CN106134492B - A kind of preparation method of hydrophilic film electrode - Google Patents
A kind of preparation method of hydrophilic film electrodeInfo
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- CN106134492B CN106134492B CN200610119769.0A CN200610119769A CN106134492B CN 106134492 B CN106134492 B CN 106134492B CN 200610119769 A CN200610119769 A CN 200610119769A CN 106134492 B CN106134492 B CN 106134492B
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- sintering
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Abstract
The present invention relates to the preparation method of a kind of hydrophilic film electrode of fuel cell field, the present invention adopt base material hydrophober hydrophobic process and carry out sintering or through hydrophobic processing carbon paper; By with carbon supported platinum catalyst in carbon carbon dust of the same type and hydrophobic emulsion be mixed into slurry and be applied on base material, sintering forms gas diffusion layers, and carries out roll extrusion leveling, catalyst pulp is applied on diffusion layer and carries out sintering, rejects not flat spot by magnifying glass; PEM is placed between two gas-diffusion electrodes with Catalytic Layer, on press, carries out hot pressing; Make the membrane electrode of preparation have good electrical property and stable life-span, compared with prior art, between each layer, combination closely, contact resistance is little, and preparation process is convenient and simple, has solved high power drainage problem, simplify membrane electrode preparation flow simultaneously, be applicable to quantize in small batches production operation.
Description
Technical field
The present invention relates to fuel cell field, be specifically related to a proton exchanging film fuel battery parentThe preparation method of water-based membrane electrode.
Background technology
Fuel cell be a kind of can be direct by containing chemical energy in hydrogen fuel and oxidantBe converted into the TRT of electric energy and product. And Proton Exchange Membrane Fuel Cells is stable because of itProperty is high, pollution-free, noise is low, energy conversion rate is high receives much concern.
For the preparation of membrane electrode assembly, the mechanism of carrying in electrode according to reacting gas is notWith, electrode conventional current PEM can be divided into hydrophobic electrode and hydrophilic electrode twoKind. Hydrophobic electrode is that in Catalytic Layer, to add hydrophober, reacting gas be to form at hydrophoberHydrophobic network in transmit, and in hydrophilic electrode, reacting gas is to be first dissolved in water or perfluorinated sulfonic acidIn sodium, then spread transmission. According to the coating method of catalyst, be mainly divided into two classes, theOne is that catalyst is covered on gas diffusion layers, forms double-decker, is called substrate transfer method,Then under certain condition, hot pressing is transferred to and on PEM, is formed membrane electrode; The second isThe disclosed catalyst of China Patent Publication No. CN 1471186A is covered in the both sides of PEMForm three-decker, be called direct coating method, first at an inertia polytetrafluoroethylene filmIn substrate, construct Catalytic Layer, transferred on PEM by the method for hot pressing subsequently.First, after catalyst, perfluorinated sulfonic acid sodium solvent, glycerine fully being mixed, be applied to polytetrafluoroethyl-neOn alkene film, after oven dry, high temperature hot pressing is transferred on PEM, divests polytetrafluoroethylene (PTFE)After film, obtain three in one membreane electrode. This hydrophily electrode, reacting gas be first dissolved in water orIn perfluorinated sulfonic acid sodium, then spread transmission, in the time that electrode moves under high power, electrode originallyThe water that body generates increases severely, and now very easily causes water logging, reduces the turnover ability of reaction gas, impactThe stability of electrode. For another example direct coating method structure, the method can be prepared low platinum load amount, hasThe features such as film is hydrophilic, continuous catalysis layer, but in the time peeling off transfer sheet, easily sticky on thin sliceLive the Catalytic Layer of part, thereby can not ensure shifting completely and Catalytic Layer smooth of Catalytic Layer,Affect electrode performance and life-span.
Summary of the invention
The object of this invention is to provide a proton exchanging film fuel battery hydrophilic film electrodePreparation method,
The object of the invention is the deficiency of the above-mentioned prior art existence solving, and proposes a kind of hydrophilicProperty membrane electrode, has good electrode performance, and stability is high, can solve high power draining and askTopic is simplified membrane electrode preparation flow simultaneously, is applicable to quantize in small batches production operation.
The present invention realizes like this; One proton exchanging film fuel battery hydrophilic film electrodePreparation method, comprises the following steps:
1, base material carbon paper concentration is that 54wt.% hydrophober hydrophobic is processed and carries out sintering,120～130 DEG C of baking 5～10min of the sintering temperature first step, sintering temperature second step exists350 DEG C of baking 5～10min,
2, mediation carbon dust
3, gas diffusion layers slip, 120～130 DEG C of baking 5～10min of first step temperature,350 DEG C of baking 5～10min of second step temperature, sintering forms gas diffusion layers, and carries out roll extrusionLeveling, rejects not flat spot by magnifying glass;
4, carry out sintering 10min for 120～130 DEG C of catalyst pulp sintering temperatures, by puttingLarge mirror is rejected not flat spot;
5, PEM is placed between two gas-diffusion electrodes with Catalytic Layer, at pressUpper with addition of protective device, pressure is 2.5～5MPa, carries out hot pressing at 140～185 DEG C, is pressingAfter machine combined pressure, continue 3s left and right, open press and release the steam of suppressing in membrane electrode, then heavyNew pressing, continues 60～120s.
The present invention compared with prior art, this hydrophily electrode strengthened membrane electrode performance andLife-span; In membrane electrode pressing process, take deflation course one time, be conducive to catalyst and protonExchange membrane is combined closely, and is not easy layering, reduces contact resistance, ensures the performance of membrane electrode.Preparation flow of the present invention is simple, easily operation, and electrode performance is good, and reduce and press the probability of wearing,Improve the homogeneity of membrane electrode simultaneously,
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail. Hydrophilic film of the present inventionThe preparation method of electrode adopts following steps:
1, bottom material carbon paper is 54wt.% with novel hydrophober vinylidene emulsion concentration) hateWater treatment is also carried out sintering, when sintering, first with 120～130 DEG C of baking 5～10min, then exists350 DEG C of baking 5～10min, the clean amount of hydrophober vinylidene emulsion is carbon paper: vinylidene breastLiquid=1: 0.25～0.66, the content of vinylidene emulsion is 20～40wt.%, or adoptsThe carbon paper (hydrophober content is 5～20wt.%) that the hydrophobic that dispatches from the factory was processed;
2, with Pt/C in carbon carbon dust of the same type be first stirred to pasty state with blender dipping, then addEnter hydrophobic emulsion vinylidene emulsion and be mixed with into gas diffusion layers slip, consumption is carbon dust
0.62mg/cm2, the clean consumption of vinylidene emulsion is 0.413mg/cm2, sonic oscillation 10minOn rear brushing or spraying base material, first, with 120～130 DEG C of baking 5～10min, then exist350 DEG C of baking 5～10min, sintering forms gas diffusion layers, and carries out roll extrusion leveling, byMagnifying glass is rejected not flat spot, and wherein vinylidene emulsion net content is gas diffusion layers
40wt.％；
3,40wt.%Pt/C catalyst is evenly mixed with 10wt.% perfluorinated sulfonic acid sodium solution,Mass ratio:
40wt.%Pt/C: perfluorinated sulfonic acid sodium=90: 10～40
Be that perfluorinated sulfonic acid sodium accounts for Catalytic Layer 10%～30%, then drip blender and stir, Under Ultrasonic VibrationSwing 10min Kaolinite Preparation of Catalyst slurry, pasty state is best;
4, agent slurry is brushed or is sprayed on diffusion layer and carries out sintering with 120～130 DEG C10min, rejects not flat spot by magnifying glass;
5, PEM is placed between two gas-diffusion electrodes with Catalytic Layer to twoOutside gas diffusion layers, respectively add an aluminium thin, on press with addition of rigid pad, the thickness of padFor being slightly less than the summation of PEM and two gas-diffusion electrode thickness with Catalytic Layer, pressPower is 2.5～5MPa, carries out hot pressing at 140～185 DEG C, continues a 3s left side after press combined pressureThe right side, opens press and releases the steam of suppressing in membrane electrode, then pressing again, continue 60～
120s。
Embodiment 1:
Select thickness 0.2mm carbon paper, process and burn with hydrophober vinylidene emulsion hydrophobicKnot, when sintering first with 120～130 DEG C of baking 5～10min, then 350 DEG C of bakings 5～
10min，
The clean amount of hydrophober vinylidene emulsion is:
Carbon paper: vinylidene emulsion=1: 0.25～0.66
The content that is vinylidene emulsion is 20～40wt.%, then by with Pt/C in carbon carbon of the same typePowder is first stirred to pasty state with blender dipping, then drips hydrophobic emulsion vinylidene emulsion and mixesBe prepared into gas diffusion layers slip, consumption is carbon dust 0.62mg/cm2, vinylidene emulsion is used onlyAmount is 0.413mg/cm2, after sonic oscillation 10min, brush or spraying base material on, first with120～130 DEG C of baking 5～10min, then, at 350 DEG C of baking 5～10min, sintering forms gasBody diffused layer, and carry out roll extrusion leveling, reject not flat spot, wherein vinylidene by magnifying glassEmulsion net content is the 40wt.% of gas diffusion layers, then take 40wt.%Pt/C catalyst with10wt.% perfluorinated sulfonic acid sodium solution evenly mixes,
Mass ratio:
40wt.%Pt/C: perfluorinated sulfonic acid sodium=90: 10～40
Be that perfluorinated sulfonic acid sodium accounts for Catalytic Layer 10%～30%, then drip a small amount of blender and stir, ultrasonicVibration 10min Kaolinite Preparation of Catalyst slurry, pasty state is best, by the catalyst pulp brush preparingBe coated with or spraying diffusion layer on and carry out sintering 10min with 120～130 DEG C, reject by magnifying glassNot flat spot, is finally placed in PEM between two gas-diffusion electrodes with Catalytic Layer,Outside two gas diffusion layers, respectively add an aluminium thin, on press with addition of rigid pad, padThickness is be slightly less than PEM and two gas-diffusion electrode thickness with Catalytic Layer totalWith, pressure is 2.5～5MPa, carries out hot pressing at 140～185 DEG C, after press combined pressure, continues3s left and right, opens press and releases the steam of suppressing in membrane electrode, and then pressing again continues60～120s. Carbon paper thickness 0.22mm under nature, PEM adopts perfluorinated sulfonic acidSodium 112 (thickness 0.05mm), the MEA thickness after hot pressing is 0.41～0.43mm.
Embodiment 2:
The carbon paper (hydrophober content is 5～20wt.%) of selecting the hydrophobic that dispatches from the factory to process, simplifiesTechnique, by with Pt/C in carbon carbon dust of the same type be first stirred to pasty state with blender dipping, connectDropping hydrophobic emulsion vinylidene emulsion and be mixed with into gas diffusion layers slip, consumption is carbonPowder 0.62mg/cm2, the clean consumption of vinylidene emulsion is 0.413mg/cm2, sonic oscillation 10minOn rear brushing or spraying base material, first, with 120～130 DEG C of baking 5～10min, then exist350 DEG C of baking 5～10min, sintering forms gas diffusion layers, and carries out roll extrusion leveling, byMagnifying glass is rejected not flat spot, and wherein vinylidene emulsion net content is gas diffusion layers40wt.%, then takes 40wt.%Pt/C catalyst and 10wt.% perfluorinated sulfonic acid sodium solution is evenMix,
Mass ratio:
40wt.%Pt/C: perfluorinated sulfonic acid sodium=90: 10～40
Be that perfluorinated sulfonic acid sodium accounts for Catalytic Layer 10%～30%, then drip a small amount of blender and stir, ultrasonicVibration 10min Kaolinite Preparation of Catalyst slurry, pasty state is best, by the catalyst pulp brush preparingBe coated with or spraying diffusion layer on and carry out sintering 10min with 120～130 DEG C, reject by magnifying glassNot flat spot, is finally placed in PEM between two gas-diffusion electrodes with Catalytic Layer,Outside two gas diffusion layers, respectively add thin a protection of aluminium, on press with addition of rigid padSheet, the thickness of pad is to be slightly less than PEM and two gas-diffusion electrodes with Catalytic LayerThe summation of thickness, pressure is 2.5～5MPa, carries out hot pressing at 140～185 DEG C, closes at pressAfter pressing, continue 3s left and right, open press and release the steam of suppressing in membrane electrode, then again pressClose, continue 60～120s. Carbon paper thickness 0.15mm under nature, PEM adoptsPerfluorinated sulfonic acid sodium 112 (thickness 0.05mm), the MEA thickness after hot pressing is 0.30～0.32mm.
Claims (1)
1. a preparation method for hydrophilic film electrode, is characterized in that the performing step of the methodAs follows:
The first step, selecting carbon paper is base material, with concentration be 54wt.% hydrophober vinylideneEmulsion hydrophobic is processed and is carried out sintering, when sintering, first toasts 5～10min with 120～130 DEG C,Then in 350 DEG C of baking 5～10min, the weight ratio of hydrophober vinylidene emulsion and carbon paper=0.25～0.66: 1, the content of vinylidene emulsion is 20～40wt.%, or adopts outThe carbon paper that factory's hydrophobic was processed, hydrophober content is 5～20wt.%;
Second step, by with Pt/C in carbon carbon dust of the same type be first stirred to pasty state with blender dipping,Add hydrophober vinylidene emulsion to be mixed with into gas diffusion layers slip, consumption is carbon dust again
0.62mg/cm2, the clean consumption of vinylidene emulsion is 0.413mg/cm2, sonic oscillation 10minOn rear brushing or spraying base material, first with 120～130 DEG C of baking 5～10min, soAfter at 350 DEG C of baking 5～10min, sintering forms gas diffusion layers, and carries out roll extrusion leveling, borrowsHelp magnifying glass to reject not flat spot, wherein vinylidene emulsion net content is gas diffusion layers 40
wt.％；
The 3rd step, by evenly mixed to 40wt.%Pt/C catalyst and 10wt.% perfluorinated sulfonic acid sodium solutionClose, mass ratio is 40wt.%Pt/C: perfluorinated sulfonic acid sodium=90: 10～40,
Perfluorinated sulfonic acid sodium accounts for Catalytic Layer 10～30%, then drips blender and stir, Under Ultrasonic VibrationSwing 10min Kaolinite Preparation of Catalyst slurry;
The 4th step, brushes catalyst pulp or be sprayed on diffusion layer, and with 120～130 DEG CCarry out sintering 10min, reject not flat spot by magnifying glass, make gas-diffusion electrode;
The 5th step, is placed in PEM between two gas-diffusion electrodes with Catalytic Layer,Outside two gas-diffusion electrodes, respectively cover again that to add an aluminium thin, on press with addition of rigid pad,The thickness of pad is to be slightly less than PEM and two gas-diffusion electrodes with Catalytic LayerThe summation of thickness, pressure is that 140～185 DEG C of 2.5～5MPa, temperature carry out hot pressing, at pressAfter combined pressure, continue 3S left and right, open press and release the steam of suppressing in membrane electrode, then againPressing, continues 60～120S.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610119769.0A CN106134492B (en) | 2006-09-13 | 2006-09-13 | A kind of preparation method of hydrophilic film electrode |
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| CN200610119769.0A CN106134492B (en) | 2006-09-13 | 2006-09-13 | A kind of preparation method of hydrophilic film electrode |
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Cited By (2)
| 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 |
| CN111162285A (en) * | 2018-11-08 | 2020-05-15 | 中国科学院大连化学物理研究所 | Conductive gas diffusion layer of fuel cell and preparation method thereof |
-
2006
- 2006-09-13 CN CN200610119769.0A patent/CN106134492B/en active Active
Cited By (2)
| 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 |
| CN111162285A (en) * | 2018-11-08 | 2020-05-15 | 中国科学院大连化学物理研究所 | Conductive gas diffusion layer of fuel cell and preparation method thereof |
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