CN101702436A - Sizing agent for proton exchange membrane fuel cell electrodes and preparation method thereof - Google Patents
Sizing agent for proton exchange membrane fuel cell electrodes and preparation method thereof Download PDFInfo
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- CN101702436A CN101702436A CN200910188223A CN200910188223A CN101702436A CN 101702436 A CN101702436 A CN 101702436A CN 200910188223 A CN200910188223 A CN 200910188223A CN 200910188223 A CN200910188223 A CN 200910188223A CN 101702436 A CN101702436 A CN 101702436A
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- 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 discloses a sizing agent for proton exchange membrane fuel cell electrodes and a preparation method thereof. The preparation method comprises: dispersing catalyst granules into an organic solvent with low boiling point and high molecular polymer solution of conductible protons to prepare mixed solution. The preparation method also comprises the step of using a high frequency oscillation probe and a high shear emulsifier probe to perform oscillation dispersion and emulsification on the mixed solution. The invention has the advantages that the high strength oscillation dispersion and emulsification method ensures that solid particles are more evenly dispersed in ethanol or isopropanol solvent and can greatly shorten the preparation time of the sizing agent. The electrodes prepared from the sizing agent prepared by the method of the invention can ensure that the materials such as the powdered carbon or catalyst and the like on the unit of the electrode surfaces are relatively evenly distributed. The utilization ratio of the catalysts is improved, and the electrode performances are greatly improved.
Description
Technical field
The present invention relates to the Proton Exchange Membrane Fuel Cells field, relate in particular to the preparation method of proton exchange membrane fuel cell electrode with slurry.
Background technology
The electrode of fuel cell is the fuel of fuel cell and the place that oxidant carries out electrochemical reaction, is the core component of fuel cell.The gas-diffusion electrode that electrode normally is made up of supporting layer, microporous layers and the Catalytic Layer of conduction with sandwich construction.Ordinary circumstance, supporting layer are through the carbon paper of hydrophobic treatment or carbon cloth, and microporous layers is made up of carbon black and PTFE, and both are called diffusion layer altogether.Catalytic Layer is made of eelctro-catalyst such as Pt/C and proton conductive resin or PTFE.For electrochemical reaction can be carried out smoothly, electrode must possess the continuous transmission channels of proton, electronics, reaction gas and generation water.
The electrode that in form can be divided into hydrophobic electrode and hydrophilic electrode and composite catalytic layer from electrode.The electrode of any form no matter, the slurry that uses during electrode is made is the key that influences electrode performance, the degree of scatter of various compositions all influences the performance of electrode in the slurry, when especially catalyst disperses inequality in slurry, can not cause electrode performance lower because of catalyst utilization is high.
The compound method of Catalytic Layer usefulness slurry in one proton exchanging film fuel battery has been described in US Patent 20090169949, it has adopted a kind of solvent that catalyst granules can be emulsified in perfluorinated resin solution and other solvent, as materials such as amine, ethers and arenes, make catalyst granules form a kind of metastable slurry by these materials.
Described a kind of compound method of slurry in Chinese patent 200610028206, having adopted some organic acid substances that contain carboxyl in the preparation of slurry is auxiliary material in the slurry.
The slurry of said method preparation has certain stability, and its deficiency is all to contain the high boiling organic solvent that makes slurry emulsification in the slurry, and various material dispersed degree are inhomogeneous in the slurry, be difficult to control, and the slurry of these methods is prepared consuming time more.
Summary of the invention
The purpose of this invention is to provide a kind of slurry compound method of various material dispersed degree in the slurry and slurry for preparing with this method of improving.
Technical solution of the present invention is: a kind of proton exchange membrane fuel cell electrode preparation method of slurry, comprise but catalyst granules is distributed in the macromolecule polymer solution of low boiling point organic solvent and proton conducting, make mixed solution, low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, the preparation method who it is characterized in that described electrode slurry also comprises popping one's head in high frequency oscillation probe and high-shear emulsion machine described mixed solution is carried out vibrating dispersion and emulsification, makes electrode emulsification slurry.
A kind of proton exchange membrane fuel cell electrode of the present invention preparation method of slurry, it is characterized in that described with high frequency oscillation probe with described mixed solution is carried out vibrating dispersion to the high-shear emulsion machine probe and emulsification may further comprise the steps: high frequency oscillation is popped one's head in is immersed in catalyst granules and the low boiling point organic solvent mixed solution earlier, concussion 30s～10min, frequency of oscillation is 50～60Hz, but the high molecular polymer and/or the polytetrafluoroethylene (PTFE) that in catalyst granules after the concussion of high frequency oscillation probe and low boiling point organic solvent mixed solution, add proton conducting then, but again high-shear emulsion machine probe is immersed in the mixed solution of the high molecular polymer that added proton conducting and/or polytetrafluoroethylene (PTFE), operation 1～5min, running speed is 2000～20000 rev/mins.
A kind of proton exchange membrane fuel cell electrode of the present invention hydrophilic slurry of a kind of proton exchange membrane fuel cell electrode of preparation method's preparation of slurry, slurry comprises catalyst, but the high molecular polymer of low boiling point organic solvent and proton conducting, it is characterized in that not containing in the described electrode slurry high boiling organic solvent, described low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, but the proton conducting high molecular polymer is perfluor sulfoacid resin solution (Nafion) or carboxylic acid resin molten (Flemion), described catalyst is institute's carbon supported platinum catalyst, and the mass percent of stating each component of electrode slurry is: platinum content is in the carbon supported platinum catalyst: 30%～70%wt; The addition of isopropyl alcohol or ethanol is 20～50 times of catalyst quality, but the high molecular polymer of proton conducting is 10%～80% (wt) of catalytic amount.
A kind of proton exchange membrane fuel cell electrode of the present invention a kind of proton exchange membrane fuel cell electrode water-repellent slurry of preparation method's preparation of slurry, slurry comprises conductive agent, low boiling point organic solvent, polytetrafluoroethylene (PTFE) and pore creating material, it is characterized in that not containing in the described electrode slurry high boiling organic solvent, described low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, described conductive agent is conductive carbon powder or carbon supported platinum catalyst, described pore creating material is an ammonium carbonate, carbonic hydroammonium, ammonium oxalate, the mixture of one or more in the urea, the mass percent of described each component of electrode slurry is: platinum content is in the carbon supported platinum catalyst: 30%～70%wt; The addition of isopropyl alcohol or ethanol is 20～50 times of catalyst quality, the mass percent of polytetrafluoroethylene (PTFE) is 10%～50% (wt), the mass ratio of conductive carbon powder or carbon supported platinum catalyst and polytetrafluoroethylene (PTFE) and pore creating material is 1: 0.2～0.35: 0.5～1.5, both conductive carbon powder or carbon supported platinum catalyst: polytetrafluoroethylene (PTFE): pore creating material=1: 0.2～0.35: 0.5～1.5 mass ratioes.
A kind of proton exchange membrane fuel cell electrode of the present invention is characterized in that with a kind of proton exchange membrane fuel cell electrode water-repellent slurry of preparation method's preparation of slurry described conductive carbon powder is VC-72 or AB-50%.
Advantage of the present invention is:
One, is to utilize high-intensity vibrating dispersion and emulsification method, makes solid particle especially be scattered in more equably in ethanol or the isopropanol solvent for the carbon supported platinum catalyst particle.Prior art is when the catalyst pulp that the preparation kind electrode is used, the method of taking is that supersonic oscillations add artificial stirring or stir with mixing plant, the very difficult complete size degradation of catalyst bulky grain that will reunite together of the mode of prior art makes the catalyst granules in the slurry disperse inhomogeneous.High-intensity vibrating dispersion and high-shear emulsion machine emulsifying technology have been adopted among the present invention, utilize stronger vibration and high shear force, weakened catalyst granules reunion bonding force together, the particles such as catalyst of reuniting together in the slurry are diminished by size degradation, make the dispersion of the catalyst granules in the slurry more even.Simultaneously, the sinking speed of particle in slurry slows down because of the raising of Dispersion of Particles degree.And, adopt high-shear emulsion machine also can shorten the preparation time of slurry greatly.
Two, utilize the slurry of described method preparation, the preparation have the electrode of layer hydrophobic catalyst and hydrophilic Catalytic Layer composite catalytic layer structure the time, can make the distribution of carbon dust on the electrode surface unit sizes or catalyst and other material even relatively, especially the utilance of catalyst is improved in the electrode, makes the performance of electrode obtain raising by a relatively large margin.
Description of drawings
The present invention has accompanying drawing 1 width of cloth, is the electrode of slurry making of the present invention and the electrode performance curve comparison diagram that conventional compound method slurry is made.The film that adopts is the NRE-212 film of E.I.Du Pont Company, and test condition is: the hydrogen/air operating pressure is a normal pressure, and battery temperature is 60 degree.Among the figure, the performance curve of the electrode that the slurry that the curve representation that round dot forms is prepared with slurry distribution of the present invention is made, the performance curve of the electrode that the slurry that the curve representation that side's point forms is prepared with conventional distribution is made.
Embodiment
Embodiment 1
The toner slurry preparation:
1. take by weighing conductive carbon powder AB50%1g, add the isopropyl alcohol of 30g, pop one's head in to taking out behind this mixed liquor vibrating dispersion 1min with high frequency oscillation;
2. in the solution of step 1, add 15% (wt) ammonium oxalate solution 7g of dissolving, with high-shear emulsion machine this solution is stirred 30s then;
3. the PTFE solution 1.5g that adds 30% (wt) again in the solution of step 2 stirs 30s with high-shear emulsion machine with this solution then, is mixed with electrode diffusion layer and makes the slurry that uses.
Implement 2
The preparation of carbon supported platinum catalyst slurry:
1. take by weighing the carbon supported platinum catalyst 1g of 50% (wt), soak into deionized water;
2. carbon supported platinum catalyst is joined in the isopropyl alcohol of 35g, pop one's head in to taking out behind this mixed liquor vibrating dispersion 1.5min with high frequency oscillation;
3. in the solution of step 2, add 15% (wt) ammonium oxalate solution 5g of dissolving again, with high-shear emulsion machine this solution is stirred 1min then;
4. the PTFE solution 1.2g that adds 30% (wt) again in the solution of step 3 stirs 30s with high-shear emulsion machine with this solution then, is mixed with the slurry that electrode diffusion layer uses.
Embodiment 3
The preparation of pole catalyze layer slurry
1. take by weighing 50% carbon supported platinum catalyst 1g, soak into deionized water.
2. add perfluorinated sulfonic resin (the Nafion solution of E.I.Du Pont Company) solution 8.5g.
3. add isopropanol solvent 35g.
4. pop one's head in to this mixed liquor vibrating dispersion 2min with high frequency oscillation earlier, with high-shear emulsion machine this solution is stirred 3min then.Be mixed with the slurry that is used for pole catalyze layer.
Use the slurry of said method preparation to carry out the making of electrode, the electrode support of making is the carbon paper of the TGP-H-060 model of Toray company, and the NRE-212 mould of the electrode of making and E.I.Du Pont Company is synthesized membrane electrode, carries out the electrode performance test.Electrode performance curve such as Fig. 1.
By the Dispersion of Particles situation in microscopically observation slurry, can find out significantly that Dispersion of Particles situation in the slurry of method preparation of the present invention is better than the Dispersion of Particles situation in the slurry of conventional distribution preparation.
Claims (5)
1. a proton exchange membrane fuel cell electrode is with the preparation method of slurry, comprise but catalyst granules is distributed in the macromolecule polymer solution of low boiling point organic solvent and proton conducting, make mixed solution, low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, the preparation method who it is characterized in that described electrode slurry also comprises popping one's head in high frequency oscillation probe and high-shear emulsion machine described mixed solution is carried out vibrating dispersion and emulsification, makes electrode emulsification slurry.
2. according to the preparation method of claim 1 described a kind of proton exchange membrane fuel cell electrode with slurry, it is characterized in that described with high frequency oscillation probe with described mixed solution is carried out vibrating dispersion to the high-shear emulsion machine probe and emulsification may further comprise the steps: high frequency oscillation is popped one's head in is immersed in catalyst granules and the low boiling point organic solvent mixed solution earlier, concussion 30s～10min, frequency of oscillation is 50～60Hz, but the high molecular polymer and/or the polytetrafluoroethylene (PTFE) that in catalyst granules after the concussion of high frequency oscillation probe and low boiling point organic solvent mixed solution, add proton conducting then, but again high-shear emulsion machine probe is immersed in the mixed solution of the high molecular polymer that added proton conducting and/or polytetrafluoroethylene (PTFE), operation 1～5min, running speed is 2000～20000 rev/mins.
3. the described a kind of proton exchange membrane fuel cell electrode of claim 1 is with the hydrophilic slurry of a kind of proton exchange membrane fuel cell electrode of preparation method's preparation of slurry, slurry comprises catalyst, but the high molecular polymer of low boiling point organic solvent and proton conducting, it is characterized in that not containing in the described electrode slurry high boiling organic solvent, described low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, but the proton conducting high molecular polymer is perfluor sulfoacid resin solution (Nafion) or carboxylic acid resin molten (Flemion), described catalyst is institute's carbon supported platinum catalyst, and the mass percent of stating each component of electrode slurry is: platinum content is in the carbon supported platinum catalyst: 30%～70%wt; The addition of isopropyl alcohol or ethanol is 20～50 times of catalyst quality, but the high molecular polymer of proton conducting is 10%～80%wt of catalytic amount.
4. the described a kind of proton exchange membrane fuel cell electrode of claim 1 is with a kind of proton exchange membrane fuel cell electrode water-repellent slurry of preparation method's preparation of slurry, slurry comprises conductive agent, low boiling point organic solvent, polytetrafluoroethylene (PTFE) and pore creating material, it is characterized in that not containing in the described electrode slurry high boiling organic solvent, described low boiling point organic solvent is absolute ethyl alcohol or isopropyl alcohol, described conductive agent is conductive carbon powder or carbon supported platinum catalyst, described pore creating material is an ammonium carbonate, carbonic hydroammonium, ammonium oxalate, the mixture of one or more in the urea, the mass percent of described each component of electrode slurry is: platinum content is in the carbon supported platinum catalyst: 30%～70%wt; The addition of isopropyl alcohol or ethanol is 20～50 times of catalyst quality, the mass percent of polytetrafluoroethylene (PTFE) is 10%～50% (wt), the mass ratio of conductive carbon powder or carbon supported platinum catalyst and polytetrafluoroethylene (PTFE) and pore creating material is 1: 0.2～0.35: 0.5～1.5, both conductive carbon powder or carbon supported platinum catalyst: polytetrafluoroethylene (PTFE): pore creating material=1: 0.2～0.35: 0.5～1.5 mass ratioes.
5. according to a kind of proton exchange membrane fuel cell electrode water-repellent slurry of claim 4 described a kind of proton exchange membrane fuel cell electrodes, it is characterized in that described conductive carbon powder is VC-72 or AB-50% with preparation method's preparation of slurry.
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Cited By (8)
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| CN101950805A (en) * | 2010-09-20 | 2011-01-19 | 江苏万力电池股份有限公司 | Size mixing method of nanometer lithium iron phosphate material |
| CN109772004A (en) * | 2019-01-21 | 2019-05-21 | 深圳市南科燃料电池有限公司 | Fuel cell catalyst slurry filter method and filtration system |
| CN112133928A (en) * | 2020-08-21 | 2020-12-25 | 同济大学 | Stable and high-performance proton exchange membrane fuel cell catalyst slurry and preparation method thereof |
| CN113871633A (en) * | 2021-09-26 | 2021-12-31 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Method for high-efficiency in-situ activation of membrane electrode of proton exchange membrane fuel cell |
| CN113871673A (en) * | 2021-09-07 | 2021-12-31 | 国家电投集团氢能科技发展有限公司 | Composite proton exchange membrane and preparation method thereof |
| CN114361476A (en) * | 2021-12-06 | 2022-04-15 | 安徽熵卡科技有限公司 | Preparation method and application of gas diffusion electrode |
| CN114373945A (en) * | 2021-12-16 | 2022-04-19 | 同济大学 | Preparation method of catalyst slurry suitable for ultrathin proton exchange membrane |
| CN114959765A (en) * | 2022-06-01 | 2022-08-30 | 润世华新能源控股集团有限公司 | Adhesive for membrane electrode, preparation method of membrane electrode slurry, membrane electrode and proton exchange membrane water electrolyzer |
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| CN1208862C (en) * | 2003-08-13 | 2005-06-29 | 中国科学院长春应用化学研究所 | Prepn of electrode for proton exchange film fuel cell |
| CN100405641C (en) * | 2004-06-23 | 2008-07-23 | 比亚迪股份有限公司 | Electrode production of fuel battery membrane with proton exchange membrane |
| CN1315221C (en) * | 2005-05-19 | 2007-05-09 | 武汉理工大学 | Full cross-linked proton exchange film fuel cell chip and preparing process |
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| CN101950805A (en) * | 2010-09-20 | 2011-01-19 | 江苏万力电池股份有限公司 | Size mixing method of nanometer lithium iron phosphate material |
| CN101950805B (en) * | 2010-09-20 | 2012-07-04 | 江苏万力电池股份有限公司 | Size mixing method of nanometer lithium iron phosphate material |
| CN109772004A (en) * | 2019-01-21 | 2019-05-21 | 深圳市南科燃料电池有限公司 | Fuel cell catalyst slurry filter method and filtration system |
| CN112133928A (en) * | 2020-08-21 | 2020-12-25 | 同济大学 | Stable and high-performance proton exchange membrane fuel cell catalyst slurry and preparation method thereof |
| CN112133928B (en) * | 2020-08-21 | 2022-08-19 | 同济大学 | Stable and high-performance proton exchange membrane fuel cell catalyst slurry and preparation method thereof |
| CN113871673A (en) * | 2021-09-07 | 2021-12-31 | 国家电投集团氢能科技发展有限公司 | Composite proton exchange membrane and preparation method thereof |
| CN113871633A (en) * | 2021-09-26 | 2021-12-31 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Method for high-efficiency in-situ activation of membrane electrode of proton exchange membrane fuel cell |
| CN114361476A (en) * | 2021-12-06 | 2022-04-15 | 安徽熵卡科技有限公司 | Preparation method and application of gas diffusion electrode |
| CN114361476B (en) * | 2021-12-06 | 2023-12-26 | 安徽熵卡科技有限公司 | Preparation method and application of gas diffusion electrode |
| CN114373945A (en) * | 2021-12-16 | 2022-04-19 | 同济大学 | Preparation method of catalyst slurry suitable for ultrathin proton exchange membrane |
| CN114959765A (en) * | 2022-06-01 | 2022-08-30 | 润世华新能源控股集团有限公司 | Adhesive for membrane electrode, preparation method of membrane electrode slurry, membrane electrode and proton exchange membrane water electrolyzer |
| CN114959765B (en) * | 2022-06-01 | 2024-05-03 | 深圳市润世华氢能源有限公司 | Adhesive for membrane electrode, membrane electrode slurry preparation method, membrane electrode and proton exchange membrane water electrolysis tank |
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