CN104056741A - Preparation method for membrane electrode of fuel cell - Google Patents
Preparation method for membrane electrode of fuel cell Download PDFInfo
- Publication number
- CN104056741A CN104056741A CN201310090903.9A CN201310090903A CN104056741A CN 104056741 A CN104056741 A CN 104056741A CN 201310090903 A CN201310090903 A CN 201310090903A CN 104056741 A CN104056741 A CN 104056741A
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- Prior art keywords
- preparation
- slurry
- electrostatic
- spraying
- electrode
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B5/00—Electrostatic spraying apparatus; Spraying apparatus with means for charging the spray electrically; Apparatus for spraying liquids or other fluent materials by other electric means
- B05B5/08—Plant for applying liquids or other fluent materials to objects
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B5/00—Electrostatic spraying apparatus; Spraying apparatus with means for charging the spray electrically; Apparatus for spraying liquids or other fluent materials by other electric means
- B05B5/025—Discharge apparatus, e.g. electrostatic spray guns
- B05B5/0255—Discharge apparatus, e.g. electrostatic spray guns spraying and depositing by electrostatic forces only
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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
- H01M4/886—Powder spraying, e.g. wet or dry powder spraying, plasma spraying
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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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
Abstract
The invention provides a preparation method for a membrane electrode of a fuel cell. In the process of spraying slurry, the slurry is loaded with electrostatic charges through an electrostatic generator, so as to increase the adsorbability between the slurry and the membrane, improve the Pt utilization rate of a catalytic layer, improve the performance of the membrane electrode and reduce the Pt loading amount.
Description
Technical field
The present invention relates to a kind of preparation method of fuel cell membrane electrode, electrostatic charge on the slurry band that makes to spray, after slurry contact spray-coating surface, electric charge is exported.
Background technology
Fuel cell is a kind of energy conversion device, can be by the electric energy that is converted into efficient, clean Hydrogen Energy.In recent years, hydrogen energy fuel battery worldwide obtains support and development energetically, at present successfully Demonstration Application in multiple fields such as electric automobile, distributed power station, stand-by power supply, aviations.Wherein, Proton Exchange Membrane Fuel Cells is high with power density, toggle speed is fast, conversion efficiency is high, advantages of environment protection receives more concern.
The battery pack of Proton Exchange Membrane Fuel Cells is made up of end plate, collector plate, bipolar plates, flow field and membrane electrode conventionally, the weight issue of its end plates, bipolar plates is the principal element that affects pile specific power, the structural design in flow field is the key factor that affects the inner gas-liquid distribution of pile and long-term operation stability, and membrane electrode is the core component that affects pile output performance.Membrane electrode is made up of the PEM in the middle of being positioned at and Catalytic Layer, the diffusion layer of both sides.PEM in membrane electrode is responsible for conducting hydrogen proton by anode to negative electrode, and the proton conductivity of film directly affects the Ohmic resistance of membrane electrode.Conventional PEM is the perfluorinated sulfonic acid root PEM that E.I.Du Pont Company produces, and the wetness degree of its proton conductivity and film is closely related.Catalytic Layer in membrane electrode is the place that hydrogen reduction and two kinds of electrochemical reactions of hydroxide occur, need to there is good catalytic activity, good proton conductivity and conductive capability, its output performance is by decisions such as catalyst activity, material proportion and microcellular structures, also needing has the proton conduction in enough wetting guarantee Catalytic Layer, but when the water yield is excessive, blockage of the micro orifice also can cause performance degradation.Diffusion layer in membrane electrode is be responsible for gas transport distribution and remove product water, the hydrophobicity in its duct and pore-size distribution are the key factors that affects battery performance, the water producing when battery exceed diffusion layer when the outlet capacity, can there is the water logging of diffusion layer, and then the transmission of obstruction gas, cause voltage drop.
Membrane electrode is mainly divided into gas-diffusion electrode (Gas Diffusion Electrode, and thin layer Film electrode (catalyst coated membrane GDE), CCM), Minnesota Mining and Manufacturing Company proposes to adopt nano structure membrane (nanostructured thin film, NSTF) ultrathin electrodes of preparing as supporter, is considered to get a good chance of becoming MEA of future generation.Gas diffusion layers electrode generally adopts the preparation technology of serigraphy at present, catalyst, hydrophober, organic solvent composition catalyst pulp are brushed on gas diffusion layers, after high-temperature process, realize electrode three-dimensional to Catalytic Layer surface spraying Naifon solution again.Thin layer Film electrode generally adopts the preparation technology of spraying at present, the pulp spraying of catalyst, ion conductor resin, organic solvent composition is coated onto on film, or first pulp spraying is coated onto on other carriers and is transferred on film again, forms film Catalytic Layer integrated electrode.The ultrathin electrodes that Minnesota Mining and Manufacturing Company proposes, development time is shorter, at present also not extensive use.
Electrostatic painting process is a kind of industrial spraying method that is applied to, and under electrostatic interaction, the utilization rate of the feed liquid that sprays improves, and the adhesion at interface is also improved.
Patents:
A kind of electrostatic spraying device of patent (publication number CN1913975A), designed spraying equipment can only spray fluid composition by the step of simplifying smoothly, and wherein the step of this simplification is used for confirming that fluid composition is ready to carry out immediately electrostatic spraying.Construct and be arranged to be dispensed to distribution locations to fluid composition electrostatic charging and by described fluid composition from source of supply according to the electrostatic spraying device of this aspect.
Summary of the invention
Different from above-mentioned Patents, spray gun conventional fuel cell membrane electrode has been added static module by the present invention, and object of the present invention is to provide a kind of spraying method of high-performance membrane electrode.
For achieving the above object, the present invention has designed the membrane electrode spraying equipment being made up of static generator controller, electrostatic gun, zero potential platform, earth connection etc.In the process of coating electrode, by coat to be painted (Nafion film, carbon paper, microporous layers etc.) be placed on the platform of ground connection, to control the electromotive force of spray-coating surface as zero, by static generator controller discharge 10 ?the static of 100kV voltage, make the slurry (comprising Nafion resin solution, catalyst pulp, toner slurry) in spray gun bring electrostatic charge, slurry touches after spray-coating surface, and electrostatic charge can be led away along earth connection.Under the effect of static, the adhesion grow between slurry and spray-coating surface, the structure that spraying forms is also finer and close.
Tool of the present invention has the following advantages
The present invention can improve the utilization rate of fuel cell membrane electrode catalyst pulp;
The present invention can improve the interfacial structure between Catalytic Layer and film;
The present invention can make sprayed electrode structure more smooth evenly.
Brief description of the drawings
Fig. 1 electrostatic spraying device schematic diagram; In figure: 1 electrostatic generator, 2 spray guns, 3 feed liquids, 4 zero potential platforms, 5 connecting lines, 6 ground connection.
Fig. 2 adopts the impact of electrostatic spraying mode on electrode pattern;
Fig. 3 adopts the impact of electrostatic spraying mode on electrode performance;
Fig. 4 adopts the impact of electrostatic spraying mode on electrode activity area.
Detailed description of the invention
Embodiment 1
Get the percentage that 10mg70%(Pt accounts for catalyst gross weight) Pt/C, 50mg Nafion resin solution, 10ml isopropyl alcohol, mixes formation catalyst pulp.Adopt respectively the electrostatic gun in common spray gun and the present invention, by above-mentioned slurry spraying (spray distance, the about 1ml/min of spraying rate, environment temperature), to Nafion film surface, the effective area of spraying is 17.5cm
2.While adopting electrostatic gun spraying, Nafion film is placed on the platform of ground connection, electrostatic generator control output voltage is 60kV, makes electrostatic charge on slurry band, sprays to behind film surface, and electrostatic charge is led away along earth connection.
Above-mentioned sprayed electrode is carried out to Pt load and measured examination.Cutting area from the electrode of above-mentioned spraying is 2*2cm
2fritter, be placed in corundum crucible in 850 ° of lower roasting 2h; In the residue after roasting, successively add hydrogen peroxide, red fuming nitric acid (RFNA) and chloroazotic acid, after residue all dissolves, with distilled water isochoric formation standard liquid.
Adopt inductively coupled plasma (ICP) test, test the concentration of Pt in above-mentioned titer, and then infer Pt load amount in electrode.Test result is as follows: adopt common spray gun to prepare electrode, Pt load amount 0.89mgcm
?2; Adopt electrostatic spraying, Pt load amount 0.82mgcm
?2.
Can find out from the above results, adopt electrostatic painting process to prepare fuel cell membrane electrode, can improve the slurry utilization rate in spraying process.
Embodiment 2
Get the percentage that 24mg50%(Pt accounts for catalyst gross weight) Pt/C, 180mgNafion resin solution, 20ml isopropyl alcohol, mixes formation catalyst pulp.Adopt respectively the electrostatic gun in common spray gun and the present invention, by above-mentioned slurry spraying (spray distance, the about 1ml/min of spraying rate, environment temperature), to Nafion film surface, the effective area of spraying is 30cm
2.While adopting electrostatic gun spraying, Nafion film is placed on the platform of ground connection, electrostatic generator control output voltage is 30kV, makes electrostatic charge on slurry band, sprays to behind film surface, and electrostatic charge is led away along earth connection.
The electrode that above-mentioned spraying is completed utilizes scalpel to cut, and utilizes the cross-section morphology of scanning electron microscopic observation electrode, as shown in Figure 2.As can be seen from the figure, adopt the Catalytic Layer prepared of electrostatic spraying (in figure in red block part) structure more fine and close, surface is more smooth,
Embodiment 3
Get the percentage that 57mg70%(Pt accounts for catalyst gross weight) Pt/C, 340mgNafion resin solution, 30ml isopropyl alcohol, mixes formation catalyst pulp.Adopt respectively the electrostatic gun in common spray gun and the present invention, by above-mentioned slurry spraying (spray distance, the about 1ml/min of spraying rate, environment temperature), to Nafion film surface, the effective area of spraying is 100cm
2.While adopting electrostatic gun spraying, Nafion film is placed on the platform of ground connection, electrostatic generator control output voltage is 90kV, makes electrostatic charge on slurry band, sprays to behind film surface, and electrostatic charge is led away along earth connection.
Two kinds of sprayed electrodes are pressed into MEA together with gas diffusion layers, assembling monocell, battery completes after activation, carries out performance test, as shown in Figure 3.As can be seen from the figure, the membrane electrode that adopts electrostatic spraying to prepare, battery performance improves in high current density region.In addition, two kinds of electrodes have been carried out to the test of electro-chemical activity surface area, as shown in Figure 4, adopted as seen the method for electrostatic spraying to improve the utilization rate of catalyst in electrode.
Embodiment 4
Get Nafion solution 50mg, utilize the isopropanol of 8ml concussion even, form the slurry of spraying Nafion coating.Adopt electrostatic spraying gun by Nafion slurry spraying (spray distance, the about 1ml/min of spraying rate, environment temperature) to Nafion film surface, film is placed on the platform of ground connection, control the voltage that electrostatic generator discharges 100kV, the electric charge discharging is led away through the platform of ground connection.
Embodiment 5
Get 10mgXC ?72, with the 300mgPTFE content emulsion that is 5wt.%, alcohol 5ml mixes, and stirs, and forms the toner slurry of preparation microporous layers.Preparation utilizes electrostatic gun that above-mentioned slurry is sprayed to (spray distance, the about 1ml/min of spraying rate, environment temperature) to carbon paper, carbon paper is placed on the platform of ground connection, control the voltage that electrostatic generator discharges 10kV, the electric charge discharging is led away through the platform of ground connection.
Claims (9)
1. a preparation method for fuel cell membrane electrode, is characterized in that:
Adopt electrostatic gun by liquid slurry be sprayed to be sprayed of solid matter upper,
In spraying slurry process, make electrostatic charge on the slurry band in spray gun;
In spraying slurry process, the electromotive force of controlling spray-coating surface is zero.
2. according to preparation method claimed in claim 1, it is characterized in that: described spraying slurry comprises the one in Nafion resin solution, catalyst pulp, toner slurry.
3. according to preparation method claimed in claim 2, it is characterized in that: the solvent that described spraying slurry adopts is isopropyl alcohol, ethanol etc., stock quality concentration be 0.1 ?10mg/ml.
4. according to preparation method claimed in claim 1, it is characterized in that: described solid matter comprise the one in Nafion film, carbon paper, microporous layers, the side that described spray-coating surface is solid matter or two side surfaces.
5. according to preparation method claimed in claim 1, it is characterized in that:
The described spraying equipment adopting in electrode method of preparing comprises static generator controller, electrostatic gun, zero potential platform, earth connection;
Static generator controller is connected with liquid electrostatic spray gun by wire, makes electrostatic charge on the slurry band in spray gun by static generator controller;
Solid matter is placed on zero potential platform, zero potential platform ground connection; To be sprayed towards spray gun spout.
6. according to preparation method claimed in claim 5, it is characterized in that: described static generator controller: can discharge 10 ?the static of 100kV voltage.
7. according to the preparation method described in claim 5 or 6, it is characterized in that: static generator controller is connected with the earth by earth connection.
8. according to preparation method claimed in claim 5, it is characterized in that: zero potential platform is connected with the earth by earth connection.
9. according to preparation method claimed in claim 1, it is characterized in that: on the slurry band in spray gun the electrostatic potential of electrostatic charge be 10 ?100kV.
Priority Applications (1)
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CN201310090903.9A CN104056741A (en) | 2013-03-20 | 2013-03-20 | Preparation method for membrane electrode of fuel cell |
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CN201310090903.9A CN104056741A (en) | 2013-03-20 | 2013-03-20 | Preparation method for membrane electrode of fuel cell |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105772252A (en) * | 2016-05-05 | 2016-07-20 | 中国工程物理研究院材料研究所 | Automatic spraying device applied to SPE film and achieving method of automatic spraying device |
CN105797895A (en) * | 2016-04-28 | 2016-07-27 | 中国工程物理研究院材料研究所 | Automatic spraying device and method for SPE film electrode assembly |
CN106848355A (en) * | 2017-02-20 | 2017-06-13 | 南京大学 | The electrostatic spinning and electrostatic spraying preparation method of a kind of membrane electrode CCM |
CN106861958A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of electrostatic spraying apparatus for preparing fuel cell membrane electrode |
CN108063267A (en) * | 2017-12-26 | 2018-05-22 | 新源动力股份有限公司 | A kind of Catalytic Layer with multi-layer structure of fuel cell and preparation method thereof |
CN109982517A (en) * | 2017-12-27 | 2019-07-05 | 北大方正集团有限公司 | The preparation method and circuit board of circuit board |
CN112020576A (en) * | 2018-07-06 | 2020-12-01 | 株式会社Lg化学 | Reduction electrode for electrolysis and method for manufacturing same |
CN114602764A (en) * | 2020-12-09 | 2022-06-10 | 中国科学院大连化学物理研究所 | Electrostatic slit coating method for preparing membrane electrode of fuel cell |
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CN1231525A (en) * | 1998-03-31 | 1999-10-13 | 松下电器产业株式会社 | Electrode for fuel cell and making method thereof |
CN1455963A (en) * | 2000-06-22 | 2003-11-12 | 松下电器产业株式会社 | Polymer electrolyte fuel cell, and method for manufacturing electrode thereof, and manufacturing apparatus |
CN1716665A (en) * | 2004-06-30 | 2006-01-04 | 三星Sdi株式会社 | Electrode for fuel cell, fuel cell comprising the same and method for making an electrode |
CN101036253A (en) * | 2004-09-02 | 2007-09-12 | 百拉得动力系统公司 | Method and apparatus for electrostatically coating an ion-exchange membrane or fluid diffusion layer with a catalyst layer |
CN101145588A (en) * | 2007-10-26 | 2008-03-19 | 东南大学 | Flexible dye sensitized solar energy cell photoanode preparation method and apparatus |
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Patent Citations (5)
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CN1231525A (en) * | 1998-03-31 | 1999-10-13 | 松下电器产业株式会社 | Electrode for fuel cell and making method thereof |
CN1455963A (en) * | 2000-06-22 | 2003-11-12 | 松下电器产业株式会社 | Polymer electrolyte fuel cell, and method for manufacturing electrode thereof, and manufacturing apparatus |
CN1716665A (en) * | 2004-06-30 | 2006-01-04 | 三星Sdi株式会社 | Electrode for fuel cell, fuel cell comprising the same and method for making an electrode |
CN101036253A (en) * | 2004-09-02 | 2007-09-12 | 百拉得动力系统公司 | Method and apparatus for electrostatically coating an ion-exchange membrane or fluid diffusion layer with a catalyst layer |
CN101145588A (en) * | 2007-10-26 | 2008-03-19 | 东南大学 | Flexible dye sensitized solar energy cell photoanode preparation method and apparatus |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106861958A (en) * | 2015-12-12 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of electrostatic spraying apparatus for preparing fuel cell membrane electrode |
CN105797895A (en) * | 2016-04-28 | 2016-07-27 | 中国工程物理研究院材料研究所 | Automatic spraying device and method for SPE film electrode assembly |
CN105772252B (en) * | 2016-05-05 | 2019-01-22 | 中国工程物理研究院材料研究所 | Automatic spraying equipment applied to SPE film |
CN105772252A (en) * | 2016-05-05 | 2016-07-20 | 中国工程物理研究院材料研究所 | Automatic spraying device applied to SPE film and achieving method of automatic spraying device |
CN106848355A (en) * | 2017-02-20 | 2017-06-13 | 南京大学 | The electrostatic spinning and electrostatic spraying preparation method of a kind of membrane electrode CCM |
CN108063267B (en) * | 2017-12-26 | 2020-06-05 | 新源动力股份有限公司 | Catalytic layer with multilayer structure for fuel cell and preparation method thereof |
CN108063267A (en) * | 2017-12-26 | 2018-05-22 | 新源动力股份有限公司 | A kind of Catalytic Layer with multi-layer structure of fuel cell and preparation method thereof |
CN109982517A (en) * | 2017-12-27 | 2019-07-05 | 北大方正集团有限公司 | The preparation method and circuit board of circuit board |
CN109982517B (en) * | 2017-12-27 | 2020-10-16 | 北大方正集团有限公司 | Preparation method of circuit board and circuit board |
CN112020576A (en) * | 2018-07-06 | 2020-12-01 | 株式会社Lg化学 | Reduction electrode for electrolysis and method for manufacturing same |
CN112020576B (en) * | 2018-07-06 | 2023-06-30 | 株式会社Lg化学 | Reduction electrode for electrolysis and method for manufacturing the same |
CN114602764A (en) * | 2020-12-09 | 2022-06-10 | 中国科学院大连化学物理研究所 | Electrostatic slit coating method for preparing membrane electrode of fuel cell |
CN114602764B (en) * | 2020-12-09 | 2023-02-28 | 中国科学院大连化学物理研究所 | Electrostatic slit coating method for preparing membrane electrode of fuel cell |
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Application publication date: 20140924 |