CN101872868A - Fuel cell membrane electrode taking conductive ceramic-carried metal as electro-catalyst and preparation method thereof - Google Patents
Fuel cell membrane electrode taking conductive ceramic-carried metal as electro-catalyst and preparation method thereof Download PDFInfo
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- CN101872868A CN101872868A CN200910138332A CN200910138332A CN101872868A CN 101872868 A CN101872868 A CN 101872868A CN 200910138332 A CN200910138332 A CN 200910138332A CN 200910138332 A CN200910138332 A CN 200910138332A CN 101872868 A CN101872868 A CN 101872868A
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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 relates to a fuel cell membrane electrode which takes conductive ceramic-carried metal as an electro-catalyst and a preparation method thereof. The membrane electrode consists of three layers, namely, a proton exchange membrane and two catalyst layers on the two sides of the proton exchange membrane. The catalyst layer consists of a conductive ceramic-carried metal catalyst and perfluorinated sulfonic resin. The electro-catalyst used in the catalyst layer is the conductive ceramic-carried metal catalyst, and the metal is platinum or a platinum alloy. The method for preparing the membrane electrode comprises the following steps of: preparing slurry from the catalyst, the perfluorinated sulfonic resin emulsion and water; uniformly coating the slurry on a Teflon membrane; and transferring to the two sides of the proton exchange membrane so as to obtain the fuel cell membrane electrode under certain pressure. The fuel cell membrane electrode of the invention can be used for producing fuel cells with low cost and high durability, and can also be used as the power source of an electric vehicle or a portable electronic device.
Description
Technical field
The present invention relates to a kind of fuel cell membrane electrode and preparation method thereof.
Background technology
Fuel cell is the device that a kind of chemical energy with fuel and oxidant is converted into electric energy.The maximum characteristics of this device are that its energy conversion efficiency is not subjected to the restriction of " Carnot cycle ", its energy conversion efficiency is up to 60%-80%, actual service efficiency be ordinary internal combustion engine 2-3 doubly, and fuel cell also has fuel variation, environmental friendliness, discharges advantages such as nitrogen oxide and sulfur oxide hardly.Just because of these outstanding superiority, the exploitation and the application of fuel cell technology enjoy attention, are considered to the cleaning of 21 century first-selection and generation mode efficiently.
Kinds of fuel cells is a lot, can be divided into according to the electrolyte type: alkaline fuel cell (AFC), phosphoric acid type fuel cell (PAFC), molten carbonate fuel cell (MCFC), Solid Oxide Fuel Cell (SOFC) and Proton Exchange Membrane Fuel Cells (PEMFC) fuel cell.That generally acknowledge at present tool application prospect is Proton Exchange Membrane Fuel Cells (PEMFC).It has, and but room temperature is capable of fast starting, specific power and the high outstanding advantage of specific energy, therefore is especially suitable for use as the power supply of electric motor car and portable electric appts.
Membrane electrode (CCM, Catalyst Coated Membrane) is the core component of fuel cell, is the position that fuel and oxidant generation electrochemical reaction produce electric energy.This membrane electrode is made up of for three layers the Catalytic Layer on proton exchange membrane and both sides.The durability of eelctro-catalyst has very important significance for fuel cell performance and useful life in the Catalytic Layer of membrane electrode.The present used main carbon-carried Pt-based catalyst of eelctro-catalyst of PEMFC is because in the running environment (high humidity, highly acid PH＜2) of Proton Exchange Membrane Fuel Cells harshness, high temperature (50～90 ℃), high voltage (0.60～1.2V) and the O of high concentration
2In, electrochemical corrosion can take place in carbon black, particularly under the Pt catalytic action, quickens the corrosion of the black carbon surface of contact with it, causes with the Pt particulate unsettledly, impels Pt migration, reunion and sintering, thereby has reduced the service efficiency and the durability of catalyst.Therefore, the service efficiency of membrane electrode catalyst system therefor and durability are the current pressing issues that need solution to improving fuel cell performance and being of great significance useful life.
Summary of the invention
The objective of the invention is at above-mentioned present situation, a kind of low cost that aims to provide and the fuel cell of high-durability are fuel cell membrane electrode of eelctro-catalyst and preparation method thereof with the conductive ceramic-carried metal.
The implementation of the object of the invention is that a kind of is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, is made up of for three layers the Catalytic Layer on proton exchange membrane and both sides thereof.
A kind of is the preparation method of the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, and concrete steps are as follows:
(1) the conductivity ceramics supported noble metal is the preparation of eelctro-catalyst: metallic compound is dissolved in the acetone, add conductive ceramic powder again, be heated to 60 ℃ after fully mixing, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 15h under 110 ℃ condition promptly gets pressed powder then; Again pressed powder is used 90%H under 250 ± 50 ℃
2/ N
2Reduction was handled 5 ± 3 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtain the conductive ceramic-carried metal catalyst;
(2) preparation of fuel cell membrane electrode: with conductive ceramic-carried metal catalyst and mass fraction is that 5-20% perfluorinated sulfonic resin emulsion is mixed and deionized water, ultrasonic dispersion 30min preparation catalyst pulp, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be the both sides that are transferred to proton exchange membrane under the 1MPa at pressure again, promptly obtaining with the conductive ceramic-carried metal is the fuel cell membrane electrode of eelctro-catalyst.
Utilize fuel cell membrane electrode of the present invention can produce the fuel cell of low-cost and high-durability, also can be used for the power supply of electric motor car and portable electric appts.
Description of drawings
Accompanying drawing 1 is a fuel cell membrane electrode structure schematic diagram of the present invention.
Accompanying drawing 2 is photos of prepared fuel battery membranes electrode in the embodiment of the invention 1.
Accompanying drawing 3 is with Pt/TiSi in the embodiment of the invention 1
2Monocell CV curve for the fuel cell membrane electrode of eelctro-catalyst.
Accompanying drawing 4 is with Pt/TiSi in the embodiment of the invention 1
2Monocell I-V curve for the fuel cell membrane electrode of eelctro-catalyst.
Embodiment
With reference to accompanying drawing, fuel cell membrane electrode of the present invention is made up of for 1 three layers the Catalytic Layer on proton exchange membrane 2 and both sides thereof.
Described catalyst layer is made up of conductive ceramic-carried metal catalyst and perfluorinated sulfonic resin, and wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 1-10: 1.
Metal is platinum or platinum alloy in the described conductive ceramic-carried metal catalyst, and wherein platinum alloy is the alloy of platinum and ruthenium, iridium, palladium, wherein platinum and ruthenium, and iridium, the mass ratio of palladium are 4-0.5: 1.The mass fraction of platinum is 5-60wt% in the conductive ceramic-carried metal catalyst.The platinum carrying capacity is 0.01-1mg/cm on the Catalytic Layer
2
The particle diameter of conductive ceramic powder is 5-3000nm in the described conductive ceramic-carried metal catalyst, and specific area is 1-1000m
2/ g.Conductivity ceramics is one or more mixtures in titanium silicide, titanium carbide, titanium boride, titanium nitride, molybdenum silicide, zirconium boride, the tungsten carbide powder.
Preparation method of the present invention is:
Concrete steps are as follows:
(1) the conductivity ceramics supported noble metal is the preparation of eelctro-catalyst: metallic compound is dissolved in the acetone, add conductive ceramic powder again, be heated to 60 ℃ after fully mixing, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 15h under 110 ℃ condition promptly gets pressed powder then; Again pressed powder is used 90%H under 250 ± 50 ℃
2/ N
2Reduction was handled 5 ± 3 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtain the conductive ceramic-carried metal catalyst.
(2) preparation of fuel cell membrane electrode: with conductive ceramic-carried metal catalyst and mass fraction is that 5-20% perfluorinated sulfonic resin emulsion is mixed and deionized water, ultrasonic dispersion 30min preparation catalyst pulp, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be the both sides that are transferred to proton exchange membrane under the 1MPa at pressure again, promptly obtaining with the conductive ceramic-carried metal is the fuel cell membrane electrode of eelctro-catalyst.
Below by specific embodiment in detail the present invention is described in detail.
Example 1, (1) conductive ceramic-carried metal are the preparation of eelctro-catalyst: with 0.34gH
2PtCl
6(containing 0.13gPt) is dissolved in the acetone, adds and 0.5gTiSi again
2(particle diameter is 3000nm to powder, and BET is 1m
2/ g) also fully mix; Above-mentioned mixed liquor is heated to 60 ℃, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 12h under 110 ℃ the condition promptly gets pressed powder then; Again pressed powder is used 90%H under 200 ℃
2/ N
2Reduction was handled 8 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtain the Pt/TiSi that the platinum mass fraction is 5wt%
2Catalyst.
(2) preparation of fuel cell membrane electrode: with 0.5g Pt/TiSi
2Catalyst and 3.3g mass fraction are 5% perfluorinated sulfonic resin emulsion (wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 3: 1) and add the 4g deionized water, make catalyst pulp behind the ultrasonic dispersion 30min, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be to be transferred to proton exchange membrane Nafion212 under the 1MPa at pressure again, and guarantee that the platinum carrying capacity in the Catalytic Layer is 0.4mg/cm
2, promptly obtain fuel cell membrane electrode.Membrane electrode and gas diffusion layers, collector plate, end plate and encapsulant are formed monocell.The monocell service conditions: hydrogen/air, air back pressure are 0; From humidification; The monocell working temperature is 35-55 ℃.The monocell test result shows that the electricity output of monocell reaches [email protected]/cm
2
Example 2, (1) conductive ceramic-carried metal are the preparation of eelctro-catalyst: with 2.02gH
2PtCl
6(containing 0.75gPt) is dissolved in the acetone, again adding and 0.4gTiN and 0.1gTiB
2((wherein particle diameter is 5nm to powder, and BET is 1000m
2/ g) also fully mix; Above-mentioned mixed liquor is heated to 60 ℃, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 12h under 110 ℃ the condition promptly gets pressed powder then; Again pressed powder is used 90%H under 300 ℃
2/ N
2Reduction was handled 2 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtain the Pt/TiN-TiB that the platinum mass fraction is 60wt%
2Catalyst.
(2) preparation of fuel cell membrane electrode: will prepare 0.5gPt/TiN-TiB
2Eelctro-catalyst and 2.5g mass fraction are 20% perfluorinated sulfonic resin emulsion (wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 1: 1) and add the 3g deionized water, make catalyst pulp behind the ultrasonic dispersion 30min, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be that 1Mpa is transferred to proton exchange membrane Nafion117 at pressure again, and guarantee that the platinum carrying capacity in the Catalytic Layer is 1mg/cm
2, promptly obtain fuel cell membrane electrode.The Integration Assembly And Checkout condition of monocell is with implementing 1, and the monocell test result shows that the electricity output of monocell reaches [email protected]/cm
2
Example 3, (1) conductive ceramic-carried metal are that the preparation of eelctro-catalyst is same: with 1gH
2PtCl
6(containing 0.37gPt) and 0.25gRuCl
3(containing 0.093gRu) is dissolved in the acetone, and (particle diameter is 50nm, and BET is 220m with the 0.5gWC powder in adding again
2/ g) also fully mix; Above-mentioned mixed liquor is heated to 60 ℃, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 12h under 110 ℃ the condition promptly gets pressed powder then; Again pressed powder is used 90%H under 250 ℃
2/ N
2Reduction was handled 3 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtaining making the platinum mass fraction is the 40wt%Pt-Ru/WC catalyst.
(2) preparation of fuel cell membrane electrode: the 0.5gPt-Ru/WC eelctro-catalyst and the 0.5g mass fraction of preparation are 10% perfluorinated sulfonic resin emulsion (wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 10: 1) and add the 4g deionized water, make catalyst pulp behind the ultrasonic dispersion 30min, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be the both sides that are transferred to Nafion211 under the 1Mpa at pressure again, and guarantee that the platinum carrying capacity in the Catalytic Layer is 0.4mg/cm
2, promptly obtain fuel cell membrane electrode.The Integration Assembly And Checkout condition of monocell is with implementing 1, and the monocell test result shows that the electricity output of monocell reaches [email protected]/cm
2
Example 4, (1) conductive ceramic-carried metal are the preparation of eelctro-catalyst: with 0.17gH
2PtCl
6(containing 0.06gPt) and 0.20gPdCl
2(containing 0.12gPd) is dissolved in the acetone, adds and 1.0g TiC and 0.1g MoSi again
2(wherein particle diameter is 100nm, and BET is 150m as ceramic monolith
2/ g) also fully mix; Above-mentioned mixed liquor is heated to 60 ℃, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 12h under 110 ℃ the condition promptly gets pressed powder then; Again pressed powder is used 90%H under 200 ℃
2/ N
2Reduction was handled 8 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, the mass fraction that promptly obtains making platinum is the Pt-Pd/TiC-MoSi of 5wt%
2Catalyst.
(2) preparation of fuel cell membrane electrode: with above-mentioned 0.5g Pt-Pd/TiC-MoSi
2Be 5% perfluorinated sulfonic resin emulsion (wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 1.5: 1) and add the 2g deionized water with the 6.7g mass fraction, make catalyst pulp behind the ultrasonic dispersion 30min, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, 80 ℃ of vacuumizes remove desolvates, be the both sides that are transferred to Nafion115 under the 1MPa at pressure again, and guarantee that the platinum carrying capacity in the Catalytic Layer is 0.01mg/cm
2, promptly obtain fuel cell membrane electrode.The Integration Assembly And Checkout condition of monocell is with implementing 1, and the monocell test result shows that the electricity output of monocell reaches [email protected]/cm
2
Example 5, (1) conductive ceramic-carried metal are the preparation of eelctro-catalyst: with 0.34gH
2PtCl
6(containing 0.13gPt) and 0.075gIrCl
3(containing 0.043gIr) is dissolved in the acetone, adds 0.3gTiSi again
2And 0.1gZrB
2(wherein particle diameter is 20nm, and BET is 300m as ceramic monolith
2/ g) also fully mix; Above-mentioned mixed liquor is heated to 60 ℃, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 12h under 110 ℃ the condition promptly gets pressed powder then; Again pressed powder is used 90%H under 250 ℃
2/ N
2Reduction was handled 5 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, the mass fraction that promptly obtains platinum is the Pt-Ir/TiSi of 30wt%
2-ZrB
2Catalyst.
(2) preparation of fuel cell membrane electrode: with above-mentioned 0.4gPt-Ir/TiSi
2-ZrB
2Be 10% perfluorinated sulfonic resin emulsion (wherein the mass ratio of eelctro-catalyst and perfluorinated sulfonic resin is 2: 1) and add the 1.5g deionized water with the 2g mass fraction, make catalyst pulp behind the ultrasonic dispersion 30min, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, 80 ℃ of vacuumizes remove desolvates, be the both sides that are transferred to Nafion112 under the 1MPa at pressure again, and guarantee that the platinum carrying capacity in the Catalytic Layer is 0.6mg/cm
2, promptly obtain fuel cell membrane electrode.The Integration Assembly And Checkout condition of monocell is with implementing 1, and the monocell test result shows that the electricity output of monocell reaches [email protected]/cm
2
Claims (8)
1. one kind is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, it is characterized in that being made up of for three layers the Catalytic Layer on proton exchange membrane and both sides thereof, and catalyst layer is made up of conductive ceramic-carried metal eelctro-catalyst and perfluorinated sulfonic resin.
2. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, and the mass ratio that it is characterized in that eelctro-catalyst and perfluorinated sulfonic resin is 1-10: 1.
3. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, it is characterized in that metal is platinum or platinum alloy in the conductive ceramic-carried metal catalyst, and wherein platinum alloy is platinum and ruthenium, iridium, the alloy of palladium, platinum and ruthenium, iridium, the mass ratio of palladium are 4-0.5: 1.
4. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, and the mass fraction that it is characterized in that platinum in the conductive ceramic-carried metal catalyst is 5-60wt%.
5. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, it is characterized in that the platinum carrying capacity is 0.01-1mg/cm on the Catalytic Layer
2
6. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, and the particle diameter that it is characterized in that conductivity ceramics in the conductive ceramic-carried metal catalyst is 5-3000nm.
7. as claimed in claim 1 is the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, and the specific area that it is characterized in that conductivity ceramics in the conductive ceramic-carried metal catalyst is 1-1000m
2/ g, conductivity ceramics are one or more mixtures in titanium silicide, titanium carbide, titanium boride, titanium nitride, molybdenum silicide, zirconium boride, the tungsten carbide powder.
Claim 1 described a kind of be the preparation method of the fuel cell membrane electrode of eelctro-catalyst with the conductive ceramic-carried metal, it is characterized in that concrete steps are as follows:
(1) the conductivity ceramics supported noble metal is the preparation of eelctro-catalyst: metallic compound is dissolved in the acetone, add conductive ceramic powder again, be heated to 60 ℃ after fully mixing, and constantly stirring makes solvent slowly evaporate into its dry tack free, vacuumize 15h under 110 ℃ condition promptly gets pressed powder then; Again pressed powder is used 90%H under 250 ± 50 ℃
2/ N
2Reduction was handled 5 ± 3 hours under the atmosphere, after under Ar atmosphere, be cooled to room temperature again, promptly obtain the conductive ceramic-carried metal catalyst,
(2) preparation of fuel cell membrane electrode: with conductive ceramic-carried metal catalyst and mass fraction is that 5-20% perfluorinated sulfonic resin emulsion is mixed and deionized water, ultrasonic dispersion 30min preparation catalyst pulp, evenly be coated on the poly-polytetrafluoroethylene membrane after 80 ℃ of vacuumizes remove and desolvate, be the both sides that are transferred to proton exchange membrane under the 1MPa at pressure again, promptly obtaining with the conductive ceramic-carried metal is the fuel cell membrane electrode of eelctro-catalyst.
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| CN200910138332A CN101872868A (en) | 2009-04-27 | 2009-04-27 | Fuel cell membrane electrode taking conductive ceramic-carried metal as electro-catalyst and preparation method thereof |
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| CN200910138332A CN101872868A (en) | 2009-04-27 | 2009-04-27 | Fuel cell membrane electrode taking conductive ceramic-carried metal as electro-catalyst and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103460470A (en) * | 2011-03-15 | 2013-12-18 | 凸版印刷株式会社 | Manufacturing method and manufacturing device for membrane electrode assembly for polymer electrolyte fuel cell, and polymer electrolyte fuel cell |
| CN103688397A (en) * | 2011-07-27 | 2014-03-26 | 丰田自动车株式会社 | Catalyst ink for fuel cell electrodes, membrane electrode assembly, fuel cell |
| CN103730665A (en) * | 2012-10-15 | 2014-04-16 | 丰田自动车株式会社 | Air cathode for air batteries and air battery |
-
2009
- 2009-04-27 CN CN200910138332A patent/CN101872868A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103460470A (en) * | 2011-03-15 | 2013-12-18 | 凸版印刷株式会社 | Manufacturing method and manufacturing device for membrane electrode assembly for polymer electrolyte fuel cell, and polymer electrolyte fuel cell |
| CN103460470B (en) * | 2011-03-15 | 2015-12-09 | 凸版印刷株式会社 | The manufacture method of membrane-electrode assembly for polymer electrolyte fuel cell and manufacturing installation, polymer electrolyte fuel cell |
| CN103688397A (en) * | 2011-07-27 | 2014-03-26 | 丰田自动车株式会社 | Catalyst ink for fuel cell electrodes, membrane electrode assembly, fuel cell |
| CN103730665A (en) * | 2012-10-15 | 2014-04-16 | 丰田自动车株式会社 | Air cathode for air batteries and air battery |
| US9225018B2 (en) | 2012-10-15 | 2015-12-29 | Toyota Jidosha Kabushiki Kaisha | Air cathode for air batteries and air battery |
| CN103730665B (en) * | 2012-10-15 | 2016-02-17 | 丰田自动车株式会社 | Air cell air pole and air cell |
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Application publication date: 20101027 |