CA2341494C - Screen-printing paste and screen-printing method of fabricating a gas diffusion electrode - Google Patents

Screen-printing paste and screen-printing method of fabricating a gas diffusion electrode Download PDF

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Publication number
CA2341494C
CA2341494C CA2341494A CA2341494A CA2341494C CA 2341494 C CA2341494 C CA 2341494C CA 2341494 A CA2341494 A CA 2341494A CA 2341494 A CA2341494 A CA 2341494A CA 2341494 C CA2341494 C CA 2341494C
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CA
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Prior art keywords
screen
printing
polymer
gas diffusion
paste
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Expired - Lifetime
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CA2341494A
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French (fr)
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CA2341494A1 (en
Inventor
Armin Datz
Barbara Schricker
Manfred Waidhas
Peter Otschik
Winfried Schaffrath
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Siemens AG
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Siemens AG
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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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8892—Impregnation or coating of the catalyst layer, e.g. by an ionomer
    • 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
    • H01M4/8807—Gas diffusion layers
    • 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
    • H01M4/8817—Treatment of supports before application of the catalytic active composition
    • 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
    • H01M4/8835—Screen printing
    • 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
    • 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
    • H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • 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
    • H01M4/928—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
    • 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
    • H01M4/88—Processes of manufacture
    • H01M4/8817—Treatment of supports before application of the catalytic active composition
    • H01M4/8821—Wet proofing
    • 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

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  • Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Sustainable Energy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Composite Materials (AREA)
  • Sustainable Development (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inert Electrodes (AREA)
  • Printing Methods (AREA)
  • Fuel Cell (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)

Abstract

The invention relates to a screen printing method for producing a gas diffusion electrode, using a polybutylacrylate--polymethacrylate copolymer as a binder in the screen-printing paste.

Description

Description Screen-printing paste and screen-printing method of fabricating a gas diffusion electrode The invention relates to a screen-printing paste for fabricating a gas diffusion electrode according to the preamble of claim 1. In addition, the invention also relates to a screen-printing method of fabricating gas diffusion electrodes suitable for fuel cells.
A PEM (polymer electrolyte membrane) fuel cell has as its core section a membrane-electrode unit each of which is composed of a membrane which on both sides has an electrode comprising an electrocatalyst layer.
The electrode preferably has a solid, gas-permeable and electroconductive support, e.g. carbon fabric or carbon paper, which preferably, for the purpose of hydrophobicization, is hydrophobicized by means of a polymer suspension. Applied to this support is an electrocatalyst layer which in turn is hydrophobicized.
The polymer for the purpose of hydrophobicization is hereinafter referred to as polymer A: this involves polymers such as e.g. PTFE, i.e. polytetrafluoroethylene, which is known under the trade name TEFLON . The polymer A can be present both in the support and in the electrocatalyst layer.
The polymer A content required for hydrophobicization of the electrocatalyst layer has hitherto, as a rule, been 20-60% by weight, a high polymer A, e.g. Teflon, content having the effect of inhibiting the activity of the platinum catalyst, increasing the contact resistances and reducing the porosity of the electrode (Watanabe, J. Elektroanal.
Chem. 195 (1985) 81-83), i.e. a detrimental effect on the system. The polymer A for the hydrophobicization of AMENDED SHEET

- la -the electrocatalyst layer can therefore also be described as a "catalyst inhibitor".

AMENDED SHEET
With the electrodes known hitherto there is not only the problem of a high polymer A content for the hydrophobicization of the electrocatalyst layer (20-60%
by weight, based on the metallic-catalyst content), but also that of the homogeneity of the thickness of the electrocatalyst layer. There is a need to provide a suitable fabrication method which, in a cost-effective manner suitable for large-scale production, permits uniform coating of the support with dry catalyst powder in small layer thicknesses of 3-40 pm.
According to the conventional method (Watanabe, J. Electroanal. Chem. 195 (1985) 81-83; J. Electroanal.
Chem. 197 (1986) 195-208, M. Uchida, J. Electrochem.
Soc. 142 (1995), 463-468), a dry powdered mixture of catalyst powder hydrophobicized beforehand with PTFE is pressed onto the likewise hydrophobicized support. To prepare the starting material, the carbon powder is first mixed intensively with the PTFE dispersion and is then dried above a temperature of 280 C. In the process, the surface-active wetting agent (Triton X
100) present in the dispersion is removed. The wetting agent is employed to counterbalance the poor processing characteristics resulting from the high polymer A
content in the catalyst paste. Then the mixture is powdered.
The latter method is laborious, and a uniform thickness of the electrocatalyst layer in small layer thicknesses can be achieved only at the expense of low productivity and subject to technical difficulties.
Other drawbacks of this method are that - a high polymer A content is present to hydrophobicize the electrocatalyst layer, and AMENDED SHEET

- 2a -- for processing purposes a wetting agent is added which has to be removed separately and leaves troublesome residues.
Screen printing is a known technique for fabricating a uniformly thin layer. The screen-printing method for AMENDED SHEET
building up an electrochemical system is already known.
According to US 4 229 490 A, the screen-printing paste, which contains Teflon dispersion, graphite and platinum black, must again, for stabilization purposes, be admixed with more than 50% by weight of the wetting agent or dispersant "Triton X 100". The Teflon fraction employed for hydrophobicization in the screen-printing paste and consequently also the proportion present in the resulting electrocatalyst layer is about 25% by weight. The paste is printed onto a solid support, e.g. carbon paper, which again contains 60% by weight Teflon. The electrode fabricated by this method not only has the drawback of the high polymer A
content in order to hydrophobicize the electrocatalyst layer, but also that of the wetting agent added in an amount of more than 50% by weight of the catalyst paste.

In addition, WO 96/29752 Al discloses a cation exchange membrane which consists of polymers and also contains further fillers. This membrane is claimed to be directly suitable for the reaction using methanol as a fuel.

On the basis of the prior art discussed it is an object of the invention to provide a screen-printing paste for fabricating a gas diffusion electrode and to specify the screen-printing method thus implemented.

In one aspect of the invention, there is provided a screen-printing paste as a starting material for fabricating a gas diffusion electrode via a screen-printing method, comprising at least one polymer and at least one metallic catalyst and a high-boiling solvent, wherein among two polymers A and B the polymer A serves for hydrophobicization and the polymer B represents a binder, 3a characterized in that the polymer B is a poly(butyl acrylate)-polymethacrylate copolymer, a poly(vinyl alcohol) and/or a poly(ethylene oxide).

In another aspect of the invention, there is provided a screen-printing method of fabricating a gas diffusion electrode for a fuel cell making use of a screen-printing paste as described herein, wherein the screen-printing paste used comprises at least one polymer and at least one metallic catalyst and a high-boiling solvent, wherein among two polymers A and B the polymer A serves for hydrophobicization and the polymer B represents a binder, comprising the following procedural steps: the screen-printing paste is applied to a base in order to form a screen-printing layer of between 3 and 40 pm, serving as the screen-printing medium are the high-boiling solvent and the polymer B in the specification as described herein, thus ensuring the uniformity of the screen-printing layer, after baking out, only such residues of the solvent or of the polymer B remain in the screen-printing layer as do not interfere with use of the gas diffusion electrode in a fuel cell.

In another aspect of the invention, there is provided a screen-printing process for producing a gas diffusion electrode employing a screen-printing paste which comprises at least one metallic catalyst and a high-boiling solvent which is suitable for screen-printing, the binder used in the screen-printing paste being a poly(butyl acrylate)-polymethacrylate copolymer.

In another aspect of the invention, there is provided a screen-printing paste for use in the production of a gas diffusion electrode, which comprises at least one metallic catalyst and a high-boiling solvent which is 3b suitable for screen-printing, also containing a poly(butyl acrylate)-polymethacrylate copolymer as binder.

According to embodiments of the invention, the screen-printing paste, as well as with the metallic catalyst and the high-boiling solvent, is admixed with a polymer B, specifically preferably a polymer which can be baked out at up to 400 C. An example of such a polymer B is a poly(butyl acrylate)-polymethacrylate copolymer, although poly(vinyl alcohol) or poly(ethylene oxide) or mixtures of these substances are possible as the polymer B. In contrast, the screen-printing paste according to the invention does not contain any proportion of polymer A
or only a proportion which is decisively reduced compared with the prior art. This proportion by weight can be limited, in the gas diffusion electrode fabricated according to the inventive method, to at most 10% by weight.
In the screen-printing paste according to the invention, the metallic catalyst, as in the prior art, is platinum black or platinum on carbon. The high-boiling solvent used comprises an ester and/or a ketone and/or an alcohol, particularly preferably butyl glycolate, cyclohexanone and/or terpineol.
The invention implements a screen-printing method of fabricating a gas diffusion electrode employing a screen-printing paste which comprises polymer A in an amount of from 0 to at most 10% by weight, based on the metallic-catalyst content, at least one metallic catalyst and a high-boiling solvent.
This means that the screen-printing paste is free from wetting agent and is either also free from polymer A or contains polymer A only in small amounts of less than 10% by weight, based on the metallic-catalyst content.
The polymer B, in contrast, is removed by the baking-out procedure in such a way that no residues remain which would interfere with the use as a gas diffusion electrode.
Further details and advantages of the invention can be gathered from the following description of illustrative embodiments in conjunction with the claims. Described is the fabrication of a gas diffusion electrode for use in a fuel cell, which consists of a support, an electrocatalyst layer and a suitable hydrophobicization.

AMENDED SHEET

- 4a -Referred to as the electrocatalyst layer is the layer which is preferably applied to a solid, gas-permeable and AMENDED SHEET
electroconductive support of the electrode and at whose catalytic surface the anodic oxidation of the fuel to produce protons or the cathodic reduction of the oxygen takes place. The electrocatalyst layer comprises at least the metallic catalyst, which preferably contains platinum and which can be employed in the catalyst paste either in pure form as platinum black or in dilute form as platinum on carbon. Preferably, the electrocatalyst layer contains no further constituents since, according to the preferred embodiment of the invention, the screen-printing medium admixed to the catalyst paste for processing purposes was removed by drying and heating of the finished, i.e. coated electrode.
For processing purposes, the screen-printing paste, also referred to as carbon paste or catalyst paste, depending on the process step, is admixed with a high-boiling solvent as a screen-printing medium, such as e.g. an ester, ketone and/or an alcohol, especially butyl glycolate, cyclohexanone and/or terpineol.
However, the screen-printing paste involves not only -as known from the prior art - the admixture of a high-boiling solvent as a screen-printing medium, but also that of a polymer B, such as e.g. poly(butyl acrylate)-poly(methyl acrylate) copolymer, poly(vinyl alcohol) and/or poly(ethylene oxide), as a binder. The polymer B
can preferably be baked out, particularly at temperatures up to 400 C, and/or only leaves residues which do not interfere with fuel cell operation.
The electrode is a gas-permeable, electroconductive layer on the membrane, which preferably comprises a support with an electrocatalyst layer. The support or substrate used AMENDED SHEET

- 5a -is preferably a carbon fabric or a carbon paper or some other porous, electroconductive substrate.
The platinum loading determined by weighing is 2-3 mg/cm2 in the case of pure platinum black as the catalyst, and is AMENDED SHEET
from 0.15 to 0.4 mg/cmZ in the case of platinum on carbon as a catalyst, depending on the platinum loading of the carbon.
In the course of fabricating the gas diffusion electrode, the screen-printing procedure and subsequent processing is followed by the finished electrode being hydrophobicized with a polymer A (e.g. Teflon).
Current-voltage curves of membrane-electrode units comprising gas diffusion electrodes according to the invention were performed, in which an extraordinarily low voltage drop at high current intensities could be observed. This can be ascribed, inter alia, to the low diffusion inhibition owing to the low polymer A content and detriment to the hydrophobicization by wetting agent residues within the porous electrocatalyst layer.
A particular advantage of the screen-printing method implemented with the screen-printing paste described is the improved homogeneity of the layer thickness, because the electrocatalyst paste with the small addition or without the addition of polymer A can be processed more easily.

AMENDED SHEET

Claims (2)

CLAIMS:
1. Screen-printing process for producing a gas diffusion electrode employing a screen-printing paste which comprises at least one metallic catalyst and a high-boiling solvent which is suitable for screen-printing, the binder used in the screen-printing paste being a poly(butyl acrylate)-polymethacrylate copolymer.
2. Screen-printing paste for use in the production of a gas diffusion electrode, which comprises at least one metallic catalyst and a high-boiling solvent which is suitable for screen-printing, also containing a poly(butyl acrylate)-polymethacrylate copolymer as binder.
CA2341494A 1998-08-26 1999-08-20 Screen-printing paste and screen-printing method of fabricating a gas diffusion electrode Expired - Lifetime CA2341494C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19838786.5 1998-08-26
DE19838786 1998-08-26
PCT/DE1999/002620 WO2000013242A2 (en) 1998-08-26 1999-08-20 Screen printing method for producing a gas diffusion electrode

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CA2341494A1 CA2341494A1 (en) 2000-03-09
CA2341494C true CA2341494C (en) 2010-06-01

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US (2) US6645660B2 (en)
EP (2) EP1118129B1 (en)
JP (2) JP4792160B2 (en)
CN (2) CN1195336C (en)
AT (2) ATE415713T1 (en)
CA (2) CA2341495C (en)
DE (2) DE59914914D1 (en)
ES (2) ES2214895T3 (en)
WO (2) WO2000013243A2 (en)

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CN1324502A (en) 2001-11-28
CA2341495A1 (en) 2000-03-09
DE59908263D1 (en) 2004-02-12
JP4707834B2 (en) 2011-06-22
ATE257621T1 (en) 2004-01-15
CN1173426C (en) 2004-10-27
EP1118130B1 (en) 2004-01-07
ATE415713T1 (en) 2008-12-15
EP1118129A2 (en) 2001-07-25
CA2341494A1 (en) 2000-03-09
ES2214895T3 (en) 2004-09-16
JP2002525811A (en) 2002-08-13
EP1118129B1 (en) 2008-11-26
ES2315020T3 (en) 2009-03-16
WO2000013242A3 (en) 2000-06-08
CN1328707A (en) 2001-12-26
US20020022083A1 (en) 2002-02-21
WO2000013243A2 (en) 2000-03-09
EP1118130A2 (en) 2001-07-25
US20010018145A1 (en) 2001-08-30
DE59914914D1 (en) 2009-01-08
WO2000013242A2 (en) 2000-03-09
US6645660B2 (en) 2003-11-11
CN1195336C (en) 2005-03-30
CA2341495C (en) 2010-07-06
WO2000013243A3 (en) 2000-08-10
JP2002525812A (en) 2002-08-13
JP4792160B2 (en) 2011-10-12

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