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WO2009034845A1 - Procédé de production d'un séparateur pour pile à combustible - Google Patents

Procédé de production d'un séparateur pour pile à combustible Download PDF

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Publication number
WO2009034845A1
WO2009034845A1 PCT/JP2008/065345 JP2008065345W WO2009034845A1 WO 2009034845 A1 WO2009034845 A1 WO 2009034845A1 JP 2008065345 W JP2008065345 W JP 2008065345W WO 2009034845 A1 WO2009034845 A1 WO 2009034845A1
Authority
WO
WIPO (PCT)
Prior art keywords
titanium
separator
fuel cell
specimen
producing
Prior art date
Application number
PCT/JP2008/065345
Other languages
English (en)
Japanese (ja)
Inventor
Kuroudo Maeda
Masahiro Mizuno
Original Assignee
Toyota Jidosha Kabushiki Kaisha
Aisin Takaoka Co., Ltd.
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
Priority claimed from JP2007262199A external-priority patent/JP2009087909A/ja
Application filed by Toyota Jidosha Kabushiki Kaisha, Aisin Takaoka Co., Ltd. filed Critical Toyota Jidosha Kabushiki Kaisha
Publication of WO2009034845A1 publication Critical patent/WO2009034845A1/fr

Links

Classifications

    • 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
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • 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
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • 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 for manufacturing a fuel cell separator, and more particularly, to a method for manufacturing a fuel cell separator that separates gas between adjacent fuel cell cells.
  • Fuel cells have been in the limelight as batteries with high efficiency and excellent environmental characteristics. Fuel cells generally produce electric energy by electrochemically reacting hydrogen, the fuel gas, with oxygen in the air, the oxidant gas. As a result of the electrochemical reaction between hydrogen and oxygen, water is generated.
  • Types of fuel cells include phosphoric acid type, molten carbonate type, solid electrolyte type, alkaline type, and solid polymer type.
  • solid polymer fuel cells that have advantages such as startup at normal temperature and quick startup time are drawing attention.
  • Such a polymer electrolyte fuel cell is used as a power source for a mobile object such as a vehicle.
  • a polymer electrolyte fuel cell is assembled by stacking a plurality of single cells, current collector plates, end plates, and the like.
  • the fuel cell includes an electrolyte membrane, a catalyst layer, a gas diffusion layer, and a separator.
  • Patent Document 1 the use of a fuel cell separator that is surface-treated with a metal made of gold or chromium on a separator base made of stainless steel or titanium prevents corrosion against the corrosive atmosphere of the battery environment. It is described that the performance is improved.
  • Patent Document 2 describes a high corrosion resistance stainless steel used as a separator for a polymer electrolyte fuel cell and a surface treatment method for reducing contact resistance against carbon to titanium, in which a passive metal is polished with a noble metal attached thereto. It describes that a noble metal is adhered to a passive metal immediately after removing the surface oxide film by polishing with a material.
  • Patent Document 3 describes a surface treatment method for a passive metal to carbon with a low contact resistance.
  • An appropriate amount of high-hardness particles partially or entirely coated with a precious metal or its alloy are mixed between the surface to be treated of the passive metal and the precious metal or its alloy facing it, and the surface is hardened by ultrasonic waves. It describes that particles are vibrated and flowed, and a noble metal or an alloy thereof is adhered to a part or all of the surface while removing a surface oxide film of a passive metal by collision of a hard particle with a surface to be treated.
  • Patent Document 1 Japanese Patent Laid-Open No. 2005-158441
  • Patent Document 2 Japanese Patent Laid-Open No. 2002-134128
  • Patent Document 3 Japanese Patent Laid-Open No. 2002-134136 Disclosure of Invention
  • an object of the present invention is to provide a method for manufacturing a fuel cell separator capable of suppressing a decrease in conductivity.
  • a method for manufacturing a fuel cell separator according to the present invention is a method for manufacturing a fuel cell separator that separates gas between adjacent fuel cell cells, wherein a titanium substrate is formed by plastically adding a titanium material.
  • the titanium substrate forming step is characterized by rolling and forming a titanium material.
  • the method for manufacturing a fuel cell separator according to the present invention is characterized by having a conductive layer forming step of forming a conductive layer on the surface of the titanium substrate after the removing step.
  • the invention's effect As described above, according to the method for manufacturing a fuel cell separator according to the present invention, since the generation of oxides formed in the fuel cell separator is reduced, the conductivity of the fuel cell separator overnight is reduced. Can be suppressed.
  • FIG. 1 is a diagram showing a cross section of a fuel cell in an embodiment of the present invention.
  • FIG. 2 is a flow chart showing a method for manufacturing a separator overnight in an embodiment of the present invention.
  • FIG. 3 is a schematic diagram showing a method of rolling a titanium material in the embodiment of the present invention.
  • FIG. 4 is a view showing a cross section of the titanium substrate after rolling in the embodiment of the present invention.
  • FIG. 5 is a diagram showing a cross section of the separator evening in the embodiment of the present invention.
  • FIG. 6 is a diagram showing a test apparatus used in the electrochemical high temperature corrosion test in the embodiment of the present invention.
  • FIG. 7 is a diagram showing a corrosion test result in a separate evening specimen in the embodiment of the present invention.
  • FIG. 8 is a diagram showing a method for measuring contact resistance in the embodiment of the present invention.
  • FIG. 9 is a graph showing the measurement results of contact resistance in a separate evening specimen in the embodiment of the present invention. Explanation of symbols
  • FIG. 1 is a cross-sectional view of a fuel cell 10.
  • a fuel cell 10 includes a membrane electrode assembly 18 (Membran e lectrode A sse mb 1) that integrates an electrolyte membrane 12, a catalyst layer 14, and a gas diffusion layer 16 to form a fuel cell electrode.
  • ME A membrane electrode assembly 18
  • an expanded molded body 20 that is a gas flow path structure that forms a gas flow path, and a separator gas that separates fuel gas or oxidant gas between adjacent cells (not shown). And including.
  • the electrolyte membrane 12 has a function of moving hydrogen ions generated on the anode electrode side to the force sword electrode side.
  • a chemically stable fluorine-based resin for example, an ion exchange membrane of perfluorocarpone sulfonic acid is used.
  • the catalyst layer 14 has a function of promoting a hydrogen oxidation reaction on the anode electrode side and an oxygen reduction reaction on the force sword electrode side.
  • the catalyst layer 14 includes a catalyst and a catalyst carrier. In order to increase the electrode area to be reacted, the catalyst is generally used in the form of particles and attached to the catalyst carrier.
  • platinum which is a platinum group element having a smaller activation overvoltage, is used for the oxidation reaction of hydrogen and the reduction reaction of oxygen.
  • a carbon material such as a car pump rack is used as the catalyst carrier.
  • the gas diffusion layer 16 has a function of diffusing hydrogen gas, which is a fuel gas, and air, which is an oxidant gas, into the catalyst layer 14 and a function of moving electrons.
  • the gas diffusion layer 16 is made of carbon fiber woven fabric, force-on-paper, or the like, which is a conductive material.
  • the expanded molded body 20 is laminated on both surfaces of the membrane electrode assembly 18 and has a function as a gas channel structure that forms a gas channel.
  • the expanded molded body 20 is laminated in contact with the gas diffusion layer 16 of the membrane electrode assembly 18 and the separator 22, and is electrically connected to the membrane electrode assembly 18 and the separator 22. Since the expanded molded body 20 has a mesh structure composed of a large number of openings, more fuel gas or the like comes into contact with the membrane electrode assembly 18 to cause a chemical reaction, thereby generating power from the fuel cell 10. Efficiency can be increased.
  • the expanded molded body 20 for example, an expanded metal shown in JISG 3351, a metal lath or a metal porous body shown in JISA 5505, or the like is used.
  • the expanded molded body 20 is preferably molded from titanium, titanium alloy stainless steel or the like. These metal materials, mechanical strength high degree of stable oxide on the surface (T I_ ⁇ , T i 2 ⁇ 3, T I_ ⁇ 2, C R_ ⁇ 2, C R_ ⁇ , C r 2 ⁇ 3 This is because an inert film such as a passive film is formed and thus has excellent corrosion resistance.
  • the stainless steel an austenitic stainless steel, a ferritic stainless steel, or the like can be used.
  • the separate evening 22 is laminated on the expanded molded body 20 and has a function of separating the fuel gas and the oxidant gas in the adjacent cell (not shown).
  • the separator overnight 22 has a function of electrically connecting adjacent cells (not shown).
  • Separate Night 22 is made of pure titanium or a titanium alloy.
  • the titanium material has high mechanical strength and has an excellent corrosion resistance because an inert film such as a passive film made of a stable oxide is formed on the surface thereof.
  • the separate evening 22 includes a titanium substrate 24 formed of a titanium material and a conductive layer 26 formed on the titanium substrate 24.
  • the conductive layer 26 is set to a thickness of 311111 to 2001 m, and has a function of reducing contact resistance between the expanded molded body 20 and the titanium substrate 24.
  • the conductive layer 26 is made of a metal material such as gold (Au), silver (Ag), copper (Cu), platinum (Pt), rhodium (Rh), iridium (Ir), palladium (Pd), etc. It is formed by. Because these metal materials have high electrical conductivity, the contact resistance can be further reduced.
  • the conductive layer 26 may be formed of an alloy such as gold (Au) or platinum (Pt).
  • FIG. 2 is a flowchart showing a method for manufacturing the separate evening 22.
  • the manufacturing method of Separat 22 includes a titanium substrate forming step (S 10), a cleaning step (S 12), a neutralization step (S 14), a removal step (S 16), and a conductive layer forming step (S 18 ) When, It is comprised including.
  • the titanium substrate forming step (S 10) is a step of forming a titanium substrate 24 by plastic working a titanium material.
  • the titanium substrate 24 is formed by, for example, roll rolling a titanium material.
  • Fig. 3 is a schematic diagram showing a method of rolling a titanium material.
  • pure titanium or a titanium alloy is used for the titanium material 30.
  • the titanium material is hot-rolled at a temperature of 700 to 900 ° C.
  • a rolling apparatus generally used for rolling titanium material can be used.
  • a lubricant containing fats and oils and carbons is used to prevent seizure and the like.
  • the plastic working of the titanium material 30 is not limited to rolling, but may be press working or the like.
  • FIG. 4 is a view showing a cross section of the titanium substrate 24 after rolling.
  • T I_ ⁇ the titanium material 3 0 is a base material was produced by oxidation, T i 2 ⁇ 3, T I_ ⁇ 2 titanium oxides such as 3 2 are formed.
  • T i C, T i C 2 , T i produced by chemical reaction with carbon produced by carbonization of oils and fats contained in the lubricant during the rolling process.
  • Titanium carbide 3 4 such as C 3 is formed.
  • titanium oxide 3 6 such as T i O, T i 2 0 3 , T i 0 2, etc. formed by oxidizing the titanium carbide 3 4 is also formed.
  • the cleaning step (S 1 2) is a step of cleaning the titanium substrate 24 formed by rolling the titanium material 30.
  • the titanium substrate 24 is cleaned by, for example, alkaline immersion degreasing.
  • alkaline immersion degreasing an alkaline solution such as caustic soda is used.
  • alkali dipping degreasing or the like oil or the like adhering to the surface of the titanium substrate 24 is removed.
  • the neutralization step (S 14) is a step of neutralizing and removing the alkali remaining on the cleaned titanium substrate 24.
  • the neutralization treatment is performed by immersing the cleaned titanium substrate 24 in a neutralizing solution.
  • a neutralizing solution sulfuric acid solution, hydrochloric acid solution, nitric acid solution, etc. are used.
  • the titanium substrate 24 taken out from the neutralized solution is washed with deionized water or the like.
  • the removal step (S 1 6) the titanium substrate 24 that has been subjected to the neutralization treatment is pickled to remove the titanium oxides 3 2 and 3 6 and the titanium carbide 3 4 from the surface of the titanium substrate 24. It is a process.
  • the productivity of the fuel cell separator can be improved as compared with the step for removal by polishing or the like.
  • the pickling treatment is performed by immersing the titanium substrate 24 in a solution containing fluoride such as a nitric hydrofluoric acid solution or a hydrofluoric acid solution.
  • a solution containing fluoride such as a nitric hydrofluoric acid solution or a hydrofluoric acid solution.
  • the titanium oxide 36, titanium carbide 34, and titanium oxide 32 on the surface of the titanium substrate 24 are etched. Thereby, the titanium oxides 3 2 and 3 6 and the titanium carbide 3 4 formed on the titanium substrate 24 are removed.
  • a solution containing a fluoride such as a nitric hydrofluoric acid solution is not used for the pickling solution unless it contains a fluoride.
  • a fluoride such as a nitric hydrofluoric acid solution
  • titanium oxide 3 2, 3 6 And titanium carbide 3 4 cannot be removed.
  • the titanium substrate 24 taken out from the nitric hydrofluoric acid solution or the like is washed with deionized water or the like.
  • the conductive layer forming step (S 1 8) is a step of forming the conductive layer 26 on the titanium substrate 24 that has been pickled.
  • the conductive layer 26 is set to a thickness of 3 nm to 200 nm, and is formed by coating a conductor such as gold (A u).
  • a conductor such as gold (A u) or the like
  • an electrolytic plating method can be used.
  • a general alkaline plating method such as gold (A u) is used. This completes the production of Separe Ichiba 22
  • the separator layer may be manufactured by omitting the conductive layer forming step (S 1 8).
  • FIG. 5 is a view showing a cross section of the manufactured separator 22.
  • the separator 22 has a titanium substrate 24 and a conductive layer 26.
  • the titanium oxides 3 2 and 3 6 and the titanium carbide 3 4 are removed in the removal step (S 16). Therefore, generation of titanium oxide due to oxidation of titanium carbide 34 can be prevented during fuel cell power generation.
  • the separate evening may be configured by omitting the conductive layer 26 from the separate evening 22 shown in FIG.
  • Example 1 A method for manufacturing the separate overnight specimen in Example 1 will be described. Pure titanium was used for the titanium material. A pure titanium material was roll-rolled to form a titanium sheet. The titanium sheet was degreased by alkali soaking and washed to remove oil adhering to the titanium sheet. The titanium sheet washed with alkali degreasing was neutralized by dipping in a sulfuric acid solution. Next, the titanium sheet was immersed in a nitric hydrofluoric acid solution and pickled, and titanium oxide and titanium carbide formed on the surface of the titanium sheet were etched and removed. In addition, the manufacturing method of the separator evening specimen in the comparative example 1 which uses what does not form a conductive layer for the separator evening specimen used for the evaluation test is explained.
  • the corrosion test was conducted in accordance with the electrochemical high temperature corrosion test method for metallic materials specified in JISZ 2 2 9 4.
  • Figure 6 shows the test equipment used in the electrochemical hot corrosion test.
  • the test was conducted in an open air system.
  • the solution used for the test was a sulfuric acid solution.
  • the temperature of the test solution was 50 ° C.
  • a corrosion test was performed by applying a constant potential for 50 hours. The corrosion resistance was evaluated by observing the appearance of the separate overnight specimen after the corrosion test.
  • Fig. 7 is a diagram showing the results of a corrosion test on a separate evening specimen.
  • the separate evening specimen of Example 1 was less discolored than the separate evening specimen of Comparative Example 1.
  • the separation overnight specimen of Comparative Example 1 has a lot of discoloration because the titanium oxide and titanium carbide remained on the surface of the separation evening specimen of Comparative Example 1, so that the titanium carbide was oxidized during the corrosion test. This is because the titanium oxide is formed thick.
  • FIG. 8 is a diagram showing a method for measuring contact resistance. After attaching the gas diffusion layer material 4 2 to the metal jig 40, sandwich the separator sample of Example 1 or Comparative Example 1 as the test piece 4 4 between the two gas diffusion layer materials 4 2, A predetermined surface pressure was applied to bring it into close contact. Then, the contact resistance was determined by measuring the voltage between the test piece 44 and the gas diffusion layer material 42 when a current of 1 A was passed.
  • Fig. 9 is a graph showing the measurement results of contact resistance of the separate overnight specimen.
  • the horizontal axis indicates the type of the specimen to be separated
  • the vertical axis indicates the relative value of contact resistance (m ⁇ ⁇ cm 2 )
  • the contact resistance before the corrosion test is indicated by a white square.
  • Corrosion test The contact resistance after 50 hours is indicated by a black square.
  • the contact resistance before the corrosion test and the corrosion resistance after the corrosion test were substantially the same level.
  • the contact resistance after the corrosion test in the separate evening specimen of Comparative Example 1 increased significantly compared to the contact resistance before the corrosion test.
  • Example 1 a separate layer specimen was manufactured by forming a conductive layer (gold or palladium having a thickness of 10 nm) on the separator specimen of Example 1, and the same as in Example 1 and Comparative Example 1. As a result, a corrosion test was performed on a separate specimen and contact resistance was obtained. Although not shown here, the present inventors have confirmed that the corrosion test results and the contact resistance measurement results were better than those in Example 1.

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

Abstract

Cette invention concerne un procédé de production d'un séparateur pour une pile à combustible qui peut séparer un gaz présent entre des piles adjacentes pour une pile à combustible. Dans la production d'un séparateur pour une pile à combustible à l'aide d'un matériau métallique tel que le titane, un conducteur ayant un haut niveau de conductivité électrique est généralement formé sur la surface du séparateur pour réduire une résistance de contact entre le séparateur et une couche de diffusion de gaz et similaires. Toutefois, il existe une possibilité que, durant la génération d'électricité dans une pile à combustible, un oxyde soit formé sur la surface du séparateur, entraînant un abaissement de la conductivité électrique du séparateur. Le problème ci-dessus peut être résolu par un procédé de production d'un séparateur pour une pile à combustible, comprenant une étape de formation de base de titane consistant à travailler plastiquement un matériau de titane pour former une base de titane et une étape d'élimination consistant à décaper la base de titane pour éliminer l'oxyde de titane et le carbure du titane de la surface de la base de titane.
PCT/JP2008/065345 2007-09-14 2008-08-20 Procédé de production d'un séparateur pour pile à combustible WO2009034845A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2007238980 2007-09-14
JP2007-238980 2007-09-14
JP2007-262199 2007-10-05
JP2007262199A JP2009087909A (ja) 2007-09-14 2007-10-05 燃料電池用セパレータの製造方法

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WO2009034845A1 true WO2009034845A1 (fr) 2009-03-19

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015182731A1 (fr) * 2014-05-28 2015-12-03 株式会社神戸製鋼所 Matériau séparateur de pile à combustible et procédé de fabrication dudit matériau
WO2020054072A1 (fr) * 2018-09-14 2020-03-19 日本製鉄株式会社 Feuille de titane et son procédé de production
KR20220029422A (ko) * 2020-08-28 2022-03-08 토와 가부시기가이샤 수지 성형 장치 및 수지 성형품의 제조 방법

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JP2002012962A (ja) * 2000-02-23 2002-01-15 Nippon Steel Corp 大気環境中において変色を生じにくいチタンおよびその製造方法
WO2005019498A2 (fr) * 2003-08-11 2005-03-03 General Motors Corporation Composition et procede pour traitement de surface d'un metal oxyde
JP2006127922A (ja) * 2004-10-29 2006-05-18 Dainippon Printing Co Ltd 燃料電池用金属部材及びその製造方法
JP2007073232A (ja) * 2005-09-05 2007-03-22 Japan Carlit Co Ltd:The 燃料電池用セパレータおよびその製造方法
JP2007146250A (ja) * 2005-11-29 2007-06-14 Nikko Kinzoku Kk 貴金属めっきを施したチタン又はチタン合金材料
JP5068537B2 (ja) * 2005-01-14 2012-11-07 三菱電機株式会社 レプリカ結合グループシャッフル反復デコーダ及びこの生成方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002012962A (ja) * 2000-02-23 2002-01-15 Nippon Steel Corp 大気環境中において変色を生じにくいチタンおよびその製造方法
WO2005019498A2 (fr) * 2003-08-11 2005-03-03 General Motors Corporation Composition et procede pour traitement de surface d'un metal oxyde
JP2006127922A (ja) * 2004-10-29 2006-05-18 Dainippon Printing Co Ltd 燃料電池用金属部材及びその製造方法
JP5068537B2 (ja) * 2005-01-14 2012-11-07 三菱電機株式会社 レプリカ結合グループシャッフル反復デコーダ及びこの生成方法
JP2007073232A (ja) * 2005-09-05 2007-03-22 Japan Carlit Co Ltd:The 燃料電池用セパレータおよびその製造方法
JP2007146250A (ja) * 2005-11-29 2007-06-14 Nikko Kinzoku Kk 貴金属めっきを施したチタン又はチタン合金材料

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015182731A1 (fr) * 2014-05-28 2015-12-03 株式会社神戸製鋼所 Matériau séparateur de pile à combustible et procédé de fabrication dudit matériau
US10236519B2 (en) 2014-05-28 2019-03-19 Kobe Steel, Ltd. Fuel cell separator material and method for manufacturing said material
WO2020054072A1 (fr) * 2018-09-14 2020-03-19 日本製鉄株式会社 Feuille de titane et son procédé de production
KR20220029422A (ko) * 2020-08-28 2022-03-08 토와 가부시기가이샤 수지 성형 장치 및 수지 성형품의 제조 방법
KR102511018B1 (ko) * 2020-08-28 2023-03-15 토와 가부시기가이샤 수지 성형 장치 및 수지 성형품의 제조 방법
US11999083B2 (en) 2020-08-28 2024-06-04 Towa Corporation Resin molding apparatus and method for producing resin molded product

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