CN100524913C - Method for preparing membrane electrode of direct methanol fuel cell - Google Patents
Method for preparing membrane electrode of direct methanol fuel cell Download PDFInfo
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- CN100524913C CN100524913C CNB2005100338165A CN200510033816A CN100524913C CN 100524913 C CN100524913 C CN 100524913C CN B2005100338165 A CNB2005100338165 A CN B2005100338165A CN 200510033816 A CN200510033816 A CN 200510033816A CN 100524913 C CN100524913 C CN 100524913C
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Abstract
The invention discloses a method for making a membrane electrode of direct methanol fuel battery. The membrane electrode comprises proton exchange membrane, positive electrode of carbon carried platinum-ruthenium catalyst and negative electrode of carbon carried platinum catalyst. The invention is characterized in that it reduces the usage of direct methanol fuel battery catalytic agent noble metal and lowers costs of fuel battery. The direct methanol fuel batteries assembled with the membrane electrode components has the advantages of high output power density, great performance test reproducibility.
Description
Technical field:
The present invention relates to the fuel cell technology field, particularly relate to and a kind ofly have higher power density and than the membrane electrode preparation method of the direct methanol solution fuel cell of low noble metal dosage.
Background technology:
Battery is used as relatively independent usually, and transportable supply unit uses.But existing secondary power supply all exists the lower problem of energy density.Wherein the lithium ion battery that energy density is the highest also is no more than 300Wh/kg, and other then more are low to moderate 100Wh/kg as ni-mh, chromium nickel, lead-acid battery etc.On the one hand, this has caused the excessive drawback of battery volume or weight; On the other hand, the energy of battery storage causes life cycle too short very little, need often charge for a long time, influences the use of battery.Fuel cell is a kind of by the primary cell operation principle, and the handle of isothermal is stored in the energy conversion device that chemical energy in fuel and the oxidant is converted into electric energy.Fuel cell has the specific energy density much larger than common secondary cell, and its speed that charges into fuel also is far longer than the charging rate of common batteries.The most suitable supply unit of movable equipment that this makes fuel cell become stream time is had relatively high expectations.At present, the range of application that can expect of fuel cell has: electric motor car, portable set, Military Electronic Equipment.In addition, because the combustion efficiency of fuel cell is very high, can be as the combustion efficiency of Proton Exchange Membrane Fuel Cells (PEMFC) up to more than 80%, fuel cell also can be used as the dispersed miniature power station and uses.
Research or developing fuel cell mainly contain following several now: alkaline fuel cell (AFC), phosphoric acid fuel cell (PAFC), molten carbonate fuel cell (MCFC), Solid Oxide Fuel Cell (SOFC) and Proton Exchange Membrane Fuel Cells (PEMFC).Wherein to have working temperature low for Proton Exchange Membrane Fuel Cells, and start-up time is fast, and is simple in structure, environmental friendliness, and in light weight and specific energy density advantages of higher more is applicable to portable set than other various fuel cells.
Directly using methyl alcohol is that the jet-propulsion test institute (JPL) of early 1990s American National aviation and space travel office (NASA) and the researcher of University of Southern California propose as the conception of the direct methanol fuel cell (DMFC) of the anode fuel of Proton Exchange Membrane Fuel Cells.Because methyl alcohol is liquid (64.51 ℃ of boiling points) at normal temperatures, the hydrogen more used than other fuel cells, methane or carbon monoxide have the energy density (combustion heat 726.83kJ/mol) of better storge quality and Geng Gao, so be the focus of research and development, and obtained significant progress always.
The electrode of direct methanol fuel cell is the place that electro-chemical reaction takes place.The half-cell reaction that takes place on anode is:
The half-cell reaction that takes place on negative electrode is:
In the reactant at the two poles of the earth or product, all there are gas and liquid as can be seen.This makes direct methanol fuel cell on three phase boundary electrochemical reaction could take place.In order to derive carbon dioxide and the required oxygen of importing negative electrode that anode produces, need the gas phase network in the electrode, this network is formed (in the minority design, the process of gas conduction is to realize by the dissolving of gas in solution) by the hydrophobic polymer in the electrode usually.In order to import the required first alcohol and water of anode and to derive the water that negative electrode produces, need the liquid phase network in the electrode, this network normally constitutes under the hydrophily effect of capillary force and charcoal.Also contain two kinds of networks in the solid phase: the electron conduction network that the first has catalyst granules and diffusion layer to constitute, and another is the proton conduction network that is made of proton exchange resins.
Electrode property has decisive influence to the performance of battery.The structure of this electrode is stacked, mainly is made up of diffusion layer and Catalytic Layer two parts.Direct methanol fuel cell generally adopts charcoal cloth or carbon paper as the diffusion layer in the electrode, and thickness generally is 100～300 μ m.Carbon paper generally need be done hydrophobisation and handle, and is that the polytetrafluoroethylene (PTFE) emulsion of 1～5wt% is soaked 10%～15wt% (anode) or the 20%～50wt% (negative electrode) that makes the weight of polytetrafluoroethylene (PTFE) account for whole diffusion layer repeatedly with concentration promptly.Catalytic Layer is (generally to be 1～10mg/cm by the mixed catalyst pulp that forms of catalyst, perfluor sulfoacid resin solution and other additives and solvent according to certain bullion content
2) be coated with diffusion layer surface and form.Proton exchange membrane and coated electrode are accurately aimed at the back at 120～150 ℃ by " electrode-proton exchange membrane-electrode " order, hot pressing promptly formed an integral body in 1～5 minute under 5～15MPa, be called membrane electrode assembly, for improving the adhesion between electrode and the film, can spray on electrode or brush the aqueous isopropanol of one deck perfluorinated sulfonic resin and dry at electrode, electrode surface dry state perfluorinated sulfonic resin solid supported amount be 1～2mg/cm
2Another method is directly catalyst pulp to be coated on the proton exchange membrane, and then becomes membrane electrode assembly with the diffusion layer hot binding.
Although electrode has bigger three-dimensional chemical reactivity scope and reasonable material conductive performance as mentioned above, but its diffusion layer porous surface has still caused a large amount of catalyst to be penetrated among the diffusion layer, leave the bigger zone of exchange membrane surface reaction activity, caused the certain decline of catalyst utilization.
Summary of the invention:
For addressing the above problem, the object of the present invention is to provide a kind of membrane electrode preparation method of direct methanol fuel cell, adopt the electrode of this method preparation to make battery have lower noble metal use amount and better power output performance.
The present invention is achieved through the following technical solutions: this membrane electrode is made of diffusion layer, regulating course and leveling processing layer, and diffusion layer soaks carbon paper repeatedly by ptfe emulsion and dries up, and makes after the baking; Regulating course adds an amount of alcoholic solvent by raw material of wood-charcoal material and polytetrafluoroethylene, is coated on the diffusion layer, makes after baking; The leveling processing layer makes after the baking for the perfluorinated sulfonic resin alcoholic solution is sprayed at regulating course.
The preparation method of described regulating course is: at first, take by weighing raw material of wood-charcoal material and ptfe emulsion or powder by solid weight than 70～90:30～10, add an amount of ethanol, isopropyl alcohol or methyl alcohol, through stirring or grinding; And then with the ultrasonic prepared Chinese ink shape that is dispersed into; Then this prepared Chinese ink shape solution is evenly brushed or is sprayed on the diffusion layer, form a densification and uniform raw material of wood-charcoal material and polytetrafluoroethylene mixed layer, i.e. regulating course.
The preparation method of described leveling processing layer is: at first will evenly spray the alcoholic solution that a spot of weight ratio is 1～5% perfluorinated sulfonic resin on the regulating course of sintering, wherein perfluorinated sulfonic resin solid supported amount is controlled at 0.1～1.0mg/cm
2, will coat perfluor sulfoacid resin solution regulating course afterwards then through 100～180 ℃ of bakings 1 hour, be bonded on the regulating course to make the perfluorinated sulfonic resin fusing.
The direct painting catalyst slurry on its regulating course of the diffusion layer of Huo Deing according to the method described above also can be pressed into membrane electrode assembly with the proton exchange membrane direct heat of coated catalyst pulp.During use, add Shangyang (the moon) utmost point flow-field plate (the passive type battery does not have this part) successively in the membrane electrode assembly outside, sun (the moon) utmost point current collection fluid and end plate just constitute direct methanol fuel cell.Direct methanol fuel cell electrode of the present invention and manufacture method thereof compared with prior art have following advantage: simple to operate, the regulating course composition is even, and regulating course combines with diffusion layer tightly, and Catalytic Layer and regulating course are bonding firmly, the catalyst utilization height, catalyst amount is little.The direct methanol fuel cell of assembling with the membrane electrode assembly of manufacturing of the present invention has shown good electrochemical, and its reappearance in performance test is better, and in use membrane electrode assembly is difficult for peeling off.
Description of drawings:
The present invention is further illustrated below in conjunction with accompanying drawing:
Fig. 1 is the structural representation of present direct methanol fuel cell membrane electrode;
Fig. 2 is the performance map of the embodiment of the invention one in forcing the streaming methanol fuel cell;
Fig. 3 is the performance map of the embodiment of the invention one in passive direct methanol fuel cell;
Fig. 4 is the performance map of the embodiment of the invention two in passive direct methanol fuel cell.
Embodiment:
Manufacture method of the present invention is applicable to makes the direct methanol fuel cell that adopts the carbonaceous diffusion layer.See Fig. 1, direct methanol fuel cell membrane electrode basic structure is by anode diffusion layer 1 usually at present, anode catalyst layer 2, proton exchange membrane 3, cathode catalyst layer 4, cathode diffusion layer 5 stacked compositions.The regulating course that adds described in the present invention just is between above-mentioned diffusion layer 1 (5) and the Catalytic Layer 2 (4).
The manufacture method of direct methanol fuel cell electrode mainly comprises the steps among the present invention.
A. the hydrophobization of diffusion layer.With concentration is that the polytetrafluoroethylene (PTFE) emulsion of 1～5wt% is soaked repeatedly and dried up 10～15wt% (anode) or the 20～50wt% (negative electrode) that makes the quality of polytetrafluoroethylene (PTFE) account for whole diffusion layer, toasted 1 hour down at 200～300 ℃ then, 300～400 ℃ were toasted 2 hours down, made the polytetrafluoroethylene (PTFE) fusing.
B. carbonaceous regulating course solid constituent chooses and preliminary treatment.Raw material of wood-charcoal material in the carbonaceous regulating course solid constituent among the present invention must be the enough tiny shot-like particle of volume.The three-dimensional dimension of carbon particle all should be controlled between 30～3000nm.The raw material of wood-charcoal material that the present invention is suitable for has carbon black, active carbon, activated carbon fiber, charcoal-aero gel, carbon nano-tube or their mixture.As when adopting active carbon, activated carbon fiber and charcoal-aero gel, need carry out ball milling or shear preliminary treatment it.The PTFE emulsion that adopts among the present invention should contain the PTFE solid masses should be more than 40wt% (weight ratio), in order to avoid too much water has a negative impact to the dispersiveness of raw material of wood-charcoal material.Calculate with solid masses, PTFE content in regulating course should be controlled between 10～30wt%, and all the other compositions are the raw material of wood-charcoal material.
C. the preparation of regulating course slurry.The regulating course slurry that the present invention uses is basic solvent with low-carbon alcohols, and the water content of alcohols needs below 5wt%.Take by weighing weight and be 5～20 parts alcohol, add weight and be 1 part raw material of wood-charcoal material, stir and ultrasonic dispersion number minute, the PTFE emulsion of the corresponding deal that takes by weighing in step a or powder are also added in the suspension-turbid liquid of ultrasonic dispersion.Then this suspension-turbid liquid is worn into shinny dense thick liquid with colloid mill, and then to add weight be 20～200 parts alcohol, ultrasonic dispersion obtained required prepared Chinese ink shape liquid in 0.5～1 hour under the frequency of 40～59kHz.
D. the coating of regulating course.Regulating course can adopt the mode of brushing, blade coating or spraying to be coated on the diffusion layer.Brush, to scrape coating method as follows: drop on the diffusion layer with the prepared Chinese ink shape fluid drips number of glue head dropper gained in the b step, thin slice with row brush or neat in edge is brushed liquid flat gently, dry up or the roaster drying liquid with hair dryer, repeat this process and get final product for 3～8 times.The method of spraying is as follows: with spray gun prepared Chinese ink shape liquid is sprayed on the surface of diffusion layer uniformly, dries up, repeat this process and get final product for 3～10 times.Regulating course (solid) quality on the every square centimeter of diffusion layer in coating back should be between 1～2mg.
E. the heat treatment of regulating course.In order to improve the adhesion of regulating course and diffusion layer, the diffusion layer of coated regulating course is placed on is heated to 200～300 ℃ in the baking oven, constant temperature 0.5～1 hour allows the activating agent of PTFE remained on surface fully decompose and gasifies; Baking oven is warming up to 300～400 ℃ then, constant temperature 1～2 hour allows PTFE fully melt, and fully merges with the raw material of wood-charcoal material.
F. improve the caking property of regulating course.Perfluor sulfoacid resin solution is diluted to mass ratio 1～5wt% in alcohols, fully stirs evenly, operable alcohols has methyl alcohol, ethanol, isopropyl alcohol, butanols etc.Evenly spray the alcoholic solution of the perfluorinated sulfonic resin that modulates on a small quantity on the regulating course surface with spray gun, dry up, repeat this process 10～20 times.Perfluorinated sulfonic resin solid supported amount should be controlled at 0.1～1.0mg/cm on the regulating course
2A spot of perfluor sulfoacid resin solution can provide adhesive property good between Catalytic Layer and the regulating course.
G. to containing the heat treatment of perfluorinated sulfonic resin regulating course.To be placed in the baking oven through the diffusion layer of the band regulating course of e step process,, make the perfluorinated sulfonic resin fusing that is sprayed on the regulating course surface and infiltrate regulating course with 130～200 ℃ of bakings 1～2 hour.This tack coat can hot pressing prepare fusing once again in the process of membrane electrode assembly and and Catalytic Layer in perfluorinated sulfonic resin
H. merge, constitute firm resin network, improved the adhesion between Catalytic Layer and the regulating course.
According to the diffusion layer process painting catalyst slurry that above method makes, spray perfluor sulfoacid resin solution and just can be pressed into membrane electrode assembly afterwards with proton exchange membrane pressure with 5～15Mpa under 130～140 ℃.Add Shangyang (the moon) utmost point flow-field plate (in the passive type battery, not having this part) successively in the membrane electrode assembly both sides, sun (the moon) utmost point current collection fluid.In forcing the streaming battery, anode flow field board closely contacts with cathode diffusion layer with the anode diffusion layer of membrane electrode assembly respectively with cathode flow field plate; In the passive type battery, the medial surface of anode current collection fluid and negative electrode current collection fluid closely contacts with cathode diffusion layer with the anode diffusion layer of membrane electrode assembly respectively.Other metallic plates that described flow-field plate and current collection fluid available heat are separated graphite, expanded graphite, stainless steel or had methanol tolerance corrosion coating are made.Outermost end plate play a part the insulation and to internal pressurization.
Following specific embodiment is prepared acquisition according to above-mentioned manufacture method.
Embodiment 1: handle carbon paper with the PTFE emulsion hydrophobization of 3wt%, make PTFE quality therein account for 10% and 30% and sintering respectively; The carbon paper that contains PTFE quality 10% is an anode diffusion layer, and what contain PTFE quality 30% is cathode diffusion layer.The PTFE emulsion of getting acetylene type carbon black and 60% than 80: 20 by solid masses adds the acetylene type carbon black of 1 part of quality in the ethanol of 10 parts of quality, stirs and ultrasonic dispersion 3 minutes; With colloid mill it is worn into shinny liquid again after adding the PTFE emulsion that takes by weighing; The ethanol that adds 100 parts of quality, ultrasonic dispersion half an hour.Blade coating is on diffusion layer repeatedly with thin PVC (polyvinyl chloride) sheet with gained prepared Chinese ink shape liquid, and drying up until the regulating course carrying capacity with hair dryer is 1.5mg/cm
2This diffusion layer was toasted 1 hour down at 240 ℃, toasted 2 hours down at 350 ℃ again.The spray solid loadings is 0.1mg/cm on regulating course after cooling
2Nafion solution, and then 150 ℃ of down bakings 1 hour.On the anode diffusion layer with thin PVC sheet blade coating on the metal carrying capacity be 3.6mg/cm
2PtRu/C (charcoal carries the platinum ruthenium) catalyst layer, scraping the matel coated carrying capacity at cathode diffusion layer is 2.4mg/cm
2Pt/C (charcoal carries platinum) Catalytic Layer.Under 140 ℃ and 15Mpa, anode, proton exchange membrane and negative electrode are compressed on the membrane electrode assembly that thickness is 0.87mm.Its performance in forcing streaming and passive direct methanol fuel cell is shown in Fig. 2,3.
Embodiment 2: roughly as embodiment 1, just be used in PTFE powder replacement PTFE emulsion when doing regulating course.Regulating course carrying capacity 1.2mg/cm
2, anode PtRu/C catalyst layer metal carrying capacity 3mg/cm
2, negative electrode Pt/C catalyst layer metal carrying capacity 1mg/cm
2Its performance in passive direct methanol fuel cell as shown in Figure 4.
Claims (3)
1, a kind of membrane electrode preparation method of direct methanol fuel cell is characterized in that: this membrane electrode comprises diffusion layer, regulating course and leveling processing layer, and diffusion layer soaks carbon paper repeatedly by ptfe emulsion and dries up, and makes after the baking; Regulating course adds an amount of alcoholic solution by the material with carbon element and the polytetrafluoroethylene of three-dimensional dimension between 20-3000nm, is coated on the diffusion layer, makes after baking; The leveling processing layer is that the alcoholic solution of perfluorinated sulfonic resin is sprayed at regulating course, makes after the baking.
2, the membrane electrode preparation method of direct methanol fuel cell according to claim 1, it is characterized in that: the preparation method of described regulating course is: at first, take by weighing material with carbon element and ptfe emulsion or powder by solid weight than 70～90:30～10, add an amount of ethanol, isopropyl alcohol or methyl alcohol, through stirring or grinding; And then with the ultrasonic prepared Chinese ink shape that is dispersed into; Then this prepared Chinese ink shape solution is evenly brushed or is sprayed on the diffusion layer, form a densification and uniform material with carbon element and polytetrafluoroethylene mixed layer, i.e. regulating course.
3, the membrane electrode preparation method of direct methanol fuel cell according to claim 1 and 2, it is characterized in that: the preparation method of described leveling processing layer is: at first will evenly spray the alcoholic solution that a spot of weight ratio is 1～5% perfluorinated sulfonic resin on the regulating course of sintering, wherein perfluorinated sulfonic resin solid supported amount is controlled at 0.1～1.0mg/cm
2, will coat perfluor sulfoacid resin solution regulating course afterwards then through 100～180 ℃ of bakings 1 hour, be bonded on the regulating course to make the perfluorinated sulfonic resin fusing.
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| CNB2005100338165A CN100524913C (en) | 2005-04-01 | 2005-04-01 | Method for preparing membrane electrode of direct methanol fuel cell |
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| CNB2005100338165A CN100524913C (en) | 2005-04-01 | 2005-04-01 | Method for preparing membrane electrode of direct methanol fuel cell |
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| CN100524913C true CN100524913C (en) | 2009-08-05 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101540405A (en) * | 2008-01-25 | 2009-09-23 | 汉能科技有限公司 | Fuel cell leveling layer composition and preparation method thereof as well as gas diffusion layer |
| CN102769141A (en) * | 2012-08-01 | 2012-11-07 | 新源动力股份有限公司 | Membrane electrode assembly of proton exchange membrane fuel cell and manufacturing method of membrane electrode assembly |
| CN103926284B (en) * | 2013-01-11 | 2016-12-28 | 深圳市深安旭传感技术有限公司 | The manufacture method of porous gas diffusive electrode |
| CN109449466B (en) * | 2018-10-23 | 2020-11-24 | 山东潍氢动力科技有限公司 | Preparation method of membrane electrode and preparation method of anode catalyst layer of membrane electrode |
| CN116742043B (en) * | 2023-06-09 | 2024-08-13 | 哈尔滨工业大学 | PDMFC with methanol solid-state storage fuel supply structure and working method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487610A (en) * | 2003-08-13 | 2004-04-07 | 中国科学院长春应用化学研究所 | Prepn of electrode for proton exchange film fuel cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1487610A (en) * | 2003-08-13 | 2004-04-07 | 中国科学院长春应用化学研究所 | Prepn of electrode for proton exchange film fuel cell |
Non-Patent Citations (2)
| Title |
|---|
| Development of high-power electrodes for a liquid-feed directmethanol fuel cell. C. Lim,C.Y.Wang.Journal of Power Sources,Vol.113 . 2003 |
| Development of high-power electrodes for a liquid-feed directmethanol fuel cell. C. Lim,C.Y.Wang.Journal of Power Sources,Vol.113 . 2003 * |
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