CN113964330A - 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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- 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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- 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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Abstract
The invention relates to a single-layer gas diffusion layer for a fuel cell, 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 a carbon-free paper and a self-supporting microporous layer are prepared by dry-method mould pressing, so that the gas diffusion layer has good hydrophobicity, gas permeability and conductivity, can reduce the resistance of water discharge, and further relieves the cathode flooding. The dry preparation method avoids the defect that cracks are generated on the surface due to solvent volatilization in the wet method, thereby avoiding flooding caused by water gathering at the cracks. The prepared carbon-free paper has controllable thickness and porosity of the self-supporting microporous layer; the preparation process is simple and the conditions are mild. The carbon-free paper and self-supporting microporous layer prepared by the method has 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, belonging to the technical field of fuel cells.
Background
The fuel cell is a power generation device which directly converts chemical energy stored in fuel and oxidant into electric energy in an electrochemical reaction mode, and compared with other conventional power generation modes, the fuel cell is not limited by Carnot cycle, has the advantages of high energy conversion efficiency reaching 60 percent, high reliability and environmental friendliness. Proton Exchange Membrane Fuel Cells (PEMFCs) are one type of fuel cells, and are clean and efficient energy conversion devices 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 discharged from the PEMFC in time, the Membrane Electrode (MEA) is flooded, which prevents hydrogen and oxygen from reaching the active sites of the catalyst to react, thereby causing a sharp decrease in the performance of the PEMFC. When the water content in the battery is low, the membrane is easy to dry, which is not favorable for proton conduction. Therefore, effective water management to maintain water balance in the cell is the key to improving the output performance of the fuel cell, and the gas diffusion layer, which is a core component of the MEA, has important research significance in supporting the functions of water drainage, gas guiding, electrical conduction, catalyst support, and the like in the fuel cell.
Currently commercialized gas diffusion layers consist of two layers, one of which is hydrophobically treated carbon paper or carbon cloth, also known as a substrate layer; the other layer is a microporous layer, typically composed of conductive carbon black and a hydrophobic binder. The carbon paper has complex preparation process, including thousands of high-temperature heat treatment, and high cost, and a large amount of organic solvent is used in the preparation process of the microporous layer, so that the preparation method is not in accordance with the healthy and green development concept on one hand, and the preparation cost is increased on the other hand. The high cost of gas diffusion layers is one of the reasons that has hindered the commercialization of proton exchange membrane fuel cells. Therefore, the preparation of a low-cost, high-performance gas diffusion layer is of great significance to fuel cells.
Disclosure of Invention
Aiming at the defects of the prior art and aiming at reducing the cost and adapting to scale production, the invention aims to provide the carbon-free paper for the fuel cell, the self-supporting microporous layer, the preparation method and the application thereof, wherein the microporous layer can be applied under different humidity conditions.
In one aspect, the invention provides a gas diffusion layer of a proton exchange membrane fuel cell, wherein the gas diffusion layer is of a single-layer structure and only comprises carbon-free paper and a self-supporting microporous layer, the microporous layer has a porous structure, the porosity is greater than 75%, the porous structure comprises micropores and macropores, and the proportion of the micropores is 60% -75%; the micropores are pores with the pore diameter of less than 1 μm, and the macropores are pores with the pore diameter of more than 5 μm.
Further, in the above technical solution, the pore size of the micropores is 100-1000nm, and the pore size of the macropores is 5-10 μm.
In another aspect, the present invention provides a method for preparing the above gas diffusion layer, wherein the microporous layer is prepared by dry molding: after mechanically grinding and uniformly mixing the raw materials, sequentially carrying out hot pressing, cooling, acid treatment, washing and drying to obtain the microporous layer; the raw materials comprise a conductive carbon material, a hydrophobic polymer binder and a pore-forming agent.
Further, in the technical scheme, the mass ratio of the conductive carbon material, the hydrophobic polymer binder and the pore-forming agent is 1:0.075-0.2: 2.
Further, in the above technical solution, the conductive material is one or a mixture of more than one of conductive carbon powder, carbon fiber and carbon nanotube.
Further, in the above technical solution, the hydrophobic polymer binder is one or a mixture of more than one of Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), and perfluoroethylene propylene copolymer (FEP).
Further, in the above technical solution, the pore-forming agent is one or a mixture of more than one of carbonate, bicarbonate and alkali.
Further, in the above technical scheme, the dry-process molding specifically includes the following steps:
1) mechanically grinding a carbon material, a hydrophobic agent and a pore-forming agent in a certain proportion to form a microporous layer mixture which is uniformly mixed;
2) flatly paving the uniformly mixed mixture in a self-made mold, and keeping the surface flat;
3) putting the die into a hot press, applying a certain pressure at room temperature to enable the raw materials to be flaky, then carrying out pressure relief and heat treatment, keeping for a certain time after the temperature reaches the target temperature to enable the binder to be uniformly dispersed, finally closing and heating to enable the binder to be naturally cooled to room temperature, and demoulding;
4) soaking the sheet microporous layer material obtained after demolding in acid to decompose the pore-forming agent, so as to generate pores in the gas diffusion layer, then soaking in deionized water, washing for multiple times, and finally drying 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 30 min.
Further, in the above technical scheme, the pressure is 0.1-1.0MPa, preferably 0.5MPa, and the pressing time is 1-60min, preferably 30 min.
Further, in the above technical scheme, the heat treatment temperature is 150-.
Further, in the above technical scheme, the acid soaking time is 1-6h, preferably 2h, and the deionized water soaking time is 1-12h, preferably 2 h.
Further, in the technical scheme, the drying time is 1-24h, and the drying temperature is 60-120 ℃.
The invention also provides an application of the single-layer gas diffusion layer for the proton exchange membrane fuel cell.
Further, in the above technical scheme, the cathode fuel and the anode fuel of the proton exchange membrane fuel cell are respectively air and hydrogen subjected to the same humidification treatment, and the humidification treatment is 40% -100% RH.
Advantageous effects
1. The carbon-free paper and self-supporting microporous layer provided by the invention has relatively flat surface, no crack, loose and porous structure, porosity of more than 75% which is higher than that of the traditional double-layer gas diffusion layer, and more channels are provided for gas-liquid mass transfer. The pore diameter of the micropores 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, so that the flooding and mass transfer polarization of the battery under large electric density can be reduced.
2. According to the preparation method of the self-supporting microporous layer, the pore-forming agent is added into the raw material of the microporous layer, and is decomposed to generate gas in the acid treatment process, so that the gas is helpful for forming more water channels and gas channels in the microporous layer when escaping; in addition, the pore-forming agent is removed by using an acid treatment mode, so that the method is greener and more thorough than the traditional heat treatment mode.
3. The microporous layer is prepared by a dry method, no organic solvent is introduced in the preparation process, high-temperature treatment is not needed, and the preparation method is healthy, green, cheap and simple and is easy for industrial production; meanwhile, the defect that cracks are generated on the surface due to solvent volatilization in a wet method is avoided, and therefore flooding caused by water gathering 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. The reason is that more than 70 percent of the traditional gas diffusion layer is macropores, the proportion of micropores in the self-supporting microporous layer is more, under the action of strong capillary force of the micropores, the breakthrough pressure of water is increased, the back diffusion of the water to the anode is enhanced, the hydration degree of the Nafion membrane is improved, and therefore the proton conduction resistance is reduced, and the self-supporting microporous layer has better water retention capacity. Under the condition of 40% low humidity, the performance of the cell assembled by the carbon-free paper and the self-supporting microporous layer as the cathode gas diffusion layer is superior to that of the traditional gas diffusion layer. The full cell performance of the sMPL-2 serving as the cathode gas diffusion layer is optimal, and the maximum output power density is improved by 37.4% compared with that of a traditional double-layer gas diffusion layer C-GDL.
Drawings
FIG. 1(A) is an SEM image of a carbon-free paper, a 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 distributions 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.
Figure 3 is a graph comparing the full cell performance of the carbonless paper, self-supporting microporous layer obtained in examples 1-3 of the present invention with the conventional gas diffusion layer of comparative example 1 at 40% humidification.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
Weighing 1.0g of carbon fiber, 0.075g of hydrophobic binder PVDF and pore-forming agent K2CO32.0g, mechanically mixing for 30min by a flour mill, and after fully grinding and mixing, flatly paving the uniformly mixed mixture in a self-made stainless steel mold to ensure that the surface is flat. Then the mould is placed in a hot press, and the mixture is pressed for 30min under the pressure of 0.5MPa at room temperature, so that the mixture is flaky. Then releasing pressure and heating, raising the temperature to 150 ℃, and carrying out heat treatment at 150 ℃ for 20min to ensure that the PVDF is uniformly distributed in the carbon-free paper self-supporting microporous layer. Closing the mold, naturally cooling the mold to room temperature, taking the obtained sheet sample out of the mold, then placing the sheet sample in HCl solution for soaking for 2 hours to remove pore-forming agents in the microporous layer and form pores in the microporous layer, wherein the concentration of the HCl solution is 2mol L-1. After acid soaking is finished, placing the sample in deionized water for soaking for 2h to remove HCl remained in the microporous layer, finally placing the sample in a vacuum drying oven for drying for 2h, wherein the drying temperature is 100 ℃, removing the deionized water in the microporous layer to obtain the carbon-free paper and the self-supporting microporous layer for the proton exchange membrane fuel cell, and the name is sMPL-1, wherein the sample is placed in deionized water for soaking for 2h to remove HCl remained in the microporous layer, and the deionized water in the microporous layer is removed to obtain the carbon-free paper and the self-supporting microporous layer for the proton exchange membrane fuel cell, and the carbon-free paper and the self-supporting microporous layer are named as sMPL-1, whereinThe 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 K2CO32.0g, mechanically mixing for 30min by a flour mill, and after fully grinding and mixing, flatly paving the uniformly mixed mixture in a self-made stainless steel mold to ensure that the surface is flat. Then the mould is placed in a hot press, and the mixture is pressed for 30min under the pressure of 0.5MPa at room temperature, so that the mixture is flaky. Then releasing pressure and heating, raising the temperature to 150 ℃, and carrying out heat treatment at 150 ℃ for 60min to ensure that the PVDF is uniformly distributed in the carbon-free paper self-supporting microporous layer. Closing the mold, naturally cooling the mold to room temperature, taking the obtained sheet sample out of the mold, then placing the sheet sample in HCl solution for soaking for 2 hours to remove pore-forming agents in the microporous layer and form pores in the microporous layer, wherein the concentration of the HCl solution is 2mol L-1. After acid soaking is finished, placing the sample in deionized water for soaking for 2h to remove HCl remained in the microporous layer, finally placing the sample in a vacuum drying oven for drying for 2h, wherein the drying temperature is 100 ℃, removing the deionized water in the microporous layer to obtain the carbon-free paper and the self-supporting microporous layer for the proton exchange membrane fuel cell, and the name is sMPL-2, wherein the carbon powder loading capacity is 28mg cm-2。
Example 3
Weighing 1.0g of carbon fiber, 0.2g of hydrophobic binder PVDF and pore-forming agent K2CO32.0g, mechanically mixing for 30min by a flour mill, and after fully grinding and mixing, flatly paving the uniformly mixed mixture in a self-made stainless steel mold to ensure that the surface is flat. Then the mould is placed in a hot press, and the mixture is pressed for 30min under the pressure of 0.5MPa at room temperature, so that the mixture is flaky. Then releasing pressure and heating, raising the temperature to 350 ℃, and carrying out heat treatment at 350 ℃ for 60min to ensure that the PVDF is uniformly distributed in the carbon-free paper self-supporting microporous layer. Closing the mold, naturally cooling the mold to room temperature, taking the obtained sheet sample out of the mold, then placing the sheet sample in HCl solution for soaking for 2 hours to remove pore-forming agents in the microporous layer and form pores in the microporous layer, wherein the concentration of the HCl solution is 2mol L-1. After the acid soaking is finished, putting the sample in deionizationSoaking in water for 2h to remove residual HCl in the microporous layer, drying in a vacuum drying oven at 100 deg.C for 2h to remove deionized water in the microporous layer to obtain carbon-free paper and self-supporting microporous layer named sMPL-3 for proton exchange membrane fuel cell, wherein the carbon powder loading is 28mg cm-2。
Comparative example 1
The preparation method comprises the specific steps of dispersing carbon powder and PTFE dispersion liquid in isopropanol solvent by ultrasonic and stirring uniformly, then coating uniformly dispersed microporous layer slurry on the surface of carbon paper subjected to hydrophobic treatment by blade, and then carrying out heat treatment at 350 ℃ for 1h to remove the organic solvent in the diffusion layer, wherein the carbon powder loading amount of the microporous layer is 1.0mg cm-2The mass fraction of PTFE is 40 wt.%, and the conventional two-layer gas diffusion layer is named 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 were characterized and the results were as follows:
FIG. 1(A) is an SEM image of sMPL-2 obtained in example 2. FIG. 1(B) is an SEM photograph of C-GDL obtained in comparative example 1. It can be seen that, compared with the gas diffusion layer prepared by the conventional wet method of comparative example 1, the novel carbon-free paper prepared by the preparation method of the present application has the advantages of relatively flat self-supporting microporous layer surface and no cracks generated by solvent volatilization.
FIG. 2 is a graph showing the pore size distribution of sMPL-1 obtained in example 1 of the present invention, sMPL-2 obtained in example 2, sMPL-3 obtained in example 3, and C-GDL obtained in comparative example 1, and it can be seen that the difference between sMPL and C-GDL is mainly the difference in the ratio of pore sizes. C-GDL is mainly macroporous, while sMPL is mostly microporous.
FIG. 3 is a graph comparing the full cell performance of sMPL-1 obtained in example 1 of the present invention, sMPL-2 obtained in example 2, sMPL-3 obtained in example 3, and C-GDL obtained in comparative example 1 under 40% humidification. Comparing the maximum power densities of the cells assembled from the 4 gas diffusion layers, it can be seen that the single cell performance of the carbon-free paper, self-supporting microporous layer slpl, is superior to that of the commercial gas diffusion layer (C-GDL).
Claims (10)
1. The gas diffusion layer of the proton exchange membrane fuel cell is characterized by being of a single-layer structure and only comprising carbon-free paper and a self-supporting microporous layer, wherein the microporous layer has a porous structure, the porosity of the microporous layer is greater than 75%, the porous structure comprises micropores and macropores, and the proportion of the micropores is 60% -75%; the micropores are pores with the pore diameter of less than 1 μm, and the macropores are pores with the pore diameter of more than 5 μm.
2. The gas diffusion layer according to claim 1, wherein the pore size of the micropores is 100-1000nm and the pore size of the macropores is 5-10 μm.
3. A method of preparing a gas diffusion layer according to claim 1, wherein the microporous layer is prepared by dry molding: after mechanically grinding and uniformly mixing the raw materials, sequentially carrying out hot pressing, cooling, acid treatment, washing and drying to obtain the microporous layer; the raw materials comprise a conductive carbon material, a hydrophobic polymer binder and a pore-forming agent.
4. The preparation method according to claim 3, 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.
5. The preparation method according to claim 3, wherein the conductive material is one or a mixture of more than one of conductive carbon powder, carbon fiber and carbon nanotube; the hydrophobic polymer binder is one or a mixture of more than one of polytetrafluoroethylene, polyvinylidene fluoride and perfluoroethylene propylene copolymer; the pore-forming agent is one or a mixture of more than one of carbonate, bicarbonate and alkali.
6. The method for preparing according to claim 3, wherein the dry-process molding specifically comprises the steps of:
1) mechanically grinding a carbon material, a hydrophobic agent and a pore-forming agent to form a microporous layer mixture which is uniformly mixed;
2) flatly paving 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 flaky, then decompressing and carrying out heat treatment, keeping for a period of time after the temperature reaches the target temperature to enable the binder to be uniformly dispersed, finally closing and heating, naturally cooling to room temperature, and demoulding;
4) and soaking the sheet-shaped microporous layer material obtained after demolding in acid to decompose the pore-forming agent, then soaking in deionized water, washing for multiple times, and finally drying in a vacuum drying oven to obtain the microporous layer.
7. The method as claimed in claim 6, wherein the mechanical polishing time is 5-60min in step (1), and the pressure is 0.1-1.0MPa, the pressure is applied for 1-60min, the heat treatment temperature is 150-350 ℃ and the heat treatment time is 20-60min in step (3).
8. The preparation method according to claim 6, wherein in the step (4), the acid soaking time is 1-6h, the deionized water soaking time is 1-12h, the drying time is 1-24h, and the drying temperature is 60-120 ℃.
9. Use of a gas diffusion layer according to claim 1 in a proton exchange membrane fuel cell.
10. The use according to claim 9, wherein the cathode and anode fuels of the PEM fuel cell are air and hydrogen respectively subjected to the same humidification treatment, and the humidification treatment is 40% -100% relative humidity.
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CN114335564A (en) * | 2021-12-30 | 2022-04-12 | 国网安徽省电力有限公司电力科学研究院 | Single-layer gas diffusion layer for proton exchange membrane fuel cell, preparation method and application |
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