CN1167832C - Preparation of three-in-one thin-layer hydrophobic catalyst electrode and membrane electrode assembly - Google Patents

Preparation of three-in-one thin-layer hydrophobic catalyst electrode and membrane electrode assembly Download PDF

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CN1167832C
CN1167832C CNB991128265A CN99112826A CN1167832C CN 1167832 C CN1167832 C CN 1167832C CN B991128265 A CNB991128265 A CN B991128265A CN 99112826 A CN99112826 A CN 99112826A CN 1167832 C CN1167832 C CN 1167832C
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membrane electrode
preparation
electrode
electrode assembly
catalyst
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CN1269429A (en
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邵志刚
衣宝廉
韩明
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SHANGHAI SUNRISE POWER CO Ltd
Sunrise Power Co Ltd
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DALIAN XINYUAN POWER Co Ltd
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Abstract

The present invention relates to a preparation method of a thin layer hydrophobic catalyst layer electrode and a three-in-one membrane electrode assembly. A catalyst is prepared into ink to be directly or indirectly brushed and printed on a proton membrane to form the three-in-one membrane electrode. The ink comprises 10 portions of catalyst, 100 to 500 portions of solvent formed by mixing water and organic solvent, 1 to 10 portions of Nafion or Flemion proton conductor polymer, 10 to 50 portions of common pore forming agent or common soluble pore forming agent which can be easily volatilized and 1 to 10 portions of hydrophobic agent, for example, PTFE, wherein the volume ratio of the water to the organic solvent is 1: (1 to 10). The electrodes have the advantages of simple preparation processes, firm combination, good properties, long service life and low cost.

Description

The preparation method of thin-layer hydrophobic catalyst electrode, three-in-one membrane electrode assembly
The present invention relates to the technology of preparing of three-in-one membrane electrode assembly.
Document 1 USP 4738741 has introduced a kind of making method of membrane electrode of electrolysis purposes, at first catalyzer and proton conductor mixed with polymers are coated on the wire netting, form Catalytic Layer, by hot pressing Catalytic Layer is transferred on the ionic membrane then, it is three-in-one to form membrane electrode.Document 2 USP 5211984 have introduced a kind of preparation method of membrane-membrane electrode for fuel cell, the proton conductor mixed with polymers of catalyzer and sodium typeization is coated on the polytetrafluoroethylene (PTFE) film, form Catalytic Layer, by hot pressing Catalytic Layer is transferred on the proton film such as Nafion again, it is three-in-one that protonated again back forms membrane electrode.Document 3 USP 5415888, document 4 USP 5547911 have introduced a kind of preparation method of membrane-membrane electrode for fuel cell, catalyzer is made ink brush to print on the proton films such as Nafion, the formation membrane electrode is three-in-one, ink composition comprises 1) catalyzer, 2) organic solvents such as ether, epoxy formula ketone series, alcohol, 3) the proton conductor polymkeric substance.Document 5 USP 5712755 have also introduced a kind of preparation method of membrane-membrane electrode for fuel cell, catalyzer is made ink brush to print on the proton films such as Nafion, the formation membrane electrode is three-in-one, ink composition comprises 1) catalyzer, 2) pKa＞18, the organic solvent of β＜0.66,3) the proton conductor polymkeric substance.
The object of the present invention is to provide the preparation method of a kind of thin-layer hydrophobic catalyst electrode, three-in-one membrane electrode assembly, its electrode production process is simple, and in conjunction with firm, electrode performance is good, and the life-span is long and cost is lower.
The invention provides the preparation method of a kind of thin-layer hydrophobic catalyst electrode, three-in-one membrane electrode assembly, is catalyzer to be made ink stencil directly or indirectly on the proton film that to form membrane electrode three-in-one, it is characterized in that ink composition comprises:
(1) catalyzer;
(2) solvent that mixes by water and organic solvent, wherein organic solvent is selected from one or more of acetonitrile, ether, epoxy formula ketone series, alcohol, and water is 1: 1～10 with the volume of organic solvent ratio;
(3) Nafion (du pont company) or Flemion (Japanese Asahi Glass company) proton conductor polymkeric substance;
(4) easy evaporable pore-forming material bicarbonate of ammonia, ammonium oxalate or solubility pore-forming material sodium-chlor, Repone K, Quilonum Retard;
(5) hydrophobizing agent PTFE;
It is catalyzer that the part by weight of above-mentioned substance closes: solvent: proton conductor polymkeric substance: pore-forming material: hydrophobizing agent=10: 100～500: 1～10: 10～50: 1～10.
When the present invention is used as fuel cell, can select metals such as Pt, Pd, Ru, Rh, Ir or its carbon supported catalyst Pt/C, Pd/C, Ru/C, Rh/C etc. for use; During as electrolysis, can select metal Ir, Rh or metal oxide RuO for use 2, IrO 2, RhO 2Deng, for improving its electroconductibility, can add metals such as a certain proportion of Pt, Pd; During as reversible regenerable fuel cell double-effect membrane electrode, can select the platinum metals and the oxide catalyst thereof of different ratios for use.During as reversible regenerable fuel cell double-effect membrane electrode, the weight ratio of platinum metals and its oxide compound is 1/3～3.Employing contains carbon paper that hydrophobizing agent such as PTFE handles or the carbon cloth diffusion layer as electrolysis electrode, economic benefits and social benefits electrode.During as electrolysis, the content of PTFE is 5%～30%; During as the reversible regenerable fuel cell membrane electrode, the content of PTFE is 10%～30%.
The present invention has following characteristics:
1. add pore-forming material in the membrane electrode preparation, help the formation of micropore in the Catalytic Layer, can increase the porosity of Catalytic Layer, help the diffusion of gas.During as electrolysis electrode, the gas that produces on the catalyst activity position can spread out soon, prevents that Catalytic Layer from coming off from film; During as fuel cell electrode, the reactant gases of outside can be diffused on the catalyst activity position smoothly, improves electrode performance.
2. add hydrophobizing agents such as PTFE in the membrane electrode preparation, help in pole catalyze layer, forming gas passage, help the diffusion in Catalytic Layer of reactant gases or product gas, thereby it is thicker that pole catalyze layer can be made, and Catalytic Layer thickness can be far longer than common hydrophilic electrode Catalytic Layer thickness (10 μ m).
3. select different catalysts for use, can be made into the membrane electrode of different purposes.Different with the membrane electrode of the described special purpose of front document, the inventive method can be made multi-purpose membrane electrode.
4. in order to make the equally distributed ink of catalyzer, help the dissolving of pore-forming material, the present invention with an organic solvent with the mixture of water as solvent, make made ink more approach colloid.For solubilizing hydrophobic agent simultaneously and hydrophilizing agent as: Nafion and PTFE, the present invention adopt a kind of new organic solvent-acetonitrile.It is to proton conductor polymkeric substance Nafion, and hydrophobizing agent PTFE can both form colloid.
5. according to the different purposes of membrane electrode, use different diffusion layers.
The present invention saves the use of wire netting with document 1 hydrophobizing agents such as using pore-forming material, PTFE of comparing, and electrode production process is simple, and hot pressing temperature, pressure can increase, and membrane electrode is in conjunction with more firm.Compare with document 2, the present invention uses hydrophobizing agents such as pore-forming material, PTFE, can make the thin-layer hydrophobic catalyst electrode.Because the electrode according to document 2 preparations is hydrophilic Catalytic Layer electrode, does not have gas passage in the Catalytic Layer, is unfavorable for the diffusion of reactant gases, the thickness of Catalytic Layer can not be greater than 10 μ m.The present invention helps the diffusion of gas in Catalytic Layer owing to introduce gas passage in Catalytic Layer, and catalyst utilization improves, and electrode performance improves.The Catalytic Layer thickness of electrode can be greater than 10 μ m, and electrode is difficult for losing efficacy ILS.Compare with document 3,4,5, the present invention adopts water and organic solvent to make solvent, and the Catalytic Layer that makes is more even, and can reduce the organic solvent usage quantity, helps reducing the electrode manufacturing cost.The present invention uses hydrophobizing agents such as pore-forming material, PTFE, introduces gas passage in Catalytic Layer, helps the diffusion of gas in Catalytic Layer, has increased the utilization ratio of catalyzer, and electrode performance is improved.And compare with document 1,2,3,4,5, the present invention not only can make membrane-membrane electrode for fuel cell, and can make electrolysis membrane electrode, regenerative fuel cell economic benefits and social benefits membrane electrode.
In a word, the present invention has following advantage:
1. add pore-forming material in the membrane electrode preparation, can increase the porosity of pole catalyze layer, save the use of wire netting, electrode production process is simple, and hot pressing temperature, pressure can increase, and membrane electrode is in conjunction with more firm.
2. add hydrophobizing agents such as PTFE in the membrane electrode preparation, can increase the gas passage in the pole catalyze layer, help the diffusion of gas in Catalytic Layer, increased the utilization ratio of catalyzer, improve electrode performance.
3. according to different needs, can be made into multi-purpose three-in-one membrane electrode assembly.
4. the present invention can make the electrode of Catalytic Layer thickness greater than 10 μ m, compares with the thin layer hydrophilic electrode, and electrode is difficult for losing efficacy, and the life-span prolongs.
5. adopt water and organic solvent to make solvent, the Catalytic Layer that makes is more even, and can reduce the organic solvent usage quantity, helps reducing the electrode manufacturing cost.
6. adopt porous carbon paper that hydrophobizing agent such as PTFE handled or carbon cloth electrolysis as electrode diffusion layer, lower than metal costs such as the porous sintered titaniums of use.
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 is to add PTFE in the electrode preparation to the electrolysis performance impact, Nafion 115 films, 80 ℃.
Accompanying drawing 2 is that the battery performance that adds pore-forming material in the electrode preparation compares 0.08mg/cm 2Pt/C, S=5cm 2, Nafion 115, P H2=P O2=0.3MPa, 80 ℃.
Accompanying drawing 3 is for adding the influence of PTFE to catalyst utilization in the membrane electrode preparation.
Accompanying drawing 4 is a reversible regenerable fuel cell double-effect electrode performance, fuel cell pattern: P O2=0.3MPa, P H2=0.3MPa, 80 ℃, Nafion 115; Electrolysis mode: normal pressure, 80 ℃, Nafion 115; Cycle index: 1,2,3,4.
Embodiment 1a
At first take by weighing 0.1 gram XC-72 carbon dust with the one-level balance, add the PTFE of 20wt%, add 30ml ethanol again, vibration is 30 minutes in ultrasonic wave, and after mixing, 70 ℃ of oven dry in vacuum drying oven are burnt 20min 340 ℃ of bakings then, and it is stand-by to mill after the cooling.Take by weighing 1.76 milligrams of catalyst Pts, IrO with the one-level balance 22.50 milligram, 5 milligrams of the above-mentioned PTFE XC-72 carbon dusts that contains 20wt% for preparing add the mixture (volume ratio 1: 1) of entry and acetonitrile, and vibration is 15 minutes in the ultrasonic wave, add the Nafion solution of 80mg 5% then, 5mg (NH 4) 2C 2O 4, the NaOH solution of 300mg 0.5M, vibration is 45 minutes in ultrasonic wave, after mixing, is applied to 10cm 2The PTFE film on, 70 ℃ of oven dry in vacuum drying oven are divided into two 5cm then 2The PTFE film, between them, sandwich Nafion 115 films of a sodium ionization, Catalytic Layer is towards the proton film, about 180 ℃, under 5～9MPa condition, hot pressing 1.5min, then the PTFE film is peeled off, in the sulfuric acid of 0.5M, made film and Catalytic Layer protonated again, make three-in-one membrane electrode assembly.Diffusion layer adopts the carbon paper contain PTFE 20wt%, is assembled into electrolyzer with two stainless steel clamping plate, carries out Electrolytic Water Experiment under 80 ℃, normal pressure.The electrolysis performance is seen Fig. 1.
Embodiment 1b
Making method is with routine 1a, unique different be not add the PTFE XC-72 carbon dust that contains 20wt% in the preparation process, experimental result is seen Fig. 1.
Embodiment 2a
Make three-in-one membrane electrode assembly according to document 2.Take by weighing 5 milligrams of catalyst Pt/C (platinum content is 20%) with the one-level balance equally, add a certain amount of 5% Nafion solution then, a certain amount of glycerine, the weight ratio that makes Nafion/ catalyzer/glycerine is 1: 3: 20, after the ultrasonic wave mixing, add the 0.5M NaOH aqueous solution, make the H among the Nafion +Be converted into Na +Type is coated on the PTFE film then, then 135 ℃ of dry 2h in vacuum drying oven.Again two PTFE films that have a Catalytic Layer and one 's sodium ionization Nafion film about 180 ℃, under 5～9MPa condition, hot pressing 1.5min has obtained a three-in-one membrane electrode assembly.Then at 0.5M H 2SO 4In boil, protonated again.Diffusion layer adopts the carbon paper contain PTFE 50wt%, is assembled into battery with two stainless steel clamping plate, is that 80 ℃, hydrogen-oxygen pressure are 0.3MPa at battery temperature, and oxyhydrogen humidification temperature is to carry out the fuel cell experiment under 90 ℃ the condition.Battery performance is seen Fig. 2.
Embodiment 2b
Take by weighing 5 milligrams of catalyst Pt/C (platinum content is 20%) with the one-level balance, add the mixture (volume ratio is 1: 1) of entry and acetonitrile, vibration is 15 minutes in the ultrasonic wave, adds the Nafion solution of 25mg 5% then, 5mg (NH 4) 2C 2O 4, the NaOH solution of 100mg 0.5M, vibration is 45 minutes in ultrasonic wave, after mixing, is applied to 10cm 2The PTFE film on, 70 ℃ of oven dry in vacuum drying oven are divided into two 5cm then 2The PTFE film, between them, sandwich Nafion 115 films of a sodium ionization, Catalytic Layer is towards the proton film, about 180 ℃, under 5～9MPa condition, hot pressing 1.5min, then the PTFE film is peeled off, in the sulfuric acid of 0.5M, made film and Catalytic Layer protonated again, make three-in-one membrane electrode assembly.Diffusion layer adopts the carbon paper contain PTFE 50wt%, is assembled into battery with two stainless steel clamping plate, is that 80 ℃, hydrogen-oxygen pressure are 0.3MPa at battery temperature, and oxyhydrogen humidification temperature is to carry out the fuel cell experiment under 90 ℃ the condition.Battery performance is seen Fig. 2.
For estimating the catalyst utilization of electrode, carry out the cyclic voltammetry curve test of electrode.One side of electrode is fed hydrogen through humidification, and opposite side feeds the argon gas through humidification, and with surveying as reference electrode and counter electrode of feeding hydrogen, a side that feeds argon gas is carried out the test of the cyclic voltammetry curve of electrode as working electrode.Test result such as Fig. 3.
Embodiment 2c
Making method is with routine 2b, unique different be to add the PTFE XC-72 carbon dust 2mg that contains 20wt% in the preparation process, carry out the mensuration of electrode cyclic voltammetry curve, condition is with routine 2b.Experimental result such as Fig. 3.
Add PTFE in the electrode preparation as can be seen from Figure 3, the adsorption peak area of hydrogen is increased, the utilization ratio of catalyzer improves.
Embodiment 3
Take by weighing catalyst Pt 2mg, IrO with the one-level balance 22mg, 2 milligrams of PTFE XC-72 carbon dusts add the mixture (volume ratio 1: 1) of entry and acetonitrile, and vibration is 15 minutes in the ultrasonic wave, adds the Nafion solution of 24mg 5% then, 4mg (NH 4) 2C 2O 4, the NaOH solution of 100mg 0.5M, vibration is 45 minutes in ultrasonic wave, after mixing, is applied to 10cm 2The PTFE film on, 70 ℃ of oven dry in vacuum drying oven are divided into two 5cm then 2The PTFE film, between them, sandwich Nafion 115 films of a sodium ionization, Catalytic Layer is towards the proton film, about 180 ℃, under 5～9MPa condition, hot pressing 1.5min, then the PTFE film is peeled off, in the sulfuric acid of 0.5M, made film and Catalytic Layer protonated again, make three-in-one membrane electrode assembly.Diffusion layer adopts the carbon paper that contains PTFE 30wt%, is assembled into battery with two stainless steel clamping plate, carries out the experiment of reversible regenerable fuel cell double-effect electrode performance then.When working in the fuel cell mode, battery temperature is that 80 ℃, hydrogen-oxygen pressure are 0.3MPa, and oxyhydrogen humidification temperature is 90 ℃; When working, under 80 ℃, normal pressure, carry out Electrolytic Water Experiment with electrolysis mode.The economic benefits and social benefits performance of membrane electrode is seen Fig. 4.

Claims (6)

1. the preparation method of a thin-layer hydrophobic catalyst electrode, three-in-one membrane electrode assembly is catalyzer to be made ink stencil directly or indirectly that to form membrane electrode on the proton film three-in-one, it is characterized in that ink composition comprises:
(1) catalyzer;
(2) solvent that mixes by water and organic solvent, wherein organic solvent is selected from one or more of acetonitrile, ether, epoxy formula ketone series, alcohol, and water is 1: 1～10 with the volume of organic solvent ratio;
(3) Nafion or Flemion proton conductor polymkeric substance;
(4) easy evaporable pore-forming material bicarbonate of ammonia, ammonium oxalate or solubility pore-forming material sodium-chlor, Repone K, Quilonum Retard;
(5) hydrophobizing agent PTFE;
It is catalyzer that the part by weight of above-mentioned substance closes: solvent: proton conductor polymkeric substance: pore-forming material: hydrophobizing agent=10: 100～500: 1～10: 10～50: 1～10.
2. according to the preparation method of the described thin-layer hydrophobic catalyst electrode of claim 1, three-in-one membrane electrode assembly, it is characterized in that: when being used as fuel cell, can select metal Pt, Pd, Ru, Rh, Ir or carbon supported catalyst Pt/C, Pd/C, Ru/C, Rh/C for use.
3. according to the preparation method of the described thin-layer hydrophobic catalyst electrode of claim 1, three-in-one membrane electrode assembly, it is characterized in that: during as electrolysis, select metal Ir, Rh or metal oxide RuO for use 2, IrO 2, RhO 2
4. according to the preparation method of the described thin-layer hydrophobic catalyst electrode of claim 3, three-in-one membrane electrode assembly, it is characterized in that: add Pt, Pd metal in the catalyzer.
5. according to the preparation method of the described thin-layer hydrophobic catalyst electrode of claim 1, three-in-one membrane electrode assembly, it is characterized in that: during as reversible regenerable fuel cell double-effect membrane electrode, can select the platinum metals and the oxide catalyst thereof of different ratios for use, the weight ratio of platinum metals and its oxide compound is 1/3～3.
6. according to the preparation method of claim 1,2,3,4 or 5 described thin layer hydrophobic catalyst electrodes, three-in-one membrane electrode assembly, it is characterized in that: solvent is selected the mixture of water and acetonitrile for use, water: acetonitrile=1: 1～3 volume ratios.
CNB991128265A 1999-04-07 1999-04-07 Preparation of three-in-one thin-layer hydrophobic catalyst electrode and membrane electrode assembly Expired - Fee Related CN1167832C (en)

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Publication number Priority date Publication date Assignee Title
US7318972B2 (en) * 2001-09-07 2008-01-15 Itm Power Ltd. Hydrophilic polymers and their use in electrochemical cells
US20050014056A1 (en) 2003-07-14 2005-01-20 Umicore Ag & Co. Kg Membrane electrode unit for electrochemical equipment
CN100375320C (en) * 2004-09-01 2008-03-12 中国科学院大连化学物理研究所 Proton exchange membrane fuel cell multi-layer membrane electrode structure and its preparing method
ATE501221T1 (en) * 2004-11-10 2011-03-15 Toyo Boseki COMPOSITION CONTAINING PROTON CONDUCTING POLYMER AND PRODUCTION METHOD THEREOF, CATALYST INK CONTAINING THE COMPOSITION CONTACTING PROTON CONDUCTING POLYMER, AND FUEL CELL CONTAINING THE CATALYST
CN101463487B (en) * 2007-12-17 2010-06-09 中国电子科技集团公司第十八研究所 Preparation of proton exchange membrane electrode for electrolyzing water
CN101728542B (en) * 2008-10-10 2012-06-20 中国科学院大连化学物理研究所 Method for preparing thin hydrophobisation layer
CN102447116B (en) * 2010-12-31 2013-11-20 山东理工大学 Preparation method for membrane electrode
CN109346728A (en) * 2018-09-25 2019-02-15 中新国际联合研究院 Non-precious Metal Catalysts electrode, membrane electrode and preparation method thereof
CN110190310B (en) * 2019-05-16 2022-08-12 华南理工大学 Method for improving durability of fuel cell catalyst and membrane electrode
CN110336042B (en) * 2019-07-05 2023-06-30 中国科学院重庆绿色智能技术研究院 Gas diffusion cathode and preparation method and application thereof
CN110729494A (en) * 2019-10-30 2020-01-24 无锡威孚高科技集团股份有限公司 Catalyst slurry for proton exchange membrane fuel cell and preparation method thereof

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