CN101145614A - Self-humidifying proton exchange film fuel cell membrane electrode preparation method - Google Patents
Self-humidifying proton exchange film fuel cell membrane electrode preparation method Download PDFInfo
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- CN101145614A CN101145614A CNA2006100156636A CN200610015663A CN101145614A CN 101145614 A CN101145614 A CN 101145614A CN A2006100156636 A CNA2006100156636 A CN A2006100156636A CN 200610015663 A CN200610015663 A CN 200610015663A CN 101145614 A CN101145614 A CN 101145614A
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- 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 invention belongs to a preparation method of a self-humidifying membrane electrode for proton exchange membrane fuel cells. The preparation method of the self-humidifying membrane electrode comprises: (1) forming a constant humidity layer on a diffusion layer; (2) forming a catalyst layer on the surface of the constant humidity layer or on two surfaces of a proton exchange membrane; (3) allowing the catalyst layers, the constant humidity layers and the diffusion layers symmetric at two surfaces of the proton exchange membrane, hot-pressing, and taking out to obtain the self-humidifying membrane electrode for the proton exchange membrane fuel cells. The hydrophilic fiber in the constant humidity layer has good water retention capability, and can not only prevent the rapid loss of water inside the membrane electrode during the operation of the fuel cell, which results in the decrease in conductivity of protons inside the proton exchange membrane and the catalyst lining, but also remove excessive water from the electrode catalyst to keep the water inside the membrane electrode in balance without affecting the gas diffusion. The assembled fuel cell has high specific power and efficiency, high catalytic activity, small internal resistance, small diffusion resistance of reactant gases, and long service life.
Description
Technical field
The invention belongs to the Proton Exchange Membrane Fuel Cells technical field, particularly relate to a kind of preparation method of self-humidifying proton exchange film fuel cell membrane electrode.
Background technology
Proton Exchange Membrane Fuel Cells is the electrochemical energy conversion equipment that can continuously the chemical energy in fuel and the oxidant directly be changed into electric energy, is considered to the environmental protection power supply of field first-selections such as following electric automobile, electronic hybrid vehicle, electric bicycle, electric moving aid vehicle, the portable power supply of communication, distributing power station.
Membrane electrode is the core component of Proton Exchange Membrane Fuel Cells, it is the place of fuel and oxidant generation electrochemical reaction, mainly constitute by diffusion layer, Catalytic Layer, proton exchange membrane, because perfluor type sulfonate film material as proton exchange membrane, have only when water exists and just can carry out proton conduction, therefore how making the proton exchange membrane humidification, guarantee higher conductivity, is one of lot of domestic and international scholar key technology of in recent years Proton Exchange Membrane Fuel Cells being fallen over each other to study.
At present knownly make that a kind of method of proton exchange membrane humidification is before gas enters battery in the membrane electrode, auxiliary equipment such as elder generation's employing gas humidification device are carried out humidification to proton exchange membrane, guaranteed higher conductivity, but this structure makes the battery system complexity, increase battery weight and power consumption, reduced the specific power and the efficient of battery; Another kind method is that the doping inorganic nano-particle makes composite membrane in perfluoro sulfonic acid membrane, and this method can improve the water retention property of film really, the nanometer SiO that will synthesize in advance as European patent EP 0926754
2Powder is doped to blend film forming in the proton exchange resins solution, and this film can also keep higher conductivity in the time of 145 ℃, but nanometer SiO
2Powder is easy to reunite in phase transition behavior takes place, and its particle diameter is difficult to control, and the mechanical strength of film is low, is difficult to be applied in the fuel cell; Another method is to increase hydrophilic layer or hydroaropic substance in electrode, disclosing particle diameter as Chinese patent CN1442913A is that the inorganic oxide that 0.1-10 μ m has a moisture-keeping functions is coated in the proton exchange membrane both sides, though this method has improved the water retention property of film, but because the proton conductivity of inorganic oxide is relatively poor, the introducing of this tunic has increased the resistance of membrane electrode, be difficult to guarantee the electrical property of fuel cell, and also difficult at the even inorganic oxide of proton exchange membrane surface preparation; Another Chinese patent CN1719653A adopts transfer method one deck that thickness is suitable with catalyst layer by SiO
2, TiO
2, Zr (HPO
4)
2Or ZrO
2Water conservation layer Deng inorganic nano-particle and proton exchange resins composition is hot-pressed onto the catalyst layer outside, add diffusion layer in the electrode both sides then, make membrane electrode with water holding capacity, this structure has strengthened the internal resistance of membrane electrode, and this layer water conservation layer moisture after, may hinder gaseous diffusion and enter catalyst layer, cause the concentration polarization of battery, reduce the electrical property of battery.
Summary of the invention
The present invention provides a kind of can make fuel cell constant humidity better function and have high ventilation and electric conductivity for solving problems of the prior art, and the preparation method of self-humidifying proton exchange film fuel cell membrane electrode simple in structure.
The present invention for the technical scheme that solves the technical problem employing that exists in the known technology is:
The preparation method of self-humidifying proton exchange film fuel cell membrane electrode comprises diffusion layer, catalyst layer, proton exchange membrane, is characterized in: be provided with the constant humidity layer between diffusion layer and the catalyst layer, described membrane electrode preparation process comprises:
1) constant humidity layered material slurry is coated to the diffusion layer one side, 80-150 ℃ of following dry 1-2h subsequently at 300-380 ℃ of following sintering 20-60min, makes diffusion layer simultaneously form the constant humidity layer;
2) the catalyst layer slip is coated to process 1) in constant humidity laminar surface or the catalyst layer slip is coated to the proton exchange membrane two sides, at 50～130 ℃ of drying 5～60min, make the constant humidity laminar surface form catalyst layer or the proton exchange membrane two sides forms catalyst layer;
3) will not have the proton exchange membrane of coating catalyst layer to be clipped in and be process 2 up and down) in be coated between the catalyst layer of constant humidity layer, the proton exchange membrane that perhaps two sides is coated with catalyst layer is clipped in and is process 1 up and down) in be coated between the constant humidity laminar surface of diffusion layer, at temperature 80-130 ℃, time 1-5 minute, hot pressing under the pressure 0.2-5Mpa is self-humidifying proton exchange film fuel cell membrane electrode after the taking-up;
Wherein constant humidity layered material slurry is 10 by mass ratio: the graphite powder of 1-5: 0.5-4: 50-100 or carbon dust: adhesive: hydrophilic fibre: dispersant stirs and forms; In the constant humidity layered material slurry:
Graphite powder or carbon dust are electrically conductive graphite powder or carbon dust;
Adhesive is rare one or more of hydrophobicity polytetrafluoroethylene, vinylidene, ethylene fluoride third;
Hydrophilic fibre is one or more of glass fibre, carbon fiber, quartz fibre or corrosion resistant metal fiber of diameter 0.02～100 μ m, length 0.2-6mm;
Dispersant is a kind of of water or organic solvent alcohol, ether, ester.
The present invention can also take following technical measures to realize:
The thickness of described constant humidity layer is 0.01-0.3mm.
Described diffusion layer is that the surface is through carbon dust leveling and a kind of in carbon cloth, carbon paper, carbon fiber felt or porous graphite paper that polytetrafluoroethylene is handled; Pt or carbon that described catalyst layer slip is mass ratio 10: 2-5: 50-100 carry the Pt catalyst: proton exchange resins: the slip that solvent becomes; Described proton exchange membrane is perfluor type sulfonate film, composite membrane or the non-carbon fluorine skeleton proton exchange membrane of thickness 15-175 μ m.
With rubbing method or print process constant humidity layered material slurry is applied or is printed onto diffusion layer; With spraying process or rubbing method or print process the catalyst layer slip is distributed to the constant humidity layer or is distributed to the proton exchange membrane two sides.
Alcohol as dispersant is a kind of in methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, glycerol, polyvinyl alcohol or the 1-methoxyl group 2-propyl alcohol; Ether is a kind of in ether, the benzinum; Ester is an ethyl acetate.
Advantage and good effect that the present invention has are: because hydrophilic fibre has water retention preferably in the thermostat layer, the interior moisture loss of membrane electrode is too fast in the time of both can preventing operation of fuel cells, causes that the proton conductivity in proton exchange membrane and the catalyst layer descends; Can under the effect of surface tension and concentration tonsure, water too much in the electrode catalyst be discharged again, make the balance of membrane electrode inner sustain water, and do not hinder gaseous diffusion by the hydrophily of fiber.Make fuel cell specific power and efficient height, catalytic activity height after the assembling, internal resistance is little, the reaction gas diffusional resistance is little, the life-span is long.
Description of drawings
Fig. 1 is the self-humidifying proton exchange film fuel cell membrane electrode structure chart of the present invention's preparation;
The performance of Fig. 2 when preparing 70 ℃ of battery temperatures with the present invention.
Label among the figure is respectively: 1, diffusion layer; 2, constant humidity layer; 3, catalyst layer; 4, proton exchange membrane.
Embodiment
For further understanding summary of the invention of the present invention, characteristics and effect, enumerate following examples now, and conjunction with figs. is described in detail as follows:
Embodiment 1
The glass fibre, carbon dust, mass concentration 60% ptfe emulsion and 50% the isopropanol water solution that with diameter are 50 μ m, length 3mm were by 1: 7: 3: 120 mix, and stir 12 hours behind the ultrasonic 30min, make constant humidity layered material slurry; Will be through the carbon paper after the content 20wt% polytetrafluoroethylene hydrophobic treatment as diffusion layer 1, adopt silk screen print method constant humidity layered material slurry to be printed onto the one side of diffusion layer 1, under 110 ℃ of temperature, dry 30min, at 350 ℃ of sintering 30min, making thickness on diffusion layer 1 is the constant humidity layer 2 of 0.08mm again.
With mass ratio is that 1: 4: 60 Pt carrying capacity 40wt% carbon carries the Pt catalyst: the 5wt% resin solution: isopropyl alcohol is made catalyst slurry, with silk screen print method catalyst slurry is printed onto constant humidity layer 2 surface, 100 ℃ of dry 40min form catalyst layer 3 on constant humidity layer 2 surface.
By structural order shown in Figure 1, the film of a perfluoro sulfonic acid membrane class is placed between two diffusion layers 1 that are loaded with catalyst layer 3, constant humidity layer 2 as proton exchange membrane 4, carry out hot pressing, hot pressing temperature is 130 ℃, 3 minutes time, pressure is 5MPa, makes membrane electrode.
Employing has the graphite flow field plates and the made membrane electrode assembling monocell of snake type runner, and carries out performance test.Effective catalysis area of membrane electrode is 25cm
2The monocell operating condition is: normal pressure, hydrogen and air be humidification not.70 ℃ of battery temperatures.The monocell performance as shown in Figure 2.
The glass fibre, carbon dust, mass concentration 60% ptfe emulsion and 50% the isopropanol water solution that with diameter are 50 μ m, length 3mm were by 1: 7: 3: 120 mix, and stir 12 hours behind the ultrasonic 30min, make constant humidity layered material slurry; Will be through the carbon paper after the content 20wt% polytetrafluoroethylene hydrophobic treatment as diffusion layer 1, adopt silk screen print method constant humidity layered material slurry to be printed onto the one side of diffusion layer 1, under 110 ℃ of temperature, dry 30min, at 350 ℃ of sintering 30min, making thickness on diffusion layer 1 is the constant humidity layer 2 of 0.08mm again.
With mass ratio is that 1: 4: 60 Pt carrying capacity 40wt% carbon carries the Pt catalyst: the 5wt% resin solution: isopropyl alcohol is made catalyst slurry, adopt silk screen print method at the film of perfluoro sulfonic acid membrane class a side printed catalyst slurry and 100 ℃ of dry 40min as proton exchange membrane 4, and then printing opposite side, dry 40min under 100 ℃ equally.The Pt carrying capacity of both sides is 0.4mg/cm
2, proton exchange membrane 4 two sides form catalyst layer 3 respectively.
By structural order shown in Figure 1,3 the proton exchange membrane 4 that the two sides is loaded with catalyst layer places between two diffusion layers 1 that are loaded with constant humidity layer 2 by structural order shown in Figure 1, utilizes the pressure of end plate to compress.The monocell performance as shown in Figure 2.
Comparing embodiment
Will be through the carbon paper after the content 20wt% polytetrafluoroethylene hydrophobic treatment as diffusion layer 1, with mass ratio is that 1: 4: 60 Pt carrying capacity 40wt% carbon carries the Pt catalyst: the 5wt% resin solution: isopropyl alcohol is made catalyst slurry, with silk screen print method catalyst slurry is printed onto diffusion layer 1 surface, 100 ℃ of dry 40min form catalyst layer 3 on diffusion layer 1 surface.
The film of a perfluoro sulfonic acid membrane class is placed between two diffusion layers 1 that are loaded with catalyst layer 3 as proton exchange membrane 4, carry out hot pressing, hot pressing temperature is 130 ℃, and 3 minutes time, pressure is 5MPa, makes membrane electrode.
Employing has the graphite flow field plates and the made membrane electrode assembling monocell of snake type runner, and carries out performance test.Effective catalysis area of membrane electrode is 25cm
2The monocell operating condition is: normal pressure, hydrogen and air be humidification not.70 ℃ of battery temperatures.The monocell performance as shown in Figure 2.
In the comparison diagram 2 embodiment 1, embodiment 2 and comparing embodiment as seen, the prepared membrane electrode of the present invention has from humidifying capacity, at reaction gas not under the humidified condition, adopts the battery performance of this membrane electrode obviously to be better than the battery of the membrane electrode of conventional method preparation.
The also available Nafion film of above-mentioned proton exchange membrane 4, Dow film, Flemion, Aciplex
Film, partially fluorinated proton exchange membrane 4 can be used the BAM3G film of Ballard company, the proton exchange membrane 4 of nonfluorinated can be used the sulfonated phenylethylene/butylene vinyl/styrene triblock copolymer film of DaiS company, and polytetrafluoroethylporous porous membrane is the porous polymers base compound proton exchange membrane 4 of substrate, as Gore-Select
TMSeries membranes.
Claims (5)
1. the preparation method of a self-humidifying proton exchange film fuel cell membrane electrode comprises diffusion layer, catalyst layer, proton exchange membrane, it is characterized in that: be provided with the constant humidity layer between diffusion layer and the catalyst layer, described membrane electrode preparation process comprises:
1) constant humidity layered material slurry is coated to the diffusion layer one side, 80-150 ℃ of following dry 1-2h subsequently at 300-380 ℃ of following sintering 20-60min, makes diffusion layer simultaneously form the constant humidity layer;
2) the catalyst layer slip is coated to process 1) in constant humidity laminar surface or the catalyst layer slip is coated to the proton exchange membrane two sides, at 50～130 ℃ of drying 5～60min, make the constant humidity laminar surface form catalyst layer or the proton exchange membrane two sides forms catalyst layer;
3) will not have the proton exchange membrane of coating catalyst layer to be clipped in and be process 2 up and down) in be coated between the catalyst layer of constant humidity layer, the proton exchange membrane that perhaps two sides is coated with catalyst layer is clipped in and is process 1 up and down) in be coated between the constant humidity laminar surface of diffusion layer, at temperature 80-130 ℃, time 1-5 minute, hot pressing under the pressure 0.2-5Mpa is self-humidifying proton exchange film fuel cell membrane electrode after the taking-up;
Wherein constant humidity layered material slurry is 10 by mass ratio: the graphite powder of 1-5: 0.5-4: 50-100 or carbon dust: adhesive: hydrophilic fibre: dispersant stirs and forms; In the constant humidity layered material slurry:
Graphite powder or carbon dust are electrically conductive graphite powder or carbon dust;
Adhesive is rare one or more of hydrophobicity polytetrafluoroethylene, vinylidene, ethylene fluoride third;
Hydrophilic fibre is one or more of glass fibre, carbon fiber, quartz fibre or corrosion resistant metal fiber of diameter 0.02～100 μ m, length 0.2-6mm;
Dispersant is a kind of of water or organic solvent alcohol, ether, ester.
2. membrane electrode preparation method according to claim 1 is characterized in that: the thickness of described constant humidity layer is 0.01-0.3mm.
3. membrane electrode preparation method according to claim 1 is characterized in that: described diffusion layer flattens through carbon dust for the surface and is a kind of in carbon cloth, carbon paper, carbon fiber felt or porous graphite paper that polytetrafluoroethylene is handled; Pt or carbon that described catalyst layer slip is mass ratio 10: 2-5: 50-100 carry the Pt catalyst: proton exchange resins: the slip that solvent becomes; Described proton exchange membrane is perfluor type sulfonate film, composite membrane or the non-carbon fluorine skeleton proton exchange membrane of thickness 15-175 μ m.
4. membrane electrode preparation method according to claim 1 is characterized in that: with rubbing method or print process constant humidity layered material slurry is applied or be printed onto diffusion layer; With spraying process or rubbing method or print process the catalyst layer slip is distributed to the constant humidity layer or is distributed to the proton exchange membrane two sides.
5. membrane electrode preparation method according to claim 1 is characterized in that: the alcohol as dispersant is a kind of in methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, glycerol, polyvinyl alcohol or the 1-methoxyl group 2-propyl alcohol; Ether is a kind of in ether, the benzinum; Ester is an ethyl acetate.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101752566B (en) * | 2008-12-18 | 2012-05-30 | 财团法人工业技术研究院 | Bonding agent and membrane electrode assembly including same |
| CN102780009A (en) * | 2012-08-03 | 2012-11-14 | 上海锦众信息科技有限公司 | Membrane electrode preparation method of fuel battery |
| CN101887979B (en) * | 2009-05-13 | 2013-01-02 | 财团法人工业技术研究院 | Proton exchange membrane with high proton conductivity |
| CN102142572B (en) * | 2010-01-28 | 2013-11-06 | 南亚电路板股份有限公司 | Direct methanol fuel cell structure and manufacturing method thereof |
| CN107681164A (en) * | 2017-09-25 | 2018-02-09 | 深圳市南科燃料电池有限公司 | Gas diffusion layers and preparation method thereof and fuel cell |
| CN110380060A (en) * | 2019-07-01 | 2019-10-25 | 江苏乾景新能源产业技术研究院有限公司 | A kind of method for preparing membrane electrode that can improve Proton Exchange Membrane Fuel Cells low humidity runnability |
| WO2023035454A1 (en) * | 2021-09-07 | 2023-03-16 | 爱德曼氢能源装备有限公司 | Fuel cell polar plate structure and cell stack |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101752566B (en) * | 2008-12-18 | 2012-05-30 | 财团法人工业技术研究院 | Bonding agent and membrane electrode assembly including same |
| CN101887979B (en) * | 2009-05-13 | 2013-01-02 | 财团法人工业技术研究院 | Proton exchange membrane with high proton conductivity |
| CN102142572B (en) * | 2010-01-28 | 2013-11-06 | 南亚电路板股份有限公司 | Direct methanol fuel cell structure and manufacturing method thereof |
| CN102780009A (en) * | 2012-08-03 | 2012-11-14 | 上海锦众信息科技有限公司 | Membrane electrode preparation method of fuel battery |
| CN107681164A (en) * | 2017-09-25 | 2018-02-09 | 深圳市南科燃料电池有限公司 | Gas diffusion layers and preparation method thereof and fuel cell |
| CN110380060A (en) * | 2019-07-01 | 2019-10-25 | 江苏乾景新能源产业技术研究院有限公司 | A kind of method for preparing membrane electrode that can improve Proton Exchange Membrane Fuel Cells low humidity runnability |
| JP7419780B2 (en) | 2019-12-09 | 2024-01-23 | Ｔｏｐｐａｎホールディングス株式会社 | Membrane electrode assembly for fuel cells and polymer electrolyte fuel cells |
| WO2023035454A1 (en) * | 2021-09-07 | 2023-03-16 | 爱德曼氢能源装备有限公司 | Fuel cell polar plate structure and cell stack |
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| CN100505395C (en) | 2009-06-24 |
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