CN109346731A - A kind of preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells - Google Patents
A kind of preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells Download PDFInfo
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- CN109346731A CN109346731A CN201811049161.4A CN201811049161A CN109346731A CN 109346731 A CN109346731 A CN 109346731A CN 201811049161 A CN201811049161 A CN 201811049161A CN 109346731 A CN109346731 A CN 109346731A
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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
- H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
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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 discloses a kind of preparation methods of gas diffusion layers for Proton Exchange Membrane Fuel Cells, the gas diffusion layers are made of supporting layer and microporous layers, microporous layers are made by electrostatic spinning, steps are as follows: (1) by conductive black, hydrophober, high molecular polymer, dispersant, through ultrasound or mechanical stirring, uniform spinning solution is formed;(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, porous support layer is covered on cathode receiver sheet and collects spinning fibre;(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5-2h is sintered under conditions of 150-360 DEG C and obtains gas diffusion layers.Because preparing using electrostatic spinning technique the evenly dispersed degree of conductive black and hydrophober in microporous layers can be improved, and then improve the electric conductivity and aqueous vapor mass-transfer performance of microporous layers in microporous layers of the present invention.
Description
Technical field
The invention belongs to field of fuel cell technology, and in particular to a kind of gas expansion for Proton Exchange Membrane Fuel Cells
Dissipate the preparation method of layer.
Background technique
In a fuel cell, between Catalytic Layer and flow field, effect essentially consists in support and urges gas diffusion layers (GDL)
Change layer, collected current, while the transmission for reaction gas and product water provides channel.Drainage performance therein is particularly important, it
It influences the diffusion of reaction gas and the discharge of product water and then influences battery performance.Typical gas diffusion layers are usually by supporting layer
It is constituted with microporous layers, supporting layer is to be made of the porous, electrically conductives dielectric material such as carbon paper or carbon cloth, and microporous layers are usually by carbon dust
It is constituted with the polytetrafluoroethylene (PTFE) of hydrophobicity.United States Patent (USP) U.S.5561000, China Patent Publication No. 98109696,
96198611,1658422 etc. think that fuel electricity can be effectively improved close to the side of Catalytic Layer coating microporous layers in supporting layer
Aqueous vapor mass transfer inside pond, and then improve battery performance.
Chinese patent 200610047931.2,200510047370.1 etc., which is described, is dispersed in low boiling for carbon powder particle
The PTFE emulsion of certain mass score in isopropanol, is then directly added into wherein formation microporous layers slurries again, most by the ethyl alcohol of point
Microporous layers slurry is coated in the processed support layer surface of hydrophobic afterwards, obtains gas diffusion layers after high temperature sintering.Chinese patent
200610068168.1 describing using dry process microporous layers.
Chinese patent 200710019376.7,201310692107.2 is described using aqueous dispersant, hydrocarbon black powder
And the method that the microporous layers slurry of hydrophober composition prepares gas diffusion layers.Although there are many research of this respect, microporous layers
Preparation is still that microporous layers slurry is directly coated in support layer surface, tradition system using traditional preparation processes such as brushing, sprayings
Carbon black and hydrophober PTFE distribution are random and unordered in microporous layers made from standby technique, it is difficult to it is logical to form continuous electron transmission
Road increases Ohmic resistance;The transmission channels of simultaneous reactions gas and liquid water are tortuous, and transmitting distance extends, and increase resistance to mass tranfer.
It may be implemented effectively by improving the preparation process of gas diffusion layers, regulating and controlling the microstructure of gas diffusion layers and surface nature
Water management improves the transmission of inside battery aqueous vapor two-phase, reduces the demand to system additional device.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of preparation side of gas diffusion layer for fuel cell
Method, method is simple, improves the evenly dispersed degree of hydrophober and carbon black in microporous layers, so that the electric conductivity of microporous layers and ventilative
Performance, which has, to be significantly improved.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells, steps are as follows:
(1) conductive black, hydrophober, high molecular polymer, dispersant are formed uniform through ultrasound or mechanical stirring
Spinning solution;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, porous support layer is covered on cathode and is connect
By collecting spinning fibre on plate;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5-2h is sintered under conditions of 200-360 DEG C and is obtained
To gas diffusion layers.
The mass ratio of conductive black and dispersing agent is 1:2-1:15, conductive black and high molecular polymerization in the step (1)
The mass ratio of object is 2:1-10:1, and the mass ratio of conductive black and hydrophober is 5:1-2:1.
Conductive black is acetylene black, Vulcan XC-72, Black pearls, carbon nanotube, graphite in the step (1)
The mixture of one or more of alkene, graphite oxide, expanded graphite, graphene oxide.
The hydrophober is copolymer (FEP), the polyvinylidene fluoride of polytetrafluoroethylene (PTFE), tetrafluoroethene and hexafluoropropene
One of organic silicons hydrophober such as fluoropolymers or polysiloxanes such as alkene (PVDF), polytrifluorochloroethylene (PCTFE) or
Two kinds of mixtures.
The dispersing agent is the mixture of one or both of isopropanol, dehydrated alcohol, deionized water.
The high molecular polymer is polyacrylonitrile, in polyacrylic acid, polyvinylpyrrolidone, polyaniline, polyvinyl alcohol
One or two kinds of mixtures.
Spinning condition in the step (2) are as follows: applied voltage 8-20kV, the spacing of syringe needle to receiver board are 8-20cm, phase
It is 10-30% to humidity, spinning flow velocity is 0.2-0.8ml/h, and the spinning time is 1-5h.
Porous support layer is the processed carbon paper of hydrophobic or carbon fiber woven cloth in the step (2).
Compared with prior art, the invention has the following advantages that
(1) the evenly dispersed degree of hydrophober and carbon black in microporous layers is improved.
(2) electric conductivity of microporous layers and permeability, which have, significantly improves.
(3) preparation method is simple.
Detailed description of the invention
Fig. 1 is gas diffusion layers of the present invention and the cell performance curve figure for being commercialized gas diffusion layers.
Specific embodiment
Combined with specific embodiments below, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
Embodiment 1
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) acetylene black 0.09g, isopropanol 0.35g, deionized water 0.1g, polyacrylic acid 0.03g are separately added into volumetric flask,
Ultrasonic disperse 0.5h after stirring 12h, is added PTFE lotion (mass fraction 60%) 0.06g, stirs evenly and obtain spinning
Liquid;
(2) spinning solution is subjected to electrostatic spinning, control voltage is 10kV, flow rate of liquid 0.3ml/h, and hydrophobic is processed
Toray carbon paper, which is covered on cathode receiver sheet, collects spinning fibre, and needle point and reception plate spacing are 10cm, when by controlling and receiving
Between, obtain the gas diffusion layers of different-thickness;
(3) entire gas diffusion is finally placed on nitrogen charging baking oven to be respectively sintered 30 minutes in 240 DEG C, 350 DEG C.
Monocell, the standby charcoal having the same with traditional law system are assembled using the gas diffusion layers as cathode gas diffusion layer
The monocell that black and hydrophober loading gas diffusion layers assemble carries out performance evaluation.Battery is surveyed with fuel battery test system
Examination, battery operating temperature are 65 DEG C, and hydrogen humidification temperature is 65 DEG C, and oxygen humidification temperature is 65 DEG C, hydrogen, oxygen pressure
0.05MPa(gauge pressure), battery work area is 5cm2.It is shown by battery performance test result (Fig. 1), it is no matter close in low current
Under degree or high current density, gas diffusion layers prepared by the present invention show more preferably battery performance, illustrate system of the present invention
Standby gas diffusion layers have smaller Ohmic resistance (mainly due in gas diffusion layers prepared by the present invention conductive black with
The distribution of hydrophober is more uniform) and more preferably aqueous vapor mass-transfer performance.In addition, using aperture tester (the high modest function material in Nanjing
Expect Science and Technology Ltd., PSDA-20 type) N is carried out to the gas diffusion layers of preparation2Flux test, as the result is shown present invention preparation
Gas diffusion layers infiltration coefficient be 1.05 × 10-12 m2, it is higher than Traditional Method gas diffusion layers (0.94 × 10-12 m2), explanation
Gas diffusion layers prepared by the present invention have the permeability more having.
Embodiment 2
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (acetylene black), hydrophober (PTFE, FEP, PVDF, PCTFE or polysiloxanes), high molecular polymer
The mixing of (polyvinylpyrrolidone), dispersing agent (deionized water) forms uniform spinning solution through ultrasound or mechanical stirring;It is conductive
The mass ratio of carbon black and dispersing agent is 1:2, and the mass ratio of conductive black and high molecular polymer is 2:1, conductive black and hydrophobic
The mass ratio of agent is 5:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon paper or carbon fiber woven cloth) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 8kV, needle
The spacing of head to receiver board is 20cm, and relative humidity 10%, spinning flow velocity is 0.8ml/h, and the spinning time is 1h.
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.2h, 360 are sintered under conditions of 330 DEG C
It is sintered 0.3h under conditions of DEG C and obtains gas diffusion layers.
Embodiment 3
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (carbon nanotube), hydrophober (PTFE), high molecular polymer (polyacrylonitrile, polyacrylic acid), dispersion
Agent (isopropanol) mixing forms uniform spinning solution through ultrasound or mechanical stirring;The mass ratio of conductive black and dispersing agent is 1:
3, the mass ratio of conductive black and high molecular polymer is 3:1, and the mass ratio of conductive black and hydrophober is 4:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon paper or carbon fiber woven cloth) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 20kV,
The spacing of syringe needle to receiver board is 8cm, and relative humidity 30%, spinning flow velocity is 0.2ml/h, and the spinning time is 5h;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5-2h is sintered under conditions of 200-360 DEG C and is obtained
To gas diffusion layers.
Embodiment 4
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (Vulcan XC-72), hydrophober (PTFE, FEP), high molecular polymer (polyacrylonitrile), dispersion
Agent (deionized water) mixing forms uniform spinning solution through ultrasound or mechanical stirring;The mass ratio of conductive black and dispersing agent is
The mass ratio of 1:4, conductive black and high molecular polymer is 4:1, and the mass ratio of conductive black and hydrophober is 3:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon fiber woven cloth) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 10kV, syringe needle arrive
The spacing of receiver board is 10cm, and relative humidity 15%, spinning flow velocity is 0.5ml/h, and the spinning time is 3h;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 1h, 320 DEG C of item are sintered under conditions of 280 DEG C
It is sintered 0.5h under part and obtains gas diffusion layers.
Embodiment 5
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (carbon nanotube, graphene), hydrophober (FEP), high molecular polymer (polyacrylonitrile), dispersing agent
(isopropanol) mixing forms uniform spinning solution through ultrasound or mechanical stirring;The mass ratio of conductive black and dispersing agent is 1:5,
The mass ratio of conductive black and high molecular polymer is 5:1, and the mass ratio of conductive black and hydrophober is 2:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon paper) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 12kV, syringe needle to receiver board
Spacing is 12cm, and relative humidity 20%, spinning flow velocity is 0.3ml/h, and the spinning time is 2h;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5h is sintered under conditions of 250 DEG C, at 300 DEG C
Under conditions of sintering 0.5h obtain gas diffusion layers.
Embodiment 6
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (graphene), hydrophober (PVDF), high molecular polymer (polyvinylpyrrolidone), dispersing agent (nothing
Water-ethanol) it mixes, through ultrasound or mechanical stirring, form uniform spinning solution;The mass ratio of conductive black and dispersing agent is 1:10,
The mass ratio of conductive black and high molecular polymer is 6:1, and the mass ratio of conductive black and hydrophober is 3:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon paper) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 18kV, syringe needle to receiver board
Spacing is 16cm, and relative humidity 20%, spinning flow velocity is 0.6ml/h, and the spinning time is 3.5h;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, it is sintered 0.5 under conditions of 200 DEG C, at 360 DEG C
Under conditions of sintering 1.5h obtain gas diffusion layers.
Embodiment 7
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (expanded graphite), hydrophober (PCTFE), high molecular polymer (polyaniline), dispersing agent (deionization
Water) it mixes, through ultrasound or mechanical stirring, form uniform spinning solution;The mass ratio of conductive black and dispersing agent is 1:12, conductive
The mass ratio of carbon black and high molecular polymer is 8:1, and the mass ratio of conductive black and hydrophober is 4:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon fiber woven cloth) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 15kV, syringe needle arrive
The spacing of receiver board is 15cm, and relative humidity 25%, spinning flow velocity is 0.4ml/h, and the spinning time is 4h;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 1h, 360 DEG C of item are sintered under conditions of 300 DEG C
It is sintered 0.5h under part and obtains gas diffusion layers.
Embodiment 8
The preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells of the present embodiment, steps are as follows:
(1) by conductive black (graphene oxide), hydrophober (polysiloxanes), high molecular polymer (polyvinyl alcohol), dispersing agent
(isopropanol) mixing forms uniform spinning solution through ultrasound or mechanical stirring;The mass ratio of conductive black and dispersing agent is 1:
15, the mass ratio of conductive black and high molecular polymer is 10:1, and the mass ratio of conductive black and hydrophober is 5:1;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, (hydrophobic is processed by porous support layer
Carbon fiber woven cloth) be covered on cathode receiver sheet and collect spinning fibre;Spinning condition are as follows: applied voltage 18kV, syringe needle arrive
The spacing of receiver board is 18cm, and relative humidity 18%, spinning flow velocity is 0.7ml/h, and the spinning time is 2.5h.
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5,350 are sintered under conditions of 330 DEG C
It is sintered 1.5h under conditions of DEG C and obtains gas diffusion layers.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (8)
1. a kind of preparation method of the gas diffusion layers for Proton Exchange Membrane Fuel Cells, it is characterised in that: the gas expands
It dissipates layer to be made of supporting layer and microporous layers, microporous layers are made by electrostatic spinning, and steps are as follows:
(1) conductive black, hydrophober, high molecular polymer, dispersant are formed uniform through ultrasound or mechanical stirring
Spinning solution;
(2) spinning solution made from step (1) is poured into and carries out electrostatic spinning in injection-tube, porous support layer is covered on cathode and is connect
By collecting spinning fibre on plate;
(3) spinning fibre is placed on together with open support and fills N2In baking oven, 0.5-2h is sintered under conditions of 200-360 DEG C and is obtained
To gas diffusion layers.
2. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: the mass ratio of conductive black and dispersing agent is 1:2-1:15 in the step (1), conductive black and high molecular polymer
Mass ratio is 2:1-10:1, and the mass ratio of conductive black and hydrophober is 5:1-2:1.
3. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: in the step (1) conductive black be acetylene black, Vulcan XC-72, Black pearls, carbon nanotube, graphene,
The mixture of one or more of graphite oxide, expanded graphite, graphene oxide.
4. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: the hydrophober is polytetrafluoroethylene (PTFE), the copolymer of tetrafluoroethene and hexafluoropropene, Kynoar, poly- trifluoro chloroethene
One or both of alkene, polysiloxanes mixture.
5. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: the dispersing agent is the mixture of one or both of isopropanol, dehydrated alcohol, deionized water.
6. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: the high molecular polymer is polyacrylonitrile, polyacrylic acid, polyvinylpyrrolidone, polyaniline, one in polyvinyl alcohol
Kind or two kinds of mixture.
7. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
It is: spinning condition in the step (2) are as follows: applied voltage 8-20kV, the spacing of syringe needle to receiver board is 8-20cm, relatively wet
Degree is 10-30%, and spinning flow velocity is 0.2-0.8ml/h, and the spinning time is 1-5h.
8. the preparation method of the gas diffusion layers according to claim 1 for Proton Exchange Membrane Fuel Cells, feature
Be: porous support layer is the processed carbon paper of hydrophobic or carbon fiber woven cloth in the step (2).
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CN114221002A (en) * | 2021-12-06 | 2022-03-22 | 极永新能源科技(上海)有限公司 | High-performance membrane electrode for proton exchange membrane fuel cell and preparation method thereof |
CN114221002B (en) * | 2021-12-06 | 2024-03-15 | 极永新能源科技(上海)有限公司 | High-performance membrane electrode for proton exchange membrane fuel cell and preparation method thereof |
CN114824298A (en) * | 2022-04-12 | 2022-07-29 | 安徽枡水新能源科技有限公司 | Preparation method of microporous layer in gas diffusion layer of hydrogen fuel cell |
CN115020736A (en) * | 2022-04-20 | 2022-09-06 | 中国科学院大连化学物理研究所 | Gas diffusion layer based on fiber arrangement type microporous layer and preparation method and application thereof |
CN115020736B (en) * | 2022-04-20 | 2024-01-26 | 中国科学院大连化学物理研究所 | Gas diffusion layer based on fiber arrangement type microporous layer and preparation method and application thereof |
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