CN1581548A - Unit combined fuel cell membrane eletrode and its preparing method - Google Patents
Unit combined fuel cell membrane eletrode and its preparing method Download PDFInfo
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- CN1581548A CN1581548A CNA200410013149XA CN200410013149A CN1581548A CN 1581548 A CN1581548 A CN 1581548A CN A200410013149X A CNA200410013149X A CN A200410013149XA CN 200410013149 A CN200410013149 A CN 200410013149A CN 1581548 A CN1581548 A CN 1581548A
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- Y02E60/30—Hydrogen technology
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Abstract
Membrane electrode is composed of secondary unit and main unit. The main unit consists of gaseous diffusion layer, catalyst layer, and proton exchange layer. The preparation method includes following steps: coating pulp of catalyst on gaseous diffusion layer to prepare catalyst layer; casting resin solution of proton exchange to prepare proton exchange layer, then coating pulp of catalyst again to prepare catalyst layer. Secondary unit is a gaseous diffusion layer. Membrane electrode is obtained by cold contact between main unit and secondary unit, or hot pressing the two units. Features are: suitable to continuous production, controllable thickness of proton exchange layer, high binding intensity between layers, low contact resistance, operatable under high temperature.
Description
Technical field
The present invention relates to a kind of membrane electrode of fuel batter with proton exchange film and preparation method thereof, particularly membrane electrode that combines by master unit and sub-cell and preparation method thereof.
Background technology
Fuel cell is a kind of cleaning, efficient, the quiet electrochemical engine that moves.People generally believe that it will become a super big industry at mid-21st Century, and the revolution that will bring energy industry.And Proton Exchange Membrane Fuel Cells (Proton Exchange Membrane Fuel Cell, PEMFC) low with its operating temperature, specific power density has good application prospects in industries such as mobile communication equipment, portable electronics, national defence critical equipment, mechanical transports greatly.But because pem fuel pond cost is still too high, be difficult at present to marketing and application.
Proton Exchange Membrane Fuel Cells is made of end plate, collector plate, sealing medium and membrane electrode usually, (the Membrane Electrode Assembly of membrane electrode wherein, MEA) be the indispensable assembly of fuel cell, mainly form by diffusion layer, catalyst layer and substrate with proton exchange function, catalyst layer wherein and proton exchange membrane are the important places of fueled electrochemical reaction, are the cores of fuel cell.The technology of preparing of tradition MEA is that catalyst material is coated on the gas diffusion layers (adopting the porous carbon paper usually), then with proton exchange membrane hot pressing, forms the membrane-electrode three-in-one component.By the analysis to the basic principle of electrochemical reaction of fuel cell, this traditional technology exists very outstanding defective:
(1) catalyst layer electrochemical reaction district and porous carbon paper fuel delivery area are overlapping.Because the electrochemical reaction district is different to the character requirement of material with the fuel delivery area, the requirement of fuel delivery area is hydrophobic as the requirement of electrochemical reaction district is hydrophilic, therefore causes taking place mutual interference, has limited the performance of battery.Simultaneously greatly waste catalyst material, the potentiality that further reduce the Pt carrying capacity are limited.
(2) combination interface of catalyst layer and proton exchange membrane is to form by hot pressing, and catalyst is to be coated on the scraggly porous carbon paper and proton exchange membrane hot pressing again, therefore can not form the good interface combination, influence proton transport, also limit battery performance.
Based on the shortcoming of traditional MEA, people have developed a kind of MEA that is made up of CCM (catalyst coated membrane) and diffusion layer.CCM is the traditional MEA structure of being different from of development in recent years, directly a kind of functional unit of the realization fuel cell electrochemical process that catalyst layer and proton exchange membrane are composited.Adopt the CCM framework, requirement design catalyst layer that can the fuel cell electrochemical reaction and and proton exchange membrane between interfacial structure, make catalyst layer do very thinly, improve reaction rate to greatest extent, reduce the Pt carrying capacity; In addition, CCM can be continuously produced, and realizes the scale manufacturing of CCM, and reduces cost.But in the CCM fuel cell framework, catalyst layer is coated or transfers on the proton exchange membrane that the interface of catalyst layer and film lacks excessively layer, has influenced proton transport; In addition, the gas diffusion layers of CCM both sides and CCM are cold joint and touch, and promptly unhot-pressing touches, and the contact resistance between them is generally all bigger.
Summary of the invention
The purpose of this invention is to provide a kind of membrane electrode of fuel batter with proton exchange film and preparation method thereof, promptly a kind of membrane electrode of fuel batter with proton exchange film that combines by master unit and sub-cell and preparation method thereof.
Membrane electrode of fuel batter with proton exchange film of the present invention is combined by master unit and sub-cell, membrane electrode for a kind of unit-combination type, described master unit is the membrane-electrode unit that is formed by the common bonding of gas diffusion layers, catalyst layer and proton exchange layer, its composition or structure are followed successively by gas diffusion layers, catalyst layer, proton exchange layer, catalyst layer, and described sub-cell is a gas diffusion layers.
The gas diffusion layers of described membrane electrode master unit and sub-cell is porous carbon paper or the carbon cloth through hydrophobic treatment, can the compound more inferior hydrophobic layer of being made up of carbon black and polytetrafluoroethylgranule granule (sublayer) through a side of the porous carbon paper of hydrophobic treatment or carbon cloth.
Described membrane electrode master unit catalyst layer mainly carries platinum or platinum alloy carbon-supported catalysts and proton exchange resins by platinum or platinum alloy or carbon to be formed, and the mass ratio of catalyst and proton exchange resins is 10: 2～5.
Described catalyst is meant Pt, Pd, Ru, Rh, Ir, Os noble metal or its carbon loading Pt/C, Pd/C, Ru/C, Rh/C, Ir/C, Os/C, Pt and Pd, Ru, Rh, Ir, the bianry alloy PtPd of Os, PtRu, PtRh, PtIr, PtOs or its carbon loading PtPd/C, PtRu/C, PtRh/C, PtIr/C, PtOs/C, Pt, Pd, Ru, Rh, Ir, Os noble metal and Fe, Cr, Ni, (N is Pt to the bianry alloy NM that Co forms, Pd, Ru, Rh, Ir or Os, M is Fe, Cr, Co or Ni) or its carbon loading NM/C (N, the definition of M is with aforementioned), Pt, Pd, Ru, Rh, Ir, Os noble metal and Fe, Cr, Ni, the ternary alloy three-partalloy NM that Co forms
1M
2(definition of N is with aforementioned, M
1, M
2Be the composition of any two kinds of metallic elements among Fe, Cr, Co and the Ni, as FeCo etc.) or its carbon loading NM
1M
2/ C (N, M
1, M
2Definition with aforementioned).Above-mentioned carrier carbon is generally conductive carbon black or carbon nano-tube, or carbon nano-fiber.
The proton exchange layer of described membrane electrode master unit is that the resin with proton exchange function is formed, described proton exchange resins is meant the perfluorinated sulfonic resin with sulfonic acid group, as the Nafion resin or the Nafion solution of du Pont company production, or sulfonation thermal stability polymer, Flemion proton conductor polymer with proton exchange function.
The preparation process of membrane electrode of fuel batter with proton exchange film of the present invention is as follows:
(1) catalyst, proton exchange resins are mixed by 10: 2～5: 100～1500 mass ratio is full and uniform with solvent, make catalyst slurry or prepared Chinese ink, described solvent is meant water or alcohol, ether, ester, ketone or nitrile.Wherein alcohol is methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, glycerol, 1-methoxyl group 2-propyl alcohol (MOP), and ether can be ether, benzinum, and ester and ketone are ethyl acetate and acetone;
(2) the part catalyst slurry that step (1) is obtained is coated to a side of gas diffusion layers, and vacuumize forms catalyst layer;
(3) the proton exchange resins solution-cast is arrived on step (3) catalyst layer,, form proton exchange layer through vacuumize;
(4) remaining catalyst slurry is coated on the proton exchange layer that has been shaped, vacuumize makes membrane electrode master unit of the present invention;
(5) the membrane electrode master unit of preparation is close to or hot pressing by contact with the sub-cell of being made up of gas diffusion layers, is promptly obtained unit-combination type membrane electrode of the present invention.
The concrete preparation method of unit-combination type membrane electrode of fuel batter with proton exchange film of the present invention, carry out as follows:
1,, makes catalyst slurry (slurry) or prepared Chinese ink (ink) with catalyst, proton exchange resins and solvent is full and uniform mixes;
2, get the part catalyst slurry, by a side that is coated with, method for printing screen is coated to a gas diffusion layers, vacuumize forms catalyst layer.Gas diffusion layers is porous carbon paper or the carbon cloth through hydrophobic treatment, the inferior hydrophobic layer of can compound again one deck being made up of carbon black and polytetrafluoroethylene (PTFE) particle in the porous carbon paper of hydrophobic treatment or carbon cloth one side;
3, by coating, method for printing screen proton exchange resins solution is coated on the prepared catalyst layer, vacuumize forms proton exchange layer on catalyst layer;
4, remaining catalyst slurry is coated on the proton exchange membrane of formation by coating, method for printing screen, vacuumize promptly makes membrane electrode master unit of the present invention;
5, the membrane electrode master unit of preparation is close to or hot pressing by contact with the sub-cell of being made up of gas diffusion layers, is promptly obtained unit-combination type membrane electrode of the present invention.
Sub-cell of the present invention is made up of gas diffusion layers.
It is one-sided that the present invention at first is coated in catalyst slurry one gas diffusion layers, form proton exchange layer at the catalyst layer surface casting proton exchange resins solution that forms then, coating catalyst slip thereon more at last, form catalyst layer, promptly obtain the master unit of fuel cell, sub-cell only is a gas diffusion layers.Master unit and sub-cell are touched or hot pressing by cold joint, promptly obtain unit-combination type membrane electrode of the present invention.The present invention compares with background technology, has the following advantages:
1) the membrane electrode preparation is highly integrated, is fit to very much continuous suitability for industrialized production;
2) proton exchange layer or proton exchange membrane controllable thickness are not subjected to the size restrictions of commercially available proton exchange membrane, so can do proton exchange layer or proton exchange membrane very thin; ,
3) diffusion layer and catalyst layer, the bond strength of catalyst layer and proton exchange interlayer is improved, and contact resistance decreases.
Monocell assembling and test.Unit-combination type membrane electrode and graphite collector plate, copper facing stainless-steel sheet are assembled into monocell.Effective catalysis area of monocell is 5cm * 5cm, and operating condition is: back pressure P
Air=P
Hydrogen=0Mpa, battery temperature room temperature-80 ℃, anode 0-100% humidification, the humidification temperature is 70-100 ℃, Pt carrying capacity≤1mg/cm
2
Description of drawings
Fig. 1 is the composition schematic diagram of membrane electrode of the present invention.
Fig. 2 is the preparation process schematic diagram of membrane electrode master unit.
Fig. 3 is the sem photograph (SEM) of membrane electrode master unit.
Fig. 4,5,6,7 is respectively embodiment 2 and 1, embodiment 3, embodiment 4, embodiment 5 mea are dressed up the V-I curve chart behind the monocell.
Number in the figure implication: first-master unit, second-sub-cell, the 1-gas diffusion layers, 2-catalyst layer, 3-proton exchange layer, the 4-catalyst layer, 5-gas diffusion layers, a-are substrate with the gas diffusion layers, and b-coating catalyst slip in substrate prepares catalyst layer, c-is at catalyst layer top casting proton exchange resins formulations prepared from solutions proton exchange layer, and d-coating catalyst slip on proton exchange layer prepares catalyst layer.
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
The preparation of membrane electrode master unit.Through the compound inferior hydrophobic layer of forming by conductive carbon black and polytetrafluoroethylene (PTFE) particle of carbon paper one side of hydrophobic treatment, under 350 ℃, calcine 20min, make gas diffusion layers.According to carbon supported platinum catalyst: Nafion
The portions of resin isopropyl alcohol is that 3: 1: 300 mass ratio prepares catalyst slurry, and half slip is printed onto inferior hydrophobic layer (sublayer) side of gas diffusion layers with silk screen print method, and vacuumize 1-10h is hardened in the diffusion layer surface with catalyst layer.Get the Nafion solution of 5wt%, concentrate the volume of half after, be printed onto the catalyst layer surface of sclerosis with silk screen print method, vacuumize 1-10h forms fine and close proton exchange layer on catalyst layer.The catalyst slurry of remainder is printed onto on the proton exchange layer with silk screen print method, and vacuumize 1-10h, catalyst layer are hardened in the surface of proton exchange layer.The average thick about 4-5 μ m of catalyst layer of preparation, the about 30 μ m of proton exchange bed thickness, the Pt carrying capacity is 0.6mg/cm
2(each 0.3mg/cm of cathode and anode catalyst layer wherein
2).The surface characteristics of membrane electrode master unit is seen accompanying drawing 3.
Getting a gas diffusion layers identical with master unit is sub-cell, and membrane electrode master unit and sub-cell cold joint are touched, and promptly gets the unit-combination type membrane electrode.The unit-combination type membrane electrode is assembled into monocell with assemblies such as Teflon seal washer, graphite collector plate, copper facing stainless-steel sheets.Effective catalysis area of monocell is 5cm * 5cm, and operating condition is: back pressure P
Air=P
Hydrogen=0Mpa, 80 ℃ of battery temperatures, anode 100% humidification, the humidification temperature is 70 ℃.The V-I curve of monocell is seen accompanying drawing 4.
Embodiment 2
The preparation method of membrane electrode master unit and monocell assembling are identical with embodiment 1 with test condition, and different is not have the compound inferior hydrophobic layer of being made up of conductive carbon black and polytetrafluoroethylene (PTFE) particle as the gas diffusion layers of membrane electrode master unit and the gaseous diffusion laminar surface of sub-cell.The V-I curve of monocell is seen accompanying drawing 4.Be not difficult to find out, as current density＞0.7A/cm
2The time, overpotential will be higher than embodiment 1.
Embodiment 3
The assembling of the preparation method of membrane electrode master unit, sub-cell material and monocell is identical with embodiment 1 with test condition, and the thickness of different is proton exchange layer is 60 μ m.The V-I curve of monocell is seen accompanying drawing 5.Be not difficult to find out, when current density is 0.7-0.2A/cm
2The time, overpotential is greater than embodiment 1.
Embodiment 4
The preparation method of membrane electrode master unit, sub-cell material and monocell assembling are identical with embodiment 1 with test condition, and different is, the thickness of cathode catalyst layer is 4 μ m, and the Pt carrying capacity is 0.4mg/cm
2, the thickness of cathode catalyst layer is 2 μ m, the Pt carrying capacity is 0.2mg/cm
2The V-I curve of monocell is seen accompanying drawing 6.
Embodiment 5
The preparation method of membrane electrode master unit, sub-cell material and monocell assembling are identical with embodiment 1 with test condition, and different is that master unit and sub-cell are by hot binding.Hot-pressing processing condition: 120 ℃ of temperature, pressure 0.2MPa, time 90s.The V-I curve of monocell is seen accompanying drawing 7.Compare with embodiment 1, after the hot pressing, the electric output performance of battery has certain improvement.
Claims (5)
1, a kind of membrane electrode of fuel batter with proton exchange film, it is characterized in that membrane electrode is combined by master unit and sub-cell, membrane electrode for unit-combination type, described master unit is the membrane-electrode unit that is formed by the common bonding of gas diffusion layers, catalyst layer and proton exchange layer, its composition or structure are followed successively by gas diffusion layers, catalyst layer, proton exchange layer, catalyst layer, and described sub-cell is a gas diffusion layers.
2, membrane electrode according to claim 1, the gas diffusion layers that it is characterized in that membrane electrode master unit and sub-cell is porous carbon paper or carbon cloth through hydrophobic treatment, can the compound more inferior hydrophobic layer of being made up of carbon black and polytetrafluoroethylgranule granule through a side of the porous carbon paper of hydrophobic treatment or carbon cloth.
3, membrane electrode according to claim 1 is characterized in that the master unit catalyst layer mainly carries platinum or platinum alloy carbon-supported catalysts and proton exchange resins by platinum or platinum alloy or carbon and forms, and the mass ratio of catalyst and proton exchange resins is 10: 2～5.
4, membrane electrode according to claim 1, the proton exchange layer that it is characterized in that master unit is made up of the resin with proton exchange function, described proton exchange resins is meant the perfluorinated sulfonic resin with sulfonic acid group, as the Nafion resin or the Nafion solution of du Pont company production, or sulfonation thermal stability polymer, Flemion proton conductor polymer with proton exchange function.
5, the described membrane electrode preparation method of claim 1, its preparation process is as follows:
(1) catalyst, proton exchange resins are mixed by 10: 2～5: 100～1500 mass ratio is full and uniform with solvent, make catalyst slurry or prepared Chinese ink, described solvent is meant water or alcohol, ether, ester, ketone or nitrile, wherein alcohol is methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, glycerol, 1-methoxyl group 2-propyl alcohol, ether is ether, benzinum, and ester and ketone are ethyl acetate and acetone;
(2) the part catalyst slurry that step (1) is obtained is coated to a side of gas diffusion layers, and vacuumize forms catalyst layer;
(3) with the proton exchange resins solution-cast to catalyst layer, vacuumize forms proton exchange layer;
(4) the remaining catalyst slurry that step (1) is obtained is coated on the proton exchange layer of step (3) formation, and vacuumize forms the membrane electrode master unit;
(5) the membrane electrode master unit of preparation is close to or hot pressing by contact with the sub-cell of being made up of gas diffusion layers, is made unit-combination type membrane electrode of the present invention.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410013149XA CN1324739C (en) | 2004-05-14 | 2004-05-14 | Unit combined fuel cell membrane eletrode and its preparing method |
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|---|---|---|---|
| CNB200410013149XA CN1324739C (en) | 2004-05-14 | 2004-05-14 | Unit combined fuel cell membrane eletrode and its preparing method |
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| CN1581548A true CN1581548A (en) | 2005-02-16 |
| CN1324739C CN1324739C (en) | 2007-07-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101841042B (en) * | 2009-03-16 | 2013-03-20 | 黄炳照 | Electrode layer of fuel cell and method of fabricating the same |
| CN108950587A (en) * | 2018-07-09 | 2018-12-07 | 国家电网有限公司 | A kind of high surface area solids polymer membrane electrode and preparation method thereof |
| CN109473706A (en) * | 2018-12-12 | 2019-03-15 | 上海懋乐新材料科技有限公司 | The electrode assembly and preparation method thereof of one proton exchanging film fuel battery |
| CN111180744A (en) * | 2018-11-09 | 2020-05-19 | 本田技研工业株式会社 | Method for forming gas diffusion layer on carbon paper and carbon paper with gas diffusion layer |
| CN112968199A (en) * | 2019-12-14 | 2021-06-15 | 中国科学院大连化学物理研究所 | Integrated membrane electrode for fuel cell and preparation and application thereof |
| CN114188551A (en) * | 2021-11-12 | 2022-03-15 | 江苏大学 | Preparation method of platinum-palladium alloy catalyst growing on gas diffusion layer in situ and application of platinum-palladium alloy catalyst to fuel cell electrode |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1276633A (en) * | 2000-07-27 | 2000-12-13 | 钟家轮 | Fuel cell with more membrane electrodes on one membrane and its preparing process |
| JP2002184428A (en) * | 2000-12-11 | 2002-06-28 | Toyota Motor Corp | Fuel cell |
| CN1405915A (en) * | 2001-08-16 | 2003-03-26 | 亚太燃料电池科技股份有限公司 | Module element of proton exchange film fuel cell and moudule cell unit |
| TW200306031A (en) * | 2002-01-22 | 2003-11-01 | Du Pont | Unitized membrane electrode assembly and process for its preparation |
| CN1492530A (en) * | 2002-10-24 | 2004-04-28 | 江苏隆源双登电源有限公司 | Process for producing fuel cell film electrode |
-
2004
- 2004-05-14 CN CNB200410013149XA patent/CN1324739C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101841042B (en) * | 2009-03-16 | 2013-03-20 | 黄炳照 | Electrode layer of fuel cell and method of fabricating the same |
| CN108950587A (en) * | 2018-07-09 | 2018-12-07 | 国家电网有限公司 | A kind of high surface area solids polymer membrane electrode and preparation method thereof |
| CN111180744A (en) * | 2018-11-09 | 2020-05-19 | 本田技研工业株式会社 | Method for forming gas diffusion layer on carbon paper and carbon paper with gas diffusion layer |
| CN109473706A (en) * | 2018-12-12 | 2019-03-15 | 上海懋乐新材料科技有限公司 | The electrode assembly and preparation method thereof of one proton exchanging film fuel battery |
| CN112968199A (en) * | 2019-12-14 | 2021-06-15 | 中国科学院大连化学物理研究所 | Integrated membrane electrode for fuel cell and preparation and application thereof |
| CN114188551A (en) * | 2021-11-12 | 2022-03-15 | 江苏大学 | Preparation method of platinum-palladium alloy catalyst growing on gas diffusion layer in situ and application of platinum-palladium alloy catalyst to fuel cell electrode |
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| CN1324739C (en) | 2007-07-04 |
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