CN107123822B - A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers - Google Patents
A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers Download PDFInfo
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- CN107123822B CN107123822B CN201710318918.4A CN201710318918A CN107123822B CN 107123822 B CN107123822 B CN 107123822B CN 201710318918 A CN201710318918 A CN 201710318918A CN 107123822 B CN107123822 B CN 107123822B
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1007—Fuel cells with solid electrolytes with both reactants being gaseous or vaporised
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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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
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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
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- Sustainable Energy (AREA)
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Abstract
The present invention relates to Proton Exchange Membrane Fuel Cells field, especially a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers.Gas diffusion layers are made of supporting layer and microporous layers, and the microporous layers are made of hydrophilic carbon dust layer and water-repellent layer.Gas diffusion layers the preparation method is as follows: conductive carbon powder is dispersed in low-boiling alcohols solvent, form uniform silica aerogel layer slurry；Using the hydrophobic agent emulsion of low concentration as the raw material of water-repellent layer.The raw material of carbon dust layer slurry and water-repellent layer is repeatedly alternately uniformly coated in the surface of the porous, electrically conductive supporting layer handled through hydrophobic respectively, finally forms gas diffusion layers through Overheating Treatment.
Description
Technical field
The present invention relates to Proton Exchange Membrane Fuel Cells field, especially a kind of used in proton exchange membrane fuel cell gas expands
Dissipate the preparation method of layer.
Background technique
Proton Exchange Membrane Fuel Cells (PEMFC) core component membrane electrode assembly (MEA) by gas diffusion layers, Catalytic Layer and
Proton exchange membrane composition.When battery operation, if vapor local partial pressure is higher than local saturation partial pressure, it just will appear liquid water.
Liquid water excessive aggregation in porous electrode seriously can hinder reactant to transmit, and influence the performance of battery.Typical gas diffusion
Layer is usually made of supporting layer and microporous layers, and supporting layer is made of the porous, electrically conductives dielectric material such as carbon paper or carbon cloth, and micropore
Layer is usually to be made of the polytetrafluoroethylene (PTFE) (PTFE) of carbon dust and hydrophobicity.PTFE is both hydrophober in microporous layers and bonds
Agent, good distribution can effectively improve the aqueous vapor mass transfer of fuel battery inside, and then improve battery performance, so PTFE
It is uniformly distributed most important.United States Patent (USP) U.S.5561000, Chinese patent 98109696,96198611,1658422,
200610047931.2,200510047370.1 etc. describe carbon powder particle being dispersed in low-boiling ethyl alcohol, isopropanol
In, the PTFE emulsion of certain mass score is then directly added into wherein formation microporous layers slurries again, finally by microporous layers slurry
Coated in the processed support layer surface of hydrophobic, gas diffusion layers are obtained after high temperature sintering.However the surface of PTFE can be very low, leads
Cause its stably dispersing performance in nonaqueous solvents poor.Therefore easy as the PTFE in the microporous layers slurries that solvent obtains using alcohols
In cohesion, dispersion is uneven.Moreover, in the heat treatment process of microporous layers, PTFE particle agglomerated together be easily formed compared with
The insulating regions of large area package, reduce the electric conductivity and permeability of diffusion layer part.But this problem does not cause to grind
The extensive concern for the person of studying carefully.In order to solve this problem, Chinese patent 200610068168.1 is described is used for using dry process
The gas diffusion layers of Proton Exchange Membrane Fuel Cells.Chinese patent 201310692107.2 is described by deionized water, carbon black powder
The method of the slurry preparation microporous layers at end, dispersing agent and hydrophober composition, uses the deionized water of addition dispersing agent as microporous layers
The dispersing agent of slurry solves the problems, such as that hydrophober agglomerates in alcohols solvent.
Summary of the invention
In view of aqueous solution is more advantageous to the fine dispersion of PTFE emulsion, and alcohols solvent is more advantageous to the dispersion of carbon dust,
The method that the present invention prepares gas diffusion layers using substep, i.e., be divided into hydrophilic layer and water-repellent layer for microporous layers, coat layer by layer, solves
The evenly dispersed problem of PTFE and carbon dust, have obtained the evenly dispersed microporous layers slurry of each component.
Specifically, its step are as follows for preparation method provided by the invention:
1) conductive carbon powder is added in low-boiling alcohols solvent, ultrasonic disperse 10-40 minutes, forms uniform carbon dust layer
Slurry；
2) deionized water or distilled water are added into the hydrophobic agent emulsion of high concentration, mechanical stirring 1-10 minutes, is formed equal
The water-repellent layer lotion of even low concentration；
3) a certain amount of above-mentioned carbon dust layer slurry is uniformly coated on to the table of the porous, electrically conductive supporting layer handled through hydrophobic
Face, drying are simultaneously weighed；Then a certain amount of above-mentioned water-repellent layer lotion is coated on its surface, drying is simultaneously weighed；
4) repeat it is above-mentioned 3) in step 2-5 times, until the loading of carbon dust powder reaches 0.4mg/cm2-1.5mg/
cm2, the loading of hydrophober reaches the 10%-60% of carbon dust quality.
5) the above-mentioned support with microporous layers is placed in nitrogen charging baking oven, is sintered 30-120 at a temperature of 150-360 DEG C
Minute obtains gas diffusion layers.
The preparation method, wherein conductive carbon powder is acetylene black, Vulcan XC-72, Black pearls, carbon nanometer
The one such or several mixture of pipe, graphene powder.
The preparation method, wherein the lotion of hydrophober is polytetrafluoroethylene (PTFE) (PTFE) lotion, tetrafluoroethene and hexafluoro
The fluoropolymers such as the copolymer (FEP) of propylene, Kynoar (PVDF) lotion, polytrifluorochloroethylene (PCTFE) suspension
One or both of mixture.
The preparation method, wherein the coating method of microporous layers is brushing, blade coating, spraying and silk-screen printing.
Detailed description of the invention
Fig. 1: cell performance curve figure
Specific embodiment
Embodiment 1
According to the method described in the present invention, 5ml ethyl alcohol is measured, the acetylene black of 62.5mg, ultrasonic disperse 20 are added into it
Minute forms uniform carbon dust layer slurry.The PTFE emulsion that mass fraction is 60% is diluted with deionized water, obtains quality point
The hydrophobic agent emulsion that number is 1%.Successively successively by carbon dust layer slurry and hydrophober lotion applicator in the processed Toray carbon of hydrophobic
Paper (loading of PTFE is the 1% of carbon paper quality) side surface, it is dry simultaneously to weigh, until the loading of carbon dust reaches 0.5mg/
cm2, the loading of PTFE reaches the 35% of carbon dust quality.Finally by entire gas diffusion be placed on nitrogen charging baking oven 240 DEG C,
350 DEG C are respectively sintered 30 minutes.
Comparative example 1
Microporous layers slurry is prepared by dispersing agent of ethyl alcohol.The acetylene black of 62.5mg, 5ml EtOH Sonicate are dispersed 40 points first
It is bell at uniform mixed liquor, then into it add 437.5mg PTFE emulsion (5wt%), be uniformly mixing to obtain microporous layers
Slurry.Above-mentioned microporous layers slurry is uniformly coated to the processed Toray carbon paper of hydrophobic, and (loading of PTFE is carbon paper quality
1%) a side surface, drying are simultaneously weighed, and then repeat the step until the loading of carbon dust reaches 0.5mg/cm2；.Most postposition
It is respectively sintered 30 minutes in nitrogen charging baking oven in 240 DEG C, 350 DEG C.
Respectively using gas diffusion layers prepared by embodiment 1 and comparative example 1 as cathode gas diffusion layer, commercialization gas
Diffusion layer (including microporous layers) is used as anode gas diffusion layer, and the CCM assembled battery with 212 film two sides spraying catalyst is surveyed
Examination.Battery is tested with fuel battery test system, and battery testing condition is that battery operating temperature is 65 DEG C, hydrogen humidification temperature
It is 65 DEG C, oxygen humidification temperature is 65 DEG C, hydrogen, oxygen pressure 0.05MPa (gauge pressure), and battery work area is 5cm2.Battery
Performance curve is as shown in Figure 1.Meanwhile online ohmage spectrum display, ohm electricity of 2500mA cm-2 example 1 group packed battery
Resistance and mass transfer resistance are respectively less than the cell resistance that comparative example 1 is assembled.
Comparative example 2
According to the method described in the present invention, the polyvinylpyrrolidone (PVP) for weighing 60mg is added in 70g deionized water
It is made into uniform aqueous solution, measures aqueous solution 5ml, the acetylene black of 62.5mg, magnetic agitation 6h are added into it, blender turns
Speed is 1600 revs/min, forms uniform suspension within ultrasonic disperse 30 minutes later, states in suspension add then up
The PTFE emulsion (5wt%) of 437.5mg, is uniformly mixing to obtain microporous layers slurry.Above-mentioned microporous layers slurry is uniformly coated to
Toray carbon paper side, drying are simultaneously weighed, and then repeat the step until the loading of carbon dust reaches 0.5mg/cm2；Then in carbon
Paper uncoated microporous layer side sprays the PTFE emulsion (0.25wt%) of low concentration, so that the loading of PTFE reaches carbon paper quality
1%.Entire diffusion is finally placed on nitrogen charging baking oven to be respectively sintered 30 minutes in 240 DEG C, 350 DEG C.
Using aperture tester (Nanjing Gao Qian functional material Science and Technology Ltd., PSDA-20 type) to embodiment 1 compared with
Gas diffusion layers prepared by example 1,2 carry out N2Flux test, and then calculate the infiltration coefficient of each gas diffusion layers.As a result it shows
Show, the infiltration coefficient of gas diffusion layers prepared by embodiment 1 is 1.096 × 10-12m2, gas prepared by Comparative Examples 1 and 2 expands
The infiltration coefficient for dissipating layer is respectively 0.876 × 10-12m2、0.932×10-12m2.By the measurement of infiltration coefficient can be found that according to
The preparation-obtained gas diffusion layers of the claims have good gas permeability.
Using drop imaging analysis instrument (Drop Shape Analyzer 100) to the microporous layers of embodiment 1 and comparative example 1
Surface measures, and the distribution of microporous layers surface contact angle prepared by discovery embodiment 1 is more uniform.
Claims (7)
1. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers, it is characterised in that: process is as follows,
1) conductive carbon powder is added in low-boiling alcohols solvent, ultrasonic disperse 10-40 minutes, forms uniform carbon dust layer slurry
Material；
2) deionized water or distilled water are added into the hydrophobic agent emulsion of high concentration, mechanical stirring 1-10 minutes, is formed uniform
The water-repellent layer lotion of low concentration；
3) a certain amount of above-mentioned carbon dust layer slurry is uniformly coated on to the surface of the porous, electrically conductive supporting layer handled through hydrophobic, is done
It is dry and weigh；Then a certain amount of above-mentioned water-repellent layer lotion is coated on its surface, drying is simultaneously weighed；
4) repeat it is above-mentioned 3) in step 2-5 time, up to the loading of carbon dust powder reaches 0.4mg/cm2-1. 5mg/cm2, hate
The loading of aqua reaches the 10%-60% of carbon dust quality；
5) support for obtaining step 4) is placed in nitrogen charging baking oven, is burnt 30-120 minutes at a temperature of 150-360 DEG C and is obtained gas
Body diffused layer.
2. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, feature exists
In the mixture of one or both of the optional ethyl alcohol of alcohols solvent, isopropanol.
3. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in accordance with the claim 1, feature
It is, conductive carbon powder is that acetylene black, Vulcan XC-72, Black pearls, carbon nanotube, graphene powder are one such
Or several mixture.
4. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in accordance with the claim 1, feature
It is, the quality of conductive carbon powder and the volume of alcohols dispersing agent meet: the quality of conductive black is added in the dispersing agent of every 1mL
For 5-15mg.
5. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in accordance with the claim 1, feature
Be, the lotion of hydrophober be polytetrafluoroethylene (PTFE) lotion, tetrafluoroethene and hexafluoropropene copolymer (FEP) lotion,
The mixing of one or both of fluoropolymers such as Kynoar (PVDF) lotion, polytrifluorochloroethylene (PCTFE) suspension
Object.
6. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in accordance with the claim 1, feature
It is, the supporting layer of microporous layers is carbon fiber paper or woven cloth.
7. a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in accordance with the claim 1, feature
It is, the coating method of microporous layers is brushing, blade coating, spraying or silk-screen printing.
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