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WO2014155929A1 - Procédé de fabrication de couche de catalyseur pour pile à combustible, couche de catalyseur pour pile à combustible et pile à combustible - Google Patents

Procédé de fabrication de couche de catalyseur pour pile à combustible, couche de catalyseur pour pile à combustible et pile à combustible Download PDF

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Publication number
WO2014155929A1
WO2014155929A1 PCT/JP2014/000637 JP2014000637W WO2014155929A1 WO 2014155929 A1 WO2014155929 A1 WO 2014155929A1 JP 2014000637 W JP2014000637 W JP 2014000637W WO 2014155929 A1 WO2014155929 A1 WO 2014155929A1
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WO
WIPO (PCT)
Prior art keywords
fuel cell
catalyst layer
catalyst
producing
cathode
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2014/000637
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English (en)
Japanese (ja)
Inventor
孝司 松岡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
JX Nippon Oil and Energy Corp
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 JX Nippon Oil and Energy Corp filed Critical JX Nippon Oil and Energy Corp
Publication of WO2014155929A1 publication Critical patent/WO2014155929A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H01M4/8882—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
    • H01M4/8605—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
    • H01M4/8807—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
    • 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]
    • 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 present invention relates to a fuel cell that generates electricity by an electrochemical reaction between hydrogen and oxygen.
  • a polymer electrolyte fuel cell has a basic structure in which a polymer electrolyte membrane, which is an electrolyte membrane, is arranged between a fuel electrode and an air electrode. It is a device that supplies the agent gas and generates power by the following electrochemical reaction.
  • Fuel electrode H 2 ⁇ 2H + + 2e ⁇ (1)
  • Air electrode 1 / 2O 2 + 2H + + 2e ⁇ ⁇ H 2 O (2)
  • the anode and the cathode each have a structure in which a catalyst layer and a gas diffusion layer (GDL) are laminated.
  • the catalyst layers of the electrodes are arranged opposite to each other with the solid polymer film interposed therebetween, thereby constituting a fuel cell.
  • the catalyst layer is a layer formed by binding carbon particles carrying a catalyst with an ion exchange resin.
  • the gas diffusion layer becomes a passage for the oxidant gas and the fuel gas.
  • hydrogen contained in the supplied fuel is decomposed into hydrogen ions and electrons as shown in the above formula (1).
  • hydrogen ions move inside the solid polymer electrolyte membrane toward the air electrode, and electrons move to the air electrode through an external circuit.
  • oxygen contained in the oxidant gas supplied to the cathode reacts with hydrogen ions and electrons that have moved from the fuel electrode, and water is generated as shown in the above formula (2). In this way, in the external circuit, electrons move from the fuel electrode toward the air electrode, so that electric power is taken out.
  • a procedure is employed in which a catalyst slurry is applied to a gas diffusion layer and then heated and dried to form a catalyst layer.
  • the catalyst layer produced by the conventional procedure has fine pores serving as reaction gas passages, and the ratio of the pores to the catalyst layer is at most about 15%. For this reason, in order to improve gas diffusivity, it was difficult to raise the ratio of a pore.
  • the present invention has been made in view of these problems, and an object thereof is to provide a technique capable of improving the gas diffusibility of a catalyst layer for a fuel cell.
  • An embodiment of the present invention is a method for producing a fuel cell catalyst layer.
  • a conductive carrier, a metal catalyst supported on the carrier, and a proton conductor made of a solid polymer material are dispersed in a dispersion containing a lower alcohol and water to obtain a water content of 20 to 60.
  • the lower alcohol may be an aliphatic alcohol or a polyhydric alcohol having 1 to 4 carbon atoms.
  • the area ratio of pores observed by a cross-sectional SEM (Scanning Electron Microscope, Scanning Electron Microscope) image may be 25 to 50%.
  • the proton conductor may have an EW of 450 or more and 900 or less.
  • the fuel cell catalyst layer includes a carrier having conductivity, a metal catalyst supported on the carrier, and a proton conductor made of a solid polymer material, and an area ratio of pores observed by a cross-sectional SEM image Is 25 to 50%.
  • the proton conductor may have an EW of 450 or more and 900 or less.
  • Yet another embodiment of the present invention is a fuel cell.
  • the fuel cell includes an electrolyte, a cathode provided on one side of the electrolyte, an anode provided on the other side of the electrolyte,
  • the fuel cell catalyst layer according to claim 7 is used only for the cathode.
  • the gas diffusibility of the catalyst layer for the fuel cell can be improved.
  • FIG. 1 is a perspective view schematically showing the structure of a fuel cell according to an embodiment. It is sectional drawing on the AA line of FIG. It is a cross-sectional SEM image of the cathode catalyst layer of an Example. It is a cross-sectional SEM image of the cathode catalyst layer of a comparative example. It is a graph which shows the relationship between the output voltage and P / C of each membrane electrode assembly of an Example and a comparative example.
  • FIG. 1 is a perspective view schematically showing the structure of the fuel cell 10 according to the first embodiment.
  • FIG. 2 is a cross-sectional view taken along the line AA in FIG.
  • the fuel cell 10 includes a flat membrane electrode assembly 50, and a separator 34 and a separator 36 are provided on both sides of the membrane electrode assembly 50. In this example, only one membrane electrode assembly 50 is shown, but a plurality of membrane electrode assemblies 50 may be stacked via the separator 34 or the separator 36 to constitute a fuel cell stack.
  • the membrane electrode assembly 50 includes a solid polymer electrolyte membrane 20, an anode 22, and a cathode 24.
  • Oxidant gas is distributed to the gas flow path 40 from an oxidant supply manifold (not shown), and the oxidant gas is supplied to the membrane electrode assembly 50 through the gas flow path 40.
  • a reformed gas containing a fuel gas for example, hydrogen gas
  • the fuel gas is supplied to 22.
  • an oxidant gas for example, air flows through the gas flow path 40 from the upper side to the lower side along the surface of the gas diffusion layer 32, whereby the oxidant gas is supplied to the cathode 24.
  • an electrochemical reaction occurs in the membrane electrode assembly 50.
  • hydrogen gas is supplied to the catalyst layer 26 via the gas diffusion layer 28
  • hydrogen in the gas becomes protons, and these protons move through the solid polymer electrolyte membrane 20 to the cathode 24 side.
  • the emitted electrons move to the external circuit and flow into the cathode 24 from the external circuit.
  • air is supplied to the catalyst layer 30 through the gas diffusion layer 32, oxygen is combined with protons to become water. As a result, electrons flow from the anode 22 toward the cathode 24 in the external circuit, and power can be taken out.
  • an alloy catalyst made of noble metal and ruthenium can be cited.
  • the noble metal used in the alloy catalyst include platinum and palladium.
  • the conductive carrier that supports the metal catalyst include acetylene black, ketjen black, carbon nanotube, and carbon nano-onion.
  • the microporous layer 29 applied to the gas diffusion base material 27 is a kneaded product (paste) obtained by kneading a conductive powder and a water repellent.
  • a kneaded product obtained by kneading a conductive powder and a water repellent.
  • carbon black can be used as the conductive powder.
  • a fluorine resin such as tetrafluoroethylene resin (PTFE) or tetrafluoroethylene / hexafluoropropylene copolymer (FEP) can be used.
  • the water repellent agent preferably has binding properties.
  • the binding property refers to a property that can be made sticky (state) by joining things that are less sticky or those that tend to break apart. Since the water repellent has binding properties, a paste can be obtained by kneading the conductive powder and the water repellent.
  • EW is greater than 900
  • the swelling of the solid polymer is reduced, and a gas diffusion path is sufficiently ensured even in a state where the porosity is low. Therefore, the effect of producing the pores of the catalyst layer 30 by the method described later becomes poor. .
  • Examples of the metal catalyst used for the catalyst layer 30 include platinum or a platinum alloy.
  • Examples of the metal used for the platinum alloy include cobalt, nickel, iron, manganese, iridium and the like.
  • Examples of the conductive carrier supporting the metal catalyst include acetylene black, ketjen black, carbon nanotube, and carbon nano-onion.
  • the microporous layer 33 applied to the gas diffusion base material 31 is a paste-like kneaded material obtained by kneading the conductive powder and the water repellent, and the micropores applied to the gas diffusion base material 27 described above. Similar to layer 29.
  • the catalyst layer 26 that constitutes the anode 22 and the catalyst layer 30 that constitutes the cathode 24 described above are formed by a manufacturing method including freeze-drying processing, which will be described later, and a cross-sectional SEM cut by an Ar ion beam, a Ga ion beam, or the like.
  • the area ratio of the pores observed by the image is 25 to 50%, preferably 35 to 40%.
  • the area ratio of the pores observed by the cross-sectional SEM image is obtained by binarizing the cross-sectional SEM image (7000 times or 15 ⁇ m square) to separate the pore portion and the portion other than the pore, and then with respect to the entire evaluation area. It is obtained by calculating the ratio of the pore portion.
  • Catalyst layer production method Here, a method for producing the catalyst layers (catalyst layer 26 and catalyst layer 30) will be described.
  • Lower alcohol has the effect of uniformly dispersing a metal catalyst and a proton conductor formed of a solid polymer material, and evaporates at a lower temperature and lower pressure than water. Do not disturb.
  • the proton conductors formed of the metal catalyst and the solid polymer material are not uniformly dispersed but form aggregates individually, so the proton conduction path in the catalyst layer and the reaction field of the fuel cell
  • the three-phase interface (catalyst, proton conductor, and gas interface) cannot be sufficiently formed, and the power generation characteristics deteriorate.
  • the obtained catalyst slurry is applied to the gas diffusion layer using a coating method such as a screen printing method.
  • the gas diffusion layer and the frozen catalyst slurry are vacuum-dried at room temperature for about 2 hours using a vacuum chamber.
  • the ice in the catalyst slurry is sublimated, and the space where the ice was present becomes pores or voids to form a catalyst layer.
  • the conditions for sublimating the ice in the catalyst slurry are determined by the temperature and pressure of the catalyst slurry in a frozen state, so that the gas diffusion layer and the frozen catalyst slurry are separated from the water in the water phase diagram.
  • the temperature may be increased so that the pressure is lower than the point of importance.
  • the gas diffusion layer can be kept on a metal flat plate made of frozen stainless steel, aluminum, aluminum alloy material, titanium, titanium alloy material, etc. It is possible to facilitate the freeze-drying process.
  • the gas diffusion layer and the catalyst layer are dried at 80 to 100 ° C. for 10 minutes to 3 hours, and then heat treated at 100 to 190 ° C. for 30 minutes to 2 hours.
  • the heat treatment temperature is preferably higher than the glass transition temperature of the solid polymer material used for the catalyst slurry and lower than the decomposition temperature.
  • a catalyst layer having a pore area ratio of 25 to 50% can be formed.
  • the catalyst layer is formed by a manufacturing method including freeze-drying, and the pore area ratio observed by a cross-sectional SEM image of a sample cut by an Ar ion beam, a Ga ion beam, or the like is 25 to 25%.
  • the catalyst layer can be made to have a porous and uniform pore structure as compared with a normal production method.
  • the gas diffusibility in the catalyst layer can be increased, and a higher concentration solid polymer can be used for the catalyst layer as a proton conductor, and as a result, the output voltage of the fuel cell 10 can be increased.
  • the pore size in the catalyst layer is uniform, when carbon is used as the catalyst carrier, the pores are not easily destroyed when the carbon corrodes, and the catalyst layer structure is destroyed when it deteriorates. It is possible to greatly suppress the gas diffusivity decrease (voltage decrease) due to the above.
  • FEP tetrafluoroethylene-hexafluoropropylene copolymer
  • the carbon paper is immersed in the FEP dispersion, dried at 60 ° C. for 1 hour, and then subjected to heat treatment (FEP water repellent treatment) at 380 ° C. for 15 minutes. Thereby, the carbon paper is subjected to water repellent treatment almost uniformly.
  • Vulcan XC-72 (manufactured by CABOT: Vulcan XC72R) and terpineol (manufactured by Kishida Chemical Co.) as a solvent and triton (manufactured by Kishida Chemical Co., Ltd.) as a solvent
  • the paste after defoaming is naturally cooled to produce cathode gas diffusion layer paste A.
  • the cathode gas diffusion layer paste B is prepared using the carbon paste B described above.
  • FEP tetrafluoroethylene-hexafluoropropylene copolymer
  • Hot pressing is performed in a state where a solid polymer electrolyte membrane having a thickness of 30 ⁇ m is sandwiched between the anode and the cathode produced by the above method.
  • Aciplex registered trademark
  • SF7202 manufactured by Asahi Kasei E-Materials
  • the membrane electrode assembly of the example was manufactured by hot pressing the anode, the solid polymer electrolyte membrane, and the cathode under the bonding conditions of 170 ° C. and 200 seconds.
  • the cathode catalyst layer of the example was subjected to cross-section cutting using ion milling (Ar ion beam, E-3500, manufactured by Hitachi High-Tech), and a cross-sectional SEM image (7000 times, see FIG. 3) was taken.
  • the obtained cross-sectional SEM image was binarized by image processing / image measurement / data processing software WinROOF (manufactured by Mitani Shoji Co., Ltd.), and the area ratio occupied by the pores was calculated. (31-39%).
  • the average porosity can be changed by changing the moisture in the catalyst layer slurry to 20 wt% to 60 wt%.
  • the present invention can be used for a fuel cell that generates electricity by an electrochemical reaction between hydrogen and oxygen.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Fuel Cell (AREA)
  • Inert Electrodes (AREA)

Abstract

Cette invention concerne un ensemble électrode à membrane (50) présentant une structure dans laquelle sont stratifiées une anode (22), une membrane électrolyte polymère solide (20), et une cathode (24). Une couche de diffusion de gaz d'anode (28) contenue dans l'anode (22) et une couche de diffusion de gaz de cathode (32) contenue dans la cathode (24) sont fabriquées par lyophilisation d'une suspension catalytique, le rapport de section des trous observés par microscopie électronique à balayage en coupe transversale allant de 25 à 50%.
PCT/JP2014/000637 2013-03-27 2014-02-06 Procédé de fabrication de couche de catalyseur pour pile à combustible, couche de catalyseur pour pile à combustible et pile à combustible Ceased WO2014155929A1 (fr)

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JP2013066501 2013-03-27
JP2013-066501 2013-03-27

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WO2014155929A1 true WO2014155929A1 (fr) 2014-10-02

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105680075A (zh) * 2014-12-08 2016-06-15 丰田自动车株式会社 制造膜电极组件的方法
CN105762374A (zh) * 2014-12-16 2016-07-13 中国科学院大连化学物理研究所 一种燃料电池催化层与膜电极组件及其制备方法

Citations (9)

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JPH08185865A (ja) * 1994-12-28 1996-07-16 Tokyo Gas Co Ltd 固体高分子型燃料電池用電極及びその製造方法
JPH09199138A (ja) * 1996-01-19 1997-07-31 Toyota Motor Corp 燃料電池用の電極または電極・電解質膜接合体の製造方法および燃料電池用の電極
JPH11167925A (ja) * 1997-10-01 1999-06-22 Tokyo Gas Co Ltd 燃料電池用電極及びその製造方法
JP2001338654A (ja) * 2000-05-29 2001-12-07 Asahi Glass Co Ltd 固体高分子型燃料電池
JP2004273257A (ja) * 2003-03-07 2004-09-30 Asahi Kasei Corp 燃料電池用の電極触媒層
JP2008047473A (ja) * 2006-08-18 2008-02-28 Nissan Motor Co Ltd 電極触媒
JP2008186798A (ja) * 2007-01-31 2008-08-14 Nissan Motor Co Ltd 電解質膜−電極接合体
JP2008269847A (ja) * 2007-04-17 2008-11-06 Toyota Motor Corp 燃料電池触媒層用インク及びその製造方法、燃料電池用膜電極接合体
JP2011077006A (ja) * 2009-10-02 2011-04-14 Toppan Printing Co Ltd 固体高分子型燃料電池用電極触媒層の製造方法および固体高分子型燃料電池用電極触媒層、ならびに膜電極接合体の製造方法および膜電極接合体

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08185865A (ja) * 1994-12-28 1996-07-16 Tokyo Gas Co Ltd 固体高分子型燃料電池用電極及びその製造方法
JPH09199138A (ja) * 1996-01-19 1997-07-31 Toyota Motor Corp 燃料電池用の電極または電極・電解質膜接合体の製造方法および燃料電池用の電極
JPH11167925A (ja) * 1997-10-01 1999-06-22 Tokyo Gas Co Ltd 燃料電池用電極及びその製造方法
JP2001338654A (ja) * 2000-05-29 2001-12-07 Asahi Glass Co Ltd 固体高分子型燃料電池
JP2004273257A (ja) * 2003-03-07 2004-09-30 Asahi Kasei Corp 燃料電池用の電極触媒層
JP2008047473A (ja) * 2006-08-18 2008-02-28 Nissan Motor Co Ltd 電極触媒
JP2008186798A (ja) * 2007-01-31 2008-08-14 Nissan Motor Co Ltd 電解質膜−電極接合体
JP2008269847A (ja) * 2007-04-17 2008-11-06 Toyota Motor Corp 燃料電池触媒層用インク及びその製造方法、燃料電池用膜電極接合体
JP2011077006A (ja) * 2009-10-02 2011-04-14 Toppan Printing Co Ltd 固体高分子型燃料電池用電極触媒層の製造方法および固体高分子型燃料電池用電極触媒層、ならびに膜電極接合体の製造方法および膜電極接合体

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105680075A (zh) * 2014-12-08 2016-06-15 丰田自动车株式会社 制造膜电极组件的方法
JP2016110855A (ja) * 2014-12-08 2016-06-20 トヨタ自動車株式会社 膜電極接合体の製造方法
US9673442B2 (en) 2014-12-08 2017-06-06 Toyota Jidosha Kabushiki Kaisha Method of manufacturing membrane electrode assembly
CN105762374A (zh) * 2014-12-16 2016-07-13 中国科学院大连化学物理研究所 一种燃料电池催化层与膜电极组件及其制备方法

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