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WO2005081352A1 - Encre de catalyseur, procede de fabrication de celle-ci et de preparation de membranes revetues de catalyseur - Google Patents

Encre de catalyseur, procede de fabrication de celle-ci et de preparation de membranes revetues de catalyseur Download PDF

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Publication number
WO2005081352A1
WO2005081352A1 PCT/US2005/005313 US2005005313W WO2005081352A1 WO 2005081352 A1 WO2005081352 A1 WO 2005081352A1 US 2005005313 W US2005005313 W US 2005005313W WO 2005081352 A1 WO2005081352 A1 WO 2005081352A1
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WO
WIPO (PCT)
Prior art keywords
catalyst
membrane
catalyst ink
pem
ink
Prior art date
Application number
PCT/US2005/005313
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English (en)
Inventor
David L. Olmeijer
Christopher G. Castledine
Jonathan D. Servaites
Douglas S. Diez
Original Assignee
Polyfuel, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Polyfuel, Inc. filed Critical Polyfuel, Inc.
Publication of WO2005081352A1 publication Critical patent/WO2005081352A1/fr

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Classifications

    • 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]
    • 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
    • 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
    • H01M4/881—Electrolytic membranes
    • 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
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to catalyst inks used in the formation of catalyst coated membranes used in fuel cells.
  • Nafion® is a common commercial ionomer used in fuel cell applications. It is a sulfonated perflorinated polymer which functions as a polymer electrolyte membrane (PEM).
  • PEM polymer electrolyte membrane
  • the PEM is typically coated with anode and cathode catalyst layers which promote chemical reactions which results in the oxidation of a fuel on the anode surface, transport of a proton across the PEM and reduction of oxygen at the cathode surface. I the process, electrons are conducted form the anode through a load and then to the cathode to complete the reduction of oxygen to water.
  • catalyst layers have been applied to Nafion® and other PEMs by applying a suspension of metal catalysts such as platinum or platinum/ruthenium, typically supported on carbon particles, and Nafion® ionomer suspended in an aqueous solution or water/alcohol solution.
  • metal catalysts such as platinum or platinum/ruthenium, typically supported on carbon particles
  • Nafion® ionomer suspended in an aqueous solution or water/alcohol solution.
  • DMFC direct methanol fuel cell
  • a significant problem with such catalyst coated membranes is the swelling of the ionomer and membranes when in contact with fuels such as methanol. This results in a weakening of the interface between the catalyst layer and the membrane.
  • Nafion® is often not compatible with such PEMs resulting in less than optimal adherence between the catalyst layer and the membrane and interfacial resistance at the catalyst layer/membrane junction.
  • the invention relates to a catalyst ink comprising a metal catalyst, an ionomer and one or more non-aqueous solvents which together comprise at least 50% of the liquid in said catalyst ink.
  • the non-aqueous solvents taken together with any other component in the liquid portion of the catalyst will have a dielectric constant of approximately 5 or greater, more preferably 15 or greater and most preferably 30 or greater.
  • Individual non-aqueous solvents also preferably have the aforementioned dielectric constants.
  • Some non-aqueous solvents may have a dielectric constant which is less than the preferred dielectric constant. However, when combined with one or more other non-aqueous solvents the resultant liquid will have the preferred dielectric constant.
  • non-aqueous solvent(s) examples include alcohols, glycols, alkyl ethers, alkyl ketones, alkyl esters, alkyl amides, alkyl sulfones, alkyl sulfoxides and alkyl carbonates.
  • the alkyl groups may be linear, branched or cyclic and may be substituted. Such alkyl groups generally have between 1 and 10 carbon atoms.
  • the non-aqueous solvent(s) generally has a boiling point between 80 and 250 degrees Celsius.
  • the non-aqueous solvent is dimethylacetamide (DMAc), dimethylformamide (DMF), N-methyl pyrrolidone, propylene carbonate, dimethyl sulfoxide, tetraniethylene sulfone, cyclohexanone, cyclopentanone, 2-butoxy ethanol, 2-methoxy ethanol, ethylene glycol, 1,2 propanediol, isopropyl alcohol, glycerol, 1-octanol, butanol, 2-methoxyethyl ether, and/or methyl propyl ketone.
  • DMAc dimethylacetamide
  • DMF dimethylformamide
  • N-methyl pyrrolidone N-methyl pyrrolidone
  • propylene carbonate dimethyl sulfoxide
  • tetraniethylene sulfone cyclohexanone
  • cyclopentanone 2-butoxy ethanol
  • 2-methoxy ethanol 2-methoxy ethanol
  • DMAc may be combined with one or more of dimethylformamide (DMF), N-methyl pyrrolidone, propylene carbonate, dimethyl sulfoxide, tetramethylene sulfone, cyclohexanone, cyclopentanone, 2-butoxy ethanol, 2-methoxy ethanol, ethylene glycol, 1,2 propanediol, isopropyl alcohol, glycerol, 1-octanol, butanol, 2-methoxyethyl ether, and/or methyl propyl ketone.
  • DMF dimethylformamide
  • N-methyl pyrrolidone propylene carbonate
  • dimethyl sulfoxide tetramethylene sulfone
  • cyclohexanone cyclopentanone
  • 2-butoxy ethanol 2-methoxy ethanol
  • ethylene glycol 1,2 propanediol
  • isopropyl alcohol glycerol
  • 1-octanol butan
  • the catalyst ink can include a conductive filler such as graphite particles, carbon particles or graphitized carbon particles.
  • the invention also includes a process for making the catalyst ink which comprises mixing the ionomer, metal catalyst and one or non-aqueous solvent(s) to form a catalytic ink.
  • the ionomer is preferably part of a mixture comprising the ionomer and the non-aqueous solvent.
  • the ionomer e.g., Nafion®
  • the ionomer is supplied as a suspension in water or water/alcohol mixture. This suspension of ionomer can be distilled under vacuum in the presence of the non-aqueous solvent to produce a solution/suspension of ionomer in the non-aqueous solvent(s).
  • the catalyst is then added to the mixture of ionomer and non-aqueous solvent(s) to form the catalyst ink.
  • the invention also includes a process for making a catalyst coated membrane.
  • a polymer electrolyte membrane (PEM) is first dried at a temperature between 50°C and 170°C to form a dehydrated membrane.
  • the membrane is then exposed to air having a temperature between 15°C and 30°C and a relative humidity between 35% and 70%. This forms a pretreated membrane.
  • PEM polymer electrolyte membrane
  • the catalyst ink is applied to a first surface of the pretreated membrane to form a first catalyst layer.
  • the first surface of the PEM is then contacted with a gas stream having a temperature between 15°C and 30°C and a relative humidity of between 35% and 70% to remove bulk fluid from the membrane.
  • the membrane is dried at a temperature between 50°C and 170°C. If necessary, the process may be repeated to apply additional layers of catalyst to the PEM to form a catalyst coated membrane (CCM).
  • CCM catalyst coated membrane
  • the CCM is annealed at a temperature between 70°C and 200°C. Pressure may also be applied, e.g, between 1 to 200 kilograms per cm 2 . Temperature and pressure may be applied by use of a hot press or heated rollers
  • the PEM is a continuous web and the process is carried out either step wise or on a continuous basis.
  • the catalyst coated membranes (CCMs) made according to the process of the invention can be used to make membrane electrode assemblies (MEAs) which can be used to fabricate fuel cells such as hydrogen and methanol fuel cells.
  • MEAs membrane electrode assemblies
  • Fig. 1 is a flow chart for an embodiment of the process for making a catalyst coated membrane.
  • Fig. 2 is a plot voltage versus current density for the catalyst coated membrane of Example 1 at various concentrations of methanol.
  • Fig. 3 is a voltage versus current density plot for a Nafion® membrane which has been coated with the anode and catalyst inks and in the same manner as set forth in Example 1.
  • the invention includes catalyst inks containing metal catalysts, ionomer and one or more non-aqueous solvent(s).
  • the non-aqueous solvent(s) taken together if more than one is present are preferably between 50 to 100 wt% of the liquid present in the catalyst ink, more preferably between 75 and 100 wt%, and still more preferably between 90 and 100 wt%.
  • the amount of non-aqueous solvent may be slightly less than 100 wt% wherein said solvent is present at between 90 and 99wt%, more preferably between 95 and 98wt%. Under such circumstances, the preferred other liquid component is water.
  • the non-aqueous solvents taken together with any other component in the liquid portion of the catalyst ink will have a dielectric constant of approximately 5 or greater, more preferably 15 or greater and most preferably 30 or greater.
  • Individual non-aqueous solvents also preferably have the aforementioned dielectric constants.
  • some non-aqueous solvents may have a dielectric constant which is less than the preferred dielectric constant.
  • the resultant liquid will have the preferred dielectric constant.
  • the non-aqueous solvent(s) may be alcohols, glycols, alkyl ethers, alkyl ketones, alkyl esters, alkyl amides, alkyl sulfones, alkyl sulfoxides and alkyl carbonates.
  • the alkyl groups may be linear, branched or cyclic and may be substituted alkyl. Such alkyl groups generally have between 1 and 10 carbon atoms.
  • the non-aqueous solvent(s) generally has a boiling point between 80 and 250°C.
  • the non-aqueous solvent is dimethylformamide (DMF), N-methyl pyrrolidone, propylene carbonate, dimethyl sulfoxide, tetramethylene sulfone, cyclohexanone, cyclopentanone, 2-butoxy ethanol, 2- methoxy ethanol, ethylene glycol, 1,2 propanediol, isopropyl alcohol, glycerol, 1-octanol, butanol, 2-methoxyethyl ether, and/or methyl propyl ketone.
  • DMAc dimethylformamide
  • DMAc may be combined with one or more of the following: N-methyl pyrrolidone, propylene carbonate, dimethyl sulfoxide, tetramethylene sulfone, cyclohexanone, cyclopentanone, 2-butoxy ethanol, 2-methoxy ethanol, ethylene glycol, 1,2 propanediol, isopropyl alcohol, glycerol, 1-octanol, butanol, 2-methoxyethyl ether, and/or methyl propyl ketone.
  • the non-aqueous solvents preferably have a boiling point of 80°C to 250°C, more preferably 125°C to 225°C, and still more preferably between 150°C and 200°C.
  • the non-aqueous solvent is capable of solubilizing the polymer electrolyte membrane (PEM) to which it is applied. This property allows for a plasticizing effect at the surface of the membrane which facilitates bonding between the components of the catalyst layer and the membrane surface.
  • the exposure time between the PEM and the non-aqueous solvent is chosen so as to maximize the strength of the junction between the catalyst layer and the PEM while minimizing the actual solubilization of the membrane during the formation of a catalyst layer.
  • the amount of ionomer present in the catalyst layers formed from the catalyst ink will be a percentage defined as the mass of the ionomer divided by the mass of ionomer plus the mass of metal catalyst and the mass of the support particles when a supported catalyst is used. These are essentially the solids which will be deposited as the catalyst layer.
  • supported metal catalysts e.g., platinum Black or platinum/ruthenium Black
  • the ionomer constitute 1-40%, more preferably between 2 and 25% and most preferably between 4 and 15%.
  • the ionomer be between 3 and 90%, more preferably between 5 and 60% and most preferably between 15 and 40%.
  • Cathode and anode inks may contain different catalysts.
  • the cathode in a PEM for a DMFC application it is preferred that the cathode contain Pt as catalyst while the anode contain Pt/Ru as catalyst.
  • the preferred catalyst is Pt which is used at both the cathode and anode.
  • Nafion® may be the ionomer of choice.
  • Commercially available Nafion® ionomer is available as a suspension in water/alcohol.
  • vacuum distillation is used for solvent exchange. See Items 1-4 of Fig. 1. For example, if it is desired to obtain Nafion® at 10% by weight in DMAc, a 5% Nafion® solution in alcohol and water is mixed with DMAc solvent and distilled in a vacuum until the liquid reaches 10% solids. The solution temperature is kept under 55°C, preferably under 40°C to avoid gelation. This results in a solvent with less than 1% water or alcohol in the mixture.
  • lonomers other than Nafion® may be used.
  • Particular ionomers are those having the same or similar formula to the polymer electrolyte membrane used to make the catalyst coated membrane. Use of compositions of the same or similar formula enhances the interface between the catalyst layer and the membrane. In addition, less stress is produced at the catalyst membrane interface when exposed to fuels such as methanol or solvents such as water, since the ionomer and membrane have substantially the same properties such as fuel permeability and swelling caused by water.
  • the overall effect of matching such properties is enhanced durability and a decreased interfacial resistance produced at the catalyst layer/membrane junction as compared to when Nafion® ionomer is applied as a catalyst layer to a membrane which is other than a Nafion® membrane.
  • Anode catalyst ink can be made by mixing a platinum/ruthenium black catalyst (50/50 atomic ratio) with the above described Nafion® solution where additional DMAc is added as necessary. See Items 5-6 of Fig. 1.
  • an additional conductive filler is added to the formula to enhance the stability of the ink dispersion, modify the ink viscosity and facilitate electrical conductivity of the catalyst layer.
  • Graphitized synthetic carbon particles with a surface area between 5 and 15 square meters per gram and a particle diameter between 5 and 15 micron diameter are preferred (Asbury Carbons, Asbury, NJ).
  • the amount of carbon additive may range from 0 to 40% by weight, preferably 3 to 20%. See Item 2 of Fig. 1.
  • Non-graphitized carbon particles may also be used.
  • Table I A preferred formulation for an anode ink is shown in Table I: Table I
  • a cathode ink may be prepared as described above using platinum black catalyst rather than platinum/ruthenium black catalyst (see, e.g., Items 8, 9 and 10 of Fig. 1).
  • platinum black catalyst rather than platinum/ruthenium black catalyst (see, e.g., Items 8, 9 and 10 of Fig. 1).
  • a preferred foimulation for a catalyst is shown in Table II:
  • Each of the catalyst inks are separately mixed by repeated sonications (see, e.g., Items 13-15 and 17-20 of Fig. 1). For production runs, more scaleable processes, such as ball milling are preferred over sonication. [035]
  • the quality of the dispersion may be assessed through the use of a "fineness of grind,” commonly called Hegman gage in the ink making industry. A reading of 1.5 ⁇ m or less is acceptable for the inks though a reading of less than 12 ⁇ m is preferred.
  • Anode ink 16 and cathode ink 21 are thereafter used to form a catalyst layer on membrane 22.
  • the membrane 22 in Fig. 2 may be any of a wide variety of membranes including those disclosed in U.S. Patent Applications Serial Nos. 09/872,770, filed June 1, 2001, Publication No. US 2002-0127454 Al, dated September 12, 2002, entitled “Polymer Composition”; 10/351,257, filed January 23, 2003, Publication No. US 2003-0219640 Al, dated November 27, 2003, entitled “Acid Base Proton Conducting Polymer Blend Membrane”; 10/438,186, filed May 13, 2003, Publication No. US 2004-0039148 Al, dated February 26, 2004, entitled “Sulfonated Copolymer”; 10/449,299, filed February 20, 2003, Publication No.
  • the ionomer correspond to the polymer electrolyte membrane, in some instances, it may appropriate to use ionomers made from any of the above identified formulations for use in catalyst inks applied to polymer electrolyte membranes having a different formula.
  • the overall process for applying a first catalyst layer to a first surface of membrane 22 involves the following steps: (1) Applying heat to dehydrate the membrane (Fig. 1, Item 24); (2) applying the catalyst ink (Fig. 1, Item 26); (3) contacting the first surface of the membrane with a gas stream to remove fluid from the membrane (Fig. 1, Item 27), and (4) drying the membrane (Fig. 1, Item 28). The process may then be repeated on a second surface of the membrane to apply a first catalyst layer to thereby form a catalyst coated membrane. See Fig. 1, Items 30, 31 and 32.
  • multiple catalyst layers are applied to the polymer electrolyte membrane. This may be achieved by repeating the aforementioned processes until the catalyst coated membrane has the desired properties. See Fig. 1, Items 34-36 and 38-40
  • an additional step is used in the preparation of the catalyst coated membrane.
  • the dried membrane Prior to the application of catalyst ink, the dried membrane is contacted with a gaseous fluid such as air which is maintained at a predetermined temperature and relative humidity.
  • the overall process includes the steps of (1) drying the polymer electrolyte membrane to between 50°C and 170°C to form a dehydrated membrane; (2) contacting the dehydrated membrane with a gas such as air having a temperature between 15°C and 30°C and a relative humidity between 35% and 70% to form a pretreated membrane; (3) contacting a first surface of said pretreated membrane with the catalyst ink of claim 1 to form a first catalyst layer on said first surface of said PEM; (4) contacting the first surface of the membrane with a gas stream having a temperature between 15°C and 30°C and a relative humidity of between 35% and 70% to remove bulk fluid from said membrane, and (5) drying the membrane at a temperature between 50°C and 170°C.
  • the drying of the membrane in step 1 is preferably carried out at between 50°C and 170°C, preferably between 100°C and 170°C and most preferably at about 140°C.
  • the drying time depends on temperature but will generally be between 2 and 15 minutes. For example, when drying at 140°C the drying step should take between 3 and 8 minutes, most preferably 5 minutes. This results in the drying of the membrane.
  • CCMs made from such membranes often fracture.
  • dehydration protects the membrane from aggressive solubilization by the solvent.
  • the drying of the catalyst coated membrane in the last step of the processes is preferably carried out at between 50°C and 170°C, preferably between 80°C and 140°C and most preferably at about 100°C.
  • the drying time depends on temperature but will generally be between 3 and 30 minutes. For example, when drying at 100°C the drying step should take between 3 and 10 minutes, most preferably 5 minutes. This results in the drying of the membrane.
  • CCMs made from such membranes often fracture.
  • dehydration protects the membrane from aggressive solubilization by the solvent.
  • the polymer electrolyte membrane may be a continuous web on which the catalyst layers may be applied in a step wise or continuous process.
  • the catalyst layers are applied to individual sections of the membrane.
  • the membrane is preferably stored at a temperature between 15°C and 30°C and at a relative humidity between 0 and 30%. See, e.g., Items 25, 29, 33 and 37 of Fig. 1.
  • the CCM may be stored under similar conditions prior to subsequent treatment. See Item 41 of Fig. 1.
  • the CCM is preferably annealing at a temperature between about 70°C and 200°C, more preferably from 90°C - 160°C , and most preferably between 100°C and 140°C .
  • Pressure may also be applied to the opposing surfaces of the CCM.
  • subjected to a hot press process see Fig. 1, Item 42
  • a particularly preferred hot press process includes the application of a pressure of about 20 kilograms per square centimeter at 120°C for 2 minutes. However, these parameters may vary depending upon the components used.
  • pressures may vary from between 1 to 200 kilograms per square centimeter, more preferably between 5 and 50, and most preferably between 10 and 25 kilograms per centimeter squared.
  • the time of the hot press process may range from 1 second to 60 minutes, more preferably from 30 seconds to 30 minutes, and most preferably between 90 seconds to 10 minutes.
  • hot rollers may be used alone or in combination with hot press to apply the necessary temperature and pressure to complete the annealing of the CCM.
  • the aforementioned catalyst coated membranes are used to make MEAs by combining the CCM with gas diffusion layers and optionally current collectors. While standard gas diffusion layers may be used, gas diffusion layers such as those disclosed in U.S. Patent Application Serial No. 60/502,024, filed September 10, 2003, entitled "Process for Application of Gas Diffusion Layer to a Catalyst Coated Membrane" can be utilized.
  • the MEAs are used in fuel cells for portable or stationary applications.
  • Portable uses include electronic devices such as portable computers, video cameras, and vehicles such as automobiles, planes, boats, aerospace vehicles, etc.
  • Stationary applications include residential and commercial power supplies.
  • the Nafion® solution was prepared by taking 200mg of a stock 5% Nafion® solution, adding 300mg of DMAc solvent, and distilling under vacuum until the bottom product reached a nominal 10% solids (actual 10.1%).
  • the anode ink was dispersed by mixing with a small spatula for 1 minute, immersing in a bath sonicator for 25 minutes, stirring by hand, sonicating in a bath for another 10 minutes, stirring, then probe sonicating for ten minutes.
  • the cathode ink was also mixed by hand with a small spatula for approximately one minute before immersing the container in a bath sonicator for 25 minutes. Afterwards, it was stirred again with the spatula, then probe sonicated for three 10-minute cycles, with stirring after each cycle.
  • the Zl membrane and Nafion® 117 membrane were prepared by baking in an oven for 5 minutes at 140°C, then storing in a desiccator filled with fresh "Drierite” (calcium sulfate) dessicant. Screens were obtained for printing 22 cm 2 square blocks using Saatilene® HiTechTM mesh with mesh counts of 125/inch and 196/inch.
  • the samples were dried under an unheated blower until visually dry (approx. 2.5 minutes), then placed in a 100°C oven for five minutes, and finally stored in a desiccator in this dried state until the next ink layer was applied. During this time, the room environment was maintained at a temperature of between 71 -75°C, with relative humidity at 55 - 60%. After the final layer was applied and dried, the samples were hot-pressed in a Carver two-post press at a pressure of 20kg cm 2 active area at 120°C for two minutes.

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Abstract

L'invention concerne des encres de catalyseur utilisées dans la formation de membranes revêtues de catalyseur utilisées dans des piles à combustible.
PCT/US2005/005313 2004-02-18 2005-02-18 Encre de catalyseur, procede de fabrication de celle-ci et de preparation de membranes revetues de catalyseur WO2005081352A1 (fr)

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US54607804P 2004-02-18 2004-02-18
US60/546,078 2004-02-18

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