CN104600325A - Fuel cell electrode on-step preparation technology - Google Patents
Fuel cell electrode on-step preparation technology Download PDFInfo
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- CN104600325A CN104600325A CN201310532409.3A CN201310532409A CN104600325A CN 104600325 A CN104600325 A CN 104600325A CN 201310532409 A CN201310532409 A CN 201310532409A CN 104600325 A CN104600325 A CN 104600325A
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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
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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
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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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
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
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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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Abstract
The invention provides a fuel cell electrode on-step preparation method, which comprises the following steps: preparing a precursor solution from a carbon carrier, a platinum source, a polymeric monomer and a solvent, and preparing the fuel cell membrane electrode by using a cyclic voltammetry method by adopting a three-electrode system under a stirring condition, wherein the precursor solution is adopted as electrolyte. According to the fuel cell electrode preparation method, the characteristics of the two kinds of substances such as the polymeric monomer and the platinum source capable of respectively generating reactive polymerization and oxidization reaction under positive and negative potentials are reasonably utilized, the preparation of a precious metal catalyst and a polymer membrane can be realized by one step, the preparation method is simple, the conductivity capability of the electrode can be improved, and the service life of the electrode can be prolonged.
Description
Technical field
What the present invention relates to is field of fuel cell technology, particularly relates to the technique that a kind of one-step method prepares fuel cell electrode.
Background technology
Fuel cell is a kind of Blast Furnace Top Gas Recovery Turbine Unit (TRT) being directly electric energy in electrochemical reaction mode by the converts chemical energy of fuel without burning, is a kind of green energy resource technology." energy shortage " and " environmental pollution " this two hang-up that fuel cell technology faces the current world of solution is significant.The advantages such as it has clean, efficient and reliable, are considered to the optimal path of fuel utilization.For carbon-based fuel (as oil gas, biological fuel processed, alcohols, fuel oil) power conversion, fuel cell has obvious advantage compared to traditional burning/internal combustion engine process, its efficiency is not by the restriction of Carnot cycle theoretical upper limit, and also avoid the pollution problem that combustion process produces, is the important step of fossil energy to high-efficiency cleaning " low-carbon economy " transition.The power output flexibility of fuel cell is very high, difference according to demand, and it can be that the occasion such as enterprise, school is powered as distributed energy that fuel cell arrives greatly, and little arriving can as the power supply of the portable equipment such as mobile phone, computer.Therefore, fuel cell will have very large development as the novel energy of advanced person; On the other hand, a large amount of uses of fuel cell-powered and fuel cell car, electric motor car, can suppress the continuous pollution of environment effectively, contain global warming simultaneously.
Electrode is the critical component of fuel cell, and its performance is the key factor affecting overall fuel cell performance.In order to improve the life-span of fuel cell, reduce the consumption of fuel-cell catalyst noble metal platinum, researcher have studied various electrode structure.Current low-temperature fuel cell catalyst used no matter cathod catalyst or anode catalyst is all the noble metal catalysts based on platinum metal.Platinum metal expensive, and larger proportion is occupied in battery cost.This is also the one of the main reasons causing fuel cell to be still difficult to large-scale promotion and application so far.In addition, this kind of catalyst is subject to the restriction of resource, very limited in the output of China's platinum metal especially.Therefore, develop highly active novel membrane electrode, improve the utilance of catalyst and reduce its consumption, be the direction that operation of fuel cells person's emphasis is made great efforts always.
According to bibliographical information, the catalyst carrier of high surface and suitable method for preparing catalyst is selected to be one of main method.The people such as Goodenough have studied the contrast that carbon carries platinum (Pt/C) electrode and pure platinum black electrode very early in document (Electrochim. Acta, 1987,32 (8)), and experiment shows that Pt/C electrode has with high current density.Henceforth, obtain using carbon as the research of fuel-cell catalyst carrier and develop fast.In recent years, conducting polymer is owing to having that specific area is higher, resistance is lower and the advantage of good stability is used as the carrier of fuel-cell catalyst, gradually as polythiophene, polyaniline, polypyrrole etc.Ren Fangfang reports the fuel cell electrode preparation method of three kinds of conducting polymers as carrier in document " electrocatalysis characteristic of conducting polymer and noble metal composite is studied ".Author adopts two steps to prepare electrode, on glass-carbon electrode material, first adopts electropolymerization mode to prepare conducting polymer support, then depositing noble metal catalyst.Experimental result shows, fuel cell electrode prepared by the method has good oxidation to methyl alcohol.
Chinese invention patent (201010606384.3) discloses a kind of preparation method of combined electrode of fuel cell.Applicant adopts arc discharge method to prepare Single Walled Carbon Nanotube ultrathin film and silk screen print method prepares multi-wall carbon nano-tube film, is then electroplated on combination electrode by metallic catalyst.Matrix prepared by this method has extra specific surface area and conductive characteristic, is applicable to efficient supported metal catalyst.
Summary of the invention
The object of the invention is to overcome that existing fuel cell membrane electrode platinum amount is more, conductive capability is poor, the deficiencies such as complex process, provides the technique that a kind of one-step method prepares fuel cell electrode.The membrane electrode prepared by the method has good catalytic activity, the feature that less by platinum amount and conductive capability is strong.
The invention provides a kind of method that one-step method prepares fuel cell membrane electrode, comprise the following steps: with carbon carrier, platinum source, polymerization single polymerization monomer and solvent preparation precursor solution, with described precursor solution for electrolyte, adopt three-electrode system, under agitation, cyclic voltammetry is used to prepare fuel cell membrane electrode.
Mass ratio 1:0.1 ~ 10:1 ~ 30 containing carbon carrier, platinum source (in simple substance platinum), polymerization single polymerization monomer three in described precursor solution, preferred 1:0.2 ~ 5:2 ~ 15; In simple substance platinum, in precursor solution, the concentration range of platinum is 1.0 ~ 15.0mmol/L, preferably 2.0 ~ 10mmol/L.
In the preparation method of fuel cell membrane electrode of the present invention, described carbon carrier can be any one in carbon black, graphite, carbon nano-tube, Graphene, carbon nanocoils, preferred carbon nano-tube or Graphene.
In the preparation method of fuel cell membrane electrode of the present invention, purification process need be carried out when described carbon carrier is carbon nano-tube, described purification treating method can carry out according to the method described in document (Electroanalysis 2011,23 (8): 1863-1869).
In the preparation method of fuel cell membrane electrode of the present invention, described platinum source is one or more in platinum chloride, platinum nitrate, chloroplatinic acid, preferred platinum chloride and/or chloroplatinic acid.
In the preparation method of fuel cell membrane electrode of the present invention, described polymerization single polymerization monomer can be one or more in o-phenylenediamine, p-phenylenediamine (PPD), resorcinol, hydroquinones, thiophene, aniline, preferred o-phenylenediamine and resorcinol.
In the preparation method of fuel cell membrane electrode of the present invention, described solvent is any one in sodium nitrate, sodium sulphate, sodium chloride, potassium sulfate solution, preferably sulfuric acid sodium or sodium nitrate.
In the preparation method of fuel cell membrane electrode of the present invention, described work electrode is: any one in graphite flake, platinized platinum, gold plaque, carbon paper, nickel foam, preferred carbon paper or nickel foam.
In the preparation method of fuel cell membrane electrode of the present invention, described can be any one in platinum plate electrode, Ti electrode, nickel sheet electrode and platinum guaze to electrode, preferred platinized platinum or platinum guaze.
In the preparation method of fuel cell membrane electrode of the present invention, described reference electrode can adopt the conventional reference electrodes such as saturated calomel electrode, Mercurous sulfate electrode or silver/silver chloride electrode.Use different reference electrode, operating voltage is different, can according to the electrode potential conversion operating voltage of this reference electrode relative to standard hydrogen electrode.
In the preparation method of fuel cell membrane electrode of the present invention, described cyclic voltammetry operating parameter is, sweep speed 5 ~ 200mV/s, preferably 20 ~ 50mV/s, potential range-2.0 ~ 3.5V, preferably-1.0 ~ 1.5V, the continuous sweep number of turns is 10 ~ 200 circles, preferably 30 ~ 100 circles.
The principle that the present invention prepares fuel cell membrane electrode is: chloroplatinic acid can be reduced to simple substance platinum under negative potential, and polymerization single polymerization monomer polymerization reaction take place under positive potential, carbon carrier can be driven simultaneously to be attached to electrode surface, to form the fuel cell membrane electrode of Surface coating polymer.
The fuel cell membrane electrode preparation method tool that the present invention relates to has the following advantages:
1, fuel cell electrode preparation method Appropriate application of the present invention polymerization single polymerization monomer and platinum source this two classes material issue the characteristic of the reaction of raw reactive polymeric and oxidation reaction respectively at positive negative potential, can realize preparing noble metal catalyst and polymer film by one-step method, preparation method is simple, is easy to large-scale promotion application.
2, in fuel cell electrode preparation method of the present invention, conducting polymer add the decentralization enhancing catalyst granules, improve the conductive capability of electrode; The interaction of platinum grain and conducting polymer decreases the formation of strong adsorbing species in course of reaction on the other hand, extends the life-span of electrode.
3, by the electrode that fuel cell electrode preparation method of the present invention obtains, catalyst granules is less, and high degree of dispersion on the carbon carrier.Thus the effective surface area of catalyst granules can be significantly improved, thus a large amount of avtive spots is provided, enhance the oxidability of electrode.
4, the carbon carrier adopted in fuel cell electrode preparation method of the present invention can promote electron transmission, adds the electric conductivity of electrode.Both act synergistically mutually can provide the crystal plane structure being conducive to electrochemical reaction more.
Accompanying drawing explanation
Fig. 1 is membrane electrode component transmission electron microscope (TEM) picture prepared in the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, and described embodiment is only for explaining the present invention, instead of limitation of the present invention.
Embodiment 1:
In the present embodiment, take multi-walled carbon nano-tubes as carbon carrier, chloroplatinic acid is platinum source, and o-phenylenediamine and resorcinol are polymerization single polymerization monomer, and metabisulfite solution is solvent.Taking carbon paper as work electrode, is to electrode with platinum plate electrode, take saturated calomel electrode as reference electrode.
In the present embodiment, first described multi-walled carbon nano-tubes carries out purification process.Weigh the multi-walled carbon nano-tubes of 1g, slowly join (concentrated sulfuric acid and red fuming nitric acid (RFNA) volume ratio 3:1) in the mixed solution of the 50mL concentrated sulfuric acid and red fuming nitric acid (RFNA), continuous stir process 6 hours, then dilute with the high purity water of 150mL, and centrifugation, repeat dilution and lock out operation 5 pH value to solution are 6.5, then use vacuum pump suction filtration system under 85kPa, carry out suction filtration concentrated, finally 50 DEG C, vacuumize 8 hours under the condition of 20kPa, obtain the multi-walled carbon nano-tubes of purifying.
Take the multi-walled carbon nano-tubes after 20mg purifying, 40mg chloroplatinic acid, 50mg o-phenylenediamine and 50mg resorcinol to join in the metabisulfite solution of 20mL 0.02 mol/L preparation and obtain precursor solution, using carbon paper as work electrode in this precursor solution, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, cyclic voltammetry is adopted to prepare fuel cell membrane electrode, sweep speed 50mV/s, potential range-1.0 ~ 1.0V, the continuous sweep number of turns is 10 circles, obtains a kind of fuel cell electrode being loaded with Pt catalyst granule of the present invention.
Electrode material portions prepared by embodiment 1 to peel off, characterized by transmission electron microscope, see accompanying drawing 1, can see that platinum grain is uniformly dispersed in carbon nano tube surface.Learn thus, catalyst prepared by the method is more stable, and avtive spot is comparatively large, can improve the performance of electrode.
Embodiment 2:
In the present embodiment, take Single Walled Carbon Nanotube as carbon carrier, platinum chloride is platinum source, and aniline is polymerization single polymerization monomer, and sodium nitrate solution is solvent.Taking graphite flake as work electrode, is to electrode with platinum plate electrode, take saturated calomel electrode as reference electrode.
In the present embodiment, first described multi-walled carbon nano-tubes carries out purification process.Weigh the multi-walled carbon nano-tubes of 1g, slowly join in the mixed solution of the 50mL concentrated sulfuric acid and red fuming nitric acid (RFNA), continuous stir process 6 hours, then dilute with the high purity water of 200mL, and centrifugation, repeat dilution and lock out operation 5 pH value to solution are 6.5, then use vacuum pump suction filtration system under 85kPa, carry out suction filtration concentrated, finally 50 DEG C, vacuumize 6 hours under the condition of 20kPa, obtain the Single Walled Carbon Nanotube of purifying.
Take the Single Walled Carbon Nanotube of 30mg purifying, 40mg platinum chloride, 100mg aniline joins preparation in the sodium nitrate solution of 50mL 0.02 mol/L and obtain precursor solution, using graphite flake as work electrode in this precursor solution, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, cyclic voltammetry is adopted to prepare fuel cell membrane electrode, sweep speed 20mV/s, potential range-1.0 ~ 1.5V, the continuous sweep number of turns is 50 circles, obtains a kind of fuel cell electrode being loaded with Pt catalyst granule of the present invention.
Embodiment 3:
In the present embodiment, take carbon black as carbon carrier, platinum chloride is platinum source, and thiophene is polymerization single polymerization monomer, and sodium chloride solution is solvent.Taking graphite flake as work electrode, is to electrode with gauze platinum electrode, take saturated calomel electrode as reference electrode.
Take the carbon black of 30mg purifying, 80mg chloroplatinic acid, 100mg thiophene join preparation in the sodium chloride solution of 50mL 0.02 mol/L and obtain precursor solution, using graphite flake as work electrode in this precursor solution, gauze platinum electrode is to electrode, silver/silver chloride electrode is reference electrode, cyclic voltammetry is adopted to prepare fuel cell membrane electrode, sweep speed 100mV/s, potential range-1.0 ~ 1.5V, the continuous sweep number of turns is 100 circles, obtains a kind of fuel cell electrode being loaded with Pt catalyst granule of the present invention.
Claims (18)
1. one-step method prepares the method for fuel cell membrane electrode, it is characterized in that: with carbon carrier, platinum source, polymerization single polymerization monomer and solvent preparation precursor solution, with described precursor solution for electrolyte, adopt three-electrode system, under agitation, cyclic voltammetry is used to prepare fuel cell membrane electrode.
2. method according to claim 1, is characterized in that: mass ratio 1:0.1 ~ 10:1 ~ 30 of carbon carrier, platinum source, polymerization single polymerization monomer three in described precursor solution, wherein platinum source is in simple substance platinum.
3. method according to claim 1, is characterized in that: mass ratio 1:0.2 ~ 5:2 ~ 15 of carbon carrier, platinum source, polymerization single polymerization monomer three in described precursor solution, wherein platinum source is in simple substance platinum.
4. method according to claim 1, is characterized in that: in simple substance platinum, and in precursor solution, the concentration range of platinum is 1.0 ~ 15.0mmol/L.
5. method according to claim 1, is characterized in that: in simple substance platinum, and in precursor solution, the concentration range of platinum is 2.0 ~ 10.0mmol/L.
6. method according to claim 1, is characterized in that: described carbon carrier is any one in carbon black, graphite, carbon nano-tube, Graphene and carbon nanocoils.
7. method according to claim 1, is characterized in that: described carbon carrier is carbon nano-tube or Graphene.
8. the method according to claim 3 or 4, is characterized in that: need carry out purification process when carbon carrier is carbon nano-tube.
9. method according to claim 1, is characterized in that: described platinum source is one or more in platinum chloride, platinum nitrate, chloroplatinic acid.
10. method according to claim 1, is characterized in that: described platinum source is platinum chloride and/or chloroplatinic acid.
11. methods according to claim 1, is characterized in that: described polymerization single polymerization monomer is one or more in o-phenylenediamine, p-phenylenediamine (PPD), resorcinol, hydroquinones, thiophene, aniline.
12. methods according to claim 1, is characterized in that: described polymerization single polymerization monomer is o-phenylenediamine and resorcinol.
13. methods according to claim 1, is characterized in that: described solvent is any one in sodium nitrate, sodium sulphate, sodium chloride, potassium sulfate.
14. methods according to claim 1, is characterized in that: described work electrode is any one in graphite flake, platinized platinum, gold plaque, carbon paper, nickel foam.
15. methods according to claim 1, is characterized in that: described is any one in platinum plate electrode, Ti electrode, nickel sheet electrode, platinum guaze to electrode.
16. methods according to claim 1, is characterized in that: described reference electrode is any one in saturated calomel electrode, Mercurous sulfate electrode, silver/silver chloride electrode.
17. methods according to claim 1, is characterized in that: described cyclic voltammetry operating parameter is, sweep speed 5 ~ 200mV/s, potential range-2.0 ~ 3.5V, and the continuous sweep number of turns is 10 ~ 200 circles.
18. methods according to claim 1, is characterized in that: described cyclic voltammetry operating parameter is, sweep speed 20 ~ 50mV/s, potential range-1.0 ~ 1.5V, and the continuous sweep number of turns is 30 ~ 100 circles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394239A (en) * | 2017-07-28 | 2017-11-24 | 李兴祥 | Fuel cell membrane electrode preparation method and preparation equipment |
| CN108155393A (en) * | 2017-12-25 | 2018-06-12 | 苏州擎动动力科技有限公司 | It is a kind of using carbon nanotube as the method for preparing catalyst of carrier |
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| US8354137B2 (en) * | 2009-06-29 | 2013-01-15 | Toppan Printing Co., Ltd. | Manufacturing method of electrode catalyst layer for fuel cell |
| US20130280419A1 (en) * | 2008-08-21 | 2013-10-24 | Board Of Trustees Of Michigan State University | Novel catalyst for oxygen reduction reaction in fuel cells |
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2013
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Patent Citations (4)
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| US20130280419A1 (en) * | 2008-08-21 | 2013-10-24 | Board Of Trustees Of Michigan State University | Novel catalyst for oxygen reduction reaction in fuel cells |
| CN101549304A (en) * | 2009-05-07 | 2009-10-07 | 浙江大学 | Method for preparing conductive polymer modified carbon based cobaltous hydroxide composite catalyst |
| US8354137B2 (en) * | 2009-06-29 | 2013-01-15 | Toppan Printing Co., Ltd. | Manufacturing method of electrode catalyst layer for fuel cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107394239A (en) * | 2017-07-28 | 2017-11-24 | 李兴祥 | Fuel cell membrane electrode preparation method and preparation equipment |
| CN107394239B (en) * | 2017-07-28 | 2023-07-07 | 李兴祥 | Fuel cell membrane electrode preparation method and preparation equipment |
| CN108155393A (en) * | 2017-12-25 | 2018-06-12 | 苏州擎动动力科技有限公司 | It is a kind of using carbon nanotube as the method for preparing catalyst of carrier |
| CN108155393B (en) * | 2017-12-25 | 2020-04-14 | 苏州擎动动力科技有限公司 | Preparation method of catalyst with carbon nano tube as carrier |
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