WO2009075037A1 - Procédé de préparation d'un catalyseur d'électrodes pour piles à combustible, et pile à combustible à électrolyte polymère - Google Patents

Procédé de préparation d'un catalyseur d'électrodes pour piles à combustible, et pile à combustible à électrolyte polymère Download PDF

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Publication number
WO2009075037A1
WO2009075037A1 PCT/JP2007/074368 JP2007074368W WO2009075037A1 WO 2009075037 A1 WO2009075037 A1 WO 2009075037A1 JP 2007074368 W JP2007074368 W JP 2007074368W WO 2009075037 A1 WO2009075037 A1 WO 2009075037A1
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WIPO (PCT)
Prior art keywords
platinum
catalyst
group element
fuel cells
electrode catalyst
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Ceased
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PCT/JP2007/074368
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English (en)
Inventor
Naoko Iwata
Hiroaki Takahashi
Hidetaka Nishikoori
Christa Barkschat
Iris Herrmann
Sebastian Fiechter
Peter Bogdanoff
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Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Toyota Motor Corp
Original Assignee
Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Toyota Motor Corp
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Application filed by Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH, Toyota Motor Corp filed Critical Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Priority to PCT/JP2007/074368 priority Critical patent/WO2009075037A1/fr
Publication of WO2009075037A1 publication Critical patent/WO2009075037A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • H01M4/921—Alloys or mixtures with metallic elements
    • 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
    • H01M4/923—Compounds thereof with non-metallic elements
    • 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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M2008/1095—Fuel cells with polymeric electrolytes
    • 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

Definitions

  • the present invention relates to a method of preparing an electrode catalyst for fuel cells having an excellent oxygen reduction activity.
  • the invention also relates to a polymer electrolyte fuel cell having such electrode catalyst in a catalyst layer of its electrode.
  • Polymer electrolyte fuel cells which comprise a polymer electrolyte membrane, are easy to reduce in size and weight For this reason, they are expected to provide power supplies for mobile vehicles such as electric vehicles, and small-sized cogeneration systems.
  • the hydrogen ion produced at the anode by the reaction of equation (1) passes (diffuses) through the solid polymer electrolyte membrane in a hydrated state OfH + (XH 2 O).
  • the hydrogen ion that has passed through the membrane is fed to the cathode for the reaction of equation (2).
  • These electrode reactions at the anode and cathode proceed at the interface between the catalyst in an electrode catalyst layer, which is closely attached to the solid polymer electrolyte membrane as a reaction site, and the solid polymer electrolyte membrane.
  • the electrode reaction in each of the catalyst layers for the anode and cathode of the polymer electrolyte fuel cell proceeds at a three-phase interface (reaction site) where the individual reaction gas, the catalyst, and a fluorine-containing ion exchange resin (electrolyte) simultaneously exist.
  • a catalyst comprising a metal-supported carbon, such as a carbon black support with a large specific surface area supporting a metal catalyst, such as platinum, is coated with the same or different kind of fluorine-containing ion exchange resin as or from the polymer electrolyte membrane and is then used as the material of the catalyst layer.
  • the production of water from proton and electron at the cathode takes place in the presence of the three phases of the catalyst, carbon particle, and electrolyte.
  • the electrolyte, which conducts proton, and the carbon particle, which conducts electron coexists, with which further the catalyst coexists, whereby the oxygen gas is reduced. Therefore, the greater the amount of catalyst supported by the carbon particle, the higher the electricity generation efficiency.
  • the catalyst used in fuel cells comprises a noble metal, such as platinum, an increase in the amount of catalyst supported by the carbon particle results in an increase in fuel cell manufacturing cost.
  • the catalyst is indispensable for promoting reactions. While as the catalyst material, platinum or platinum alloys have been the major candidates for both the hydrogen electrode and the oxygen electrode, there is a large overpotential, particularly at the oxygen electrode (cathode). The overpotential could be reduced by increasing the supported amount of platinum or platinum alloy in the catalyst. However, increasing the amount of catalyst does not lead to much reduction in overpotential, while creating the bigger problem of an increase in cost Thus, there is the major question of how cost and catalyst performance can be balanced.
  • the disclosed catalyst comprises a catalyst material derived from a noble metal-containing macrocyclic compound precursor.
  • the catalyst material which is supported by a high-surface-area carbon, comprises a noble metal in a zero-oxidation state.
  • a disclosed preparation method involves dissolving a noble metal macrocyclic compound in water or an organic solvent, adding an electrically conductive carbon to the resultant solution, causing the macrocyclic material to be adsorbed on the carbon support, and separating the macrocyclic material supported by the carbon.
  • PtNx (2 ⁇ x ⁇ 4) centres are assumed to be present in the carbon, which has been formed by the pyrolysis of the organic part of the precursor.
  • a practical application may involve an electrode comprising, as a catalyst, a pyrolysed platinum-based PtNx (2 ⁇ x ⁇ 4) centre catalyst material in which platinum (Pt) is coordinated to the two ⁇ four nitrogen atoms.
  • JP Patent Publication (Kohyo) No. 2004-532734 A indicated below discloses a non-platinum-containing chelate catalyst in which metal porphyrin is used.
  • JP Patent Publication (Kokai) No. 2006-035186 A 4 indicated below discloses an electrode catalyst in which a macrocyclic metal complex is highly adsorbed on to the carbon support and subsequently pyrolysed by a heat treatment.
  • JP Patent Publication (Kokai) No. 2003-168442 A indicated below discloses a fuel electrode for polymer electrolyte fuel cells comprising an ion-conductive substance, an electron conductive substance, and a catalyst substance, in which a metal complex, such as metallotetra porphyrin, is added.
  • JP Patent Publication (Kokai) No. 03-030838 A (1991) indicated below discloses a reducing catalyst comprising a tetraphenylporphyrin derivative and the compound.
  • a platinum-supported catalyst is prepared as follows. In a wet reduction method, a Pt complex is adsorbed on a support dispersed in a solution and then reduced by a reducing agent into a supported Pt metal. When an alloy catalyst (such as PtFe) is to be prepared, a Pt particle is supported on a carbon support and then an alloy seed is supported by reduction.
  • an alloy catalyst such as PtFe
  • an electrode catalyst comprising a pyrolysed platinum-based PtNx (2 ⁇ x ⁇ 4) centre catalyst material which is composed of small platinum particles deposited within the pyrolytic carbon, which has additionally PtNx (2 ⁇ x ⁇ 4) chelate structure embedded in the pyrolytic carbon, in which a platinum group element or a platinum group element and another element are coordinated to the each four nitrogen atoms, thereby an improved utilization efficiency and enhanced electricity generation performance can be obtained.
  • the inventors realized that, in an electrode catalyst for fuel cells comprising a pyrolysed containing platinum-based PtNx (2 ⁇ x ⁇ 4) complex having small platinum particles and additional PtNx (2 ⁇ x ⁇ 4) chelate centres in which a platinum-group element or a platinum-group element and another element are coordinated to the each four nitrogen atoms separately, the particle size of the platinum particle can be adjusted by performing a specific process, thereby achieving the aforementioned object.
  • the invention provides a method of preparing a platinum group-supported carbon electrode catalyst for fuel cells, comprising the steps of: mixing a pyrolysed containing platinum-based PtNx (2 ⁇ x ⁇ 4) complex having small platinum particles and additional PtNx (2 ⁇ x ⁇ 4) chelate centres in which a platinum-group element or a platinum-group element and another element are coordinated to the each four nitrogen atoms, separately with a pore-forming agent, such as iron oxalate, by crushing and/or milling; calcining a mixture obtained by the crushing and/or milling in an inert gas atmosphere; dipping a calcined product in a strong acid; and filtering, washing, and drying the calcined product after dipping.
  • a pore-forming agent such as iron oxalate
  • the optimum calcination temperature in the step of calcining the mixture obtained by the crushing and/or milling in an inert gas atmosphere was determined to range from 700 0 C to 900°C.
  • the platinum-based PtNx (2 ⁇ x ⁇ 4) structure is not particularly limited.
  • a preferable example is a nitrogen-containing transition metal complex comprising one or more kinds of macrocyclic compound selected from porphyrin (PP) or its derivatives, phthalocyanine (Pc) or its derivatives, and tetraazaannulene (TAA) or its derivatives, in which one or more kinds of platinum-group element selected from platinum, ruthenium, rhodium, palladium, osmium, and iridium, or such platinum-group element and one or more kinds of other elements, are coordinated.
  • PP porphyrin
  • Pc phthalocyanine
  • TAA tetraazaannulene
  • the pore-forming agent in the present invention refers to a compound that act for itself or by its calcination products as a framework for the calc of the macrocyclic precursor. Gaseous products of the pore forming agent lead a forming effect during the pyrolysis of the macrocycle precursor. The framework is removed after calcination. So that a porus matrix of carbon black is remained. Some of the compound remains in the pores.
  • the pore-forming agent are transition metal oxide and transition metal oxalate. Among others, preferable examples are iron oxalate, cobalt oxalate, calcium oxalate, calcium carbonate, iron oxide, and copper oxide.
  • the invention provides a polymer electrolyte fuel cell comprising an electrode catalyst for fuel cells prepared by the above method.
  • a platinum group-supported carbon electrode catalyst for fuel cells which involves mixing a precursor, a pyrolysed containing platinum-based PiNx (2 ⁇ x ⁇ 4) complex having small platinum particles and additional PtNx (2 ⁇ x ⁇ 4) chelate centres with a pore-forming agent, such as iron oxalate, by crushing and/or milling, calcining the crushed and/or ground mixture in an inert gas atmosphere, dipping a calcined product in a strong acid, and filtering, washing, and drying the calcined product after dipping, provides the following actions and effects:
  • Fine particles of Pt can be prepared, so that the Pt utilization ratio can be improved and the amount of Pt used in the system as well as cost can be reduced.
  • the electrode catalyst comprising a pyrolysed catalyst which is prepared from a nitrogen-containing platinum-based complex having a PtNx chelate structure in which a platinum-group element or a platinum-group element and another element are coordinated to the each four nitrogen atoms, and to achieve improved electricity generation performance.
  • PtNx precursor is calcinated to a carbon matrix with embedded PtNx precursor centres. Parts of precursor art transferred to platinum particles with good dispersion and small particle size. This is due to the good features of the carbon and the mechanism of particle formation from PtNx structures.
  • Fig. 1 shows the electricity generation performance of a pyrolysed PtTTP/FeOx catalyst (example) and a Pt(40wt%)-supported carbon catalyst (comparative example).
  • Fig 2 shows the relationship between the calcination temperature of the PtTTP/FeOx catalyst and electricity generation performance (J km ).
  • Fig. 3 shows the relationship between the Pt feeding amount of the pyrolysed PtTTP/FeOx catalyst and electricity generation performance (J km ).
  • a schematic of a nitrogen-containing transition metal complex having a PtNx (2 ⁇ x ⁇ 4) chelate structure in which a platinum group element or a platinum group element and another element are coordinated to the each four nitrogen atoms separately is shown below.
  • a platinum-group element or a platinum-group element and another element (Pt) are coordinated to the each four nitrogen atoms separately in a macrocyclic compound, thus forming a macrocyclic compound complex (MCC).
  • Nx-chelate structures such as porphyrin and its derivatives, phthalocyanine and its derivatives, azaporphyrin and its derivatives, tetraazaannulene and its derivatives, and a Schiff base.
  • platinum-based PtNx (2 ⁇ x ⁇ 4) centre catalyst material in which a platinum-group element or a platinum-group element and another element (Pt) are coordinated to the two ⁇ four nitrogen atoms separately.
  • the carbon-based platinum-based PtNx (2 ⁇ x ⁇ 4) centre catalyst material in which a platinum-group element or each platinum-group element and another element (Pt) are coordinated to the four nitrogen atoms, may be either supported by a support or not; catalyst performance can be provided even without a support.
  • the nitrogen-containing compound used in the present invention is carbonized by calcination, so that the compound by itself can constitute a support, providing the advantage that no separate support is required. And more the sage of forming agent like Fe-oxalate, leads to very sutable prosity and a special molecular structure of the carbon.
  • the electrically conductive support there are no limitations as to the electrically conductive support. Examples are carbon black, carbon nanotube, and carbon nanofiber.
  • the method of mixing the nitrogen-containing platinum-based complex having a PtN4 chelate structure and an iron oxalate by crushing and/or milling is not particularly limited, and a variety of known methods may be employed for obtaining fine particles and mixing them. Among others, a method involving milling in a mortar is preferable from a laboratory point of view.
  • the 5, 10, 15, 20-tetrakis tolyl platinum (II) porphyrin (PtTTP) is a complex compound expressed by the following chemical formula:
  • Fig. 1 shows the electricity generation performance of the PtTTP/FeOx catalyst (example) and the Pt(40wt%)-supported carbon catalyst (comparative example).
  • the result of Fig. 1 indicates that the pyrolysed PtTTP/FeOx catalyst obtained by the preparation method of the present invention provides an improvement over the conventional Pt(40wt%)-supported carbon catalyst in electricity generation performance.
  • Fig. 2 shows the relationship between calcination temperature and ORR activity (J km ). It was learned from the result of Fig. 2 that improved activity is obtained in the range of calcination temperature from 700 0 C to 900 0 C.
  • Various pyrolysed PtITlVFeOx catalysts were prepared by varying the ratio of the tetrakis tolyl Pt porphyrin (PtTTP) to the iron oxalate (FeC 2 O 4 ) in step (1) of the above preparation method.
  • Fig. 3 shows the relationship between the Pt feeding amount and ORR activity (Ji ⁇ n ). It was learned from the result of Fig. 2 that improved performance is obtained when the Pt feeding proportion is 5 mol% or greater.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inert Electrodes (AREA)
  • Catalysts (AREA)

Abstract

Selon l'invention, l'efficacité de l'utilisation du platine et les performances de production d'électricité sont améliorées dans un catalyseur d'électrodes comprenant un catalyseur pyrolysé fabriqué dans un matériau catalytique central à base de platine PtNx (2 ≤x ≤4), dans lequel un élément du groupe platine ou un élément du groupe platine et tout autre élément sont associés séparément à chacun des quatre atomes d'azote. Selon l'invention, un procédé de fabrication d'un catalyseur d'électrodes en carbone supporté sur un groupe platine comprend les étapes suivantes: mélange d'un complexe à base de platine contenant de l'azote présentant une structure chélate PtNx (2 ≤x ≤ 4), dans lequel l'élément du groupe platine ou un élément du groupe platine et un autre élément sont associés à chacun des quatre atomes d'azote séparément, avec un agent de formation de pores par écrasement ou broyage; calcination du mélange obtenu par écrasement et/ou broyage dans une atmosphère de gaz inerte; trempage d'un produit calciné dans un acide fort; filtrage; lavage et séchage du produit calciné après trempage.
PCT/JP2007/074368 2007-12-12 2007-12-12 Procédé de préparation d'un catalyseur d'électrodes pour piles à combustible, et pile à combustible à électrolyte polymère Ceased WO2009075037A1 (fr)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011045869A1 (fr) 2009-10-16 2011-04-21 Toyota Jidosha Kabushiki Kaisha Procédé de fabrication de catalyseur d'électrode pour pile à combustible
US20140011102A1 (en) * 2011-03-24 2014-01-09 Yokohama National University Oxygen reduction catalyst and method for producing the same
US10566631B2 (en) 2016-07-27 2020-02-18 Industrial Technology Research Institute Electrocatalyst and fuel cell employing the same
CN114628706A (zh) * 2022-04-11 2022-06-14 西安凯立新材料股份有限公司 质子交换膜燃料电池用催化剂及其制备方法
CN118039944A (zh) * 2024-01-23 2024-05-14 中南大学 铂基金属间化合物催化剂及其制备方法和应用
CN120280507A (zh) * 2025-06-09 2025-07-08 温州大学碳材料与氢能产业技术研究院 共价有机框架衍生的低载量Pt/C催化剂及其制备方法和应用

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EP0176831A2 (fr) * 1984-09-27 1986-04-09 Eltech Systems Corporation Electrode à diffusion gazeuse à réponse rapide destinée à une forte intensité et procédé pour sa fabrication
EP0512413A2 (fr) * 1991-05-08 1992-11-11 R.R. DONNELLEY & SONS COMPANY Procédé d'identification des usagers de coupons
WO2003004156A2 (fr) * 2001-07-03 2003-01-16 Hahn-Meitner-Institut Berlin Gmbh Materiau catalyseur au chelate, exempt de platine, pour reduction selective par l'oxygene, et son procede de fabrication
WO2006121191A1 (fr) * 2005-05-10 2006-11-16 Toyota Jidosha Kabushiki Kaisha Catalyseur d’électrode à base de porphyrine

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0176831A2 (fr) * 1984-09-27 1986-04-09 Eltech Systems Corporation Electrode à diffusion gazeuse à réponse rapide destinée à une forte intensité et procédé pour sa fabrication
EP0512413A2 (fr) * 1991-05-08 1992-11-11 R.R. DONNELLEY & SONS COMPANY Procédé d'identification des usagers de coupons
WO2003004156A2 (fr) * 2001-07-03 2003-01-16 Hahn-Meitner-Institut Berlin Gmbh Materiau catalyseur au chelate, exempt de platine, pour reduction selective par l'oxygene, et son procede de fabrication
WO2006121191A1 (fr) * 2005-05-10 2006-11-16 Toyota Jidosha Kabushiki Kaisha Catalyseur d’électrode à base de porphyrine

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Title
LEFEVRE M ET AL: "O2 reduction in PEM fuel cells: activity site structural information for catalysts obtained by the pyrolysis at high temperature of Fe precursors", JOURNAL OF PHYSICAL CHEMISTRY. B, MATERIALS, SURFACES, INTERFACES AND BIOPHYSICAL, WASHINGTON, DC, US, vol. 104, 1 January 2000 (2000-01-01), pages 11238 - 11247, XP002229709, ISSN: 1089-5647 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011045869A1 (fr) 2009-10-16 2011-04-21 Toyota Jidosha Kabushiki Kaisha Procédé de fabrication de catalyseur d'électrode pour pile à combustible
CN102511099A (zh) * 2009-10-16 2012-06-20 丰田自动车株式会社 生产用于燃料电池的电极催化剂的方法
JP2013507723A (ja) * 2009-10-16 2013-03-04 トヨタ自動車株式会社 燃料電池用電極触媒の製造方法
US20140011102A1 (en) * 2011-03-24 2014-01-09 Yokohama National University Oxygen reduction catalyst and method for producing the same
US9748580B2 (en) * 2011-03-24 2017-08-29 Yokohama National University Oxygen reduction catalyst and method for producing the same
US10566631B2 (en) 2016-07-27 2020-02-18 Industrial Technology Research Institute Electrocatalyst and fuel cell employing the same
CN114628706A (zh) * 2022-04-11 2022-06-14 西安凯立新材料股份有限公司 质子交换膜燃料电池用催化剂及其制备方法
CN114628706B (zh) * 2022-04-11 2024-02-13 西安凯立新材料股份有限公司 质子交换膜燃料电池用催化剂及其制备方法
CN118039944A (zh) * 2024-01-23 2024-05-14 中南大学 铂基金属间化合物催化剂及其制备方法和应用
CN120280507A (zh) * 2025-06-09 2025-07-08 温州大学碳材料与氢能产业技术研究院 共价有机框架衍生的低载量Pt/C催化剂及其制备方法和应用

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