CN100486006C - Production method of membrane electrode of proton-exchange membrane fuel battery - Google Patents
Production method of membrane electrode of proton-exchange membrane fuel battery Download PDFInfo
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- CN100486006C CN100486006C CNB200510047984XA CN200510047984A CN100486006C CN 100486006 C CN100486006 C CN 100486006C CN B200510047984X A CNB200510047984X A CN B200510047984XA CN 200510047984 A CN200510047984 A CN 200510047984A CN 100486006 C CN100486006 C CN 100486006C
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Abstract
The invention is concerned with the film electrode preparation method for the proton exchanging film fuel battery, it is: the organic multi-hole film is the electrode supporter, the thickness of the multi-hole film is 1-20 mu meter, the hole rate is 50%-99%, adheres the activator to the multi-hole film directly, prepares the electrode catalyzing layer; combines the catalyzing layer and the electrolyzing film to be the film electrode groupware by heat pressure. The activator of the invention is high using rate, better active, higher intensity.
Description
Technical field
It is three-in-one to the present invention relates to the used in proton exchange membrane fuel cell membrane electrode, the method for preparing membrane electrode of a proton exchanging film fuel battery specifically, it uses porous membrane as supporter, the mixture of eelctro-catalyst and proton conductor is prepared into formation electrode activity layer on the film, then it and dielectric film is gathered the method that becomes MEA.
Background technology
Fuel cell is a kind of Blast Furnace Top Gas Recovery Turbine Unit (TRT) that chemical energy in fuel and the oxidant is converted into electric energy by the electrocatalytic reaction on the electrode.It is not subjected to the restriction of Carnot cycle, can efficiently chemical energy be converted into electric energy.So far people have developed the fuel cell of five types of alkalescence, phosphatic type, fused carbonate type, high-temperature solid electrolyte type and proton exchange models etc.Wherein Proton Exchange Membrane Fuel Cells (Proton Exchange Membrane Fuel Cell is called for short PEMFC) has wide application prospect, its energy cold-starting, and no electrolyte corrosion and leakage, simple in structure, easy to operate; Be acknowledged as electric automobile, regional power station, portable power supply, submarine, spacecraft etc. the first-selected energy (document 1: the clothing treasured is honest and clean. fuel cell-efficient, eco-friendly generation mode. Beijing: Chemical Industry Press, 2000.).
Membrane electrode three-in-one (Membrane electrode assembly) is the core component of Proton Exchange Membrane Fuel Cells, and its performance quality directly influences the performance and the stability of battery.
United States Patent (USP) (document 2:US 5211984) has been described the manufacture method of a proton exchanging film fuel battery.The Catalytic Layer of this battery is very thin, between the electrode bottom of solid electrolyte (SPE) and porous.The thickness of Catalytic Layer is less than 10 μ m, and the load amount of carrier platinum catalyst is less than 0.35mg/cm
2Catalyst feed is formulated into printing ink and is sprayed on the film to be transferred, solidifies then, and the Catalytic Layer after the curing is transferred on the proton film and is hot pressed into membrane electrode.In addition, Catalytic Layer can adopt Na
+The perfluorosulfonic acid ionomer accomplish directly on the proton film that high temperature drying converts H again to then
+Type.This Catalytic Layer has enough gas passages to make that battery performance does not descend under the condition of low platinum load amount.
European patent (document 3:EP 1318559 A2) has been described the manufacture method of a kind of membrane electrode assembly (MEA).This MEA is made of polymer dielectric film and negative electrode (being made up of Catalytic Layer and gas diffusion layers), anode (being made up of Catalytic Layer and gas diffusion layers).Catalytic Layer is between film and gas diffusion layers.Negative electrode or anode catalyst layer comprise two sublayers at least.In this patent, negative electrode or anode catalyst layer have at least a sublayer directly to be implemented on the film, and remaining sublayer is implemented on the corresponding gas diffusion layers.To smear the film of Catalytic Layer at last and smear the gas diffusion layers assembling MEA of Catalytic Layer.In this piece patent, there is not the description of aspect of performance.
United States Patent (USP) (document 4:US 2003/0224233 A1) has been described the manufacture craft of a proton exchanging film fuel battery (PEMFC) MEA, exactly, is the laminating technology of MEA, and this technology has simply, characteristics efficiently.This MEA structure that is of five storeys, 5 layer MEAs contain bonded assemblies and press together by laminating.Anode gas diffusion layer, membrane electrode and cathode gas diffusion layer are pressed onto together in the condition lower floor of low-temp low-pressure. and this has simplified the processing of MEA and the assembling of pile.And membrane electrode is damaged because of hot pressing or the phenomenon of boring a hole has reduced, and the performance of MEA is improved.
Summary of the invention
The object of the present invention is to provide the method for preparing membrane electrode of a proton exchanging film fuel battery. it is electrode support with the organic porous films, directly affact electroactive substance on the supporter, making the electrode activity layer is an independently assembly, this structure had both helped the preparation of electrode, also help active layer is modified, increase its function.
For achieving the above object, the technical solution used in the present invention is:
A kind of method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells, it is characterized in that: be electrode support with the organic porous films, perforated membrane thickness is 1～20 μ m, and porosity is 50%～99%, catalyst feed is directly adhered on the perforated membrane preparation pole catalyze layer; This Catalytic Layer and dielectric film are combined into membrane electrode assembly by means such as hot pressing.
Described organic porous films is polytetrafluoroethylene, inclined to one side tetrafluoroethene, polypropylene, polyethylene, polyimides or polysulfones perforated membrane etc.; Catalyst feed is the mixture of eelctro-catalyst and proton conductive resin, catalyst concentration can also can be the black or black catalyst of PtRu of Pt for 10%～80% Pt/C or PtRu/C catalyst, proton conductor solution (for example perfluorinated sulfonic resin), mixed proportion is a catalyst: resin solution is 10:1～1:1; Eelctro-catalyst can be the black or black catalyst of PtRu of Pt/C, PtRu/C, the Pt of weight content 10～80%; Proton conductor is the material with proton conduction function with the perfluorinated sulfonic resin class; Catalyst feed directly adheres to and is meant on the perforated membrane that catalyst feed can be prepared on the perforated membrane by means such as spraying, blade coating or printings;
The pore creating material that can add its weight 10-90% in the described catalyst feed, described pore creating material for can mix with the catalyst feed liquid, 100～300 ℃ can decompose volatilization, and can in Catalytic Layer, form the material of pore structure, as ammonium oxalate, ammonium carbonate, pyrazolone, histamine, n-valeramide, hexamethylene diamine, pyrrolidones, urea or lower alcohol etc.; Can also add in the catalyst feed its weight 1-50% have absorbent function from humidizer (hygroscopic agent), then prepared active layer has better moisture-retaining capacity, if add the Pt catalyst, under the Pt catalyst action, 2H reacts
2+ O
2→ 2H
2O makes MEA have self-moistening function; Described is silicon dioxide, titanium dioxide, water-absorbing resin or sulfonation organic substance from humidizer; What add in the catalyst feed can be used as the carrier that supports fuel cell eelctro-catalyst commonly used from humidizer, and the eelctro-catalyst as Pt, Ru and PtRu etc. have electro-chemical activity has from humidification MEA;
Described catalyst feed adheres on the perforated membrane, after the perforated membrane that has catalyst feed of preparation is shaped, need obtain pole catalyze layer through 120～320 ℃ processing procedure; Wherein perforated membrane can play the catalyst supporting role, form gas passage effect and the electrolytical multiple action of reinforcing membrane.
The technical solution used in the present invention has been compared following characteristics with aforesaid background technology:
1) patent US5211984 A adopts transfer method to prepare electrode, and active layer is prepared on the film electrolyte, and technology is numerous and diverse, and repeatability is relatively poor, damage the film electrolyte easily, and manufacturing cycle is long, is not suitable for commercially producing.In the electrode preparation method of the present invention, catalyst feed prepares easily, and operation is simple, and manufacturing cycle is short, the favorable repeatability of production, and battery is easy to assembly, possesses the condition of commercially producing.
2) patent US 2003/0224233 A1 and patent EP 1318559 A2 directly are prepared into Catalytic Layer on the film, then by adhesive and low pressure combined method combination MEA, active layer can't independently prepare, among the present invention active layer is prepared as independent assembly, rather than directly accomplish on the film electrolyte, avoided in the operation injury that may cause the film electrolyte, supporting the perforated membrane and the dielectric film of active layer simultaneously combines closely, both improve the MEA performance, played the humidification of electrolyte strength again.
The present invention has following advantage:
1. the present invention is electrode support with the organic porous films, and the electrode activity layer is an independently assembly, and this structure had both helped the preparation of electrode; In the independent preparation process of active layer, can add composition, improve the MEA performance, can realize self-moistening function, add the environmental suitability that anti-impurity catalyst can improve MEA as adding water absorbing agent with various functions.
2. the perforated membrane that supports active layer (being Catalytic Layer) can play the function that strengthens MEA.In the middle of the electrode for preparing is an organic porous films, and catalyst granules is distributed in the hole of film, has both helped catalyst feed and has evenly distributed, and helps electrochemical reaction again.
3. accomplish directly that with catalyst the electrode on the proton film compares, organic porous films can not resemble the Nafion film because of running into solvent swelling rapidly, has good dimensional stability, is convenient to make.
4.MEA middle catalyst utilization height.On gas diffusion layers, catalyst feed leaks in the hole of diffusion layer traditional method unavoidably, has both influenced the pore structure in the diffusion layer, has reduced the utilance of catalyst again with the Catalytic Layer preparation.And the present invention is when preparation electrode activity layer, and catalyst feed all is prepared on the organic porous films, has avoided the shortcoming of conventional method, has reduced the catalyst loading amount, has reduced cost when improving performance, possesses business-like condition; Prepare MEA by the inventive method, make MEA have better catalyst utilization, better intensity, be convenient to large-scale continuous production simultaneously, help the amplification production of MEA.
Advantages such as in a word, it is simple that technology of the present invention has technology, easy and simple to handle, and repeatability is strong can be produced in batches.
Description of drawings
Fig. 1 is the structural representation of MEA among the present invention; Wherein: 1 is cathode diffusion layer, and 2 are the cathodic protection frame, 3 adhesive sublayers, and 4 is anode diffusion layer, and 5 is cathode catalysis layer, and 6 is proton exchange membrane, and 7 is anode catalyst layer, 8 are the anodic protection frame;
Fig. 2 is the MEA volt-ampere curve of the embodiment of the invention 1;
Fig. 3 is the MEA volt-ampere curve of the embodiment of the invention 2;
Fig. 4 is the MEA volt-ampere curve of the embodiment of the invention 3.
Embodiment
Embodiment 1
1) polytetrafluoroethylporous porous membrane (porosity of film is 90%, and thickness is 5 μ m) with 5 μ m is cut into suitable dimensions, is placed in the alcohol solvent, places ultrasonic wave ultrasonic cleaning half an hour, repeats, and it is standby to carry out clean;
2) will contain the solution of 5% perfluorinated sulfonic resin (as Nafion) and the Pt/C catalyst of 70%WT and press Nafion: the ratio of catalyst=1:3 mixes. and the anode catalyst consumption is pressed 0.5mg/cm
2Calculate, the cathod catalyst consumption is pressed 0.3mg/cm
2Calculate, and add a certain amount of isopropyl alcohol.In order to allow catalyst feed evenly disperse in solution, it is big that the ratio of isopropyl alcohol is wanted, and adds in the ratio of catalyst: isopropyl alcohol=1:100:
3) use the ultrasonic wave mixed solution, catalyst feed is evenly spread in the solution, standby;
4) at the both sides of perforated membrane spraying skim bonding agent, as the mixture of Nafion and carbon dust;
5) catalyst feed is sprayed to a side of porous membrane electrode;
6) in opposite side repeating step (2)～(4) of film:
7) membrane electrode is dried 4h under 140 ℃ environment;
8) both sides that membrane electrode are placed on Nafion film precompressed 1min, hot pressing 1min under 160 ℃, the condition of 0.35MPa makes membrane electrode assembly;
9) both sides that diffusion layer and bearer bar are placed on membrane electrode precompressed 1min, hot pressing 1min under 160 ℃, the condition of 0.7MPa, preparation MEA.
The performance of this MEA is seen Fig. 1.As seen from Figure 1, under condition of normal pressure, reached 0.65V@500mA/cm
2
1) step 1) among the repetition embodiment one;
2) will contain the solution of 5% perfluorinated sulfonic resin (as Nafion) and the Pt/C catalyst of 70%WT and press Nafion: the ratio of catalyst=1:3 mixes, and the cathod catalyst consumption is pressed 0.75mg/cm
2Calculate, the anode catalyst consumption is pressed 0.75mg/cm
2Calculate, at the isopropyl alcohol of adding with embodiment one same ratio.
3) step (3)～(9) among the repetition embodiment one.
The performance of present embodiment MEA is seen Fig. 2.As seen from Figure 2, the performance of condition of normal pressure bottom electrode has reached 0.66V@500mA/cm
2, be better than the performance of embodiment 1 slightly.
Embodiment 3
1) step 1) among the repetition embodiment one;
2) press the step 2 of embodiment one) the preparation catalyst feed, add simultaneously catalyst feed total weight 10% from humidizer silicon dioxide, be uniformly dispersed;
3) step (3)～(9) among the repetition embodiment one.
The performance of present embodiment MEA is seen Fig. 3.As seen from Figure 3, add behind humidizer, the performance that feeds dry air is better than the performance of humidification air slightly.Therefore, played effect from humidification.
Embodiment 4
1) the polyethylene perforated membrane (porosity of film is 55%, and thickness is 2 μ m) with 2 μ m is cut into suitable dimensions, is placed in the alcohol solvent, places ultrasonic wave ultrasonic cleaning half an hour, repeats, and it is standby to carry out clean;
2) will contain the solution of 5% perfluorinated sulfonic resin (as Nafion) and the Pt/C catalyst of 10%WT and press Nafion: the ratio of catalyst=1:10 mixes, add in the catalyst feed material total weight 1% from humidizer titanium dioxide, be uniformly dispersed; The anode catalyst consumption is pressed 0.5mg/cm
2Calculate, the cathod catalyst consumption is pressed 0.3mg/cm
2Calculate, and add a certain amount of isopropyl alcohol.In order to allow catalyst feed in solution, evenly disperse. the ratio of isopropyl alcohol wants big, adds in the ratio of catalyst: isopropyl alcohol=1:100;
3) use the ultrasonic wave mixed solution, catalyst feed is evenly spread in the solution, standby;
1) at the both sides of perforated membrane spraying skim bonding agent. as the mixture of Nafion and carbon dust;
5) with the side of catalyst feed blade coating to porous membrane electrode;
6) in opposite side repeating step (2)～(4) of film;
7) membrane electrode is dried 4h under 320 ℃ environment;
8) both sides that membrane electrode are placed on Nafion film precompressed 1min, hot pressing 1min under 160 ℃, the condition of 0.35MPa makes membrane electrode assembly;
9) both sides that diffusion layer and bearer bar are placed on membrane electrode precompressed 1min, hot pressing 1min under 160 ℃, the condition of 0.7MPa, preparation MEA.
Embodiment 5
Difference from Example 4 is,
In the step 1), perforated membrane is the polysulfones perforated membrane, and the porosity of film is 70%, and thickness is 18 μ m;
Step 2) in, the solution of perfluorinated sulfonic resin (as Nafion) and Pt are black, and catalyst is pressed Nafion: the weight rate of catalyst=1:8 mixes; Add in the catalyst feed catalyst feed total weight 4% from humidizer water-absorbing resin (as silicon dioxide colloid), be uniformly dispersed;
In the step 7), 260 ℃ of the bake out temperatures of membrane electrode.
Embodiment 6
Difference from Example 4 is,
In the step 1), perforated membrane is a polyimide porous membrane, and the porosity of film is 60%, and thickness is 12 μ m;
Step 2) in, the solution of perfluorinated sulfonic resin (as Nafion) and PtRu are black, and catalyst is pressed Nafion: the weight rate of catalyst=1:5 mixes; Add in the catalyst feed catalyst feed total weight 4% from humidizer sulfonation organic substance (as SPSF), be uniformly dispersed;
In the step 7), 180 ℃ of the bake out temperatures of membrane electrode.
Claims (5)
1. method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells, it is characterized in that: be electrode support with the organic porous films, perforated membrane thickness is 1～20 μ m, and porosity is 50%～99%, catalyst feed is directly adhered on the perforated membrane preparation pole catalyze layer; This Catalytic Layer and dielectric film are combined into membrane electrode assembly by hot pressing;
Described organic porous films is polytetrafluoroethylene, polypropylene, polyethylene, polyimides or polysulfones perforated membrane;
Described catalyst feed adheres on the perforated membrane, and after the perforated membrane that has catalyst feed of preparation was shaped, the processing procedure through 120～320 ℃ obtained pole catalyze layer;
The pore creating material that adds its weight 10-90% in the described catalyst feed, described pore creating material for mix with the catalyst feed liquid, can decompose material volatilization and that in Catalytic Layer, form pore structure at 100～300 ℃;
Add in the described catalyst feed its weight 1-50% have absorbent function from humidizer, described is silicon dioxide, titanium dioxide or SPSF from humidizer.
2. according to the described method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells of claim 1, it is characterized in that: described catalyst feed is the mixture of eelctro-catalyst and proton conductive resin, eelctro-catalyst is the Pt/C of weight content 10～80%, the black or black catalyst of PtRu of PtRu/C, Pt of weight content 10～80%, and the weight mixed proportion is a catalyst: resin is 10:1～1:4.
3. according to the described method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells of claim 1, it is characterized in that: described catalyst feed directly adheres to and is meant on the perforated membrane that catalyst feed is prepared on the perforated membrane by spraying, blade coating or printing.
4. according to the described method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells of claim 1, it is characterized in that: described pore creating material is ammonium oxalate, ammonium carbonate, pyrazolone, histamine, n-valeramide, hexamethylene diamine, pyrrolidones or urea.
5. according to the described method for preparing membrane electrode that is used for Proton Exchange Membrane Fuel Cells of claim 1, it is characterized in that: what add in the described catalyst feed uses the carrier of eelctro-catalyst from humidizer always as supporting fuel cell, and membrane electrode is had from humidification; Described eelctro-catalyst is Pt, Ru or PtRu.
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| CN111584880A (en) * | 2020-05-15 | 2020-08-25 | 无锡威孚高科技集团股份有限公司 | Low-platinum proton exchange membrane fuel cell membrane electrode and preparation method thereof |
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| CN109585859A (en) * | 2018-10-08 | 2019-04-05 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of film electrode component of proton exchange film fuel battery |
| CN112144076B (en) * | 2020-09-18 | 2023-08-22 | 碳能科技（北京）有限公司 | Integrated membrane electrode and preparation method and application thereof |
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| Influence of electrode structure on the performance of adirectmethanol fuel cell. Zhaobin Wei,Suli Wang,Baolian Yi,et al.Journal of Power Sources,Vol.106 . 2002 |
| Influence of electrode structure on the performance of adirectmethanol fuel cell. Zhaobin Wei,Suli Wang,Baolian Yi,et al.Journal of Power Sources,Vol.106 . 2002 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111584880A (en) * | 2020-05-15 | 2020-08-25 | 无锡威孚高科技集团股份有限公司 | Low-platinum proton exchange membrane fuel cell membrane electrode and preparation method thereof |
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