WO2016103494A1 - Catalyseur d'électrode pour des piles à combustible et procédé permettant de fabriquer ce dernier - Google Patents

Catalyseur d'électrode pour des piles à combustible et procédé permettant de fabriquer ce dernier Download PDF

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Publication number
WO2016103494A1
WO2016103494A1 PCT/JP2014/084654 JP2014084654W WO2016103494A1 WO 2016103494 A1 WO2016103494 A1 WO 2016103494A1 JP 2014084654 W JP2014084654 W JP 2014084654W WO 2016103494 A1 WO2016103494 A1 WO 2016103494A1
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Prior art keywords
electrode catalyst
catalyst
ruthenium
fuel cell
nanosheet
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PCT/JP2014/084654
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English (en)
Japanese (ja)
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渉 杉本
智弘 大西
大裕 滝本
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国立大学法人信州大学
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Priority to PCT/JP2014/084654 priority Critical patent/WO2016103494A1/fr
Publication of WO2016103494A1 publication Critical patent/WO2016103494A1/fr

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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
    • 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
    • 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
    • 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
    • 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 an electrode catalyst for a fuel cell and a method for producing the same, and more specifically, a fuel that is preferably used as an electrode catalyst for a polymer electrolyte fuel cell, and that can further improve CO resistance and catalyst deterioration suppression ability.
  • the present invention relates to an electrode catalyst for a battery and a method for producing the same.
  • Ruthenium platinum alloy particles are widely used as an electrode catalyst with high CO resistance. It is known that the ruthenium platinum alloy particles change to a Pt electronic state due to alloying of ruthenium and platinum, so that the ruthenium platinum alloy particles become an electrode catalyst having high CO resistance due to a ligand effect or a dual function mechanism.
  • Non-patent Document 2 In response to this problem, it has been reported that CO resistance is drastically increased by mixing 100% of Pt atoms and Ru atoms in the alloy particles (Non-patent Document 2). In addition, this electrode catalyst is obtained by rapidly cooling after firing at a high temperature in order to synthesize alloy particles of Pt atoms and Ru atoms.
  • the electrode catalyst used for a home polymer electrolyte fuel cell not only to improve the CO resistance but also to have a characteristic that the electrode catalyst performance is not easily deteriorated.
  • the deterioration of the electrocatalytic performance is known as Ru ions are eluted from ruthenium platinum alloy particles due to a voltage load that occurs when the fuel cell is started or stopped, resulting in a decrease in CO resistance.
  • the present invention has been made in order to solve the above-mentioned problems, and the object thereof is preferably used as an electrode catalyst used in a home-use polymer electrolyte fuel cell, and has improved CO resistance and catalyst deterioration suppression ability.
  • An object of the present invention is to provide an electrode catalyst for a fuel cell that can be further improved and a method for producing the same.
  • the present inventor researches an electrode catalyst in which Ru atoms are present in the vicinity of Pt atoms, and also studies an electrode catalyst that can suppress Ru ion elution in order to further improve the catalyst deterioration suppression ability. did.
  • the present inventor thinks that if CO can be adsorbed to Ru atoms before CO is adsorbed to Pt atoms, CO resistance can be further improved.
  • the use of a Ru sheet having a large specific surface area was examined.
  • the electrode catalyst for a fuel cell according to the present invention for solving the above-mentioned problems is a composite electrode catalyst comprising a ruthenium nanosheet and an electrode catalyst having ruthenium platinum alloy particles supported on carbon black.
  • the ruthenium nanosheet is a metal sheet having a huge specific surface area
  • Ru atoms of the ruthenium nanosheet can be present in the vicinity of the Pt atoms on the surface of the ruthenium platinum alloy particles.
  • Ru of the ruthenium nanosheet is poisoned with CO before Pt is poisoned with CO, so that the CO resistance of Pt can be increased.
  • Ru ions are eluted from the ruthenium platinum alloy particles, it is expected that the eluted Ru ions are adsorbed on the ruthenium nanosheet and reprecipitated as Ru metal.
  • the reprecipitated Ru metal contributes to CO poisoning, and it is possible to improve the catalyst deterioration suppressing ability with respect to the CO resistance of Pt.
  • the composite electrode catalyst is preferably an anode electrode catalyst having hydrogen oxidation ability.
  • the hydrogen oxidation reaction activity retention rate is preferably 83% or more and the catalyst deterioration rate is preferably 10% or less.
  • the fuel cell electrode catalyst according to the present invention it is preferably used for CO tolerance use and catalyst deterioration suppression use.
  • a method for producing an electrode catalyst for a fuel cell comprises producing a composite electrode catalyst comprising a ruthenium nanosheet and an electrode catalyst carrying ruthenium platinum alloy particles on carbon black as an electrode catalyst for a fuel cell.
  • a method for producing a composite electrode catalyst comprising a RuO 2 nanosheet and an electrode catalyst having ruthenium platinum alloy particles supported on carbon black, and after producing the composite electrode catalyst, And a step of reducing by baking in a hydrogen atmosphere.
  • the RuO 2 nanosheet can be obtained by exfoliating a layered ruthenium oxide prepared in advance.
  • the fuel cell electrode catalyst of the present invention is preferably used as an electrode catalyst used in a polymer electrolyte fuel cell for home use, particularly as an anode electrode catalyst having hydrogen oxidation ability, and is resistant to CO and suppresses catalyst deterioration. Performance can be further improved.
  • Each electrode catalyst is an image observed by a transmission electron microscope, (A) is a Pt 1 Ru 1 / C, ( B) is a RuO 2 ns-Pt 1 Ru 1 / C, (C) is Runs -Pt 1 Ru 1 / C. Is an explanatory diagram showing a spectrum of binding energy relating Pt4f and Ru3d at each electrode catalyst, (a) is a Pt 1 Ru 1 / C, ( b) is a RuO 2 ns-Pt 1 Ru 1 / C, ( c) is Runs-Pt 1 Ru 1 / C.
  • the electrode catalyst for a fuel cell and the production method thereof according to the present invention will be described in detail.
  • the present invention is not limited to the following description as long as it is included in the technical scope.
  • the fuel cell electrode catalyst according to the present invention is characterized in that it is a composite electrode catalyst comprising a ruthenium nanosheet and an electrode catalyst having ruthenium platinum alloy particles supported on carbon black.
  • This composite electrode catalyst is preferably used as an anode electrode catalyst having hydrogen oxidation ability.
  • the ruthenium nanosheet is a metal sheet having a huge specific surface area
  • Ru atoms of the ruthenium nanosheet can be present in the vicinity of the Pt atoms on the surface of the ruthenium platinum alloy particles.
  • Ru of the ruthenium nanosheet is poisoned with CO before Pt is poisoned with CO, so that the CO resistance of Pt can be increased.
  • Ru ions are eluted from the ruthenium platinum alloy particles, it is expected that the eluted Ru ions are adsorbed on the ruthenium nanosheet and reprecipitated as Ru metal.
  • the reprecipitated Ru metal contributes to CO poisoning, and it is possible to improve the catalyst deterioration suppressing ability with respect to the CO resistance of Pt.
  • the ruthenium nanosheet is a metal nanosheet (also referred to as a metal nanosheet).
  • the ruthenium nanosheet has a scaly shape with a thickness of about 1 nm, a planar direction is several ⁇ m in size, and has a huge specific surface area. Therefore, it can be used not only as an electrode catalyst but also as a thin film material or a coating agent.
  • the fuel cell electrode catalyst preferably has a hydrogen oxidation reaction activity retention rate of 83% or more and a catalyst deterioration rate of 10% or less.
  • the fuel cell electrode catalyst having such characteristics is preferably used as a CO resistant use and a catalyst deterioration suppressing use.
  • the one where the upper limit of hydrogen oxidation reaction activity retention rate is larger is desirable, and it does not specifically limit.
  • Pt 2 Ru 3 / C widely used is about 72%.
  • the lower limit of the catalyst deterioration rate is desirably small, and is not particularly limited. In the Pt 2 Ru 3 / C, it is about 23%.
  • the method for producing a fuel cell electrode catalyst according to the present invention is a method for producing the above-described fuel cell electrode catalyst according to the present invention. That is, this is a method for producing a composite electrode catalyst of a ruthenium nanosheet and an electrode catalyst having ruthenium platinum alloy particles supported on carbon black as an electrode catalyst for a fuel cell. Specifically, after the step of manufacturing a composite electrode catalyst of a RuO 2 nanosheet and an electrode catalyst supporting ruthenium platinum alloy particles on carbon black, and the step of manufacturing the composite electrode catalyst, the composite electrode catalyst is treated with hydrogen. And a step of baking and reducing in an atmosphere.
  • the ruthenium oxide nanosheet (RuO 2 nanosheet) is obtained by peeling off a layer of ruthenium oxide prepared in advance, or between layers of ruthenium oxide (hydrogen type: H 0.2 RuO 2.1 ) as described in the examples below. It can be obtained by peeling off an alkylammonium-layered ruthenate intercalation compound containing alkylammonium ions.
  • Ruthenium nanosheets can be obtained by reducing such ruthenium oxide nanosheets.
  • a method for producing such a ruthenium nanosheet for example, a conventionally known method described in JP2010-280977A can be applied.
  • the electrode catalyst in which ruthenium platinum alloy particles are supported on a carbon black support a conventionally known one described in, for example, Japanese Patent Application Laid-Open No. 2011-134477 can be applied.
  • layered ruthenium oxide is a complex oxide of ruthenium oxide and an alkali metal (sodium, potassium, etc.).
  • K 0.2 RuO 2.1 ⁇ nH 2 O and Na 0.2 RuO 2 ⁇ nH 2 O have ion exchange capacity. By using it, it is possible to delaminate the layer as a single unit, so that it was possible to obtain a ruthenium oxide nanosheet.
  • ruthenium oxide (RuO 2 ) and potassium carbonate (K 2 CO 3 ) are weighed in a molar ratio of 8: 5 and wetted in acetone for 1 hour using an agate mortar. Mixed. Thereafter, the mixed powder was pelletized using a tablet molding machine. The pellets were placed on an alumina boat and baked at 850 ° C. for 12 hours in a tubular furnace under an argon atmosphere. After firing, the pellets were pulverized, washed with ion exchange distilled water, and the supernatant was removed. This operation was repeated until the supernatant became neutral to obtain layered ruthenium oxide (potassium type).
  • RuO 2 ruthenium oxide
  • K 2 CO 3 potassium carbonate
  • layered ruthenium oxide (potassium type)
  • acid treatment is performed in a water bath at 60 ° C. for 72 hours, so that K + ions contained in layered ruthenium oxide (potassium type) are converted into hydrogen ions (protons). ).
  • the supernatant was removed by washing with ion-exchanged distilled water. This operation was repeated until the supernatant became neutral.
  • layered ruthenium oxide hydrogen type: H 0.2 RuO 2.1
  • layered ruthenium oxide (hydrogen type: H 0.2 RuO 2.1 )
  • 10% TBAOH aqueous solution as a release agent for obtaining a ruthenium oxide nanosheet was added.
  • layered ruthenium oxide (hydrogen type: H 0.2 RuO 2.1 ) was added to distilled water and shaken for 10 days.
  • the ruthenium oxide nanosheet peeled off by this method was centrifuged at 2000 rpm for 30 minutes, and then the supernatant was collected and the aqueous dispersion of ruthenium oxide nanosheet diluted with ultrapure water to a concentration of 0.02 g / L ( Ruthenium oxide nanosheet colloid) was obtained.
  • the ruthenium oxide nanosheet is described as RuO 2 ns.
  • a test dispersion for a polymer electrolyte fuel cell was prepared by applying a catalyst dispersion to such glassy carbon. The catalyst dispersion was applied so that the carbon content was 5.5 ⁇ g / cm 2 regardless of the content of RuO 2 ns contained in the composite electrode catalyst provided on the test electrode.
  • the nanosheets of RuO 2 ns-Pt 1 Ru 1 / C and Runs-Pt 1 Ru 1 / C partially covered the Pt 1 Ru 1 particles.
  • the nanosheet of Runs-Pt 1 Ru 1 / C maintained the sheet form even after reduction.
  • FIG. 2 is an explanatory diagram showing the spectrum of the binding energy related to Pt4f and Ru3d in each electrode catalyst, where (a) shows Pt 1 Ru 1 / C and (b) shows RuO 2 ns-Pt 1 Ru 1 / C. , (C) is Runs-Pt 1 Ru 1 / C.
  • the Pt4f binding energy of Runs-Pt 1 Ru 1 / C was lower than Pt 1 Ru 1 / C and RuO 2 ns-Pt 1 Ru 1 / C. This is because the reduction of RuO 2 ns can predict that the Pt atom on the surface of the alloy particle and the Ru atom of Runs are metal-bonded, and therefore it is possible that the energy shift has occurred. This energy shift tendency is generally considered to be effective in improving CO tolerance.
  • FIG. 3 is an explanatory view showing an X-ray diffraction pattern of each electrocatalyst, wherein (a) is Pt 2 Ru 3 / C, (b) is Pt 1 Ru 1 / C, and (c) is RuO. 2 ns-Pt 1 Ru 1 / C, and (d) is Runs-Pt 1 Ru 1 / C.
  • the amount of hydrogen desorption electricity of Runs-Pt 1 Ru 1 / C is about three times larger than Pt 1 Ru 1 / C and RuO 2 ns-Pt 1 Ru 1 / C. This increase in the amount of electricity desorbed from hydrogen is thought to be due to the formation of ruthenium nanosheets.
  • the composite electrode catalyst composed of ruthenium nanosheets has improved CO resistance.
  • Runs-Pt 1 Ru 1 / C The hydrogen oxidation reaction activity of Runs-Pt 1 Ru 1 / C after the endurance test was repeated 5000 cycles under the same conditions was 93A (g-PtRu) ⁇ 1 . This was higher than Pt 2 Ru 3 / C and Pt 1 Ru 1 / C after 1000 cycles endurance test, and was similar to RuO 2 ns-Pt 1 Ru 1 / C after 1000 cycles endurance test. From this, it is understood that Runs-Pt 1 Ru 1 / C has high catalyst durability, and can be expected to be an electrode catalyst that can be operated for a long time.
  • Ru ions eluted in the durability test may have re-deposited as Ru metal on the nanosheet, which is considered to improve the catalyst durability.
  • the improvement in CO tolerance of the composite electrocatalyst of Runs and Pt 1 Ru 1 / C is considered to be due to the ligand effect accompanying the change in the electronic state of Pt. As a result, it is expected that CO molecules adsorbed on Pt are easily oxidized and removed. In addition, there is a possibility that CO is first adsorbed to the Ru atoms of Runs before CO adsorption to Pt with the conversion to Runs, and this point is also considered to contribute to the improvement of CO resistance.

Abstract

Le problème à résoudre dans le cadre de la présente invention consiste à fournir : un catalyseur d'électrode pour des piles à combustible, qui convient pour être utilisé comme catalyseur d'électrode pour des piles à combustible à polymère solide à usage domestique et qui présente une meilleure résistance au monoxyde de carbone (CO) et une meilleure capacité de suppression de détérioration de catalyseur ; et un procédé permettant de produire ce catalyseur d'électrode pour des piles à combustible. La solution consiste en ce que le problème mentionné ci-dessus a été résolu par un catalyseur d'électrode pour des piles à combustible, qui est un catalyseur d'électrode composite composé d'une nanofeuille de ruthénium et un catalyseur d'électrode obtenu en ayant des particules d'alliage de platine et de ruthénium de support du noir de charbon. Il est préférable que ce catalyseur d'électrode pour des piles à combustible soit un catalyseur d'électrode anodique ayant une capacité d'oxydation de l'hydrogène. Il est également préférable que ce catalyseur d'électrode pour des piles à combustible présente un rapport de maintien d'activité de réaction d'oxydation de l'hydrogène égal ou supérieur à 83 % et un rapport de détérioration du catalyseur égal ou inférieur à 10 %. Ce catalyseur d'électrode pour des piles à combustible convient pour être utilisé comme catalyseur d'électrode pour des applications résistantes au CO et des applications de suppression de détérioration du catalyseur.
PCT/JP2014/084654 2014-12-26 2014-12-26 Catalyseur d'électrode pour des piles à combustible et procédé permettant de fabriquer ce dernier WO2016103494A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007046279A1 (fr) * 2005-10-19 2007-04-26 Shin-Etsu Chemical Co., Ltd. Catalyseur d’électrode pour pile à combustible
JP2010280977A (ja) * 2009-06-08 2010-12-16 Shinshu Univ 金属ナノシートの製造方法、および金属ナノシート
JP2011134477A (ja) * 2009-12-22 2011-07-07 Shinshu Univ 燃料電池用電極触媒の製造方法
JP2011253627A (ja) * 2010-05-31 2011-12-15 National Institute For Materials Science 燃料電池用電極触媒およびその製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007046279A1 (fr) * 2005-10-19 2007-04-26 Shin-Etsu Chemical Co., Ltd. Catalyseur d’électrode pour pile à combustible
JP2010280977A (ja) * 2009-06-08 2010-12-16 Shinshu Univ 金属ナノシートの製造方法、および金属ナノシート
JP2011134477A (ja) * 2009-12-22 2011-07-07 Shinshu Univ 燃料電池用電極触媒の製造方法
JP2011253627A (ja) * 2010-05-31 2011-12-15 National Institute For Materials Science 燃料電池用電極触媒およびその製造方法

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