CN112259746A - Metal tin bonded fuel cell flexible gas diffusion membrane and preparation method thereof - Google Patents
Metal tin bonded fuel cell flexible gas diffusion membrane and preparation method thereof Download PDFInfo
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- CN112259746A CN112259746A CN202011114606.XA CN202011114606A CN112259746A CN 112259746 A CN112259746 A CN 112259746A CN 202011114606 A CN202011114606 A CN 202011114606A CN 112259746 A CN112259746 A CN 112259746A
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- fuel cell
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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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
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8668—Binders
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention belongs to the technical field of fuel cell membrane electrodes, and provides a metal tin bonded fuel cell flexible gas diffusion membrane and a preparation method thereof. According to the method, metallic tin powder, a conductive carbon material, coke powder, a foaming agent, wood fiber and cellulose ether colloid are used as raw materials to prepare a paste, then cold rolling and foaming shaping are carried out to obtain a fluffy sheet, and then the fluffy sheet is heated, sintered, treated by steam and dried to prepare the flexible fuel cell gas diffusion membrane. Compared with the traditional method, the prepared gas diffusion membrane has the advantages of good flexibility and toughness, reservation of network gaps of the conductive carbon material, avoidance of the defect that the conductivity and the air permeability are influenced by using a polymer, simple preparation process, easiness in large-scale continuous production, low energy consumption and low cost.
Description
Technical Field
The invention belongs to the technical field of fuel cell membrane electrodes, and provides a metal tin bonded fuel cell flexible gas diffusion membrane and a preparation method thereof.
Background
The fuel cell is a zero-emission, high-efficiency and high-power-density power generation device, and particularly has an extremely attractive prospect in the aspect of new energy traffic power application. The key technical core component of a fuel cell is the membrane electrode, which serves as the "core" of the fuel cell. Membrane electrodes are the site for heterogeneous mass transport and electrochemical reactions, and determine the performance, life, and cost of fuel cells.
The membrane electrode assembly is an assembly of a diffusion layer-catalyst layer-proton exchange membrane-catalyst layer and a diffusion layer structure, wherein the diffusion layer-catalyst layer-proton exchange membrane-catalyst layer and the diffusion layer structure are formed by respectively compounding a catalyst layer and a gas diffusion layer on two sides by taking a proton exchange membrane as an interlayer center. The fuel cell diffusion layer is a key component affecting the cell performance, and has the main functions of: supporting the catalyst and the membrane structure; uniformly distributing gas; support the whole structure and simultaneously require the diffusion layer to be a transmission channel of gas, electrons and water. Therefore, the diffusion layer is required to have the comprehensive characteristics of conductivity, air permeability, hydrophobicity and strength.
At present, carbon paper is mostly used for a diffusion layer of a fuel cell, but the existing carbon paper preparation technology has defects in the aspect of industrial preparation of carbon paper, preforming of carbon fibers is difficult, energy consumption of subsequent high-temperature carbonization is high, and the prepared carbon fiber paper is brittle and not folding-resistant and is difficult to produce in large scale in batches. In particular, when used for a gas diffusion layer, the carbon paper is likely to be damaged due to the adhesion. How to ensure good conductivity and air permeability of the carbon paper and good flexibility is the problem which needs to be solved in the large-scale application of the carbon paper in the fuel cell at present. In addition, the problem of brittle fracture can be better solved by preparing the fuel cell carbon paper by calendering the conductive carbon material and the polymer.
At present, the membrane electrode technology of the fuel cell, especially the gas diffusion layer of the fuel cell, has achieved certain effect at home and abroad. Among them, wang biao et al invented a preparation of carbon fiber paper for a gas diffusion layer of a proton exchange membrane fuel cell (chinese patent application No. 200910053648.4), the invention includes: (1) performing water treatment on the pitch-based carbon fiber, and performing activation treatment on the PAN-based pre-oxidized fiber; (2) chopping; (3) mixing and carrying out wet papermaking forming to obtain base paper; (4) dispersing carbon nano tubes and/or conductive carbon black particles in a resin solution (5), spraying the resin solution on the upper surface and the lower surface of the base paper, drying and then hot-pressing to obtain a semi-finished product; (6) and carrying out heat treatment on the semi-finished product to obtain the product. Further, a gas diffusion layer material for a proton exchange membrane fuel cell has been invented by people like liuhuan (chinese patent application No. 201721695602.9), and the gas diffusion layer carbon includes: carbon fiber layer, micropore conductive coating. The carbon fiber layer is distributed with nano carbon fiber and short carbon fiber, and the upper part and the lower part of the carbon fiber layer are provided with a micropore conductive coating consisting of graphene and PETE.
Therefore, in the prior art, the carbon paper for the fuel cell, which is prepared by calendering the conductive carbon material and the polymer, has certain toughness, but has the defects of poor conductivity and poor air permeability due to the influence of the polymer.
Disclosure of Invention
Aiming at the situation, the flexible gas diffusion membrane of the fuel cell bonded by the metal tin and the preparation method are provided, so that the flexibility and the toughness of the gas diffusion layer can be effectively ensured, and the conductivity and the air permeability are improved.
In order to achieve the purpose, the invention relates to the following specific technical scheme:
a preparation method of a flexible gas diffusion membrane of a metal tin bonded fuel cell comprises the following steps of preparing paste by using metal tin powder, a conductive carbon material, coke powder, a foaming agent, wood fibers and cellulose ether colloid as raw materials, carrying out cold rolling and foaming shaping to obtain a fluffy sheet, heating and sintering the fluffy sheet, carrying out steam treatment and drying to obtain the flexible gas diffusion membrane of the fuel cell, wherein the preparation method comprises the following specific steps:
(1) adding metallic tin powder, a conductive carbon material, coke powder, a foaming agent, wood fiber and cellulose ether colloid into a mixer, and stirring at the temperature of 40-50 ℃ and the rotating speed of 100-200 r/min for 2-3 h to prepare a paste;
(2) adding the paste prepared in the step (1) into a three-roller cold calender, preparing a sheet by using a cold calendering process, slowly heating to 190-210 ℃ at a heating rate of 10-15 ℃/min, foaming and shaping for 30-40 min, and preparing a fluffy sheet;
(3) and (3) loosening the fluffy sheet prepared in the step (2), placing the fluffy sheet in a temperature sintering furnace for sintering, enabling the dispersed metal tin powder to be molten and bonded with a carbon material, immediately sending the sheet into a steam chamber for processing for 10-30 min, processing the sheet by using gas generated by the reaction of red hot coke powder and water vapor to prevent metal tin from blocking micropores, then introducing the sheet into a drying tunnel through a traction roller, and drying to obtain the metal tin bonded fuel cell flexible gas diffusion membrane.
Tin is a silvery-white soft metal, is easy to bend, rich in malleability, low in melting point, stable in chemical property, not easy to be oxidized by oxygen at normal temperature and non-toxic; the foaming agent is selected in consideration of the stable foaming effect, a simple foaming process and an easily controlled gas release amount, an azo compound and a sulfonyl hydrazine compound in the organic foaming agent are selected as the foaming agent, and in addition, the addition amount of the foaming agent needs to be effectively controlled so as to ensure stable foaming and achieve a fluffy effect; the conductive filler can be selected from common conductive carbon materials. Preferably, the conductive carbon material is at least one of carbon fiber, carbon nanotube, mesoporous carbon, carbon black, carbon aerogel, graphite and graphene; the foaming agent is at least one of azodicarbonamide, azodiisobutyronitrile, diphenyl sulfonyl hydrazide ether, p-toluene sulfonyl hydrazide and 4, 4' -oxybis-benzenesulfonyl hydrazide; the cellulose ether colloid is at least one of methyl cellulose ether colloid, hydroxyethyl methyl cellulose ether colloid, carboxymethyl cellulose ether colloid, ethyl cellulose ether colloid, benzyl cellulose ether colloid, hydroxyethyl cellulose ether colloid, carboxymethyl hydroxyethyl cellulose ether colloid and phenyl cellulose ether colloid with the mass concentration of 5%.
The amount of each raw material added is related to the performance of the gas diffusion layer of the fuel cell, and may even affect the cell performance of the fuel cell, so the ratio of each raw material is important. More preferably, in the step (1), the weight parts of the raw materials include 8-12 parts of metallic tin powder, 30-35 parts of conductive carbon material, 6-10 parts of coke powder, 3-6 parts of foaming agent, 12-15 parts of wood fiber and 22-41 parts of cellulose ether colloid.
The cold rolling process is selected, the temperature in the rolling process is controlled, and the high temperature can be prevented from damaging the active ingredients such as cellulose ether colloid and the like in the raw materials; preferably, the cold rolling temperature is room temperature, and the pressure is 2-4 MPa.
In the foaming process of the foaming agent, the temperature is a critical quantity, so that the effect of stable foaming is achieved, the uncontrollable release of foaming agent gas caused by rapid temperature rise is avoided, the uniformity of foam holes is influenced, and the gas permeability of the material is further influenced. Preferably, in the step (2), the temperature is slowly increased to 190-210 ℃ at the temperature increase rate of 10-15 ℃/min, and the foaming and shaping are carried out for 30-40 min.
Sintering the material at 235-240 ℃, wherein the tin powder has a low melting point, so that the metal tin powder dispersed in the sheet is melted and firmly bonded with the carbon material, thereby ensuring the connection and flexibility of the carbon material, improving the toughness of the gas diffusion layer, keeping network gaps of the conductive carbon material in the gas diffusion layer, and avoiding the defects that the conductivity and the air permeability are influenced by using a polymer; the coke powder and the water vapor can react at high temperature to generate carbon monoxide and hydrogen, and the generated gas is used for impacting micropores to prevent the micropores of the fluffy sheet material from being blocked by tin. Preferably, the sintering temperature is 235-240 ℃, and the time is 3-5 min; the drying temperature is 120-150 ℃, and the drying time is 60-80 min.
The invention also provides the metal tin bonded fuel cell flexible gas diffusion membrane prepared by the preparation method. The gas diffusion layer is formed by uniformly dispersing metal tin powder, a conductive carbon material, coke powder, a foaming agent, wood fiber and cellulose ether colloid into paste; then cold-pressing and rolling the paste into sheets, foaming and shaping to form fluffy sheets; then loose and sinter the fluffy sheet, send into the steam chamber immediately, and then introduce into the drying tunnel through the carry-over pinch rolls and dry to get final product. Not only has good flexibility and toughness, but also has the similar conductivity and air permeability of carbon fiber paper.
Compared with the prior art, the invention provides a metal tin bonded fuel cell flexible gas diffusion membrane and a preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. the gas diffusion membrane prepared by the invention has excellent performance and can be widely used for the gas diffusion layer of the membrane electrode of the fuel cell.
2. According to the preparation method disclosed by the invention, metal tin is used as the binder, so that the toughness of the gas diffusion layer is improved, and the defect that the conductivity and the air permeability are influenced by using a polymer is avoided.
3. The preparation method has the advantages of simple preparation process, easy large-scale continuous production, low energy consumption and low cost.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
Adding 10g of metallic tin powder, 33g of carbon fiber, 7g of coke powder, 5g of azodicarbonamide, 13g of wood fiber and 33g of methyl cellulose ether colloid with the mass concentration of 5% into a mixer, and stirring at 47 ℃ at the rotating speed of 160r/min for 2.5h to prepare paste; then adding the paste into a three-roller cold calender, cold-rolling at room temperature and under the pressure of 3MPa to prepare a sheet with the thickness of 0.1mm, heating to 200 ℃ at the heating rate of 12 ℃/min, and carrying out heat preservation treatment for 35min to carry out foaming and shaping to prepare a fluffy sheet; and then loosening the fluffy sheet, placing the fluffy sheet in a sintering furnace at the temperature of 237 ℃ for 5min, immediately sending the fluffy sheet into a steam chamber for treatment for 18min, and introducing the fluffy sheet into a drying tunnel at the temperature of 130 ℃ for 68min through a traction roller to obtain the metal tin bonded fuel cell flexible gas diffusion membrane with the average thickness of 0.3 mm.
The test method comprises the following steps:
air permeability: the air permeability of the gas diffusion membrane prepared by the invention at normal temperature is obtained by testing under the pressure difference of 80 Pa;
resistivity: testing according to a four-probe method;
flexibility, referring to the folding resistance of the paper, and testing the folding resistance times.
The data obtained are shown in Table 1.
Example 2
Adding 11g of metallic tin powder, 34g of carbon nano tube, 9g of coke powder, 5g of azodiisobutyronitrile, 14g of wood fiber and 27g of hydroxyethyl methyl cellulose ether colloid with the mass concentration of 5% into a mixer, and stirring at the temperature of 48 ℃ at the rotating speed of 180r/min for 2 hours to prepare a paste; then adding the paste into a three-roller cold calender, cold-rolling at room temperature and under the pressure of 3.5MPa to prepare a sheet with the average thickness of 0.1mm, raising the temperature to 208 ℃ at the heating rate of 14 ℃/min, and carrying out heat preservation treatment for 32min for foaming and shaping; and then loosening the fluffy sheet, placing the fluffy sheet in a sintering furnace at the temperature of 238 ℃ for 4min, immediately sending the fluffy sheet into a steam chamber for treatment for 15min, and introducing the fluffy sheet into a drying tunnel at the temperature of 140 ℃ for 65min through a traction roller to obtain the metal tin bonded fuel cell flexible gas diffusion membrane with the average thickness of 0.4 mm.
The test method was in accordance with example 1, and the data obtained are shown in Table 1.
Example 3
Adding 9g of metallic tin powder, 31g of mesoporous carbon, 7g of coke powder, 4g of diphenyl sulfonyl hydrazide ether, 13g of wood fiber and 36g of carboxymethyl cellulose ether colloid with the mass concentration of 5% into a mixer, and stirring at 42 ℃ for 2 hours at the rotating speed of 180r/min to prepare a paste; then adding the paste into a three-roller cold calender, cold-rolling at room temperature and under the pressure of 2.5MPa to prepare a sheet with the average thickness of 0.1mm, raising the temperature to 200 ℃ at the heating rate of 12 ℃/min, and carrying out heat preservation treatment for 38min for foaming and shaping; and then loosening the fluffy sheet, placing the fluffy sheet in a sintering furnace at the temperature of 236 ℃ for 5min, immediately sending the fluffy sheet into a steam chamber for treatment for 25min, and introducing the fluffy sheet into a drying tunnel at the temperature of 130 ℃ for 75min through a traction roller to obtain the metal tin bonded fuel cell flexible gas diffusion membrane with the average thickness of 0.4 mm.
The test method was in accordance with example 1, and the data obtained are shown in Table 1.
Example 4
Adding 12g of metallic tin powder, 35g of carbon black, 10g of coke powder, 6g of p-toluenesulfonyl hydrazide, 15g of wood fiber and 28g of ethyl cellulose ether colloid with the mass concentration of 5% into a mixer, and stirring at the temperature of 50 ℃ and the rotating speed of 200r/min for 2 hours to prepare a paste; then adding the paste into a three-roller cold calender, cold-rolling at room temperature and under the pressure of 4MPa to prepare a sheet with the average thickness of 0.1mm, heating to 210 ℃ at the heating rate of 15 ℃/min, and carrying out heat preservation treatment for 30min for foaming and shaping to prepare a fluffy sheet; and then loosening the fluffy sheet, placing the fluffy sheet in a sintering furnace at the temperature of 240 ℃ for 5min, then sending the fluffy sheet into a steam chamber, and introducing the fluffy sheet into a drying tunnel at the temperature of 150 ℃ for 60min through a traction roller to obtain the metal tin bonded fuel cell flexible gas diffusion membrane with the average thickness of 0.5 mm.
The test method was in accordance with example 1, and the data obtained are shown in Table 1.
Comparative example 1
Commercially available Dongli carbon fiber paper.
The test method was in accordance with example 1, and the data obtained are shown in Table 1.
Table 1:
Claims (10)
1. a preparation method of a metal tin bonded fuel cell flexible gas diffusion membrane is characterized in that metal tin powder, a conductive carbon material, coke powder, a foaming agent, wood fibers and cellulose ether colloid are used as raw materials to prepare a paste, then the paste is subjected to cold rolling and foaming sizing to obtain a fluffy sheet, and then the fluffy sheet is subjected to heating sintering, water vapor treatment and drying to prepare the flexible fuel cell gas diffusion membrane, wherein the preparation method comprises the following specific steps:
(1) adding metallic tin powder, a conductive carbon material, coke powder, a foaming agent, wood fiber and cellulose ether colloid into a mixer, and stirring at the temperature of 40-50 ℃ and the rotating speed of 100-200 r/min for 2-3 h to prepare a paste;
(2) adding the paste prepared in the step (1) into a three-roller cold calender, preparing a sheet by using a cold calendering process, slowly heating to 190-210 ℃ at a heating rate of 10-15 ℃/min, foaming and shaping for 30-40 min, and preparing a fluffy sheet;
(3) and (3) loosening the fluffy sheet prepared in the step (2), placing the fluffy sheet in a sintering furnace for sintering, enabling the dispersed metal tin powder to be molten and bonded with a carbon material, immediately sending the sheet into a steam chamber for processing for 10-30 min, processing the sheet by using gas generated by the reaction of red hot coke powder and water vapor to prevent metal tin from blocking micropores, then introducing the sheet into a drying tunnel through a traction roller, and drying to obtain the metal tin bonded fuel cell flexible gas diffusion membrane.
2. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: the conductive carbon material in the step (1) is at least one of carbon fiber, carbon nano tube, mesoporous carbon, carbon black, carbon aerogel, graphite and graphene.
3. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: the foaming agent in the step (1) is at least one of azodicarbonamide, azodiisobutyronitrile, diphenyl sulfonyl hydrazide ether, p-toluenesulfonyl hydrazide and 4, 4' -oxybis-benzenesulfonyl hydrazide.
4. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: the cellulose ether colloid in the step (1) is at least one of methyl cellulose ether colloid, hydroxyethyl methyl cellulose ether colloid, carboxymethyl cellulose ether colloid, ethyl cellulose ether colloid, benzyl cellulose ether colloid, hydroxyethyl cellulose ether colloid, carboxymethyl hydroxyethyl cellulose ether colloid and phenyl cellulose ether colloid with the mass concentration of 5%.
5. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: the weight parts of the raw materials in the step (1) are 8-12 parts of metallic tin powder, 30-35 parts of conductive carbon material, 6-10 parts of coke powder, 3-6 parts of foaming agent, 12-15 parts of wood fiber and 22-41 parts of cellulose ether colloid.
6. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: and (3) performing cold rolling in the step (2) at room temperature and under the pressure of 2-4 MPa.
7. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: and (2) slowly raising the temperature to 200 ℃ at the temperature rise rate of 12 ℃/min, and foaming and shaping for 35 min.
8. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: and (3) sintering at 235-240 ℃ for 3-5 min.
9. The method of claim 1, wherein the step of forming a flexible gas diffusion membrane for a metal tin bonded fuel cell comprises: and (4) drying at the temperature of 120-150 ℃ for 60-80 min.
10. A metal tin bonded fuel cell flexible gas diffusion membrane, characterized in that the metal tin bonded fuel cell flexible gas diffusion membrane prepared by the preparation method of any one of claims 1 to 9.
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Application publication date: 20210122 |