CN113629281A - Preparation method of fuel cell membrane electrode - Google Patents
Preparation method of fuel cell membrane electrode Download PDFInfo
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- H01—ELECTRIC ELEMENTS
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- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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Abstract
The invention discloses a preparation method of a fuel cell membrane electrode, which specifically comprises the steps of coating a large-area proton-conducting polymer solution on a coating substrate by adopting a coating technology; placing a gas diffusion electrode with the same coating area as the proton conducting polymer solution coated on the proton conducting polymer solution; stripping from the coating substrate after drying and forming, and cutting into a plurality of film coating electrodes with required sizes for later use; and placing the insulating airtight frame on the membrane sides of the two membrane coating electrodes to form a membrane electrode blank, and performing hot pressing treatment to obtain the integrated membrane electrode. The method can optimize the three-phase interface of the membrane electrode and reduce the material transmission resistance of the interface of the membrane electrode; the penetration of proton conduction polymer solution to the pores and cracks of the catalyst layer in the direct film deposition process is reduced, and the catalytic activity of the film electrode and the gas blocking capability of the proton exchange film are improved. The method is an extensible membrane electrode preparation method based on a coating technology, optimizes the membrane electrode preparation technology, and can be used for continuous production or intermittent production.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and relates to a preparation method of an integrated fuel cell membrane electrode; in particular to a preparation method of an integrated membrane electrode based on a direct membrane deposition technology, which can reduce the penetration of proton-conducting polymer solution.
Background
Fuel cells are considered to be an important green energy technology capable of directly converting chemical energy into electrical energy through electrochemical reactions. The membrane electrode is the most central component of a Proton Exchange Membrane Fuel Cell (PEMFC), and plays a key role in the fuel cell as a site where electrochemical reaction occurs, and the characteristics of the membrane electrode directly determine the overall performance of the fuel cell. The structural design and preparation process of the membrane electrode are always the core technology in the field of PEMFC.
The preparation method of the membrane electrode and various functional layers comprise: the structural design of the Proton Exchange Membrane (PEM), the cathode and anode catalysts, and the gas diffusion layers all contribute to the performance of the fuel cell. At present, most of membrane electrode preparation methods are to treat each functional layer as an independent unit for processing and manufacturing respectively, and each functional layer has an obvious interface. The interfaces of the functional layers of the membrane electrode prepared by the method have larger interfacial resistance, which affects the transmission of reactants and products (gas, electrons, protons and water) in the membrane electrode, and the interfaces of the functional layers are easy to be layered or dislocated in long-time work, thereby causing the reduction of the output performance of the battery. Chinese patent CN109638298A adopts slit die head casting technology to coat cathode catalyst, Nafion solution and anode catalyst in sequence, to prepare cathode catalyst layer, proton exchange membrane and anode catalyst layer, and after preparing catalyst layer each time, a layer of support frame is placed at the edge of catalyst layer, to prepare 3D structure membrane electrode. Chinese patent CN110247062A directly coats a perfluorosulfonic acid resin (PFSA) solution on a gas diffusion electrode, and coats another catalytic layer after drying to form a film, thereby preparing a membrane electrode. According to the method for preparing the membrane electrode, the proton conducting polymer is directly coated on the catalyst layer or the gas diffusion layer to form a membrane, so that the material transmission resistance between the catalyst layer and the PEM interface can be reduced. However, in the proton conducting polymer coating process, due to the existence of considerable pores and cracks on the surface of the catalytic layer or the gas diffusion layer, liquid proton conducting polymer is easy to permeate into the pores and cracks of the catalytic layer, so that the proton conducting polymer is over-filled, and the prepared PEM has defects, so that the catalytic performance of the catalyst and the gas-blocking capability of the PEM are affected, and the electric output performance and durability of the membrane electrode are reduced.
Disclosure of Invention
The invention provides a membrane electrode preparation method aiming at the problems of large membrane electrode interface transmission resistance, easy permeation of liquid proton conducting polymer into pores and cracks of a catalyst layer or a gas diffusion layer in the membrane electrode preparation process, excessive filling of the proton conducting polymer and defects of a prepared proton exchange membrane in the prior art. The method comprises the steps of coating a proton conducting polymer on a substrate, then placing a gas diffusion electrode, drying and molding, and then stripping the gas diffusion electrode from the substrate to obtain the membrane coating electrode. And assembling and hot-pressing the two membrane coating electrodes and the insulating airtight frame to obtain the membrane electrode. The method optimizes the membrane electrode preparation technology, can reduce the transmission resistance of the membrane electrode interface and simultaneously reduce the problem that liquid proton conduction polymer permeates into pores and cracks of a catalyst layer under the action of gravity, thereby improving the electric output performance of the membrane electrode and the gas blocking capability of a proton exchange membrane in the direct membrane deposition technology.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a fuel cell membrane electrode comprises the following steps:
s1, coating a large-area proton conducting polymer solution on the coated substrate by using a coating device;
s2 preparation of film-coated electrode
a) Placing a gas diffusion electrode having the same size as the proton-conducting polymer solution coated on the proton-conducting polymer solution coated in step S1, wherein the catalyst layer side of the gas diffusion electrode is in contact with the proton-conducting polymer solution;
b) drying, molding and annealing the sample prepared in the step a), and peeling the sample from the coating substrate to obtain a film coating electrode;
s3, cutting for later use: cutting the large-area film coating electrode prepared in the step S2 into required sizes for later use;
s4, assembling a membrane electrode blank: placing an insulating airtight frame at the circumferential edge of the film coating electrode, aligning another film coating electrode on the other side of the insulating airtight frame, and aligning the two film coating electrodes to form a film electrode blank;
s5, hot press forming: and carrying out hot-pressing treatment on the membrane electrode blank to obtain the integrated membrane electrode.
As an embodiment of the present invention, the coating process of step S1 is spray coating, ultrasonic spray coating, blade coating or slit extrusion coating.
As an embodiment of the present invention, the coating substrate of step S1 is any one of a glass plate, a Polytetrafluoroethylene (PTFE), a silicon oil film, and a Polydimethylsiloxane (PDMS) plate.
As an embodiment of the present invention, the proton conducting polymer solution in step S1 is one or more of a combination of a perfluorosulfonic acid solution, a sulfonated polyetheretherketone solution, and a sulfonated trifluorostyrene solution.
As an embodiment of the present invention, the gas diffusion electrode of step S2 includes a catalytic layer and a gas diffusion layer; the catalyst layer consists of a Pt-based catalyst, deionized water, Nafion solution, a dispersing solvent and a forming additive, and the Pt loading capacity in the catalyst layer is 0.1-0.4mg/cm2。
As an embodiment of the invention, the drying treatment temperature of the step S2 is 60-100 ℃, and the time is 1-4 h; the annealing heat treatment temperature is 110-150 ℃, and the time is 5-120 min.
As an embodiment of the present invention, the insulating airtight rim of step S4 is placed on the proton exchange membrane side of the membrane-coated electrode;
as an embodiment of the present invention, the insulating airtight frame in step S4 sequentially includes an inner frame and an outer frame in a radial direction of the membrane electrode, the outer frame is exposed out of the membrane coating electrode, the inner frame is embedded in a proton exchange membrane layer of the membrane electrode, and a space in the middle of the inner frame is an active reaction region.
In one embodiment of the present invention, the material of the insulating and airtight rim in step S4 is one or more of polyethylene terephthalate (PET), glass fiber reinforced polytetrafluoroethylene (frptfe), polyimide, and silicone rubber, and has a thickness of 5-50 μm.
As an embodiment of the present invention, the heat treatment temperature of the hot press molding in the step S5 is 100-150 ℃, the pressure is 0.1-1MPa, and the hot press time is 0.5-3 min.
Compared with the prior art, the invention has the following beneficial effects:
1) the method directly coats the proton conduction polymer solution on the substrate, and can control the thickness and the flatness of the finally formed proton exchange membrane by controlling the solution amount;
2) the method directly places the gas diffusion electrode on the coated proton conduction polymer solution, can reduce the permeation of the proton conduction polymer to the pores and cracks of the catalyst layer and reduce the manufacturing defects of the proton exchange membrane while ensuring that the proton exchange membrane in the prepared membrane electrode is well contacted with the interface of the catalyst layer; the influence on the catalytic activity of the catalyst and the gas blocking capability of the proton exchange membrane in the direct membrane deposition process is reduced;
3) the method can prepare the film-coated electrode with larger size at one time, and can cut the film-coated electrode into film-coated electrodes with certain size according to the requirements; the prepared membrane coating electrode can be directly used or placed for standby, the membrane electrode preparation process can be continuously operated or discontinuously operated, the operation is flexible, and the mass production of the membrane electrode can be realized.
The key technical points of the application are as follows:
1. the method of preparing the membrane-coated electrode by directly coating the proton-conducting polymer on the substrate and then placing the gas diffusion electrode can comprise the following steps:
a) the interlayer contact and the interface bonding force between the catalyst layer and the proton exchange membrane are effectively improved (the proton conductive polymer in a solution state has a certain bonding effect);
b) the problems that each functional layer is independently manufactured and the material transmission resistance of an interlayer interface is large in the preparation process of the membrane electrode by the traditional CCM method or CCS method are solved;
c) the problem that the catalytic activity of a membrane electrode and the gas blocking capability of a proton exchange membrane are influenced by the fact that a proton conducting polymer in a solution state permeates into pores and cracks of a catalytic layer under the action of gravity in the direct membrane deposition process is solved;
2. the preparation process of the proton exchange membrane is directly integrated into the preparation process of the membrane electrode, the preparation process is simple, and the time and the production cost are saved;
3. the film coating electrode with larger size can be prepared at one time; the film-coated electrode can be cut into film-coated electrodes with required sizes according to requirements; the prepared membrane coating electrode can be directly used or placed for standby, and the membrane electrode preparation process can be continuous operation or discontinuous operation; the preparation method of the membrane electrode can realize the mass production of the membrane electrode.
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 flow chart of the steps in the fuel cell membrane electrode preparation process of the present invention;
FIG. 2 is a schematic view of a membrane electrode structure prepared by the method of the present invention;
wherein 1 is a gas diffusion electrode, 11 is a gas diffusion layer, 12 is a catalyst layer, 2 is a proton exchange membrane, and 3 is an insulating airtight frame layer;
FIG. 3 is a graph comparing the performance curves of the membrane electrode assembly fuel cell prepared in example 1 and the membrane electrode assembly fuel cell prepared in comparative example 1;
FIG. 4 is a linear scan plot of a membrane electrode assembly fuel cell prepared in example 1;
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
In the following examples, materials and instruments used are commercially available unless otherwise specified.
Example 1
In the preparation method of the fuel cell membrane electrode related in this embodiment, the membrane electrode structure is shown in fig. 2, and includes, from bottom to top, a gas diffusion electrode 1, a proton exchange membrane layer 2, an insulating airtight frame layer 3, a proton exchange membrane layer 2, and a gas diffusion electrode 1; the gas diffusion electrode 1 includes a gas diffusion layer 11 and a catalytic layer 12; the proton exchange membrane layer 2 is located on the catalytic layer 12 side of the gas diffusion electrode 1.
The process flow of the membrane electrode of the embodiment is shown in fig. 1, and specifically comprises the following steps:
a) coating a 20 wt% Nafion solution on the PTFE substrate uniformly using a doctor blade coating apparatus, the coating size of the Nafion solution in this example being 10cm by 30 cm;
b) preparation of film-coated electrode: placing a gas diffusion electrode coated with 20 wt% of Nafion solution in the same size as the proton-conducting polymer solution coated in step a), wherein the catalytic layer side of the gas diffusion electrode is in contact with the proton-conducting polymer solution; then putting the prepared sample into a 100 ℃ oven for drying for 1h, then carrying out annealing heat treatment at 120 ℃ for 15min, and peeling the sample from the PTFE substrate to obtain a membrane coating electrode;
c) cutting for later use: cutting the large-size film coating electrode prepared in the step b) into required sizes for later use, wherein the size is cut to be 3.3 x 3.3cm in the embodiment;
d) assembling a membrane electrode blank: placing an insulating airtight frame (made of PET, the size of the outer frame is 4.5 x 4.5cm, the size of the inner frame is 2.7 x 2.7cm, and the thickness is 20 micrometers) at the peripheral edge of the film coating electrode, aligning another film coating electrode at the other side of the insulating airtight frame, and aligning the two film coating electrodes to form a film electrode blank;
e) hot-press molding: hot-pressing the membrane electrode blank assembled in the step d) in a hot press, setting the hot-pressing temperature to be 120 ℃, setting the pressure to be 0.3MPa, and setting the time to be 2min, thus obtaining the membrane electrode after the hot pressing is finished.
Example 2
The process flow of the membrane electrode of the embodiment is shown in fig. 1, and specifically comprises the following steps;
a) coating a 20 wt% Nafion solution on a glass substrate uniformly using a slit extrusion coating apparatus, the coating size of the Nafion solution in this example being 10cm by 30 cm;
b) preparation of film-coated electrode: placing a gas diffusion electrode coated with 20 wt% of Nafion solution in the same size as the proton-conducting polymer solution coated in step a), wherein the catalytic layer side of the gas diffusion electrode is in contact with the proton-conducting polymer solution; then, drying the prepared sample in an oven at 80 ℃ for 4h, then carrying out annealing heat treatment at 120 ℃ for 60min, and stripping the sample from the glass substrate to obtain a film-coated electrode;
c) cutting for later use: cutting the large-size film coating electrode prepared in the step b) into required sizes for later use, wherein the size is cut to be 3.3 x 3.3cm in the embodiment;
d) assembling a membrane electrode blank: placing an insulating airtight frame (made of glass fiber reinforced polytetrafluoroethylene, the size of the outer frame is 4.5 x 4.5cm, the size of the inner frame is 2.7 x 2.7cm, and the thickness is 50 μm) at the circumferential edge of the film coating electrode, then placing another film coating electrode on the other side of the insulating airtight frame in an aligned manner, and placing the two film coating electrodes in an aligned manner to form a film electrode blank;
e) hot-press molding: hot-pressing the membrane electrode blank assembled in the step d) in a hot press, setting the hot-pressing temperature to be 120 ℃, setting the pressure to be 0.4MPa, and setting the time to be 2min, thus obtaining the membrane electrode after the hot pressing is finished.
Comparative example 1
Two gas diffusion electrodes (Pt loading 0.4 mg/cm) with a size of 3.3X 3.3cm were taken2) A sheet of 4.5 x 4.5cm sizeAnd (3) a proton exchange membrane, wherein two gas diffusion electrodes are symmetrically arranged on two sides of the proton exchange membrane to form a sandwich structure, and hot pressing is carried out (the hot pressing conditions are that the temperature is 120 ℃, the pressure is 0.4MPa, and the time is 2min) to prepare the membrane electrode of the CCS method.
Performance testing of examples and comparative examples
Single cell performance testing of example 1 and comparative example 1: and respectively introducing hydrogen and air into the anode and the cathode of the single cell, wherein the gas flow of the hydrogen is 400mL/min, the gas flow of the air is 800mL/min, the humidification humidity of the anode and the cathode is 100%, the temperature of the fuel cell is 80 ℃, and no back pressure exists. Example 1 single cell hydrogen permeation current test: and respectively introducing hydrogen and nitrogen into the anode and the cathode of the single cell, wherein the hydrogen flow is 400mL/min, the nitrogen flow is 400mL/min, the humidification humidity of the anode and the cathode is 100%, the temperature of the fuel cell is 80 ℃, and no back pressure exists.
As can be seen from FIG. 3, the membrane electrode assembly cell prepared in example 1 measured an open circuit voltage of 0.947V and a peak power density of 480mW/cm2(ii) a The CCS type membrane electrode assembled single cell in the comparative example 1 measures that the open-circuit voltage is 0.865V and the peak power density is 322mW/cm2. Obviously, compared with the CCS type membrane electrode, the open-circuit voltage and the peak power of the membrane electrode prepared in the comparative example are obviously improved. As can be seen from FIG. 4, the membrane electrode prepared in example 1 measured a hydrogen permeation current of about 1.6mA/cm2Is superior to the conventional CCS type membrane electrode (about 2 mA/cm)2). In the embodiment, the proton conduction polymer solution is coated on the bottom membrane, and then the gas diffusion electrode is directly placed on the coated proton conduction polymer solution, so that the proton conduction polymer can be reduced from permeating into pores and cracks of the catalyst layer while ensuring good contact between the proton exchange membrane and the interface of the catalyst layer in the prepared membrane electrode, the manufacturing defects of the proton exchange membrane are reduced, the influence on the catalytic activity of the catalyst and the gas blocking capability of the proton exchange membrane in the direct membrane deposition process is reduced, and the electrical output performance of the membrane electrode is improved.
The number and main features of the integrated type membrane electrode prepared in each example, and the performance of the fuel cell assembled using the integrated type membrane electrode are shown in table 1.
TABLE 1
In summary, the method for preparing the membrane electrode provided by the invention directly coats the large-area proton exchange membrane coating on the coating substrate, then places the gas diffusion electrode, dries and anneals to form the large-size membrane coating, can cut into semi-finished products with certain sizes according to requirements for later use, and assembles and hot-presses the two membrane coating electrodes and the insulating airtight frame to form the membrane electrode when in use. The method can ensure good contact between the proton exchange membrane and the interface of the catalyst layer in the prepared membrane electrode, reduce the permeation of the proton conduction polymer to the pores and cracks of the catalyst layer, and reduce the influence of the direct membrane deposition process on the catalytic activity of the catalyst and the gas blocking capability of the proton exchange membrane; the method can prepare the film-coated electrode with larger size at one time, and then cut the film-coated electrode into the film-coated electrode with the required size according to the requirement, the prepared film-coated electrode can be directly used or placed for standby, and the film electrode preparation process can be continuous operation or discontinuous operation; the method has simple preparation process, breaks through the size limit and the time limit in the membrane electrode manufacturing process, and can realize the batch production of the membrane electrode.
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 fuel cell membrane electrode is characterized by comprising the following steps;
1) coating a large area of proton-conducting polymer solution on a coated substrate using a coating apparatus;
2) preparation of film-coated electrodes
a) Placing a gas diffusion electrode having the same size as the proton-conducting polymer solution coated on the proton-conducting polymer solution coated in step 1), wherein the catalyst layer side of the gas diffusion electrode is in contact with the proton-conducting polymer solution;
b) drying, molding and annealing the sample prepared in the step a), and peeling the sample from the coating substrate to obtain a film coating electrode;
3) cutting for later use: cutting the large-size film coating electrode prepared in the step 2) into required sizes for later use;
4) assembling a membrane electrode blank: placing an insulating airtight frame at the circumferential edge of the film coating electrode, aligning another film coating electrode on the other side of the insulating airtight frame, and aligning the two film coating electrodes to form a film electrode blank;
5) hot-press molding: and carrying out hot-pressing treatment on the membrane electrode blank to obtain the integrated membrane electrode.
2. The method according to claim 1, wherein the coating is spray coating, ultrasonic spray coating, blade coating, or slit extrusion coating.
3. The method of claim 1, wherein the coating substrate is any one of a glass plate, a teflon, a silicon oil film, and a polydimethylsiloxane plate.
4. The method according to claim 1, wherein the proton conducting polymer solution is one or more of a combination of perfluorosulfonic acid solution, sulfonated polyetheretherketone solution, and sulfonated trifluorostyrene solution.
5. The production method according to claim 1, wherein the gas diffusion electrode comprises a catalytic layer and a gas diffusion layer; the Pt loading capacity in the catalytic layer is 0.1-0.4mg/cm2。
6. The preparation method according to claim 1, wherein the drying treatment temperature is 60-100 ℃ and the time is 1-4 h; the annealing heat treatment temperature is 110-150 ℃, and the time is 5-120 min.
7. The method of claim 1, wherein the insulating gas-tight frame is placed on the proton exchange membrane side of the membrane-coated electrode.
8. The preparation method according to claim 1, wherein the insulating airtight frame comprises an inner frame and an outer frame in sequence in the radial direction of the membrane electrode, the outer frame is exposed out of the membrane coating electrode, the inner frame is embedded into the proton exchange membrane layer of the membrane electrode, and the space in the middle of the inner frame is an active reaction area.
9. The method as claimed in claim 1, wherein the material of the insulating and airtight frame is one or more of polyethylene terephthalate, glass fiber reinforced polytetrafluoroethylene, polyimide, and silicone rubber, and the thickness is 5-50 μm.
10. The method as claimed in claim 1, wherein the heat treatment temperature of the hot press molding is 100-150 ℃, the pressure is 0.1-1MPa, and the hot press time is 0.5-3 min.
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