CN102142563A - Method for preparing slurry for catalyst coating membrane electrode of proton exchange membrane fuel cell - Google Patents
Method for preparing slurry for catalyst coating membrane electrode of proton exchange membrane fuel cell Download PDFInfo
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Abstract
The invention discloses a method for preparing slurry for a catalyst coating membrane electrode of a proton exchange membrane fuel cell. The method is characterized in that: the slurry has uniform dispersion and good stability, is not easy to settle, can be used for preparing the electrode by a method of spraying, brushing, blade coating, silk screen printing and the like, and is suitable for mechanized production. The electrode slurry contains a catalyst, proton exchange resin, a dispersant and an auxiliary agent added in a ratio; and the preparation method comprises four processes of material adding, dispersion, concentration and activating treatment. Because the slurry contains a thickening agent or a stabilizing agent, the slurry has good stability and is not easy to settle after dispersion, concentration and activating treatment. The catalyst coating membrane electrode prepared by adopting the electrode slurry has good discharge performance, and the electrode slurry is suitable for preparing the electrode by a process of spraying, brushing, blade coating, silk screen printing and the like.
Description
Technical field
The present invention relates to the Proton Exchange Membrane Fuel Cells field, relate in particular to the preparation method of catalyst of fuel batter with proton exchange film coated membrane electrode, particularly the preparation method of catalyst coated membrane electrode slurry.
Background technology
Electrode is the critical component of fuel cell, is the key factor that influences fuel battery performance.In order to improve fuel battery performance, reduce the consumption of the noble metal platinum of the cell catalyst that acts as a fuel, the researcher has studied various electrode structures.Commonly used is catalyst coated membrane electrode (CCM) structure at present, is about to Catalytic Layer and is made on the proton exchange membrane, and Catalytic Layer is separated with gas diffusion layers (GDL).Because catalyst coated membrane electrode is that Catalytic Layer is linked to each other with the proton exchange film close, and does not contain hydrophobic substance in the Catalytic Layer, Catalytic Layer can be done very thinly, and low platinum carrying capacity just can have higher discharge performance.In order to prepare the electrode of low platinum, efficient, stable performance, the researcher adopts the high electrode slurry of prepared in various methods good dispersion, stability to achieve the goal.
The patent No. is the patent of CN200910206184.6, discloses a kind of by using the higher boiling point cosolvent to improve the method for electrode structure in electrode slurry.Except eelctro-catalyst and electrolyte, also comprise solvent and cosolvent in the electrode slurry of this patent, the boiling point of cosolvent is higher than the boiling point of solvent.Cosolvent is selected from propylene glycol butyl ether, ethylene glycol, 1 amylalcohol, 2, the mixture that 3-butanediol and dipropyl alcohol ketone are formed.By heating described solvent is removed from diffusion layer, but make at least a portion of cosolvent residual with liquid form.Residual liquid has reduced the possibility that the electrode that may form breaks in the subsequent electrode course of processing, thereby improves the performance and the life-span of electrode.
The patent No. be WO 2009086364 (A1) patent disclosure a kind of preparation method of electrode slurry.Solid content of slurry is 10～20%, and the electrolyte dispersion liquid is water miscible, also can add ethanol or polyalcohol, as glycerine or ethylene glycol.Regulate the rheological properties of slurry by the ratio of regulating water, pure and mild polyalcohol.Contain 0～50% pure and mild 0～20% polyalcohol and 0～2% dispersant in the general slurry.Slurry is diluted to the state that can spray continuously after stirring under heating condition.Contain the cosolvent that compatibility is arranged with electrolyte in the slurry.The vitrification point that cosolvent can reduce polymer dielectric makes its film forming at low temperatures.Suitable cosolvent is alkane and alkene, ammonia, ester class or aromatic compound, and its boiling point is insoluble in water greater than 120 ℃.
Chinese patent CN200580038417.6 provides a kind of protonically conductive polymer composition and the manufacture method thereof of catalyst for fuel cell performance and method that adopts the preparation of compositions catalyst pulp of this protonically conductive polymer of improving.This proton-conducting polymer composition is the aromatic hydrocarbon based proton-conducting polymer that contains at least at 1～30%wt, and the molecular weight that converts with polyethylene glycol in this proton-conducting polymer is 2, the content of the composition in 000～23,000 scope is more than the 10%wt with respect to this proton-conducting polymer total amount.Electrode by this pulp preparation has good discharge performance and durability.
The deficiencies in the prior art are poor stabilities of electrode slurry, and the short time places will sedimentation, and lamination just appearred in disposed slurry in two or three hours, and the upper strata is the solvent of clarification, and lower floor is the mixture of catalyst and ion exchange resin.Adopt such electrode slurry to produce electrode continuously, can cause measuring on the catalyst inhomogeneous.Amount is lower on the electrode catalyst of producing earlier, and amount is higher on the electrode catalyst that the back produces.
Summary of the invention
The purpose of this invention is to provide the preparing electrode paste method of a kind of good dispersion, the high catalyst coated membrane electrode of stability, make it and to prepare electrode by modes such as spraying, brushing, blade coating, silk screen printings.
Technical scheme of the present invention is: a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry, comprise catalyst, proton exchange resins, dispersant and auxiliary agent, catalyst comprise that Pt/C, Pt-Pd/C, Pt-Ru/C, the Pt of 10～80%wt is black or PtPd is black and the black catalyst of PtRu in one or more mixture; Proton exchange resins is one or more the mixture in the sulfonate resin of perfluor or partially fluorinated sulfonate resin or non-fluorine; Dispersant is one or more the mixture in deionized water, absolute ethyl alcohol, the isopropyl alcohol; It is characterized in that also comprising auxiliary agent in the described catalyst coated membrane electrode slurry, described auxiliary agent is thickener or stabilizer, and thickener is a kind of in ethylene glycol, glycerol and the polyethylene glycol, and stabilizer is Triton X-100.The addition of thickener is the 0.2%wt-0.5%wt of catalyst, proton exchange resins and dispersant quality summation, and the addition of stabilizer is the 0.2%wt-0.8%wt of catalyst, proton exchange resins and dispersant quality summation.
A kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry preparation method, the catalyst coated membrane electrode slurry comprises catalyst, proton exchange resins, dispersant and auxiliary agent, catalyst comprise that Pt/C, Pt-Pd/C, Pt-Ru/C, the Pt of 10～80%wt is black or PtPd is black and the black catalyst of PtRu in one or more mixture; Proton exchange resins is one or more the mixture in the sulfonate resin of perfluor or partially fluorinated sulfonate resin or non-fluorine; Dispersant is one or more the mixture in deionized water, absolute ethyl alcohol, the isopropyl alcohol; Auxiliary agent is thickener or stabilizer, and thickener is a kind of in ethylene glycol, glycerol and the polyethylene glycol, and stabilizer is Triton X-100; It is characterized in that described catalyst coated membrane electrode slurry preparation method comprises the material interpolation, disperses, concentrates and increase processing 4 procedures of living, described material interpolation operation is meant adds pulp components catalyst, proton exchange resins, dispersant and auxiliary agent in the container to by said sequence; Described dispersion step is to adopt high speed dispersor, supersonic generator and electric mixing device will place load weighted catalyst, proton exchange resins, dispersant and auxiliary agent in the container to disperse; Described enrichment process is to make the quality of slurry reach predetermined value through the electrode slurry of dispersion step with heating means or low pressure method volatile fraction solvent; It is described that to increase treatment process alive be to activate with high pressure method or the logically true short side method of constant temperature through the electrode slurry of concentration operation.The high speed dispersor of described dispersion step and the rotating speed of electric mixing device are at 15000rpm-25000rpm, and the vibration frequency of the supersonic generator of described dispersion step is 48Hz, and jitter time is 30 minutes-120 minutes.It is that will to be placed on temperature through the electrode slurry of concentration be 30～240 ℃ that the described high pressure method that increases treatment process alive activates, and pressure is that the environment of 2～8Mpa is handled down, and the processing time is 2～24 hours; It is that will to be placed on temperature through the electrode slurry of concentration be 30～120 ℃ that the logically true short side method of the described constant temperature that increases treatment process alive activates, and vacuum degree is that the environment of 0～0.05MPa is handled down, and the processing time is 2～24 hours.Described enrichment process be with through the electrode slurry of dispersion step with heating means or low pressure method volatile fraction solvent, make the quality of slurry reach predetermined value, be that will to place temperature through the slurry of dispersion step be under 50-80 ℃, perhaps will place the environment of 0～0.05MPa to handle down through the slurry of dispersion step, handle the 70%-80% that reduces to proper mass to stock quality.
The mechanism of method of the present invention is: in the microstructure of Catalytic Layer, mainly contain two class holes: a class is the main aperture of aperture less than 0.1 μ m, i.e. hole between the catalyst granules in the catalyst agglomeration body; The another kind of inferior hole that is the aperture greater than 0.1 μ m, i.e. hole between the catalyst agglomeration body.Want to improve catalyst utilization, will allow the proton exchange resins filling but not in the inferior hole in main aperture.Slurry of the present invention contains thickener or stabilizer, by dispersion step catalyst feed is uniformly distributed in the slurry system, make the proton exchange resins in the slurry be filled in more in the main aperture by activation, improve the dispersiveness of slurry, improve the utilance of catalyst.Simultaneously, the slurry through disperse concentrating is improved stability of slurry, free settling not in put procedure.
The advantage of the inventive method is: by adding thickener or stabilizer and adopt distinctive method to prepare electrode slurry in slurry, make electrode slurry have the characteristics of high dispersive, high stability, electrode discharge performance by this pulp preparation is high and uniform and stable, this slurry can prepare electrode by modes such as spraying, brushing, blade coating, silk screen printings, is fit to mechanization production.
Description of drawings
The present invention has accompanying drawing 1 width of cloth, is the I-V curve chart with the comparative example 1 of the battery of the embodiment 1 of the battery of the membrane electrode of pulp preparation of the present invention assembling and the assembling of prior art membrane electrode.
In the accompanying drawing, the I-V curve of single pond under the 0.1MPa condition that curve representation embodiment 1 membrane electrode assembly that the ■ point forms is assembled into, ● the I-V curve of single pond under condition of normal pressure that curve representation embodiment 1 membrane electrode assembly that point forms is assembled into, the I-V curve of single pond under the 0.1MPa condition that curve representation comparative example 1 membrane electrode assembly an of ▲ formation is assembled into
The I-V curve of single pond under condition of normal pressure that curve representation comparative example 1 membrane electrode assembly that point forms is assembled into.
Embodiment
Embodiment 1
1), take by weighing 50%wt.Pt/C catalyst 2g, the Nafion solution of 80g deionized water, 60g isopropyl alcohol and 18g5%, 0.5g ethylene glycol solution place the screw socket bottle of 250ml.
2), catalyst feed is disperseed with dispersion machine, the rotating speed of dispersion machine is controlled to be 25000rpm, and jitter time is 60 minutes, adopts the recirculated water cooling to guarantee the unlikely rising of the temperature of electrode slurry under the high-speed stirred state simultaneously.
3), the electrode slurry after will disperseing is placed in 60 ℃ the water-bath and concentrates, and stirs with electric mixer simultaneously, guarantees that the solvent in the slurry evenly volatilizees.The quality for the treatment of slurry stops to concentrate when being kept to 125.625g.
4) electrode slurry after will concentrating is placed in the autoclave, and the temperature of autoclave is set at 80 ℃, pressure transfer to 6MPa and constant voltage after 10 hours pressure release take out.
5) slurry of handling well is linked to each other with the syringe pump and the pipe-line system of flush coater, adopting NRE211 film preparation Pt load amount is 0.6mg/cm
2Catalyst coated membrane electrode and suppress MEA.
This membrane electrode assembly be assembled into curve that performance behind single pond sees that the ■ point of Fig. 1 forms and ● the curve that point forms.
Comparative example 1
1), take by weighing 50%wt.Pt/C catalyst 2g, the Nafion solution of 80g deionized water, 60g isopropyl alcohol and 18g5% places the screw socket bottle of 250ml.
2), catalyst feed is disperseed with supersonic generator, jitter time is 30 minutes, adopts the water in the ice cube cooling ultrasonic wave to guarantee the temperature unlikely rising of electrode slurry when ultrasonic the dispersion simultaneously.
3) scattered slurry is linked to each other with the syringe pump and the pipe-line system of flush coater, adopting NRE211 film preparation Pt load amount is 0.6mg/cm
2Catalyst coated membrane electrode and suppress MEA.
This membrane electrode assembly be assembled into performance behind single pond see among Fig. 1 ▲ curve of a formation and
The curve that point forms.
Claims (6)
1. catalyst of fuel batter with proton exchange film coated membrane electrode slurry, comprise catalyst, proton exchange resins, dispersant and auxiliary agent, catalyst comprise that Pt/C, Pt-Pd/C, Pt-Ru/C, the Pt of 10～80%wt is black or PtPd is black and the black catalyst of PtRu in one or more mixture; Proton exchange resins is one or more the mixture in the sulfonate resin of perfluor or partially fluorinated sulfonate resin or non-fluorine; Dispersant is one or more the mixture in deionized water, absolute ethyl alcohol, the isopropyl alcohol; It is characterized in that also comprising auxiliary agent in the described catalyst coated membrane electrode slurry, described auxiliary agent is thickener or stabilizer, and thickener is a kind of in ethylene glycol, glycerol and the polyethylene glycol, and stabilizer is TritonX-100.
2. according to the described a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry of claim 1, the addition that it is characterized in that described thickener is the 0.2%wt-0.5%wt of catalyst, proton exchange resins and dispersant quality summation, and the addition of stabilizer is the 0.2%wt-0.8%wt of catalyst, proton exchange resins and dispersant quality summation.
3. the described a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry preparation method of claim 1, the catalyst coated membrane electrode slurry comprises catalyst, proton exchange resins, dispersant and auxiliary agent, catalyst comprise that Pt/C, Pt-Pd/C, Pt-Ru/C, the Pt of 10～80%wt is black or PtPd is black and the black catalyst of PtRu in one or more mixture; Proton exchange resins is one or more the mixture in the sulfonate resin of perfluor or partially fluorinated sulfonate resin or non-fluorine; Dispersant is one or more the mixture in deionized water, absolute ethyl alcohol, the isopropyl alcohol; Auxiliary agent is thickener or stabilizer, and thickener is a kind of in ethylene glycol, glycerol and the polyethylene glycol, and stabilizer is Triton X-100; It is characterized in that described catalyst coated membrane electrode slurry preparation method comprises the material interpolation, disperses, concentrates and increase processing 4 procedures of living, described material interpolation operation is meant adds pulp components catalyst, proton exchange resins, dispersant and auxiliary agent in the container to by said sequence; Described dispersion step is to adopt high speed dispersor, supersonic generator and electric mixing device will place load weighted catalyst, proton exchange resins, dispersant and auxiliary agent in the container to disperse; Described enrichment process is to make the quality of slurry reach predetermined value through the electrode slurry of dispersion step with heating means or low pressure method volatile fraction solvent; It is described that to increase treatment process alive be to activate with high pressure method or the logically true short side method of constant temperature through the electrode slurry of concentration operation.
4. according to the described a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry preparation method of claim 3, the rotating speed that it is characterized in that the high speed dispersor of described dispersion step and electric mixing device is at 15000rpm-25000rpm, the vibration frequency of the supersonic generator of described dispersion step is 48Hz, and jitter time is 30 minutes-120 minutes.
5. according to the described a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry preparation method of claim 3, the heating process volatile fraction solvent that it is characterized in that described enrichment process, make the quality of slurry reach predetermined value, be that will to place temperature through the slurry of dispersion step be under 50-80 ℃, handle the 70%-80% that reduces to proper mass to stock quality;
6. according to the described a kind of catalyst of fuel batter with proton exchange film coated membrane electrode slurry preparation method of claim 3, it is characterized in that it is that will to be placed on temperature through the electrode slurry of concentration be 30～240 ℃ that the described high pressure method that increases treatment process alive activates, pressure is that the environment of 2～8Mpa is handled down, and the processing time is 2～24 hours; It is that will to be placed on temperature through the electrode slurry of concentration be 30～120 ℃ that the logically true short side method of the described constant temperature that increases treatment process alive activates, and vacuum degree is that the environment of 0～0.05MPa is handled down, and the processing time is 2～24 hours.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103782430A (en) * | 2011-09-26 | 2014-05-07 | 日产自动车株式会社 | Catalytic ink adjustment method |
| CN104600332A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Membraneless fuel cell catalyst slurry and methods for preparing catalyst slurry and electrode |
| CN107925091A (en) * | 2016-03-29 | 2018-04-17 | 株式会社Lg化学 | The method for preparing electrode slurry |
| CN108075158A (en) * | 2016-11-18 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of preparation method of fuel cell CCM membrane electrodes |
| CN109088073A (en) * | 2018-07-13 | 2018-12-25 | 东莞众创新能源科技有限公司 | Proton Exchange Membrane Fuel Cells ccm membrane electrode and preparation method thereof |
| CN109301265A (en) * | 2018-09-11 | 2019-02-01 | 先进储能材料国家工程研究中心有限责任公司 | Fuel cell coating catalyst pulp and preparation method thereof |
| CN110783578A (en) * | 2019-10-11 | 2020-02-11 | 成都新柯力化工科技有限公司 | Pre-dispersion method of fuel cell catalyst slurry |
| CN112599803A (en) * | 2020-12-16 | 2021-04-02 | 浙江博氢新能源有限公司 | Catalyst slurry for membrane electrode of fuel cell and preparation method thereof |
| CN112599799A (en) * | 2020-12-16 | 2021-04-02 | 浙江博氢新能源有限公司 | Preparation method of HT-PEMFC gas diffusion electrode, membrane electrode and preparation method thereof |
| CN116005184A (en) * | 2022-12-19 | 2023-04-25 | 东北农业大学 | Method for chemically modifying fullerene C60 carrier and application of fullerene C60 carrier in electrochemical hydrogenation of soybean oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103782430A (en) * | 2011-09-26 | 2014-05-07 | 日产自动车株式会社 | Catalytic ink adjustment method |
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| CN109301265A (en) * | 2018-09-11 | 2019-02-01 | 先进储能材料国家工程研究中心有限责任公司 | Fuel cell coating catalyst pulp and preparation method thereof |
| CN110783578A (en) * | 2019-10-11 | 2020-02-11 | 成都新柯力化工科技有限公司 | Pre-dispersion method of fuel cell catalyst slurry |
| CN110783578B (en) * | 2019-10-11 | 2021-03-02 | 成都新柯力化工科技有限公司 | Pre-dispersion method of fuel cell catalyst slurry |
| CN112599803A (en) * | 2020-12-16 | 2021-04-02 | 浙江博氢新能源有限公司 | Catalyst slurry for membrane electrode of fuel cell and preparation method thereof |
| CN112599799A (en) * | 2020-12-16 | 2021-04-02 | 浙江博氢新能源有限公司 | Preparation method of HT-PEMFC gas diffusion electrode, membrane electrode and preparation method thereof |
| CN116005184A (en) * | 2022-12-19 | 2023-04-25 | 东北农业大学 | Method for chemically modifying fullerene C60 carrier and application of fullerene C60 carrier in electrochemical hydrogenation of soybean oil |
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Application publication date: 20110803 |