CN107123822A - 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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- CN107123822A CN107123822A CN201710318918.4A CN201710318918A CN107123822A CN 107123822 A CN107123822 A CN 107123822A CN 201710318918 A CN201710318918 A CN 201710318918A CN 107123822 A CN107123822 A CN 107123822A
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- gas diffusion
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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
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 up of supporting layer and microporous layers, and the microporous layers are made up of hydrophilic carbon dust layer and water-repellent layer.The preparation method of gas diffusion layers is as follows：Conductive carbon powder is dispersed in lower boiling alcohols solvent, uniform silica aerogel layer slurry is formed；Using the hydrophobic agent emulsion of low concentration as water-repellent layer raw material.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, heat treatment is eventually passed and forms gas diffusion layers.
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 technology
Proton Exchange Membrane Fuel Cells (PEMFC) core component membrane electrode assembly (MEA) by gas diffusion layers, Catalytic Layer and
PEM is constituted.During battery operation, if vapor local partial pressure is higher than local saturation partial pressure, aqueous water just occurs.
Aqueous water excessive aggregation in porous electrode seriously can hinder reactant to transmit, and influence the performance of battery.Typical gas diffusion
Layer is generally made up of supporting layer and microporous layers, and supporting layer is made up of the porous, electrically conductive dielectric material such as carbon paper or carbon cloth, and micropore
Layer is usually to be made up of carbon dust and the polytetrafluoroethylene (PTFE) of hydrophobicity (PTFE).PTFE is both hydrophober in microporous layers and cohesive
Agent, its is well distributed can effectively to improve the aqueous vapor mass transfer of fuel battery inside, and then improves 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 lower boiling ethanol, isopropanol
In, the PTFE emulsion of certain mass fraction is then directly added into wherein formation microporous layers slurries again, finally by microporous layers slurry
Gas diffusion layers are obtained after being coated in the treated support layer surface of hydrophobic, high temperature sintering.But PTFE surface can be very low, leads
Cause its stably dispersing performance in nonaqueous solvents poor.Therefore the PTFE in the microporous layers slurries obtained using alcohols as solvent is easy
In cohesion, disperse uneven.Moreover, in the heat treatment process of microporous layers, PTFE particles agglomerated together be easily formed compared with
The insulating regions of large area parcel, reduce diffusion layer local electric conductivity and permeability.But this problem, which does not cause, grinds
The extensive concern for the person of studying carefully.In order to solve this problem, Chinese patent 200610068168.1 is described to be 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 powder
The method that the slurry at end, dispersant and hydrophober composition prepares microporous layers, microporous layers are used as with the deionized water of addition dispersant
The dispersant of slurry, solves the problem of hydrophober condenses in alcohols solvent.
The content of the invention
The fine dispersion of PTFE emulsion is more beneficial in view of the aqueous solution, and alcohols solvent is more beneficial for the scattered 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 by microporous layers, coat layer by layer, solves
PTFE and carbon dust dispersed problem, have obtained the dispersed microporous layers slurry of each component.
Specifically, preparation method its step that the present invention is provided is as follows：
1) conductive carbon powder is added in lower 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 agitation 1-10 minutes forms equal
The water-repellent layer emulsion 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, dries and weighs；Then a certain amount of above-mentioned water-repellent layer emulsion is coated on its surface, dries and weigh；
4) step 2-5 time during repetition is above-mentioned 3), 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, 30-120 is sintered at a temperature of 150-360 DEG C
Minute obtains gas diffusion layers.
Described preparation method, wherein conductive carbon powder are acetylene black, Vulcan XC-72, Black pearls, carbon nanometer
Pipe, graphene powder one or more of mixture therein.
The emulsion of described preparation method, wherein hydrophober is polytetrafluoroethylene (PTFE) (PTFE) emulsion, tetrafluoroethene and hexafluoro
The fluoropolymers such as copolymer (FEP), Kynoar (PVDF) emulsion, polytrifluorochloroethylene (PCTFE) suspension of propylene
One or both of mixture.
The coating method of described preparation method, wherein microporous layers is brushing, scratches, sprayed and silk-screen printing.
Brief description of the drawings
Fig. 1：Cell performance curve figure
Embodiment
Embodiment 1
According to the method described in the present invention, 5ml ethanol is measured, to its interior acetylene black for adding 62.5mg, ultrasonic disperse 20
Minute forms uniform carbon dust layer slurry.Mass fraction is diluted for 60% PTFE emulsion with deionized water, quality point is obtained
Number is 1% hydrophobic agent emulsion.The Toray carbon for successively successively treating carbon dust layer slurry and hydrophober lotion applicator in hydrophobic
Paper (PTFE loading is the 1% of carbon paper quality) side surface, dries and weighs, until the loading of carbon dust reaches 0.5mg/
cm2, PTFE loading reaches the 35% of carbon dust quality.Finally by whole gas diffusion be placed on nitrogen charging baking oven 240 DEG C,
350 DEG C respectively sinter 30 minutes.
Comparative example 1
Microporous layers slurry is prepared by dispersant of ethanol.It is first that 62.5mg acetylene black, 5ml EtOH Sonicates is scattered 40 points
It is bell into uniform mixed liquor, then into it addition 437.5mg PTFE emulsion (5wt%), be uniformly mixing to obtain microporous layers
Slurry.Above-mentioned microporous layers slurry is uniformly coated into the treated Toray carbon papers of hydrophobic, and (PTFE loading is carbon paper quality
1%) a side surface, dries and weighs, then repeat the step until the loading of carbon dust reaches 0.5mg/cm2；.It is most rearmounted
Respectively sintered 30 minutes in 240 DEG C, 350 DEG C in nitrogen charging baking oven.
It regard the gas diffusion layers prepared by embodiment 1 and comparative example 1 as cathode gas diffusion layer, commercialization gas respectively
Diffusion layer (including microporous layers) is as anode gas diffusion layer, and the CCM assembled batteries for spraying catalyst with 212 film two sides are 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
For 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 the assembled battery of 2500mA cm-2 embodiments 1
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 waters
The uniform aqueous solution is made into, aqueous solution 5ml is measured, to its interior acetylene black for adding 62.5mg, magnetic agitation 6h, agitator turns
Speed is 1600 revs/min, and ultrasonic disperse forms uniform suspension in 30 minutes afterwards, states in suspension and adds then up
437.5mg PTFE emulsion (5wt%), is uniformly mixing to obtain microporous layers slurry.Above-mentioned microporous layers slurry is uniformly coated to
Toray carbon papers side, dries and weighs, 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 PTFE loading reaches carbon paper quality
1%.Whole diffusion finally is placed on into nitrogen charging baking oven respectively to sinter 30 minutes in 240 DEG C, 350 DEG C.
Using aperture tester (Nanjing Gao Qian functional materials Science and Technology Ltd., PSDA-20 types) to embodiment 1 with being compared
Gas diffusion layers prepared by example 1,2 carry out N2Flux is tested, and then calculates the infiltration coefficient of each gas diffusion layers.As a result show
Show, the infiltration coefficient of the gas diffusion layers prepared by embodiment 1 is 1.096 × 10-12m2, the gas expansion prepared by comparative example 1,2
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 embodiment 1 and the microporous layers of comparative example 1
Surface is measured, it is found that the distribution of microporous layers surface contact angle prepared by 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 lower 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 agitation 1-10 minutes forms uniform
The water-repellent layer emulsion 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, done
It is dry and weigh；Then a certain amount of above-mentioned water-repellent layer emulsion is coated on its surface, dries and weigh；
4) step 2-5 time during repetition is above-mentioned 3), until 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) the above-mentioned support with microporous layers is placed in nitrogen charging baking oven, sintered 30-120 minutes at a temperature of 150-360 DEG C
Obtain gas diffusion layers.
2. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature exists
In the mixture of one or both of the optional ethanol of alcohols solvent, isopropanol.
3. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature
It is, conductive carbon powder is acetylene black, Vulcan XC-72, Black pearls, CNT, graphene powder one kind therein
Or several mixtures.
4. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature
It is, the quality of conductive carbon powder is met with the volume of alcohols dispersant：The quality of addition conductive black is in dispersant per 1ml
5-15mg。
5. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature
It is, the emulsion of hydrophober is polytetrafluoroethylene (PTFE) (PTFE) emulsion, the copolymer (FEP) of tetrafluoroethene and hexafluoropropene, gathers inclined
One or both of the fluoropolymers such as PVF (PVDF) emulsion, polytrifluorochloroethylene (PCTFE) suspension mixture.
6. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature
It is, the supporting layer of microporous layers is carbon fiber paper or woven cloth.
7. according to a kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers described in claim 1, its feature
It is, the coating method of microporous layers is brushing, scratches, sprayed and silk-screen printing.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842162A (en) * | 2018-06-15 | 2018-11-20 | 重庆大学 | For electrochemical reduction CO2SnO2Nanometer sheet gas-diffusion electrode and method |
| CN109585863A (en) * | 2018-12-14 | 2019-04-05 | 广东工业大学 | A kind of preparation method of gas diffusion layer of proton exchange membrane fuel cell |
| CN110085878A (en) * | 2019-05-09 | 2019-08-02 | 武汉雄韬氢雄燃料电池科技有限公司 | A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers |
| CN110289438A (en) * | 2019-07-01 | 2019-09-27 | 江苏乾景新能源产业技术研究院有限公司 | A kind of preparation method of fuel cell self-humidifying membrane electrode |
| CN110311142A (en) * | 2019-06-20 | 2019-10-08 | 一汽解放汽车有限公司 | A kind of fuel battery gas diffusion layer and preparation method thereof |
| CN110380061A (en) * | 2019-07-03 | 2019-10-25 | 上海交通大学 | A kind of matched fuel battery diffusion layer of full working scope and preparation method thereof |
| CN110416557A (en) * | 2019-07-12 | 2019-11-05 | 成都新柯力化工科技有限公司 | A kind of method that roll-to-roll printing low cost prepares fuel battery gas diffusion layer |
| CN110890555A (en) * | 2019-12-03 | 2020-03-17 | 清华大学 | Preparation method of gradient hydrophilic or hydrophobic diffusion layer |
| CN111384422A (en) * | 2018-12-28 | 2020-07-07 | 博西华电器（江苏）有限公司 | Redox device, gas conditioning system and refrigeration appliance |
| CN112909278A (en) * | 2021-01-21 | 2021-06-04 | 上海神力科技有限公司 | Preparation method of gas diffusion layer for fuel cell |
| CN114068974A (en) * | 2021-10-25 | 2022-02-18 | 上海远瞩新能源科技有限公司 | Fuel cell gas diffusion layer with functional structure and preparation method thereof |
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| US20220181645A1 (en) * | 2020-12-09 | 2022-06-09 | Hyzon Motors Inc. | Catalyst, electrode, and method of preparing the same for pem fuel cells |
| CN114824311A (en) * | 2022-03-31 | 2022-07-29 | 东风汽车集团股份有限公司 | Preparation method of gas diffusion layer |
| CN114864966A (en) * | 2022-05-31 | 2022-08-05 | 华工丽颜(广东)新材料科技有限公司 | Preparation method of gas diffusion layer of proton exchange membrane fuel cell and product thereof |
| CN114976050A (en) * | 2022-05-13 | 2022-08-30 | 上海碳际实业集团有限公司 | Gas diffusion layer for fuel cell and preparation process thereof |
| CN115513477A (en) * | 2022-11-11 | 2022-12-23 | 国家电投集团氢能科技发展有限公司 | Microporous layer slurry of proton exchange membrane fuel cell, gas diffusion layer and preparation method of microporous layer slurry |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108842162A (en) * | 2018-06-15 | 2018-11-20 | 重庆大学 | For electrochemical reduction CO2SnO2Nanometer sheet gas-diffusion electrode and method |
| CN109585863A (en) * | 2018-12-14 | 2019-04-05 | 广东工业大学 | A kind of preparation method of gas diffusion layer of proton exchange membrane fuel cell |
| CN111384422A (en) * | 2018-12-28 | 2020-07-07 | 博西华电器（江苏）有限公司 | Redox device, gas conditioning system and refrigeration appliance |
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| CN110085878A (en) * | 2019-05-09 | 2019-08-02 | 武汉雄韬氢雄燃料电池科技有限公司 | A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers |
| CN110311142A (en) * | 2019-06-20 | 2019-10-08 | 一汽解放汽车有限公司 | A kind of fuel battery gas diffusion layer and preparation method thereof |
| CN110289438A (en) * | 2019-07-01 | 2019-09-27 | 江苏乾景新能源产业技术研究院有限公司 | A kind of preparation method of fuel cell self-humidifying membrane electrode |
| CN110380061A (en) * | 2019-07-03 | 2019-10-25 | 上海交通大学 | A kind of matched fuel battery diffusion layer of full working scope and preparation method thereof |
| CN110416557A (en) * | 2019-07-12 | 2019-11-05 | 成都新柯力化工科技有限公司 | A kind of method that roll-to-roll printing low cost prepares fuel battery gas diffusion layer |
| CN110890555A (en) * | 2019-12-03 | 2020-03-17 | 清华大学 | Preparation method of gradient hydrophilic or hydrophobic diffusion layer |
| US20220181645A1 (en) * | 2020-12-09 | 2022-06-09 | Hyzon Motors Inc. | Catalyst, electrode, and method of preparing the same for pem fuel cells |
| CN112909278A (en) * | 2021-01-21 | 2021-06-04 | 上海神力科技有限公司 | Preparation method of gas diffusion layer for fuel cell |
| CN114068974A (en) * | 2021-10-25 | 2022-02-18 | 上海远瞩新能源科技有限公司 | Fuel cell gas diffusion layer with functional structure and preparation method thereof |
| CN114293211A (en) * | 2021-12-30 | 2022-04-08 | 深圳康诚博信科技有限公司 | Ozone generator with quick-dismounting structure and preparation method of cathode prefabricated film of ozone generator |
| CN114293211B (en) * | 2021-12-30 | 2023-09-05 | 深圳康诚博信科技有限公司 | Ozone generator with rapid disassembly and assembly structure and preparation method of cathode prefabricated film of ozone generator |
| CN114824311A (en) * | 2022-03-31 | 2022-07-29 | 东风汽车集团股份有限公司 | Preparation method of gas diffusion layer |
| CN114976050A (en) * | 2022-05-13 | 2022-08-30 | 上海碳际实业集团有限公司 | Gas diffusion layer for fuel cell and preparation process thereof |
| CN114864966A (en) * | 2022-05-31 | 2022-08-05 | 华工丽颜(广东)新材料科技有限公司 | Preparation method of gas diffusion layer of proton exchange membrane fuel cell and product thereof |
| CN115513477A (en) * | 2022-11-11 | 2022-12-23 | 国家电投集团氢能科技发展有限公司 | Microporous layer slurry of proton exchange membrane fuel cell, gas diffusion layer and preparation method of microporous layer slurry |
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