CN116230962A - Fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and preparation process thereof - Google Patents

Fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and preparation process thereof Download PDF

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Publication number
CN116230962A
CN116230962A CN202211569316.3A CN202211569316A CN116230962A CN 116230962 A CN116230962 A CN 116230962A CN 202211569316 A CN202211569316 A CN 202211569316A CN 116230962 A CN116230962 A CN 116230962A
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catalyst
coating
fuel cell
chemical stability
excellent chemical
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周向阳
叶涵琦
余卓平
张若婧
朱皓民
王浩
李佳俊
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Shanghai Intelligent New Energy Vehicle Technology Innovation Platform Co ltd
Shanghai Motor Vehicle Inspection Certification and Tech Innovation Center Co Ltd
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Shanghai Intelligent New Energy Vehicle Technology Innovation Platform Co ltd
Shanghai Motor Vehicle Inspection Certification and Tech Innovation Center Co Ltd
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Priority to CN202211569316.3A priority Critical patent/CN116230962A/en
Publication of CN116230962A publication Critical patent/CN116230962A/en
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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
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • 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
    • H01M4/8828—Coating with slurry or ink
    • 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
    • H01M4/921—Alloys or mixtures with metallic elements
    • 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
    • H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • 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]
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Inert Electrodes (AREA)
  • Fuel Cell (AREA)

Abstract

The invention relates to a fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and a preparation process thereof. The catalytic layer comprises a proton exchange membrane, a C1 coating and a C2 coating which are sequentially attached to the cathode side of the proton exchange membrane, and an A1 coating and an A2 coating which are sequentially attached to the anode side of the proton exchange membrane. The preparation process comprises the following steps: the cathode side of the proton exchange membrane is coated with free radical slurry, and a C1 coating is formed after drying; coating cathode slurry on the C1 layer, and drying to form a C2 coating; coating anode slurry on the anode side of the proton exchange membrane, and drying to form an A1 coating; and (3) brushing anti-reverse pole slurry on the A1 layer, and drying to form an A2 coating, thereby finally obtaining the fuel cell catalytic layer with excellent chemical stability and long anti-reverse pole time. Compared with the prior art, the invention has the advantages of obviously improving the stability and the anti-counter-electrode time of the fuel cell under the open-circuit working condition, being helpful for improving the durability of the fuel cell, and the like.

Description

Fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and preparation process thereof
Technical Field
The invention relates to the field of fuel cells, in particular to a fuel cell catalytic layer with excellent chemical stability and long anti-counter time and a preparation process thereof.
Background
The fuel cell can convert chemical energy in fuel into electric energy through electrochemical reaction, and is an important device for realizing high-efficiency utilization of hydrogen energy. The membrane electrode is used as a core component of the fuel cell and is mainly formed by stacking layered materials with different functions, such as a gas diffusion layer, a catalytic layer, a proton exchange membrane and the like, and the catalytic layer in the membrane electrode is a main place for electrochemical reaction of hydrogen and oxygen. At present, the main production flow of the catalytic layer comprises the following steps: the catalyst is fully mixed with the ionomer and the solvent and stirred to prepare slurry which is uniformly dispersed, and then the slurry is sprayed, directly coated or transferred to two sides of a Proton Exchange Membrane (PEM) to form the CCM.
During operation of the fuel cell, particularly in open circuit conditions, radicals, which are byproducts or side reaction products, attack perfluorosulfonic acid (PFSA) molecules in the PEM and cause pinhole formation and thinning of the PEM, increasing the permeation of reactant gases through the PEM, thereby causing cell failure. In addition, when the fuel cell vehicle is operated under transient conditions such as start-up and rapid loading, hydrogen starvation may be induced, resulting in higher anode potential than the cathode, i.e., counter-electrode, and further resulting in damage such as corrosion of the carbon support, affecting the safety of the overall fuel cell system. At present, a preparation process of a catalytic layer with counter electrode resistance and high chemical stability is lacking.
Disclosure of Invention
The invention aims to overcome at least one of the defects in the prior art and provide a fuel cell catalytic layer with excellent chemical stability and long anti-counter-electrode time and a preparation process thereof, wherein the stability and the anti-counter-electrode time of the fuel cell under an open-circuit working condition can be obviously improved, and the improvement of the durability of the fuel cell is greatly facilitated.
The aim of the invention can be achieved by the following technical scheme:
a fuel cell catalytic layer having both excellent chemical stability and long anti-counter time, the catalytic layer comprising a proton exchange membrane, a C1 coating and a C2 coating sequentially attached to the cathode side of the proton exchange membrane, and an A1 coating and an A2 coating sequentially attached to the anode side of the proton exchange membrane;
the C1 coating contains a free radical quenching catalyst, the C2 coating contains a cathode catalyst, the A1 coating contains an anode catalyst, and the A2 coating contains an anti-counter electrode catalyst.
The radical quencher and the anti-counter electrode catalyst do not significantly reduce the power generation performance and durability of the single cell itself. The free radical quencher can improve the chemical stability of the single cell: irreversible degradation during cell chemical stability testing is mainly affected by peroxy radicals and hydroxyl groups, which react with functional groups on the perfluorosulfonic acid in the catalytic layer and proton exchange membrane to cause ionomer degradation, proton exchange membrane thinning, pinhole formation. Thereby increasing the gas permeation quantity of the proton exchange membrane and reducing the ECSA of the single cell catalyst, and further reducing the power generation performance of the single cell. The introduction of the free radical quencher can reduce the content of free radicals in the durability test process, thereby improving the chemical stability
The anti-counter electrode catalyst can improve the anti-counter electrode performance of the single cell: in the case of fuel starvation, protons and electrons required for the unit cell are provided by water electrolysis and carbon corrosion, which damages the catalytic layer structure, reducing the durability of the unit cell. The introduction of the anti-counter electrode catalyst can improve the water electrolysis capacity and further improve the anti-counter electrode performance of the single cell.
Further, the free radical quenching Catalyst (CZO) is Zr x Ce 1-x O 2 Wherein x=0-1, the cathode catalyst and/or anode catalyst is Pt/C, and the anti-counter electrode catalyst is Ir y Ru 1-y O 2 Wherein y=0-1; the proton exchange membrane comprises a perfluorinated sulfonic acid type solid polymer which is used for isolating electrons and gases and transmitting protons;
the content of the free radical quenching catalyst is 5-15wt% of the cathode catalyst, and the content of the anti-counter electrode catalyst is 15-25wt% of the anode catalyst.
Further, the mass ratio of Pt in the Pt/C is 50-70wt%, and the mass ratio of y=0.4-0.6; the Pt content on the cathode and anode sides is 0.2-0.4mg/cm 2 。
Further, x=0.2, the mass ratio of Pt in the Pt/C is 60wt%, and y=0.5; the Pt content on the cathode side was 0.4mg/cm 2 The Pt content on the anode side was 0.2mg/cm 2 ；
The content of the free radical quenching catalyst is 20wt% of the cathode catalyst, and the content of the anti-counter electrode catalyst is 20wt% of the anode catalyst.
A process for preparing a catalytic layer for a fuel cell having both excellent chemical stability and long counter electrode time as described above, the process comprising the steps of:
the cathode side of the proton exchange membrane is coated with free radical slurry, and a C1 coating is formed after drying;
coating cathode slurry on the C1 layer, and drying to form a C2 coating;
coating anode slurry on the anode side of the proton exchange membrane, and drying to form an A1 coating;
and (3) brushing anti-reverse pole slurry on the A1 layer, and drying to form an A2 coating, thereby finally obtaining the fuel cell catalytic layer with excellent chemical stability and long anti-reverse pole time.
Further, the free radical removing slurry comprises a free radical quenching catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the cathode slurry comprises a cathode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the anode slurry comprises an anode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the anti-reverse electrode slurry comprises an anti-reverse electrode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%.
Further, the ionomer is a polymer composed of ionomer molecules, the solvent is a mixture of water and alcohol, and the mass ratio of the catalyst to the ionomer in the coating is (2-4): 1.
Further, the ionomer comprises Nafion, the alcohol comprises isopropanol or methanol, and the mass ratio of the catalyst to the ionomer in the coating is 3:1.
Further, the brushing mode comprises spraying, direct coating or transfer printing.
Further, the free radical quenching catalyst is Ce 0.8 Zr 0.2 O 2 The anti-reverse electrode catalyst is IrO with the mass ratio of 1:1 2 And RuO (Ruo) 2 。
Compared with the prior art, the invention has the following advantages:
(1) In the present invention, the radical quencher and the counter electrode catalyst do not significantly reduce the power generation performance and durability of the single cell itself. The preparation process can have the chemical stability and the anti-counter-electrode performance of the fuel cell, and can obviously improve the durability of the fuel cell;
(2) In the invention, the free radical quencher can improve the chemical stability of the single cell: irreversible degradation during cell chemical stability testing is mainly affected by peroxy radicals and hydroxyl groups, which react with functional groups on the perfluorosulfonic acid in the catalytic layer and proton exchange membrane to cause ionomer degradation, proton exchange membrane thinning, pinhole formation. Thereby increasing the gas permeation quantity of the proton exchange membrane and reducing the ECSA of the single cell catalyst, and further reducing the power generation performance of the single cell. The introduction of the free radical quencher can reduce the content of free radicals in the durability test process, thereby improving the chemical stability;
(3) In the invention, the anti-counter electrode catalyst can improve the anti-counter electrode performance of the single cell: in the case of fuel starvation, protons and electrons required for the unit cell are provided by water electrolysis and carbon corrosion, which damages the catalytic layer structure, reducing the durability of the unit cell. The introduction of the anti-counter electrode catalyst can improve the water electrolysis capacity and further improve the anti-counter electrode performance of the single cell.
Drawings
FIG. 1 is a schematic view of the structure of a catalyst layer of the present invention;
FIG. 2 is a graph showing voltage versus time during the reverse polarity test of the MEA in example 1;
FIG. 3 is a graph showing the variation of (a) voltage and (b) hydrogen permeation current density over time during an open-circuit operation durability test of the MEA of example 1;
FIG. 4 is a graph showing the voltage and hydrogen permeation current densities over time during an MEA-C open circuit condition durability test of comparative example 1;
FIG. 5 is a graph showing the voltage over time during the counter electrode test of MEA-C in comparative example 1.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
A fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and a preparation process thereof are disclosed in fig. 1, wherein the preparation process of the catalytic layer comprises the following steps: spraying/directly coating/transferring the free radical scavenger slurry on the cathode side of the proton exchange membrane, and drying to form a C1 coating; then spraying/directly coating/transferring cathode slurry on the C1 layer, and drying to form a C2 coating; and spraying/directly coating/transferring anode slurry on the anode side of the proton exchange membrane, drying to form an A1 coating, then spraying/directly coating/transferring anti-reverse-electrode slurry on the A1 layer, drying to form an A2 coating, and finally obtaining the structure schematically shown in figure 1.
Wherein the radical scavenger slurry comprises radical scavenger (CeO) 2 And Zr (Zr) x Ce 1-x O 2 Isocitrate), ionomer, and a mixture of alcohol and water (the alcohol may be an easily dispersible solvent such as isopropyl alcohol, methanol, etc.), the solids content being 0.5-10%; the cathode slurry comprises a free cathode catalyst, an ionomer and a mixture of alcohol and water (the alcohol can be isopropanol, methanol and other easily dispersible solvents), and the solid content is 0.5-10%; the anode slurry comprises a free anode catalyst, an ionomer and a mixture of alcohol and water (the alcohol can be isopropanol, methanol and other easily dispersible solvents), and the solid content is 0.5-10%; the anti-reverse electrode slurry comprises free anti-reverse electrode catalyst (IrO) 2 、RuO 2 Or IrRuO 4 Etc.), ionomer, and a mixture of alcohol and water (the alcohol may be an easily dispersible solvent such as isopropyl alcohol, methanol, etc.), the solids content being 0.5-10%. The proton exchange membrane mainly comprises perfluorosulfonic acid type solid polymer, and is used for isolating electrons and gases and transmitting protons. Ionomers are polymers composed of ionomer molecules, including principally Nafion and the like. The cathode catalyst and the anode catalyst mainly consist of Pt/C.
Example 1
A fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time, wherein the mass ratio of catalyst to Nafion in the coating is 3:1, and the Pt content in the anode and the cathode is 0.4mg/cm and 0.2mg/cm respectively 2 Free radical quencher CZO (Ce 0.8 Zr 0.2 O 2 ) The content of the catalyst was 10wt% of the content of Pt/C (Pt mass ratio: 60 wt%) of the cathode, and the anti-counter electrode catalyst OER (IrO) 2 /RuO 2 The mass ratio 1:1) was 20wt% of the anode Pt/C content.
Fig. 2 is a battery cell reversed polarity performance test under the following test conditions: the temperature of the battery is 80 ℃, the relative humidity is 100%, the inlet pressure of the cathode and anode is 130/120kPa, and the counter current density is 200mA/cm 2 ，H 2 The flow rate of the air is 0.3/0.3L/min 1 . It can be seen that the counter electrode time of the single cell is up to 742 minutes.
FIG. 3 is an open circuit process of a single cellThe test conditions for the condition durability test are as follows: the cell temperature was 90℃and the cathode/anode inlet flow was 0.35/0.83L/min, inlet backpressure was 150/150kPa, and inlet relative humidity was 30/30%. From the above results, it can be seen that the voltage decay of the single cell is almost reversible and the hydrogen permeation current density is 5-8mA cm during the 500-hour open-circuit condition durability test -2 And fluctuates up and down. The results show that the prepared single cell has good electrochemical stability.
Comparative example 1
A fuel cell catalyst layer and process for its preparation differs from example 1 in that the free radical quencher and anti-counter electrode catalyst are removed during the preparation to give MEA-C, the performance characteristics of which are shown in FIGS. 4-5.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (10)

1. A fuel cell catalytic layer having excellent chemical stability and long anti-counter time, characterized in that the catalytic layer comprises a proton exchange membrane, a C1 coating and a C2 coating sequentially attached to the cathode side of the proton exchange membrane, and an A1 coating and an A2 coating sequentially attached to the anode side of the proton exchange membrane;
the C1 coating contains a free radical quenching catalyst, the C2 coating contains a cathode catalyst, the A1 coating contains an anode catalyst, and the A2 coating contains an anti-counter electrode catalyst.
2. The fuel cell catalyst layer having excellent chemical stability and long anti-counter electrode time according to claim 1, wherein the radical quenching catalyst is Zr x Ce 1-x O 2 Wherein x=0-1, said cathodeThe catalyst and/or anode catalyst is Pt/C, and the anti-counter electrode catalyst is Ir y Ru 1-y O 2 Wherein y=0-1;
the content of the free radical quenching catalyst is 5-15wt% of the cathode catalyst, and the content of the anti-counter electrode catalyst is 15-25wt% of the anode catalyst.
3. The fuel cell catalyst layer having both excellent chemical stability and long anti-reflection time according to claim 2, wherein x=0 to 0.2, the mass ratio of Pt in Pt/C is 50 to 70wt%, and y=0.4 to 0.6; the Pt content on the cathode and anode sides is 0.2-0.4mg/cm 2 。
4. A fuel cell catalyst layer having both excellent chemical stability and long anti-reflection time according to claim 3, wherein x=0.2, the Pt mass ratio in Pt/C is 60wt%, and y=0.5; the Pt content on the cathode side was 0.4mg/cm 2 The Pt content on the anode side was 0.2mg/cm 2 ；
The content of the free radical quenching catalyst is 20wt% of the cathode catalyst, and the content of the anti-counter electrode catalyst is 20wt% of the anode catalyst.
5. A process for the preparation of a catalytic layer for a fuel cell having both excellent chemical stability and long anti-counter electrode time as claimed in any one of claims 1 to 4, characterized in that it comprises the steps of:
the cathode side of the proton exchange membrane is coated with free radical slurry, and a C1 coating is formed after drying;
coating cathode slurry on the C1 layer, and drying to form a C2 coating;
coating anode slurry on the anode side of the proton exchange membrane, and drying to form an A1 coating;
and (3) brushing anti-reverse pole slurry on the A1 layer, and drying to form an A2 coating, thereby finally obtaining the fuel cell catalytic layer with excellent chemical stability and long anti-reverse pole time.
6. The process for preparing a catalytic layer for a fuel cell having excellent chemical stability and long anti-reflection time as claimed in claim 5, wherein,
the free radical removal slurry comprises a free radical quenching catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the cathode slurry comprises a cathode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the anode slurry comprises an anode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%;
the anti-reverse electrode slurry comprises an anti-reverse electrode catalyst, an ionomer and a solvent, wherein the solid content is 0.5-10wt%.
7. The process for preparing a catalytic layer for a fuel cell having excellent chemical stability and long anti-reflection time as claimed in claim 6, wherein the ionomer is a polymer composed of ionomer molecules, the solvent is a mixture of water and alcohol, and the mass ratio of catalyst to ionomer in the coating is (2-4): 1.
8. The process for preparing a catalytic layer for a fuel cell having excellent chemical stability and long anti-reflection time according to claim 7, wherein the ionomer comprises Nafion, the alcohol comprises isopropanol or methanol, and the mass ratio of catalyst to ionomer in the coating is 3:1.
9. The process for preparing a catalytic layer for a fuel cell having excellent chemical stability and long anti-reflection time according to claim 5, wherein the brushing means comprises spraying, direct coating or transfer printing.
10. The process for preparing a catalytic layer for a fuel cell having excellent chemical stability and long anti-reflection time as claimed in claim 5, wherein the radical quenching catalyst is Ce 0.8 Zr 0.2 O 2 The anti-reverse electrode catalyst is IrO with the mass ratio of 1:1 2 And RuO (Ruo) 2 。
CN202211569316.3A 2022-12-08 2022-12-08 Fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and preparation process thereof Pending CN116230962A (en)

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CN202211569316.3A CN116230962A (en) 2022-12-08 2022-12-08 Fuel cell catalytic layer with excellent chemical stability and long anti-counter electrode time and preparation process thereof

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