CN113964330B - Novel single-layer gas diffusion layer for fuel cell and preparation method and application thereof - Google Patents
Novel single-layer gas diffusion layer for fuel cell and preparation method and application thereof Download PDFInfo
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- CN113964330B CN113964330B CN202111235400.7A CN202111235400A CN113964330B CN 113964330 B CN113964330 B CN 113964330B CN 202111235400 A CN202111235400 A CN 202111235400A CN 113964330 B CN113964330 B CN 113964330B
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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
- H01M4/8605—Porous electrodes
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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
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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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- 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 relates to a single-layer gas diffusion layer for a fuel cell and a preparation method and application thereof, wherein the gas diffusion layer only comprises a microporous layer, the microporous layer takes a carbon material, a hydrophobic binder and a pore-forming agent as raw materials, and the carbon-free paper and self-supporting microporous layer is prepared by dry compression molding, so that the gas diffusion layer has good hydrophobicity, gas permeability and electrical conductivity, and can reduce the resistance of water discharge, thereby relieving cathode flooding. The dry preparation avoids the defect that cracks are generated on the surface of the solvent volatilized by the wet method, thereby avoiding flooding caused by water collection at the cracks. The thickness and the porosity of the prepared carbon-free paper and self-supporting microporous layer are controllable; the preparation process is simple and the condition is mild. The carbon-free paper and the self-supporting microporous layer prepared by the invention have better electrochemical performance when being used as a gas diffusion layer of a fuel cell. The invention has wide application value in the field of fuel cells.
Description
Technical Field
The invention relates to a single-layer gas diffusion layer for a fuel cell, and a preparation method and application thereof, and belongs to the technical field of fuel cells.
Background
The fuel cell is a power generation device for directly converting chemical energy stored in fuel and oxidant into electric energy through electrochemical reaction, and compared with other conventional power generation modes, the fuel cell is not limited by Carnot cycle, the energy conversion efficiency can reach 60%, the reliability is high, and the environment is friendly. Proton Exchange Membrane Fuel Cell (PEMFC) is a kind of fuel cell, is a clean and efficient energy conversion device capable of directly converting chemical energy of hydrogen into electric energy, and can be widely applied to the fields of automobiles, power stations, portable power supplies and the like.
When the proton exchange membrane fuel cell is operated at high current density, if the produced water cannot be timely discharged from the PEMFC, the Membrane Electrode (MEA) is flooded, and the hydrogen and the oxygen are prevented from reaching the active site of the catalyst to react, so that the performance of the PEMFC is drastically reduced. And when the water content in the battery is low, the membrane is easy to dry, and the conduction of protons is not facilitated. Therefore, effective water management to maintain water balance within the cell is a key to improving the output performance of the fuel cell, and the gas diffusion layer serves as a core component of the MEA, and has important research significance in carrying the roles of water drainage, gas guide, electrical conduction, catalyst support, and the like in the fuel cell.
The current commercialized gas diffusion layer consists of two layers, wherein one layer is hydrophobic treated carbon paper or carbon cloth, also called a basal layer; the other layer is a microporous layer, typically composed of conductive carbon black and a hydrophobic binder. Because the preparation process of the carbon paper is complex and comprises thousands of high-temperature heat treatment, the cost is high, and a large amount of organic solvents are used in the preparation process of the microporous layer, on one hand, the preparation process does not conform to the healthy green development concept, and on the other hand, the preparation cost is increased. The high cost of the gas diffusion layer is one of the reasons that the commercialization of proton exchange membrane fuel cells is hindered. Therefore, the preparation of a low-cost, high-performance gas diffusion layer is of great importance to fuel cells.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a carbon-free paper for a fuel cell, a self-supporting microporous layer, a preparation method and application thereof, and aims to reduce cost and adapt to mass production.
In one aspect, the invention provides a proton exchange membrane fuel cell gas diffusion layer, which has a single-layer structure and only comprises carbon-free paper and a self-supporting microporous layer, wherein the microporous layer has a porous structure with the porosity of more than 75%, and the porous structure comprises micropores and macropores, wherein the micropore accounts for 60% -75%; the micropores are pores with the pore diameter smaller than 1 mu m, and the macropores are pores with the pore diameter larger than 5 mu m.
Further, in the above technical scheme, the pore diameter of the micropores is 100-1000nm, and the pore diameter of the macropores is 5-10 μm.
In another aspect, the present invention provides a method for preparing the gas diffusion layer, wherein the microporous layer is prepared by dry molding, and the dry molding is as follows: the raw materials are mechanically ground and uniformly mixed, and then are sequentially subjected to hot pressing, cooling, acid treatment, washing and drying to obtain the microporous layer; the raw materials comprise conductive carbon materials, hydrophobic polymer binders and pore formers.
Further, in the technical scheme, the mass ratio of the conductive carbon material to the hydrophobic polymer binder to the pore-forming agent is 1:0.075-0.2:2.
Further, in the above technical solution, the conductive material is one or more of conductive carbon powder, carbon fiber, and carbon nanotube.
Further, in the above technical solution, the hydrophobic polymer binder is one or more of Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), and perfluoroethylene propylene copolymer (FEP).
Further, in the above technical scheme, the pore-forming agent is one or more of carbonate, bicarbonate and alkali.
Further, in the above technical solution, the dry molding specifically includes the following steps:
1) Mechanically grinding a certain proportion of carbon material, a hydrophobic agent and a pore-forming agent to form a uniformly mixed microporous layer mixture;
2) Spreading the uniformly mixed mixture in a self-made mold, and keeping the surface flat;
3) Putting the die into a hot press, firstly applying a certain pressure at room temperature to enable the raw materials to be in a sheet shape, then releasing pressure, carrying out heat treatment, keeping for a certain time after the temperature reaches a target temperature to enable the binder to be uniformly dispersed, finally closing and heating to enable the binder to be naturally cooled to the room temperature, and demoulding;
4) And soaking the obtained microporous layer material pressed into a sheet shape after demolding in acid to decompose a pore-forming agent, so that pores are generated in the gas diffusion layer, then soaking the microporous layer material in deionized water, washing the microporous layer material for the proton exchange membrane fuel cell for multiple times, and finally drying the microporous layer material in a vacuum drying oven to obtain the carbon-free paper and the self-supporting microporous layer for the proton exchange membrane fuel cell.
Further, in the above technical solution, the mechanical grinding time is 5-60min, preferably 30min.
Further, in the above technical scheme, the pressure is 0.1-1.0MPa, preferably 0.5MPa, and the pressing time is 1-60min, preferably 30min.
Further, in the technical scheme, the heat treatment temperature is 150-350 ℃, and the heat treatment time is 20-60min.
Further, in the above technical scheme, the acid soaking time is 1-6 hours, preferably 2 hours, and the deionized water soaking time is 1-12 hours, preferably 2 hours.
Further, in the technical scheme, the drying time is 1-24h, and the drying temperature is 60-120 ℃.
The invention also provides application of the single-layer gas diffusion layer for the proton exchange membrane fuel cell.
In the technical scheme, the cathode fuel and the anode fuel of the proton exchange membrane fuel cell are respectively air and hydrogen which are subjected to the same humidification treatment, and the humidification treatment is 40% -100% RH.
Advantageous effects
1. The surface of the carbon-free paper and self-supporting microporous layer provided by the invention is relatively flat and has no cracks, the porous structure is realized, the porosity is more than 75%, and the porosity is higher than that of the traditional double-layer gas diffusion layer, so that more channels are provided for gas-liquid mass transfer. Wherein the aperture of the micropore is 100-1000nm, which is beneficial to the transmission of liquid water, and the macropores with the diameter of 5-10 μm are beneficial to the transmission of reaction gas, thereby reducing the flooding and mass transfer polarization of the battery under large electric density.
2. According to the preparation method of the self-supporting microporous layer, the pore-forming agent is added into the microporous layer raw material, so that the pore-forming agent is decomposed to generate gas in the acid treatment process, and the gas is helpful for the microporous layer to form more water channels and gas channels when escaping; in addition, the pore-forming agent is removed by acid treatment, which is more green and thorough than the traditional heat treatment.
3. According to the invention, the microporous layer is prepared by a dry method, an organic solvent is not introduced in the preparation process, high-temperature treatment is not needed, and the preparation method is healthy, green, cheap and concise and easy for industrial production; meanwhile, the defect that cracks are generated on the surface of the solvent volatilized by the wet method is avoided, so that flooding caused by water collection at the cracks is avoided.
4. Compared with the traditional double-layer gas diffusion layer, the carbon-free paper and the self-supporting microporous layer provided by the invention have better electrochemical performance. This is because the conventional gas diffusion layer is 70% or more macroporous, and the self-supporting microporous layer has a larger proportion of micropores, and under the action of strong capillary force of the micropores, the breakthrough pressure of water becomes large, the back diffusion of water to the anode is enhanced, and the hydration degree of the Nafion membrane is improved, so that the proton conduction resistance is reduced, and therefore, the self-supporting microporous layer has better water retention capacity. Under the condition of 40% low humidification, the battery assembled by taking the carbon-free paper and the self-supporting microporous layer as the cathode gas diffusion layer has better performance than the traditional gas diffusion layer. Wherein, the whole cell performance of the sMPL-2 as the cathode gas diffusion layer is optimal, and the maximum output power density is improved by 37.4% compared with that of the traditional double-layer gas diffusion layer C-GDL.
Drawings
FIG. 1 (A) is an SEM image of the carbon-free paper and self-supporting microporous layer obtained in example 2 of the present invention; fig. 1 (B) is an SEM image of comparative example 1.
FIG. 2 is a graph showing pore size distribution of the carbon-free paper, the self-supporting microporous layer and the conventional gas diffusion layer of comparative example 1 obtained in examples 1 to 3 of the present invention.
FIG. 3 is a graph showing a comparison of the performance of a full cell at 40% humidification of the carbon-free paper, self-supporting microporous layer obtained in examples 1-3 of the present invention, and a conventional gas diffusion layer of comparative example 1.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
Weighing carbon fiberVitamin 1.0g, hydrophobic binder PVDF 0.075g, pore-forming agent K 2 CO 3 2.0g, mechanically mixing for 30min by a pulverizer, and spreading the uniformly mixed mixture in a self-made stainless steel die after fully grinding and mixing to ensure the surface to be smooth. The mold was then placed in a hot press and was first pressed at room temperature under a pressure of 0.5MPa for 30min to make the mixture into a tablet. Then releasing pressure and heating to raise the temperature to 150 ℃, and heat treating for 20min at 150 ℃ to uniformly distribute PVDF in the carbon-free paper and self-supporting microporous layer. Naturally cooling the mold to room temperature by closing and heating, taking out the obtained sheet sample from the mold, soaking in HCl solution for 2h to remove pore-forming agent in the microporous layer, and forming pores inside the microporous layer, wherein the concentration of the HCl solution is 2mol L -1 . After the acid soaking is finished, soaking the sample in deionized water for 2 hours to remove residual HCl in the microporous layer, finally drying the sample in a vacuum drying oven for 2 hours at the drying temperature of 100 ℃, and removing the deionized water in the microporous layer to obtain a carbon-free paper and self-supporting microporous layer for a proton exchange membrane fuel cell, which is named sMPL-1, wherein the carbon powder loading amount is 28mg cm -2 。
Example 2
Weighing 1.0g of carbon fiber, 0.1111g of hydrophobic binder PVDF and pore-forming agent K 2 CO 3 2.0g, mechanically mixing for 30min by a pulverizer, and spreading the uniformly mixed mixture in a self-made stainless steel die after fully grinding and mixing to ensure the surface to be smooth. The mold was then placed in a hot press and was first pressed at room temperature under a pressure of 0.5MPa for 30min to make the mixture into a tablet. Then releasing pressure and heating to raise the temperature to 150 ℃, and heat treating for 60min at 150 ℃ to uniformly distribute PVDF in the carbon-free paper and self-supporting microporous layer. Naturally cooling the mold to room temperature by closing and heating, taking out the obtained sheet sample from the mold, soaking in HCl solution for 2h to remove pore-forming agent in the microporous layer, and forming pores inside the microporous layer, wherein the concentration of the HCl solution is 2mol L -1 . After the acid soaking is finished, soaking the sample in deionized water for 2 hours to remove residual HCl in the microporous layer, and finally drying in a vacuum drying oven for 2 hours at a drying temperature of 100 ℃ to remove the inside of the microporous layerIs named sMPL-2, wherein the carbon powder loading amount is 28mg cm -2 。
Example 3
Weighing 1.0g of carbon fiber, 0.2g of hydrophobic binder PVDF and pore-forming agent K 2 CO 3 2.0g, mechanically mixing for 30min by a pulverizer, and spreading the uniformly mixed mixture in a self-made stainless steel die after fully grinding and mixing to ensure the surface to be smooth. The mold was then placed in a hot press and was first pressed at room temperature under a pressure of 0.5MPa for 30min to make the mixture into a tablet. Then releasing pressure and heating to make its temperature rise to 350 deg.C, heat-treating at 350 deg.C for 60min so as to uniformly distribute PVDF in the carbon-free paper and self-supporting microporous layer. Naturally cooling the mold to room temperature by closing and heating, taking out the obtained sheet sample from the mold, soaking in HCl solution for 2h to remove pore-forming agent in the microporous layer, and forming pores inside the microporous layer, wherein the concentration of the HCl solution is 2mol L -1 . After the acid soaking is finished, soaking the sample in deionized water for 2 hours to remove residual HCl in the microporous layer, finally drying the sample in a vacuum drying oven for 2 hours at the drying temperature of 100 ℃, and removing the deionized water in the microporous layer to obtain a carbon-free paper and self-supporting microporous layer for a proton exchange membrane fuel cell, which is named sMPL-3, wherein the carbon powder loading amount is 28mg cm -2 。
Comparative example 1
The traditional double-layer gas diffusion layer is characterized in that a substrate layer of the traditional double-layer gas diffusion layer is made of PTFE treated carbon paper, a microporous layer is made of carbon powder and PTFE, the specific preparation steps are that carbon powder and PTFE dispersion liquid are uniformly dispersed in isopropanol solvent through ultrasonic and stirring, then uniformly dispersed microporous layer slurry is scraped and coated on the surface of the carbon paper after hydrophobic treatment, and then heat treatment is carried out for 1h at 350 ℃ to remove organic solvent in the diffusion layer, wherein the carbon powder loading of the microporous layer is 1.0mg cm -2 The mass fraction of PTFE was 40wt.%, and the conventional double gas diffusion layer was designated C-GDL. The traditional double-layer gas diffusion layer is used as a comparison sample of the carbon-free paper and the self-supporting microporous layer prepared by the preparation method.
The above examples and comparative examples are characterized and experimental results are as follows:
FIG. 1 (A) is an SEM image of sMPL-2 obtained in example 2. FIG. 1 (B) is an SEM image of the C-GDL obtained in comparative example 1. It can be seen that compared with the gas diffusion layer prepared by the traditional wet method of the comparative example 1, the novel carbon-free paper and the self-supporting microporous layer prepared by the preparation method have relatively flat surfaces and no cracks generated by solvent volatilization.
FIG. 2 shows pore size distribution diagrams of sMPL-1 obtained in example 1, sMPL-2 obtained in example 2, sMPL-3 obtained in example 3, and C-GDL obtained in comparative example 1 of the present invention, and it can be seen that the main difference between sMPL and C-GDL is the difference in pore size ratio. The C-GDL is mainly macroporous, while the vast majority of sMPL is microporous.
FIG. 3 is a graph showing the full cell performance of sMPL-1 obtained in example 1, sMPL-2 obtained in example 2, sMPL-3 obtained in example 3, and C-GDL obtained in comparative example 1 of the present invention under 40% humidification. Comparing the maximum power densities of the cells assembled with the 4 gas diffusion layers, it can be seen that the cell performance of the carbon-free paper, self-supporting microporous layer sMPL is superior to that of the commercial gas diffusion layer (C-GDL).
Claims (8)
1. The preparation method of the proton exchange membrane fuel cell gas diffusion layer is characterized in that the gas diffusion layer is of a single-layer structure and only comprises a carbon-free paper and a self-supporting microporous layer, the microporous layer is prepared by dry molding, and the dry molding comprises the following steps:
1) Mechanically grinding the conductive carbon material, the hydrophobic polymer binder and the pore-forming agent to form a uniformly mixed microporous layer mixture;
2) Spreading the uniformly mixed mixture in a self-made mold, and keeping the surface flat;
3) Putting the die into a hot press, firstly applying pressure at room temperature to enable the raw materials to be in a sheet shape, then releasing pressure, carrying out heat treatment, keeping for a period of time after the temperature reaches a target temperature to enable the binder to be uniformly dispersed, finally closing heating, naturally cooling to room temperature, and demoulding;
4) Soaking the obtained microporous layer material pressed into a sheet shape after demolding in acid to decompose a pore-forming agent, soaking the microporous layer material in deionized water, washing the microporous layer material for multiple times, and finally drying the microporous layer material in a vacuum drying oven to obtain the microporous layer;
the microporous layer has a porous structure with porosity greater than 75%, the porous structure comprises micropores and macropores, wherein the proportion of the micropores is 60% -75%; the micropores are pores with the pore diameter smaller than 1 mu m, and the macropores are pores with the pore diameter larger than 5 mu m.
2. The method according to claim 1, wherein the micropores have a pore size of 100 to 1000. 1000nm, and the macropores have a pore size of 5 to 10 μm.
3. The method according to claim 1, wherein the mass ratio of the conductive carbon material, the hydrophobic polymer binder and the pore-forming agent is 1:0.075-0.2:2.
4. The method according to claim 1, wherein the conductive carbon material is one or a mixture of two or more of conductive carbon powder, carbon fiber, and carbon nanotube; the hydrophobic polymer binder is one or a mixture of more than two of polytetrafluoroethylene, polyvinylidene fluoride and perfluoroethylene propylene copolymer; the pore-forming agent is one or a mixture of more than two of carbonate, bicarbonate and alkali.
5. The method according to claim 1, wherein in the step (1), the mechanical grinding time is 5 to 60 minutes, and in the step (3), the pressure is 0.1 to 1.0MPa, the pressing time is 1 to 60 minutes, the heat treatment temperature is 150 to 350 ℃, and the heat treatment time is 20 to 60 minutes.
6. The method according to claim 1, wherein in the step (4), the acid soaking time is 1-6h, the deionized water soaking time is 1-12h, the drying time is 1-24 hours, and the drying temperature is 60-120 ℃.
7. Use of a gas diffusion layer prepared by the method of claim 1 in a proton exchange membrane fuel cell.
8. The use according to claim 7, wherein the anode and cathode fuels of the pem fuel cell are air and hydrogen, respectively, which are subjected to the same humidification treatment, said humidification treatment being between 40% and 100% relative humidity.
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