CN110289438A - A kind of preparation method of fuel cell self-humidifying membrane electrode - Google Patents
A kind of preparation method of fuel cell self-humidifying membrane electrode Download PDFInfo
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- CN110289438A CN110289438A CN201910585701.9A CN201910585701A CN110289438A CN 110289438 A CN110289438 A CN 110289438A CN 201910585701 A CN201910585701 A CN 201910585701A CN 110289438 A CN110289438 A CN 110289438A
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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
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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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
- H01M2008/1095—Fuel cells with polymeric electrolytes
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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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Abstract
The present invention relates to a kind of preparation methods of fuel cell self-humidifying membrane electrode.The preparation process of membrane electrode includes the pretreatment of proton exchange membrane；The hydrophilic Catalytic Layer preparation of anode；Cathode catalysis layer preparation；It is bonded respectively with gas diffusion layers again and self-humidifying membrane electrode is made；Its Anodic water wetted material chitin can play the role of being retained well, and the moisture absorption that generation is reacted in cathode catalysis layer is kept, proton exchange membrane is allowed to be sufficiently humidified so as to, and keep its good proton conductivity；The self-humidifying membrane electrode can have excellent performance under low humidity conditions, and reduce influence of the addition hydroaropic substance to electrode conductivuty and resistance, also simplify the preparation process of membrane electrode.
Description
Technical field
The present invention relates to field of fuel cell technology, and in particular to a kind of preparation side of fuel cell self-humidifying membrane electrode
Method.
Background technique
In today that global fossil energy growing tension and environmental problem are increasingly serious, Hydrogen Energy and fuel cell technology are ground
Study carefully the great attention received in global range.China " National Program for Medium-to Long-term Scientific and Technological Development (2006-
2020) " many places are placed on fuel cell in important developing direction, and the preparation of fuel cell basis critical component and pile are integrated
Technology is classified as cutting edge technology.Polyelectrolyte membrane cell (PEMFC) is used as latest generation fuel cell, high with specific energy,
Operating temperature is low, it is environmental-friendly, can quick start, the advantages that service life is long at room temperature, be mobile device and portable device
Ideal source has extremely wide application prospect, is known as being one of this century most promising clean energy resource.
Currently, the low-temperature fuel cell based on perfluorinated sulfonic acid polymer is most successful one kind in PEMFC.Although perfluor sulphur
Acid polymer as a kind of super acids have extremely strong proton conductivity, but its proton transport ability heavy dependence its be hydrated journey
Degree.Therefore, usual PEMFC system needs to humidify into reaction gas, to guarantee perfluorinated sulfonic acid polymer in film and catalysis
Well-hydrated state in layer, to maintain high proton efficiency of transmission in film and electrode.Meanwhile gas humidification and electrode reaction institute
The excessive moisture of generation must be discharged in time, in case blocking gas delivery passage, causes " liquid flooding ".Generally using it is outer humidification and it is interior
The mode of humidification is humidified to proton exchange membrane.The technology of outer humidification and interior humidification is all needed using humidification ancillary equipment, this nothing
Cost, quality, volume and the complexity for increasing battery system are doubted, while also resulting in the quality specific power and volume ratio function of battery
Rate decline.Therefore, there is the self-humidification of PEMFC, realize can simplify the structure of system from humidification, reducing for PEMFC
The volume and weight of system, the energy consumption for reducing system itself and the energy delivery efficiency for improving fuel cell system reduce fuel
The cost of battery system is advantageously implemented the commercialization of Proton Exchange Membrane Fuel Cells.
More about the document patent from humidification at present, Chinese patent ZL200510037575.1 discloses " a kind of from increasing
Wet film electrode and preparation method thereof ", this method are to pre-process proton exchange membrane, and carbon supported platinum catalyst, perfluorinated sulfonic resin are molten
Liquid, hydroaropic substance and low boiling point solvent mixing, are coated in the side of proton exchange membrane, dry and hydrophily hydrogen electrode is made；Again will
Carbon supported platinum catalyst, perfluor sulfoacid resin solution, lyophobic dust and low boiling point solvent mixing, are coated in the another of proton exchange membrane
Side dries and hydrophobicity oxygen electrode is made；Two panels carbon paper and proton exchange membrane are pressed into self-humidifying membrane electrode.In that patent,
Due to hydrophilic particle only simple incorporation, rather than be fixed in Catalytic Layer, thus be easy in battery operation to be lost or
Reunite, this is greatly lowered the stability of battery operation.
Chinese patent ZL20131069005.7 disclose " a proton exchanging film fuel battery self-humidifying membrane electrode and its
Preparation method ", this method are by platinum carbon catalyst, inorganic hydrophilic type metal oxide nanoparticles, perfluorinated sulfonic acid polymer, low
Boiling solvent mixture is coated in the side of Nafion membrane as anode catalyst layer, by platinum carbon catalyst, inorganic hydrophilic type metal oxygen
Compound nanoparticle, perfluorinated sulfonic acid polymer, low boiling point solvent mixture are coated in the another of Nafion membrane as cathode catalysis layer
CCM is made in side.Anode-catalyzed by CCM is placed under ultraviolet lamp after progress ultraviolet lighting processing, is made then at diffusion layer hot pressing
Membrane electrode.In that patent, prepare the hydrophilic Catalytic Layer of anode have to wavelength less than 387nm purple light illumination under irradiate it is longer
Time, preparation procedure is more complex, and simply adulterates these oxide particles for neither leading proton and non-conductive son, can also reduce
The electric conductivity of entire electrode, increases charge transfer resistance, influences the performance of battery.
Up to the present, there are no can significantly weaken the side adulterating nonconducting hydrophilic substance and influencing on cell resistance
Method.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of improved fuel cell self-humidifying membrane electrode, should be from increasing
Wet film electrode can have excellent performance under low humidity conditions, and reduce addition hydroaropic substance to electrode conductivuty and
The influence of resistance also simplifies the preparation process of membrane electrode.
For achieving the above object, technical scheme is as follows:
A kind of preparation method of fuel cell self-humidifying membrane electrode, it is characterised in that: the following steps are included:
It (1) in the hydrogenperoxide steam generator and mass concentration that mass concentration is 3 ~ 5wt.% is successively 0.5 ~ 1mol/ by proton exchange membrane
It is pre-processed, be then washed with distilled water clean and be stored in spare in distilled water in the sulfuric acid solution of L；
(2) catalyst, binder, chitin and solvent are separated by 4 ~ 10: 2~4: 1~5: 100~1000 mass ratio
Even catalyst pulp is supported on the side of proton exchange membrane, and the carrying capacity of catalyst metals is controlled in 0.1~0.5mg/
cm2, then the proton exchange membrane prepared is dried to get the hydrophilic Catalytic Layer of anode is arrived；
(3) catalyst, binder and solvent are separated into uniform catalyst slurry by 4 ~ 10: 2~4: 100~1000 mass ratio
Material is supported on the proton exchange membrane other side, and the carrying capacity of catalyst metals is controlled in 0.1~0.5mg/cm2, then will preparation
Good proton exchange membrane dries to arrive cathode catalysis layer；
(4) gas diffusion layers that two have sprayed in advance are bonded to the two sides of proton exchange membrane after being like this respectively,
Obtain self-humidifying membrane electrode.
In order to which the present invention is better achieved, the chitin particle size is 8 ~ 50 μm, and water absorption quality accounts for after water suction always
The percentage of quality is 30% ~ 80%；The proton exchange membrane select the perfluoro sulfonic acid membrane with a thickness of 40-150 μm, with a thickness of 5~
40 μm of polytetrafluoroethylene (PTFE) perfluoro sulfonic acid membrane, with a thickness of any one of 5~40 μm sulfonation trifluorostyrene co-polymer membranes；Institute
Stating catalyst selects carbon supported platinum catalyst, carbon to carry one of ruthenium catalyst or pallium-on-carbon iridium catalyst；The gas diffusion layers
It to be handled through polytetrafluoroethylene (PTFE) or fluorinated ethylene propylene copolymer (FEP) hydrophobicity, wherein polytetrafluoroethylene (PTFE) or perfluor
Mass percentage of the ethylene propylene copolymer in gas diffusion layers is 10 ~ 30 wt.%；The binder selection Nafion,
Any one of PTFE, PVDF；The mixture that the solvent selects isopropanol, acetone, dehydrated alcohol any one or more of；
The proton exchange membrane drying operation is to dry 60 ~ 180 minutes under the conditions of 50~90 DEG C.
The technical effect that the invention is realized are as follows:
Chitin in the hydrophilic Catalytic Layer of anode can play the role of being retained well, and reaction in cathode catalysis layer is generated
Moisture absorption is kept, and proton exchange membrane is allowed to be sufficiently humidified so as to, and keeps its good proton conductivity；The self-humidifying membrane electrode can be with
There is excellent performance under low humidity conditions, and reduce influence of the addition hydroaropic substance to electrode conductivuty and resistance,
Also simplify the preparation process of membrane electrode.
Detailed description of the invention:
Fig. 1 is performance curve of 1 fuel cell of the embodiment of the present invention under 60% and 80% relative humidity；
Fig. 2 is performance curve of 2 fuel cell of the embodiment of the present invention under 60% and 80% relative humidity；
Fig. 3 is performance curve of 1 fuel cell of comparative example of the present invention under 60% and 80% relative humidity.
Specific embodiment
It is further described with reference to the accompanying drawing and with embodiment to the present invention.But embodiment below is only limitted to explain
The present invention, protection scope of the present invention should include the full content of claim, be not only restricted to following embodiment.
Embodiment 1
(1) pretreatment of proton exchange membrane
The Nafion212 proton exchange membrane for taking 3 × 3cm is initially positioned at 80 DEG C of processing in the hydrogen peroxide that mass fraction is 5wt.%
1 hour, distilled water washes clean was handled 1 hour in the sulfuric acid solution of 0.5mol/L, was then washed with distilled water completely,
The proton exchange membrane handled well is placed in the organic glass center that two panels has the 10 × 10cm in the hole 2 × 2cm, clamps, prevents from loading
Contraction distortion during catalyst.
(2) the hydrophilic Catalytic Layer preparation of anode
Pt/C catalyst (40 wt.%, Johnson Matthey) is weighed respectively according to the mass ratio of mass ratio 6:3:1:500
4mg, Nafion solution (5 wt.%, DuPont) 40mg, chitin (aladdin) 0.67mg, isopropanol 0.5g, sonic oscillation 30
Minute, it is sprayed on the side of proton exchange membrane, is dried 3 hours in 75 DEG C of baking ovens, obtains the hydrophilic Catalytic Layer of anode.Wherein Pt is negative
Carry 0.2mg/cm2, chitin additive amount is 10wt.%.
(3) prepared by cathode catalysis layer
According to the mass ratio of mass ratio 7:3:500 weigh respectively Pt/C catalyst (40 wt.%, Johnson Matthey) 8mg,
Nafion solution (5 wt.%, DuPont) 68.5mg, isopropanol 0.5g, sonic oscillation 30 minutes, it is another to be sprayed on proton exchange membrane
Side dries 3 hours in 75 DEG C of baking ovens, obtains cathode catalysis layer, and wherein Pt loads 0.4mg/cm2。
(4) battery assembly is tested
Proton exchange membrane two sides are fitted in pre-prepd gas diffusion layers and gasket is put into togerther test fixture, with 6N m
Power tighten fixture.Test condition are as follows: 60 DEG C of battery operating temperature, normal pressure, anode reaction gas is hydrogen, and cathode reaction gas is oxygen
Gas, stoichiometric ratio are that 2:2(minimum discharge is 0.1slpm), the opposite humidity that humidifies is 60% and 80%.Test result such as Fig. 1,
It can be seen that battery maximum power density in 60% opposite humidification can reach 450mW/cm2, 0.6V current density reaches 601
mA/cm2；In 80% opposite humidification, maximum power density can reach 465mW/cm2, 0.6V current density reaches 623mA/
cm2。
Embodiment 2
Chitin additive amount is changed to 30 wt.%, remaining experimental procedure and assembling test condition are all identical with embodiment 1.Test knot
Fruit such as Fig. 2, it can be seen that battery maximum power density in 60% opposite humidification reaches 435mW/cm2, 0.6V current density reaches
597 mA/cm2；In 80% opposite humidification, maximum power density reaches 480mW/cm2, 0.6V current density reaches 707 mA/
cm2。
Embodiment 3
Chitin additive amount is changed to 20 wt.%, remaining experimental procedure and assembling test condition are all identical with embodiment 1.Test knot
Fruit finds that battery maximum power density in 60% opposite humidification reaches 459mW/cm2, 0.6V current density reaches 611 mA/cm2；
In 80% opposite humidification, maximum power density reaches 469mW/cm2, 0.6V current density reaches 628mA/cm2。
Comparative example 1
Chitin is not added in anode catalyst layer, remaining experimental procedure and assembling test condition are all identical with embodiment 1.Test knot
Fruit such as Fig. 3, it can be seen that battery maximum power density in 60% opposite humidification can only achieve 249mW/cm2, 0.6V current density
It can only achieve 290mA/cm2；In 80% opposite humidification, maximum power density reaches 267mW/cm2, 0.6V current density reaches
367mA/cm2。
It can be seen that a kind of fuel cell self-humidifying membrane electrode of the present invention and its preparation side from above-mentioned comparative example
Method has excellent performance in low humidity.
It should be noted that according to each embodiment of the present invention, the present invention is may be implemented in those skilled in the art completely
The full scope of independent claims and dependent claims realizes process and the same the various embodiments described above of method；And the present invention is not
It elaborates and partly belongs to techniques well known.
The above, part specific embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, appoints
What those skilled in the art in the technical scope disclosed by the present invention, replaces in the variation that can be readily occurred in, should cover
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of fuel cell self-humidifying membrane electrode, it is characterised in that: the following steps are included:
It (1) in the hydrogenperoxide steam generator and mass concentration that mass concentration is 3 ~ 5wt.% is successively 0.5 ~ 1mol/ by proton exchange membrane
It is pre-processed, be then washed with distilled water clean and be stored in spare in distilled water in the sulfuric acid solution of L；
(2) catalyst, binder, chitin and solvent are separated by 4 ~ 10: 2~4: 1~5: 100~1000 mass ratio
Even catalyst pulp is supported on the side of proton exchange membrane, and the carrying capacity of catalyst metals is controlled in 0.1~0.5mg/
cm2, then the proton exchange membrane prepared is dried to get the hydrophilic Catalytic Layer of anode is arrived；
(3) catalyst, binder and solvent are separated into uniform catalyst slurry by 4 ~ 10: 2~4: 100~1000 mass ratio
Material is supported on the proton exchange membrane other side, and the carrying capacity of catalyst metals is controlled in 0.1~0.5mg/cm2, then will preparation
Good proton exchange membrane dries to arrive cathode catalysis layer；
(4) gas diffusion layers that two have sprayed in advance are bonded to the two sides of proton exchange membrane after being like this respectively,
Obtain self-humidifying membrane electrode.
2. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Chitin particle size be 8 ~ 50 μm, water absorption quality account for water suction after gross mass percentage be 30% ~ 80%.
3. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Proton exchange membrane select the perfluoro sulfonic acid membrane with a thickness of 40-150 μm, the polytetrafluoroethylene (PTFE) perfluoro sulfonic acid membrane with a thickness of 5~40 μm,
With a thickness of 5~40 μm of any one of sulfonation trifluorostyrene co-polymer membrane.
4. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Catalyst selects carbon supported platinum catalyst, carbon to carry any one of ruthenium catalyst or pallium-on-carbon iridium catalyst.
5. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Gas diffusion layers will be handled through polytetrafluoroethylene (PTFE) or fluorinated ethylene propylene copolymer (FEP) hydrophobicity, wherein polytetrafluoro
The mass percentage of ethylene or fluorinated ethylene propylene copolymer in gas diffusion layers is 10 ~ 30 wt.%.
6. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Binder selects any one of Nafion, PTFE, PVDF.
7. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
The mixture that solvent selects isopropanol, acetone, dehydrated alcohol any one or more of.
8. a kind of preparation method of fuel cell self-humidifying membrane electrode according to claim 1, it is characterised in that: described
Proton exchange membrane drying operation is to dry 60 ~ 180 minutes under the conditions of 50~90 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112072120A (en) * | 2020-09-07 | 2020-12-11 | 贵州梅岭电源有限公司 | Hydrophilic/hydrophobic membrane electrode relating to ionic liquid |
| CN114094121A (en) * | 2021-10-07 | 2022-02-25 | 江苏大学 | Preparation method of fuel cell self-humidifying membrane electrode with catalytic layer water management area and membrane electrode thereof |
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| CN103078122A (en) * | 2012-12-20 | 2013-05-01 | 华南理工大学 | Self-humidification membrane electrode for proton exchange membrane fuel cell and preparation method thereof |
| CN107123822A (en) * | 2017-05-08 | 2017-09-01 | 黄河科技学院 | A kind of preparation method of used in proton exchange membrane fuel cell gas diffusion layers |
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| CN1949570A (en) * | 2005-10-10 | 2007-04-18 | 中国科学院大连化学物理研究所 | Gas diffusion layer for low temp fuel cell and preparing process thereof |
| CN102437343A (en) * | 2011-11-17 | 2012-05-02 | 华南理工大学 | Membrane electrode containing hydrophilic high polymer in anode catalytic layer and preparation method thereof |
| CN103078122A (en) * | 2012-12-20 | 2013-05-01 | 华南理工大学 | Self-humidification membrane electrode for proton exchange membrane fuel cell and preparation method thereof |
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Cited By (3)
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| CN112072120A (en) * | 2020-09-07 | 2020-12-11 | 贵州梅岭电源有限公司 | Hydrophilic/hydrophobic membrane electrode relating to ionic liquid |
| CN112072120B (en) * | 2020-09-07 | 2021-07-20 | 贵州梅岭电源有限公司 | Hydrophilic/hydrophobic membrane electrode relating to ionic liquid |
| CN114094121A (en) * | 2021-10-07 | 2022-02-25 | 江苏大学 | Preparation method of fuel cell self-humidifying membrane electrode with catalytic layer water management area and membrane electrode thereof |
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Application publication date: 20190927 |