CN101483241A - Preparation for membrane electrode of fuel cell with proton exchange film - Google Patents
Preparation for membrane electrode of fuel cell with proton exchange film Download PDFInfo
- Publication number
- CN101483241A CN101483241A CNA200810300046XA CN200810300046A CN101483241A CN 101483241 A CN101483241 A CN 101483241A CN A200810300046X A CNA200810300046X A CN A200810300046XA CN 200810300046 A CN200810300046 A CN 200810300046A CN 101483241 A CN101483241 A CN 101483241A
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- ink
- proton exchange
- membrane electrode
- preparation
- exchange film
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 method for preparing a membrane electrode of a fuel batter with a proton exchange film comprising: preparing a jet ink by using a catalyst, a proton exchange film resin, a solvent, a pH regulating agent and a dispersant, and at 30-40 DEG C, printing the ink into a printing stock through an ink jet printer. The membrane electrode prepared by the method of the invention does not have a membrane swelling problem, good catalyst evenness and high controllable accuracy of loading amount.
Description
Technical field
The present invention relates to the preparation method of a proton exchanging film fuel battery, relate to a kind of preparation method of membrane electrode of fuel batter with proton exchange film concretely.
Background technology
Fuel cell be can be directly with the chemical energy high-efficiency cleaning of fuel be converted into the device of electric energy, fuel cell technology is one of new and high technology that receives much concern now.But Proton Exchange Membrane Fuel Cells with its start fast room temperature-operating, no electrolyte loss, the specific power advantages of higher becomes the widest fuel cell of adaptability, also is current fuel cell of greatest concern, have a wide range of applications.
Membrane electrode (being called for short MEA) is the core component of fuel cell, and by proton exchange membrane, Catalytic Layer, gas diffusion layers are formed, to the fuel cell performance decisive role.The performance of MEA is except outside the Pass having with raw material, and is also closely related with structure, and therefore the preparation method to MEA studies very necessary.Fuel cell the three phase boundary that responds all in Catalytic Layer carry out, the structure of Catalytic Layer directly determines the performance of membrane electrode.Therefore the preparation method who improves Catalytic Layer is one of important channel of improving the MEA performance.
The Catalytic Layer preparation method has multiple, comprises spraying process, scraper coating, silk screen printing etc.
Chinese patent CN1838456A discloses the method that a kind of direct spraying prepares fuel cell membrane electrode, he is after proton exchange membrane is done preliminary treatment, be fixed in the film fixture, under illumination, the cathode and anode catalyst slurry be sprayed on the both sides of film then respectively, make by low temperature drying.Zhi Bei membrane electrode has catalyst and combines with proton exchange membrane closely, need not film is carried out pre-swelling treatment by this method, need not the advantage of hot pressing.But be to use the spray gun spraying to be difficult to accomplish coating evenly, also be difficult to resolve the problem that the slip of determining splashes, cause catalyst loss.In addition, the swelling of proton exchange membrane must take place, and fixes with the film fixed frame by force, and this mandatory stress stretching action can make membrane structure cause to a certain degree destruction.
Japan Patent JP5538934 mentions Pt directly is deposited on the film surface by chemical reduction reaction, and the advantage of this method is that technology is simple, but the film swelling is more serious.
Advantages such as a kind of method commonly used is silk screen printing, and it is simple that it has technology, and the equipment maturation is low to the slip requirement, and last carrying capacity is big.But silk screen printing has its unavoidable problem, the Catalytic Layer total surface that has been coated with is to have striped, this is the marking in silk screen silk footpath, relatively large at the pressure that wire mark place Catalytic Layer is subjected to, it is solid especially that catalyst is pressed, cause overall distribution inhomogeneous, be easy to generate crackle during oven dry around these wire marks.
Chinese patent CN1560950A discloses the method for the synthetic ultra-thin core component of Proton Exchange Membrane Fuel Cells of a kind of direct method, it is that the slip that will contain catalyst, proton exchange film resin, water-repelling agent, solvent and surfactant is prepared into powder, by laser printing technology or Xeroxing powder is transferred on the proton exchange membrane.The advantage of this method is that proton exchange membrane does not have swelling and distortion, and uniformity is better.Can cause each component distributing inhomogeneous but slip is prepared into powder, owing to be that powder is printed, the fastness that combines of catalyst and film can be very not high, the very difficult assurance of the last carrying capacity of catalyst.
Summary of the invention
It is even to the purpose of this invention is to provide a kind of catalyst distribution, and last carrying capacity is controlled, and the method for preparing membrane electrode of crackle can not appear in Catalytic Layer.
To achieve these goals, technical scheme of the present invention is as follows:
The method for preparing membrane electrode of one proton exchanging film fuel battery comprises the steps:
(1) catalyst, proton exchange membrane resin solution, solvent, pH value conditioning agent and dispersant are made ink-jet ink;
(2) with ink-jet printer with the ink-jet ink in the step (1), under 30 ℃～45 ℃, print on the stock.
The mass ratio of described catalyst, proton exchange membrane resin solution, solvent, pH value conditioning agent and dispersant is 1～5:10～30:80～1000:0.1～1.0:0.05～0.1.
Described step can also comprise surfactant in (1), and described surfactant can be the water soluble surfactant active, as dodecyl sodium sulfate, nonyl phenolic compound, multicomponent alcoholics compound.
Described catalyst is meant any suitable catalyst, can be to support or non-supported platinum or platinum Quito unit metallic catalyst, and as PtM or PtM/C, wherein M is one or more simple substance or its oxide that is selected from transition metal.
Described proton exchange film resin is meant the perfluorinated sulfonic resin with sulfonic acid group, as the nafion resin of E.I.Du Pont Company, and the Kraton G1650 resin of Dias company, or other have the polymer of proton exchange function.
Described solvent is meant one or more the mixture in deionized water, alcohol, ether, ester, the ketone.
Described pH value conditioning agent is Na0H, Na
2CO
3, NaHCO
3, NH
3, in the organic ammonium one or more.
Described dispersant is a waterborne pigment dispersant.
Printer of the present invention can adopt the piezoelectric type printer; be externally connected to heating element; mode by the heating while printing prints to ink-jet ink on the proton exchange membrane, promptly beats the promptly dried proton exchange membrane swelling set of having avoided, and guard catalyst is not damaged effectively.
Described stock can be proton exchange membrane or gaseous diffusion subgrade.
When described stock is proton exchange membrane, its main operational steps is: 1. the print cartridge with printer takes out, with behind the cleaning fluid cleaning printer pipeline ink-jet ink being poured in the continuous ink-supply system (supplying hereinafter to be referred as connecting), select the pipeline of original black ink, the company of installing is for system; 2. make black or grey figure, the size of figure is the required active catalyst area of membrane electrode; 3. heating element is heated to 30 ℃～45 ℃, the open printing program prints to a side of proton exchange membrane with ink-jet ink, repeats above-mentioned technology, ink-jet ink is printed to the opposite side of proton exchange membrane; 4. the thickness and the last carrying capacity of the Catalytic Layer of ink-jet ink formation can be controlled by the gray scale and the printing times of figure.
When described stock was the gaseous diffusion subgrade, its main operational steps was: 1. ink-jet ink is irritated
Go into the print cartridge of printer; 2. make black or grey figure, the size of figure is the required active catalyst area of membrane electrode; 3. on the diffusion subgrade, spray one deck water-soluble resin (prevent that catalyst is penetrated into the diffusion subgrade, this layer resin can dissolve) as thin as a wafer in advance in activation process; 4. heating element is heated to 30 ℃～45 ℃, the open printing program prints to the diffusion subgrade with ink-jet ink; 5. the thickness and the last carrying capacity of the Catalytic Layer of ink-jet ink formation can be controlled by the gray scale and the printing times of figure.
Described water-soluble resin can be any water-soluble material preferably, as polyvinyl alcohol, polyvinyl butyral resin, polyethylene glycol, polyvinylpyrrolidone, polyacrylamide, polymine, polyethylene glycol oxide, polyacrylic acid, native starch, natural plant gum, animal glue (casein), be used to prevent that catalyst is penetrated into the diffusion subgrade, this layer resin can dissolve in activation process.
The present invention is applied to fuel cell field with inkjet technology, and the last carrying capacity by the digital technology control catalyst, the thickness of Catalytic Layer, area shape etc. are guaranteed the homogeneity and the consistency of Catalytic Layer can realize suitability for industrialized production; Spread on the subgrade spraying water-soluble resin in addition and can prevent effectively that catalyst is to the infiltration of diffusion subgrade.
Therefore compared with prior art, the present invention has following advantage: (1) is simple to operate, and cost is low, can realize suitability for industrialized production; (2) high conformity, the precision height; (3) the catalyst layer thin and thick is controlled, and thickness in monolayer can reach below 1 micron, and Catalytic Layer thickness is reached more than 5 microns, and very even; (4) because the present invention heats, quickened the rate of drying of the Catalytic Layer of ink-jet ink formation, and inkjet printing itself has ink droplet little, promptly beats the characteristics of promptly doing in the process of printing, so eliminate the proton exchange membrane swelling set substantially, the catalyst loss amount is little; (5) each ink droplet and proton exchange membrane are in conjunction with very tight, and final whole Catalytic Layer and proton exchange membrane are in conjunction with tight.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail, but the present invention is not limited only to the following examples.
Embodiment 1:
Get 0.1gJoncryl68 (production of Johnson polymer Co., Ltd.) and add the water stirring, after the uniform dissolution, to wherein adding 1g Pt/C catalyst, treat evenly wetting after, the Nafion solution (E.I.Du Pont Company's production) that adds 80ml deionized water and 10g5wt%, sand milling 120min adds 0.05gNa0H again and regulates pH value to 7, adds then and makes ink-jet ink after the 0.06g dodecyl sodium sulfate mixes.
The print cartridge of piezoelectric type printer is taken out, clean the printer pipeline after, the ink-jet ink of making poured into connect in the system, select the pipeline of original black ink, companys of installing supplies system; Then make a black graphics, the size of figure is the required active catalyst area of membrane electrode; External heating element is heated to 42 ℃, and the open printing program prints to a side of Nafion film (E.I.Du Pont Company's production) with ink-jet ink, repeats above-mentioned technology, ink-jet ink is printed to the opposite side of Nafion film; Then made membrane electrode in 30 minutes 80 ℃ of following vacuumizes.
Embodiment 2:
Get the 14g carbon dust, with putting into vacuum drying chamber after the grinder grinding, take out at 80 ℃ of freeze-day with constant temperature 2h, add 200gl, the 2-propylene glycol, slowly stirring the back ultrasonic wave disperseed 30 minutes, the PTFE emulsion that adds 30g 20wt% more slowly stirred under the frozen water cooling condition ultrasonic dispersion 30 minutes at glass bar, was applied to the carbon paper surface with silk screen then, 365 ℃ of dryings make the gaseous diffusion subgrade.
Get 0.5gSolsperse 27000 (three Co., Ltd. of Japan produce) and add the water stirring, after the uniform dissolution, to wherein adding 5g PtRu/C catalyst, treat evenly wetting after, add the Nafion solution (E.I.Du Pont Company's production) of 500ml ethanol and 25g5wt%, sand milling 120min adds 0.07g Na again
2CO
3Regulate pH value to 8, add then and make ink-jet ink after 0.3g nonyl phenol mixes.
The print cartridge of piezoelectric type printer is taken out, clean the printer pipeline after, the ink-jet ink of making poured into connect in the system, select the pipeline of original black ink, companys of installing supplies system; Then make a grey figure, the size of figure is the required active catalyst area of membrane electrode; External heating element is heated to 30 ℃, and the open printing program prints to ink-jet ink the gaseous diffusion subgrade for preparing; Then made membrane electrode in 30 minutes 80 ℃ of following vacuumizes.
Embodiment 3:
Get 1.0gTrilon X100 (production of Switzerland lark waffle company) and add the water stirring, after the uniform dissolution, to wherein adding 4g Pt/C catalyst, treat evenly wetting after, add 1000ml deionized water and the mixed solution of methyl ether and the Nafion solution (E.I.Du Pont Company's production) of 30g5wt%, sand milling 120min adds 0.1g NaHCO again
3Regulate pH value to 7, add then and make ink-jet ink after the 0.5g polyoxyethylene mixes.
The print cartridge of piezoelectric type printer is taken out, clean the printer pipeline after, the ink-jet ink of making poured into connect in the system, select the pipeline of original black ink, companys of installing supplies system; Then make a black graphics, the size of figure is the required active catalyst area of membrane electrode; External heating element is heated to 36 ℃, and the open printing program prints to a side of Nafion film (E.I.Du Pont Company's production) with ink-jet ink, repeats above-mentioned (printing) technology, ink-jet ink is printed to the opposite side of Nafion film; Then made membrane electrode in 30 minutes 80 ℃ of following vacuumizes.
Embodiment 4:
Get 1.0gTrilon X100 (production of Switzerland lark waffle company) and add the water stirring, after the uniform dissolution, to wherein adding 4.5g Pt/C catalyst, treat evenly wetting after, add 1000ml deionized water and the mixed solution of methyl ether and the Nafion solution (E.I.Du Pont Company's production) of 30g5wt%, sand milling 100min adds 0.07gNH3 and organic ammonium again and regulates pH value to 7, adds then and makes ink-jet ink after the 0.5g polyoxyethylene mixes.
The print cartridge of piezoelectric type printer is taken out, clean the printer pipeline after, the ink-jet ink of making poured into connect in the system, select the pipeline of original black ink, companys of installing supplies system; Then make a black graphics, the size of figure is the required active catalyst area of membrane electrode; The open printing program is heated to 45 ℃ with heating element, and ink-jet ink is printed to a side of KratonG1650 resin (production of Dias company), repeats above-mentioned technology, ink-jet ink is printed to the opposite side of Nafion film; Then made membrane electrode in 30 minutes 80 ℃ of following vacuumizes.
Claims (10)
- The preparation method of [claim 1] a kind of membrane electrode of fuel batter with proton exchange film is characterized in that:(1) catalyst, proton exchange membrane resin solution, solvent, pH value conditioning agent and dispersant are made ink-jet ink;(2) with ink-jet printer with the ink-jet ink in the step (1), under 30 ℃～45 ℃, print on the stock.
- The preparation method of [claim 2] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that described ink-jet printer is the piezoelectric type printer.
- The preparation method of [claim 3] membrane electrode of fuel batter with proton exchange film according to claim 1 and 2 is characterized in that described ink-jet printer is connected with heating element.
- The preparation method of [claim 4] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that described stock is proton exchange membrane or gaseous diffusion subgrade.
- The preparation method of [claim 5] membrane electrode of fuel batter with proton exchange film according to claim 4 is characterized in that:When described stock was proton exchange membrane, described operating procedure was: (1) pours into ink-jet ink in the continuous ink-supply system; (2) make black or grey figure; (3) heating element is heated to 30 ℃～45 ℃, the open printing program prints to ink-jet ink the both sides of proton exchange membrane;When described stock was the gaseous diffusion subgrade, described operating procedure was: (1) is spraying one deck water-soluble resin on the diffusion subgrade; (2) ink-jet ink is poured into the print cartridge of printer; (3) make black or grey figure; (4) heating element is heated to 30 ℃～45 ℃, the open printing program prints to ink-jet ink on the diffusion subgrade.
- The preparation method of [claim 6] membrane electrode of fuel batter with proton exchange film according to claim 1, the mass ratio that it is characterized in that described catalyst, proton exchange membrane resin solution, solvent, pH value conditioning agent and dispersant is 1～5:10～30:80～1000:0.1～1.0:0.05～0.1.
- The preparation method of [claim 7] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that also comprising surfactant in the described step (1) that described surfactant is the water soluble surfactant active.
- The preparation method of [claim 8] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that described proton exchange film resin is meant the perfluorinated sulfonic resin with sulfonic acid group.
- The preparation method of [claim 9] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that described pH value conditioning agent is NaOH, Na 2CO 3, NaHCO 3, NH 3, one or more the mixture in the organic ammonium.
- The preparation method of [claim 10] membrane electrode of fuel batter with proton exchange film according to claim 1 is characterized in that described dispersant is a waterborne pigment dispersant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810300046XA CN101483241A (en) | 2008-01-09 | 2008-01-09 | Preparation for membrane electrode of fuel cell with proton exchange film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810300046XA CN101483241A (en) | 2008-01-09 | 2008-01-09 | Preparation for membrane electrode of fuel cell with proton exchange film |
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|---|---|
| CN101483241A true CN101483241A (en) | 2009-07-15 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102986068A (en) * | 2010-09-29 | 2013-03-20 | 原子能与替代能源委员会 | Refrigerated ink jet device and method implementing such a device |
| CN108767297A (en) * | 2018-05-25 | 2018-11-06 | 上海交通大学 | A kind of preparation method of fuel cell membrane electrode |
| CN109921031A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of alkaline anion-exchange membrane fuel cell membrane electrode |
| 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 |
| CN112259753A (en) * | 2020-10-21 | 2021-01-22 | 鸿基创能科技(广州)有限公司 | Catalyst slurry for membrane electrode, method for producing same, catalyst-coated membrane, and membrane electrode |
| CN112980247A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | High-stability ink-jet printing ink for fuel cell and preparation and application thereof |
| CN113314720A (en) * | 2021-06-03 | 2021-08-27 | 中国科学院化学研究所 | Preparation method and application of patterned membrane electrode |
| CN113594472A (en) * | 2021-09-16 | 2021-11-02 | 无锡威孚高科技集团股份有限公司 | Ink for membrane electrode of proton exchange membrane fuel cell and preparation method thereof |
| CN113871761A (en) * | 2021-09-23 | 2021-12-31 | 嘉兴南湖学院 | Air cathode catalyst layer ink suitable for aerosol printing and preparation method thereof |
| CN115537068A (en) * | 2022-09-06 | 2022-12-30 | 中国科学院大连化学物理研究所 | Membrane electrode catalysis layer ink-jet printing ink and preparation method and application thereof |
-
2008
- 2008-01-09 CN CNA200810300046XA patent/CN101483241A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102986068A (en) * | 2010-09-29 | 2013-03-20 | 原子能与替代能源委员会 | Refrigerated ink jet device and method implementing such a device |
| CN109921031A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of alkaline anion-exchange membrane fuel cell membrane electrode |
| CN108767297B (en) * | 2018-05-25 | 2021-11-23 | 上海交通大学 | Preparation method of fuel cell membrane electrode |
| CN108767297A (en) * | 2018-05-25 | 2018-11-06 | 上海交通大学 | A kind of preparation method of fuel cell membrane electrode |
| 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 |
| CN112980247A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | High-stability ink-jet printing ink for fuel cell and preparation and application thereof |
| CN112259753A (en) * | 2020-10-21 | 2021-01-22 | 鸿基创能科技(广州)有限公司 | Catalyst slurry for membrane electrode, method for producing same, catalyst-coated membrane, and membrane electrode |
| CN113314720A (en) * | 2021-06-03 | 2021-08-27 | 中国科学院化学研究所 | Preparation method and application of patterned membrane electrode |
| CN113594472A (en) * | 2021-09-16 | 2021-11-02 | 无锡威孚高科技集团股份有限公司 | Ink for membrane electrode of proton exchange membrane fuel cell and preparation method thereof |
| CN113871761A (en) * | 2021-09-23 | 2021-12-31 | 嘉兴南湖学院 | Air cathode catalyst layer ink suitable for aerosol printing and preparation method thereof |
| CN113871761B (en) * | 2021-09-23 | 2023-04-28 | 嘉兴南湖学院 | Air cathode catalytic layer ink suitable for aerosol printing and preparation method thereof |
| CN115537068A (en) * | 2022-09-06 | 2022-12-30 | 中国科学院大连化学物理研究所 | Membrane electrode catalysis layer ink-jet printing ink and preparation method and application thereof |
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Open date: 20090715 |