CN110212224A - A method of porous membrane electrode is prepared using ice template method - Google Patents
A method of porous membrane electrode is prepared using ice template method Download PDFInfo
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- CN110212224A CN110212224A CN201910434431.1A CN201910434431A CN110212224A CN 110212224 A CN110212224 A CN 110212224A CN 201910434431 A CN201910434431 A CN 201910434431A CN 110212224 A CN110212224 A CN 110212224A
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- electrode layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8605—Porous electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8814—Temporary supports, e.g. decal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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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 kind of methods for preparing porous membrane electrode using ice template method, which comprises S1 mixes catalyst, binder and dispersion solvent, obtains cathode and Anode inks；The cathode inks are coated on release film by S2, obtain undried negative electrode layer；S3 will carry out vacuum freeze drying after the electrode layer freeze forming, obtain dry negative electrode layer；The Anode inks are coated on release film and are dried by S4, obtain dry anode electrode layer；The cathode and anode electrode layer are transferred to proton exchange membrane two sides and form membrane electrode by S5.In S3, use ice particle as template, the removal of ice granular formwork is realized by the vacuum freeze drying.The solvent includes deionized water and alcohols solvent.For the present invention using ice particle as template, orderly electrode structure is constructed in the pore-creating in fuel battery cathode with proton exchange film electrode layer, reduces resistance to mass tranfer, improves battery performance.
Description
Technical field
The present invention relates to field of fuel cell technology, are related to a kind of preparation side of membrane electrode of fuel batter with proton exchange film
Method more particularly to a kind of method for preparing porous membrane electrode using ice template method.
Background technique
Today of rapid economic development, energy environment issues have become major issue closely related to human life.
Proton Exchange Membrane Fuel Cells is as a kind of energy conversion device, under isothermal conditions directly will storage by redox reaction
There are the chemical energy in various fuel and oxidant to be converted into electric energy, have energy conversion efficiency it is high, it is environmental-friendly, noiseless and
The features such as high reliablity, is considered as the ultimate solution of future automobile power resources.Fancy price is always to hinder fuel
It the main reason for battery car large-scale commercial, searches to the bottom, fuel cell car pile cost is mainly derived from membrane electrode
In the platinum based catalyst that generallys use.
However, reducing the usage amount of platinum based catalyst in membrane electrode, the activation polarization of battery, Geng Huizeng not only will increase
The concentration polarization of big battery, in low platinum or ultralow platinum film electrode, slowly, mass transfer problem is prominent for the diffusion of electrode interior oxygen, at
For the factor of attention for limiting cell power density.
The method of common improvement mass transfer problem has the composition proportion adjusted in slurry, improves membrane electrode moulding process and add
Add pore creating material etc., but the former two's effect is not obvious, and pore creating material is often difficult to remove and poison catalyst granules, causes instead
Fuel battery performance decline.
Summary of the invention
In view of this, a kind of preparing porous membrane electrode using ice template method the technical problem to be solved in the present invention is that providing
Method reduce resistance to mass tranfer by constructing orderly electrode structure, improve battery performance.
The purpose of the present invention is what is be achieved through the following technical solutions:
The present invention provides a kind of methods for preparing porous membrane electrode using ice template method, which comprises
S1 mixes catalyst, binder and dispersion solvent, and ball milling disperses after stirring；Cathode inks are made respectively
And Anode inks；
The cathode inks are coated on release film by S2, obtain undried negative electrode layer；
S3 will carry out vacuum freeze drying after the undried negative electrode layer freeze forming, obtain dry cathode electricity
Pole layer；
The Anode inks are coated on release film and are dried by S4, obtain dry anode electrode layer；
S5 is by the negative electrode layer of the drying and dry anode electrode layer hot-pressing transfer printing to proton exchange membrane two sides shape
At membrane electrode.
Preferably, dispersion solvent described in S1 is the mixed solvent of deionized water and alcohols that mass ratio is 1:1~100.
Preferably, the alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol and tertiary fourth
At least one of alcohol.
Preferably, in S3, the water freezing when freeze forming in slurry forms ice granular formwork；Ice granular formwork
Removal is realized by the vacuum freeze drying.
Preferably, in S1, the mass ratio of the catalyst, binder and dispersion solvent is 1:1~10:10~1000.
Preferably, in S1, the catalyst is selected from carbon-supported Pt catalyst, carbon-supported Pt alloy catalyst or carbon load
The Pt single-layer catalyst of load.Wherein, Pt catalyst refers to the catalyst of pure Pt particle；Pt single-layer catalyst refers in a non-Pt
Core outside deposition have the catalyst of one layer of monolayer Pt.
Preferably, binder described in S1 in perfluorosulfonic acid ion resin solution and polytetrafluoroethylsolution solution at least
It is a kind of.
Preferably, in S1, then the catalyst pulp was divided using ultrasonic agitation 10-60 minutes using ball mill
It dissipates 1-24 hours.
Preferably, the method for coating described in S2 and S4 is respectively selected from spray coating method, silk screen print method, doctor-blade casting process, brush
Coating or slit casting die.
Preferably, the temperature of freeze forming described in S3 is -200 DEG C~0 DEG C, the temperature of the vacuum freeze drying is -
60 DEG C~-40 DEG C.
Preferably, the temperature of hot-pressing transfer printing described in S5 is 80 DEG C~150 DEG C, and pressure is 1MPa~15MPa, and the time is
60s~600s.
Compared with prior art, the invention has the following beneficial effects:
The present invention using ice particle as template, constructed by the pore-creating in fuel battery cathode with proton exchange film electrode layer
Resistance to mass tranfer is greatly reduced in sequence electrode structure, improves battery performance；Clean ice particle, which will not pollute, simultaneously poisons catalyst,
And can be completely removed under conditions of vacuum freeze drying, it ensure that catalyst activity is without damage.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the test performance figure of porous membrane electrode prepared by embodiment 1；
Fig. 2 is the test performance figure of traditional membrane electrode prepared by comparative example 1.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection scope.
Following embodiment provides a kind of method for preparing porous membrane electrode using ice template method, the preparation method packet
It includes:
S1 mixes catalyst, binder and dispersion solvent, and ball milling disperses after stirring；Cathode inks are made respectively
And Anode inks；
The cathode inks are coated on release film by S2, obtain undried negative electrode layer；
S3 will carry out vacuum freeze drying after the undried negative electrode layer freeze forming, obtain dry cathode electricity
Pole layer；
The Anode inks are coated on release film and are dried by S4, obtain dry anode electrode layer；
S5 is by the negative electrode layer of the drying and dry anode electrode layer hot-pressing transfer printing to proton exchange membrane two sides shape
At membrane electrode.
Preferably, dispersion solvent described in S1 is the mixed solvent of deionized water and alcohols that mass ratio is 1:1~100.
Preferably, the alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol and tertiary fourth
At least one of alcohol.
Preferably, in S3, the water freezing when freeze forming in slurry forms ice granular formwork；Ice granular formwork
Removal is realized by the vacuum freeze drying.
Preferably, in S1, the mass ratio of the catalyst, binder and dispersion solvent is 1:1~10:10~1000.
Preferably, in S1, the catalyst is selected from carbon-supported Pt catalyst, carbon-supported Pt alloy catalyst or carbon
The Pt single-layer catalyst supported.Wherein, Pt catalyst refers to the catalyst of pure Pt particle；Pt single-layer catalyst refers to non-at one
The core outside deposition of Pt has the catalyst of one layer of monolayer Pt.
Preferably, binder described in S1 in perfluorosulfonic acid ion resin solution and polytetrafluoroethylsolution solution at least
It is a kind of.
Preferably, in S1, then the catalyst pulp was divided using ultrasonic agitation 10-60 minutes using ball mill
It dissipates 1-24 hours.
Preferably, the method for coating described in S2 and S4 is respectively selected from spray coating method, silk screen print method, doctor-blade casting process, brush
Coating or slit casting die.
Preferably, the temperature of freeze forming described in S3 is -200 DEG C~0 DEG C, the temperature of the vacuum freeze drying is -
60 DEG C~-40 DEG C.
Preferably, the temperature of hot-pressing transfer printing described in S5 is 80 DEG C~150 DEG C, and pressure is 1MPa~15MPa, and the time is
60s~600s.
Embodiment 1
The preparation step for preparing porous membrane electrode using ice template method of the present embodiment is as follows:
1, the preparation of catalyst pulp
Sequentially add business Pt/C catalyst, deionized water, Nafion solution and isopropanol, the quality of above 4 kinds of ingredients
Than preparing cathode and Anode inks for 1:40:2:240；Wherein, the mass ratio of Nafion and carbon is 0.8:1 (matter
Amount ratio also can largely influence pore structure, and the value is constant just to can guarantee that ice template method pore-creating technique is the list for changing mass transfer
One variable), it is stirred by ultrasonic after mixing 20 minutes, is then dispersed 5 hours using ball mill；
The mass ratio of Nafion and carbon, according to experiment it is found that its range of choice be 0.1~5:1, preferably 0.5~1.5:
1；
2, negative electrode layer is coated with
On clean workbench, catalyst pulp is cast in release film using scraper on the level board of coating machine
On, obtain undried negative electrode layer.The platinum carrying capacity of cathode catalysis layer is controlled in 0.1mg Pt/cm2Left and right；
3, negative electrode layer is freeze-dried
Undried negative electrode layer after freeze forming, is carried out vacuum freeze drying at -50 DEG C, obtained at -196 DEG C
To dry negative electrode layer；
4, anode electrode layer is coated with
On clean workbench, catalyst pulp is cast on release film using scraper on the level board of coating machine
And dry, obtain dry anode electrode layer.The platinum carrying capacity of anode catalyst layer is controlled in 0.1mg Pt/cm2Left and right；
5, membrane electrode is hot-forming
Dry cathode and anode electrode are placed on proton exchange membrane two sides, in 100 DEG C, under the conditions of 5MPa, hot pressing
500s is transferred to Surface modification of proton exchange membrane.
Catalytic Layer sheet as nanoscale porous structure, the present invention using ice template method realize pore-creating, construct efficient biography
The cellular structure of matter,.Since the battery performance under high current is mainly controlled by oxygen mass transfer, i.e., mainly by electrode microstructure
It influences, therefore the pore-creating effect can be observed by performance boost of the monocell under high current.Therefore, by obtained sample
Electrochemical property test is carried out, as a result referring to Fig. 1.
Electro-chemical test is in 850e fuel cell full battery test macro (Scribner Associates company, the U.S.)
It carries out.Cell reaction temperature is 80 DEG C in this example, and relative humidity 100%, anode reaction gas is high-purity hydrogen, cathode reaction
Gas is air.Runner selected by battery is 2cm*2cm serpentine flow path.It can be seen that embodiment 1 from analysis result figure on piece to prepare
The polarization of porous membrane electrode cathode mass-transfer it is substantially reduced, and reach higher peak power.
Embodiment 2
The present embodiment prepares the preparation step of porous membrane electrode with embodiment 1 using ice template method, and institute's difference exists
In:
1, the preparation of catalyst pulp
Sequentially add business Pt/C catalyst, deionized water, Nafion solution and isopropanol, the quality of above 4 kinds of ingredients
Than for 1:1:1:9, preparing cathode and anode catalyst slurry.Wherein, the mass ratio of Nafion and carbon is 0.8.It is super after mixing
Sound stirs 10 minutes, is then dispersed 1 hour using ball mill；
2, negative electrode layer is freeze-dried
Undried negative electrode layer after freeze forming, is carried out vacuum freeze drying at -60 DEG C, obtained at -200 DEG C
To dry negative electrode layer；
3, membrane electrode is hot-forming
Dry cathode and anode electrode are placed on proton exchange membrane two sides, at 80 DEG C, under the conditions of 1MPa, hot pressing 60s,
It is transferred to Surface modification of proton exchange membrane.
The porous membrane electrode electrochemical property test manufactured in the present embodiment prepared using ice template method shows that mass transfer polarizes
Mitigate, compared with Example 1, peak power is smaller, but still better than conventional film electrode.
Embodiment 3
The present embodiment prepares the preparation step of porous membrane electrode with embodiment 1 using ice template method, and institute's difference exists
In:
1, the preparation of catalyst pulp
Sequentially add business Pt/C catalyst, deionized water, Nafion solution and isopropanol, the quality of above 4 kinds of ingredients
Than preparing cathode and Anode inks for 1:240:10:760.Wherein, the mass ratio of Nafion and carbon is 0.8, mixing
It is stirred by ultrasonic 60 minutes, is then dispersed 24 hours using ball mill afterwards；
2, negative electrode layer is freeze-dried
Undried negative electrode layer after freeze forming, vacuum freeze drying is carried out at -40 DEG C, is obtained at 0 DEG C
Dry negative electrode layer；
3, membrane electrode is hot-forming
Dry cathode and anode electrode are placed on proton exchange membrane two sides, in 150 DEG C, under the conditions of 15MPa, hot pressing
600s is transferred to Surface modification of proton exchange membrane.
The porous membrane electrode electrochemical property test manufactured in the present embodiment prepared using ice template method shows that mass transfer polarizes
Mitigate, compared with Example 1, peak power is smaller, but still better than conventional film electrode.
Embodiment 4
The present embodiment prepares the preparation step of porous membrane electrode with embodiment 1 using ice template method, and institute's difference exists
In:
1, the preparation of catalyst pulp
Sequentially add business Pt/C catalyst, deionized water, polytetrafluoroethylsolution solution and ethyl alcohol, the matter of above 4 kinds of ingredients
Amount prepares cathode and Anode inks than being 1:1:10:100.Wherein, the mass ratio of Nafion and carbon is 0.8, mixing
It is stirred by ultrasonic 60 minutes, is then dispersed 24 hours using ball mill afterwards；
The porous membrane electrode electrochemical property test manufactured in the present embodiment prepared using ice template method shows that mass transfer polarizes
Mitigate, compared with Example 1, peak power is smaller, but still better than conventional film electrode.
Comparative example 1
The preparation step of traditional membrane electrode of this comparative example 1 is as follows:
1, the preparation of catalyst pulp
Sequentially add business Pt/C catalyst, deionized water, Nafion solution and isopropanol, the quality of above 4 kinds of ingredients
Than preparing anode and cathode catalyst pulp, wherein the mass ratio of Nafion and carbon is 0.8 for 1:40:2:240.After mixing
It is stirred by ultrasonic 20 minutes, then disperses 5h using ball mill；
2, cathode and anode electrode layer coating
On clean workbench, catalyst pulp is cast on release film using scraper on the level board of coating machine
And dry, obtain dry cathode and anode electrode layer.The platinum carrying capacity of cathode and anode catalyst layer is controlled in 0.1mgPt/cm2It is left
It is right；
3, membrane electrode is hot-forming
Dry cathode and anode electrode are placed on proton exchange membrane two sides, in 100 DEG C, under the conditions of 5MPa, hot pressing
500s is transferred to Surface modification of proton exchange membrane.
Obtained sample is subjected to electrochemical property test, as a result referring to fig. 2.
Electro-chemical test is in 850e fuel cell full battery test macro (Scribner Associates company, the U.S.)
It carries out.Cell reaction temperature is 80 DEG C in this example, and relative humidity 100%, anode reaction gas is high-purity hydrogen, cathode reaction
Gas is air.Runner selected by battery is 2cm*2cm serpentine flow path.It can be seen that comparative example 1 from analysis result figure on piece to prepare
Traditional membrane electrode mass transfer serious polarization, peak power is lower.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
1. a kind of method for preparing porous membrane electrode using ice template method, which comprises
S1 mixes catalyst, binder and dispersion solvent, and ball milling disperses after stirring；Cathode inks and sun are made respectively
Electrode catalyst slurry；
The cathode inks are coated on release film by S2, obtain undried negative electrode layer；
S3 will carry out vacuum freeze drying after the undried negative electrode layer freeze forming, obtain dry cathode electrode
Layer；
The Anode inks are coated on release film and are dried by S4, obtain dry anode electrode layer；
The negative electrode layer of the drying and dry anode electrode layer hot-pressing transfer printing to proton exchange membrane two sides are formed film by S5
Electrode.
2. the method according to claim 1 for preparing porous membrane electrode using ice template method, which is characterized in that described in S1
Dispersion solvent is the mixed solvent of the deionized water that mass ratio is 1:1~100 and alcohols.
3. the method according to claim 2 for preparing porous membrane electrode using ice template method, which is characterized in that the alcohols
Selected from least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol and tert-butyl alcohol.
4. the method according to claim 1 or 2 for preparing porous membrane electrode using ice template method, which is characterized in that in S3
In, the water freezing when freeze forming in slurry forms ice granular formwork；The removal of ice granular formwork is cold by the vacuum
Dry realization is lyophilized.
5. the method according to claim 1 or 2 for preparing porous membrane electrode using ice template method, which is characterized in that in S1,
The mass ratio of the catalyst, binder and dispersion solvent is 1:1~10:10~1000.
6. the method according to claim 1 or 2 for preparing porous membrane electrode using ice template method, which is characterized in that in S1
The catalyst is selected from carbon-supported Pt catalyst, carbon-supported Pt alloy catalyst or carbon-supported Pt single-layer catalyst.
7. the method according to claim 1 or 2 for preparing porous membrane electrode using ice template method, which is characterized in that in S1
The binder is selected from least one of perfluorosulfonic acid ion resin solution and polytetrafluoroethylsolution solution.
8. the method according to claim 1 for preparing porous membrane electrode using ice template method, which is characterized in that in S2 and S4
The method of the coating is respectively selected from spray coating method, silk screen print method, doctor-blade casting process, spread coating or slit casting die.
9. the method according to claim 1 for preparing porous membrane electrode using ice template method, which is characterized in that described in S3
The temperature of freeze forming is -200 DEG C~0 DEG C, and the temperature of the vacuum freeze drying is -60 DEG C~-40 DEG C.
10. the method according to claim 1 for preparing porous membrane electrode using ice template method, which is characterized in that institute in S5
The temperature for stating hot-pressing transfer printing is 80 DEG C~150 DEG C, and pressure is 1MPa~15MPa, and the time is 60s~600s.
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Application publication date: 20190906 |