by compression joint according to the sequence of the cathode gas diffusion electrode, the proton exchange membrane and the anode gas diffusion electrode.
2. The method for preparing a membrane electrode assembly for a low-temperature proton exchange membrane fuel cell according to claim 1, wherein in step S1, the hydrophobic treatment comprises immersing carbon paper in 2 wt% -20 wt% PTFE emulsion.
3. The method for preparing a membrane electrode assembly of a proton exchange membrane fuel cell according to claim 1, wherein in step S1, the carbon powder is one or more of XC-72R, Super P, EC300J, EC600J, acetylene black, graphene, carbon nanotubes, and BP 2000.
4. The method for preparing a membrane electrode assembly for a low-temperature proton exchange membrane fuel cell according to claim 1, wherein in step S1, the processing temperature of the high-temperature treatment is 300-400 ℃.
5. The preparation method of the membrane electrode of the low-temperature proton exchange membrane fuel cell according to claim 1, wherein in the step S1, the mass ratio of the PTFE emulsion to the carbon powder is 10: 1-2: 1.
6. The method for preparing a membrane electrode assembly of a low-temperature proton exchange membrane fuel cell according to claim 1, wherein step S2 specifically includes the following steps:
A. placing the carbon paper with the microporous layer on the surface in an ALD reactor, vacuumizing, and starting to heat the reactor and a platinum source bottle;
B. after the vacuum degree and the temperature reach set values, opening a platinum source bottle, opening a platinum source control valve, enabling a platinum source to enter the microporous layer in a steam mode, then closing the platinum source control valve, opening an oxygen valve, introducing oxygen, and controlling the reaction time;
C. and closing the oxygen valve, opening the nitrogen valve, cooling the reactor to room temperature, and taking out to obtain the electrode loaded with the Pt nanoparticles.
7. The method for preparing a membrane electrode of a low-temperature proton exchange membrane fuel cell according to claim 6, wherein in the step A, the heating temperature of the reactor is 200-300 ℃, and the gas pressure in the reactor is lower than 0.01 atm; the heating temperature of the platinum source is 200-250 ℃.
8. The preparation method of the membrane electrode of the low-temperature proton exchange membrane fuel cell according to claim 6, wherein in the step B, the opening time of the platinum source control valve is 0.05-0.5 s; the opening time of the oxygen valve is 5-30 min.
9. The method for preparing the membrane electrode assembly of the low-temperature proton exchange membrane fuel cell according to claim 6, wherein in the step C, the loading amount of Pt on the electrode loaded with the Pt nanoparticles is 0.025-1.0 mg/cm2(ii) a The size of the Pt nano-particles is 2-10 nm.
10. The method for preparing a membrane electrode assembly for a low-temperature proton exchange membrane fuel cell according to claim 1, wherein in step S3, the concentration of the ionic resin solution is 5 wt% to 20 wt%.
CN201911413174.XA 2019-12-31 2019-12-31 Method for preparing membrane electrode of low-temperature proton exchange membrane fuel cell Pending CN111162299A (en)

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CN112382767A (en) * 2020-10-26 2021-02-19 江苏大学 Fuel cell electrode in-situ preparation method based on double-layer ordered structure microporous layer
CN112382767B (en) * 2020-10-26 2021-10-12 江苏大学 Fuel cell electrode in-situ preparation method based on double-layer ordered structure microporous layer
CN112838251A (en) * 2021-01-25 2021-05-25 武汉绿知行环保科技有限公司 Fuel cell membrane electrode and preparation method thereof
CN113270593A (en) * 2021-04-22 2021-08-17 上海唐锋能源科技有限公司 Membrane electrode for proton exchange membrane fuel cell and preparation method thereof
CN113782796A (en) * 2021-08-19 2021-12-10 广西大学 Method for preparing membrane electrode of ultralow platinum fuel cell based on graphene porous membrane
CN113964356A (en) * 2021-09-28 2022-01-21 三一汽车制造有限公司 Fuel cell membrane electrode, membrane electrode preparation method, fuel cell system and vehicle
CN114079071A (en) * 2021-10-12 2022-02-22 江苏大学 Preparation method and application of self-supporting membrane electrode
CN114079071B (en) * 2021-10-12 2022-12-16 江苏大学 Preparation method and application of self-supporting membrane electrode

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