WO2017081910A1 - Catalyseur pour électrodes à gaz et batterie - Google Patents

Catalyseur pour électrodes à gaz et batterie Download PDF

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Publication number
WO2017081910A1
WO2017081910A1 PCT/JP2016/074858 JP2016074858W WO2017081910A1 WO 2017081910 A1 WO2017081910 A1 WO 2017081910A1 JP 2016074858 W JP2016074858 W JP 2016074858W WO 2017081910 A1 WO2017081910 A1 WO 2017081910A1
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Prior art keywords
gas
catalyst
gas electrode
carrier
electrode catalyst
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PCT/JP2016/074858
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English (en)
Japanese (ja)
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裕輝 名古
峻 園田
横田　博
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デンカ株式会社
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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
    • H01M4/90—Selection of catalytic material
    • 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
    • H01M4/96—Carbon-based electrodes
    • 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

Definitions

  • the present invention relates to a gas electrode catalyst and a battery.
  • a battery using gas as a reactant is useful as a device capable of obtaining electric energy larger than the volume of the battery itself.
  • fuel cells are considered promising as clean power generators that consume hydrogen and air and discharge only water.
  • polymer electrolyte fuel cells (PEFC) that use polymer electrolytes as ion conductors have room temperature. From the advantages of being able to operate in the vicinity and being relatively easy to downsize, it is promising as a new power generator for home use or automobile use.
  • a gas electrode catalyst is generally used to promote the reaction of the reactant gas and efficiently extract a current.
  • the gas electrode catalyst there is a form in which a substance having catalytic activity is attached and supported on a porous carrier having conductivity.
  • metal particles such as platinum are widely used as a substance having catalytic activity, and carbon materials such as carbon black are widely used as a porous carrier having conductivity.
  • PEFC is designed to form three types of conduction paths of gas, ions and electrons for each metal fine particle by coating this type of gas electrode catalyst with a thin film of polymer electrolyte. Yes.
  • PEFC In PEFC, there is a problem that the power generation performance gradually decreases because the carbon material as a support is corroded. In particular, since oxygen and moisture in the air promote the corrosion of the carbon material, the corrosion deterioration of the air electrode is one factor that determines the life performance of the PEFC.
  • Patent Document 1 In order to suppress the corrosion deterioration of the carbon material in the air electrode and improve the life performance of the PEFC, for example, in Patent Document 1, a metal oxide or metal nitride having conductivity that is less susceptible to corrosion by oxygen or moisture than the carbon material is disclosed. A method of using as a carrier is disclosed.
  • metal oxides and metal nitrides are not necessarily stable in the entire potential range in the battery usage environment, and there is a problem that they are easily corroded when the potential varies greatly.
  • Patent Document 2 discloses a method using a carbon material coated with a silicon-based polymer as a carrier.
  • the method according to the prior art described in Patent Document 2 does not improve the corrosion resistance depending on the pore distribution of the carbon material, or may result in a decrease in output performance. .
  • JP 2014-1112569 A Japanese Patent No. 3613330
  • the present invention provides a gas electrode catalyst that suppresses corrosion deterioration of a carbon material and realizes high catalytic activity in a battery using a gas such as PEFC as a reactant, and uses the same.
  • the purpose is to provide a battery having excellent life performance and output performance.
  • the present invention employs the following means in order to solve the above problems.
  • a gas electrode catalyst comprising a support having a form in which a part or all of the surface of conductive carbon is coated with an inorganic oxide and metal fine particles having catalytic activity attached to the surface of the support,
  • a catalyst for a gas electrode wherein a pore volume having a pore radius of 10 to 40 mm measured by a nitrogen adsorption method of the conductive carbon is 0.3 mL / g or less.
  • the pH measured at 25 ° C. is 3.0 or more and 6.5 or less after the carrier is dispersed in ion-exchanged water.
  • the catalyst for gas electrodes as described.
  • FIG. 1 is a schematic view of a gas electrode catalyst of the present invention.
  • FIG. 2 is a diagram illustrating a state in which a thin-film inorganic oxide covers the surface of conductive carbon.
  • FIG. 3 is a diagram for explaining a state in which the particulate inorganic oxide covers the surface of the conductive carbon.
  • FIG. 4 is a view for explaining a state in which oxygen or moisture penetrates into pores having a pore radius of not less than 10 and not more than 40.
  • FIG. 5 is a diagram for explaining a state in which a reaction gas cannot enter a closed pore having a radius of 10 to 40 mm.
  • FIG. 6 is a diagram for explaining a state in which the path of hydrogen ions is interrupted at a position where the polymer electrolyte is interrupted.
  • FIG. 7 is a diagram for explaining a mode of mediating a hydrogen ion pathway when an acidic functional group is present at a position where the polymer electrolyte is interrupted.
  • a gas electrode catalyst comprising a support having a form in which a part or all of the surface of conductive carbon is coated with an inorganic oxide, and fine metal particles having catalytic activity attached to the surface of the conductive carbon.
  • a catalyst for a gas electrode wherein a pore volume having a pore radius of 10 to 40 mm measured by a nitrogen adsorption method is 0.3 mL / g or less.
  • the pore volume measured by the nitrogen adsorption method in the present invention with a pore radius of 10 to 40 mm is measured by the measurement method defined in JIS Z 8831-2: 2010, and is 14.3. 2
  • BJH method mesopore size distribution determination method
  • the gas electrode catalyst in the present invention comprises a carrier having a form in which a part or all of the surface of conductive carbon is coated with an inorganic oxide, and metal fine particles having catalytic activity attached to the surface.
  • the inorganic oxide covers part or all of the surface of the conductive carbon, as shown in FIG. 2 and FIG.
  • the metal fine particles adhere to the surface of the carrier means that the metal fine particles come into contact with the carrier surface (which may be a region coated with an inorganic oxide or a region not coated) by chemical bonding or physical adsorption. Means that the electrons are held at positions where mutual movement is possible.
  • the inorganic oxide in the present invention is one or more selected from solid oxides such as silica, phosphorus oxide, titanium oxide, and alumina among oxides of various typical elements or transition elements.
  • silica is particularly preferable from the viewpoints of stability and acidity.
  • Inorganic oxides are less susceptible to corrosion by oxygen and moisture than conductive carbon, and this coats the surface of the carbon material, making it difficult for the conductive carbon to come into contact with oxygen and moisture and suppressing the corrosion deterioration of the conductive carbon. can do.
  • the conductive carbon in the present invention is selected from carbon black, carbon nanotubes, carbon nanofibers, graphite, graphene, carbon fibers, elemental carbon, glassy carbon and the like, as in the case of a general gas electrode catalyst carrier. is there.
  • carbon black is preferable from the viewpoints of electronic conductivity, specific surface area that greatly affects the amount of metal fine particles attached, porosity that greatly affects gas transport, and among them, acetylene black or furnace black is more preferable.
  • the pore volume having a pore radius of 10 to 40 mm measured by the nitrogen adsorption method is 0.3 mL / g or less, and more preferably 0.25 mL / g or less.
  • the inner surface of the pore may be in direct contact with oxygen or moisture. Therefore, the effect of suppressing the corrosion deterioration of the present invention is reduced.
  • the metal fine particles attached to the inner surface of the pore cannot contact the reactant gas, and thus cannot function as a catalyst.
  • the catalytic activity of the gas electrode catalyst as a whole is reduced.
  • the pore volume having a pore radius of 10 to 40 mm is large, and conversely, it is preferable that the pore volume is small because both the effect of suppressing corrosion deterioration and the catalytic activity are increased.
  • the metal fine particles having catalytic activity in the present invention are metal fine particles having a function of catalyzing a chemical reaction (electrode reaction) that oxidizes or reduces a reactant gas to generate a flow of electrons and ions, that is, an electric current.
  • a chemical reaction electrode reaction
  • an electrode reaction that oxidizes a fuel gas (typically hydrogen) to extract electrons and hydrogen ions, and an electrode reaction that consumes electrons and hydrogen ions to reduce oxygen gas are used.
  • Metal fine particles that catalyze seed electrode reactions are each required.
  • platinum fine particles, platinum fine particles, alloy fine particles of platinum and different metals iron, cobalt, nickel, ruthenium, rhodium, palladium, gold, etc.
  • platinum and foreign elements titanium are used for any electrode reaction.
  • the number average diameter is preferably 5 nm or less, and more preferably 3 nm or less.
  • the surface coverage of the conductive carbon by the inorganic oxide in the present invention is preferably 20 area% or more and 80 area% or less, and more preferably 40 area% or more and 70 area% or less.
  • the surface coverage is preferably 20 area% or more and 80 area% or less, and more preferably 40 area% or more and 70 area% or less.
  • the pH measured at 25 ° C. is preferably 3.0 or more and 6.5 or less, and more preferably 4.0 or more and 6.0 or less.
  • the electrode is manufactured by coating the surface of the gas electrode catalyst with a polymer electrolyte thin film in order to deliver hydrogen ions to the metal fine particles.
  • the polymer electrolyte rarely completely covers the surface of the gas electrode catalyst, and a portion in which the path of hydrogen ions is partially interrupted is generally generated.
  • the path of hydrogen ions can be mediated.
  • the amount of acidic functional groups necessary to mediate the hydrogen ion pathway can be obtained, and the entire catalyst for gas electrodes As a result, the catalytic activity increases.
  • the pH measured at 25 ° C. after dispersing the carrier in ion-exchanged water is preferably 3.0 or more.
  • the gas electrode catalyst When producing a battery using a gas as a reactant using the gas electrode catalyst of the present invention, the gas electrode catalyst is mixed with a binder and formed into a flat plate to form a gas electrode, which is an ion conductor.
  • the battery is brought into contact with one or two surfaces of the electrolyte. When contacting only one surface, another type of gas electrode or an electrode that is not a gas electrode is brought into contact with the opposite surface.
  • the electrolyte that is an ionic conductor is a solid polymer electrolyte
  • the ions that are conducted are typically hydrogen ions.
  • the solid polymer electrolyte may be any one that conducts hydrogen ions or other desired ions. From the viewpoint of oxidation-reduction stability and ionic conductivity, a sulfonic acid-modified polyfluorinated olefin (for example, Nafion®) Etc.) is particularly preferred.
  • a solid polymer electrolyte as a binder used when manufacturing a gas electrode, and to make the solid polymer electrolyte coat
  • Example 1 (Measurement of pore volume)
  • acetylene black manufactured by Denka Co., BET specific surface area of 740 m 2 / g
  • the pore volume of acetylene black having a pore radius of 10 to 40 mm was measured by the nitrogen adsorption method described below. After 0.03 g of the sample was vacuum degassed at 100 ° C. for 14 hours, a fully automatic gas adsorption / desorption measuring device OMISORP360CX (manufactured by Beckman Coulter) was used, and adsorption / desorption curves by a continuous capacity method using nitrogen as an adsorption gas. Got. Using this, the pore size distribution was calculated based on the BJH method, and the cumulative pore volume in the range of the pore radius of 10 to 40 cm was calculated to be 0.219 mL / g.
  • a carrier was produced in the following manner.
  • 1N ammonia water (manufactured by Kanto Chemical Co., Inc.) was added to adjust the pH to 11.
  • [PH] 0.2 g of the carrier was mixed with 100 mL of ion exchanged water, allowed to stand in a constant temperature room at 25 ° C. for 24 hours, and then measured for pH using a desktop pH meter F-71 (manufactured by Horiba, Ltd.). .9.
  • Catalytic activity The following operations were all carried out in a constant temperature room at 25 ° C. A half cell was prepared using the catalyst evaluation electrode as a working electrode, platinum as a counter electrode, a standard hydrogen electrode as a reference electrode, and a 0.1 M perchloric acid aqueous solution as an electrolyte. First, nitrogen bubbling was performed on the electrolyte solution for 30 minutes, and cyclic voltammetry was performed for 5 cycles under the conditions of 0.05 to 1.20 V and 50 mV / s for pretreatment in a state where the number of rotations of the working electrode was zero.
  • Manufacturing PEFC 50 ⁇ L of an ink prepared by mixing 18.5 mg of the gas electrode catalyst and 100 ⁇ L of 5% Nafion (registered trademark) dispersion in a mixed solution of 19 mL of ultrapure water and 6 mL of 2-propanol was dropped onto 1 cm ⁇ 1 cm carbon paper.
  • the electrode for evaluation was dried at 15 ° C. for 15 minutes.
  • As a counter electrode an electrode produced in the same manner as the evaluation electrode was used except that the gas electrode catalyst was changed to a commercially available catalyst (TEC10E50E, manufactured by Tanaka Kikinzoku Kogyo Co., Ltd.).
  • An electrolyte membrane (Nafion (registered trademark) NR211, manufactured by DuPont) is cut into 1 cm ⁇ 1 cm, and an evaluation electrode is provided on one side, a counter electrode is provided on the opposite side, and the surface on which the ink is dropped is attached to the electrolyte membrane side.
  • the membrane electrode assembly was obtained by hot pressing at 120 ° C. This was attached to a standard cell (manufactured by Japan Automobile Research Institute) to obtain PEFC.
  • the PEFC temperature is adjusted to 80 ° C., and as a pre-treatment, 100% relative humidity oxygen is introduced into the gas electrode catalyst side (cathode) and 100% relative humidity hydrogen is introduced into the gas electrode catalyst side (anode). And aging was performed for 30 minutes. Next, after blocking only oxygen on the cathode side and allowing to stand until the open circuit voltage was stabilized at around 0 V, oxygen was introduced and the open circuit potential was measured for 2 minutes. The potential was measured for 15 minutes at 0, 0.2, 0.1, 0.08, 0.06, 0.04, and 0.02 A / cm 2 , respectively.
  • the obtained potential value was plotted against the current, and a current value (unit: A / cm 2 ) at a potential of 0.9 V was obtained by extrapolation, and this value was used as output characteristics. In this example, it was 1.30 A / cm 2 .
  • Examples 2 to 5 A support was produced and evaluated in the same manner as in Example 1 except that the amount of hexadecyltrimethylammonium chloride added in Example 1 was changed to 180 mg, 450 mg, 900 mg, and 1800 mg. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 6 A carrier was produced and evaluated in the same manner as in Example 1 except that acetylene black in Example 1 was changed to acetylene black (Denka Co., BET specific surface area 750 m 2 / g). In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Examples 7 to 8> A carrier was produced and evaluated in the same manner as in Example 6 except that the amount of hexadecyltrimethylammonium chloride added in Example 6 was changed to 450 mg and 1800 mg. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 9 The same as Example 1 except that 80 g of tetraethoxysilane (manufactured by Tokyo Chemical Industry Co., Ltd.) was changed to 60 g of trimethyl phosphate (manufactured by Tokyo Chemical Industry Co., Ltd.) and the amount of hexadecyltrimethylammonium chloride added was changed to 900 mg.
  • the carrier was produced by the method described above and evaluated.
  • a gas electrode catalyst, PEFC was prepared and evaluated. The results are shown in Table 1.
  • Example 10 A carrier was produced in the same manner as in Example 1 except that 80 g of tetraethoxysilane of Example 1 was changed to 80 g of tetraethoxytitanium (manufactured by Tokyo Chemical Industry Co., Ltd.) and the addition amount of hexadecyltrimethylammonium chloride was changed to 900 mg. And evaluated. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 11 The carrier was prepared in the same manner as in Example 1 except that 80 g of tetraethoxysilane of Example 1 was changed to 110 g of aluminum triisopropoxide (manufactured by Tokyo Chemical Industry Co., Ltd.) and the addition amount of hexadecyltrimethylammonium chloride was changed to 900 mg. Manufactured and evaluated. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 1 A support was produced and evaluated in the same manner as in Example 1 except that 80 g of tetraethoxysilane in Example 1 was changed to 80 g of ethanol. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 2 A support was produced in the same manner as in Example 1 except that the acetylene black of Example 1 was changed to Ketjen Black EC600JD (manufactured by Lion Corporation, specific surface area 1190 m 2 / g), and 80 g of tetraethoxysilane was changed to 80 g of ethanol. And evaluated. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • Example 3 A carrier was produced and evaluated in the same manner as in Example 1 except that the acetylene black in Example 1 was changed to Ketjen Black EC600JD. In addition, a gas electrode catalyst, PEFC, was prepared and evaluated. The results are shown in Table 1.
  • the gas electrode catalyst of the present invention in a battery using gas as a reactant, it is possible to achieve both suppression of corrosion deterioration of the carbon material and excellent catalytic activity. Thereby, a battery using a gas excellent in output characteristics and life performance as a reactant can be obtained.

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

Abstract

La présente invention concerne un catalyseur pour électrodes à gaz, qui est susceptible de prolonger la durée de vie d'une batterie qui utilise un gaz comme réactif en supprimant la détérioration par corrosion d'un matériau carboné, et qui permet d'obtenir d'excellentes caractéristiques de sortie. Un catalyseur pour électrodes à gaz selon l'invention est constitué de : un support qui est obtenu en couvrant une partie ou la totalité de la surface d'un carbone conducteur avec un oxyde inorganique ; et des particules métalliques fines qui adhèrent à la surface du support et qui ont une activité catalytique. Ce catalyseur pour électrodes à gaz est caractérisé en ce que le volume des pores ayant un rayon de pore de 10 Å à 40 Å (inclus) du carbone conducteur déterminé par un procédé d'adsorption d'azote est inférieur ou égal à 0,3 ml/g.
PCT/JP2016/074858 2015-11-10 2016-08-25 Catalyseur pour électrodes à gaz et batterie WO2017081910A1 (fr)

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JP2015-220559 2015-11-10
JP2015220559A JP2019008864A (ja) 2015-11-10 2015-11-10 ガス電極用触媒および電池

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62132548A (ja) * 1985-12-04 1987-06-15 Hitachi Ltd 触媒の調製方法
JPH05174838A (ja) * 1991-12-26 1993-07-13 Matsushita Electric Ind Co Ltd 触媒担持構造とそれを用いた燃料電池用電極及び燃料電池
JP2000100448A (ja) * 1998-09-24 2000-04-07 Tanaka Kikinzoku Kogyo Kk 高分子固体電解質型燃料電池用触媒
JP2000273351A (ja) * 1999-03-23 2000-10-03 Osaka Gas Co Ltd 黒鉛化カーボンブラックの製造方法
JP2007250274A (ja) * 2006-03-14 2007-09-27 Cataler Corp 貴金属利用効率を向上させた燃料電池用電極触媒、その製造方法、及びこれを備えた固体高分子型燃料電池
JP2009259492A (ja) * 2008-04-14 2009-11-05 Ricoh Co Ltd 直接アルコール型燃料電池用触媒、直接アルコール型燃料電池および電子機器
JP2010186678A (ja) * 2009-02-13 2010-08-26 Equos Research Co Ltd 燃料電池用触媒層
JP2011222132A (ja) * 2010-04-02 2011-11-04 Hitachi Ltd 電極触媒材料およびその製造方法
JP2013109856A (ja) * 2011-11-17 2013-06-06 Nissan Motor Co Ltd 燃料電池用電極触媒層
JP2014007158A (ja) * 2012-06-26 2014-01-16 Samsung Sdi Co Ltd 燃料電池用担体、これを含む燃料電池用電極、燃料電池用膜−電極接合体および燃料電池システム

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62132548A (ja) * 1985-12-04 1987-06-15 Hitachi Ltd 触媒の調製方法
JPH05174838A (ja) * 1991-12-26 1993-07-13 Matsushita Electric Ind Co Ltd 触媒担持構造とそれを用いた燃料電池用電極及び燃料電池
JP2000100448A (ja) * 1998-09-24 2000-04-07 Tanaka Kikinzoku Kogyo Kk 高分子固体電解質型燃料電池用触媒
JP2000273351A (ja) * 1999-03-23 2000-10-03 Osaka Gas Co Ltd 黒鉛化カーボンブラックの製造方法
JP2007250274A (ja) * 2006-03-14 2007-09-27 Cataler Corp 貴金属利用効率を向上させた燃料電池用電極触媒、その製造方法、及びこれを備えた固体高分子型燃料電池
JP2009259492A (ja) * 2008-04-14 2009-11-05 Ricoh Co Ltd 直接アルコール型燃料電池用触媒、直接アルコール型燃料電池および電子機器
JP2010186678A (ja) * 2009-02-13 2010-08-26 Equos Research Co Ltd 燃料電池用触媒層
JP2011222132A (ja) * 2010-04-02 2011-11-04 Hitachi Ltd 電極触媒材料およびその製造方法
JP2013109856A (ja) * 2011-11-17 2013-06-06 Nissan Motor Co Ltd 燃料電池用電極触媒層
JP2014007158A (ja) * 2012-06-26 2014-01-16 Samsung Sdi Co Ltd 燃料電池用担体、これを含む燃料電池用電極、燃料電池用膜−電極接合体および燃料電池システム

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