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Oxygen Permeable Membrane Europaisches Patentamt 0154 468 J European Patent Office Publication number: B1 Office europeen des brevets EUROPEAN PATENT SPECIFICATION M 12/06 Date of publication of patent specification: 04.10.89 intci.4: H 01 M 4/86, H 01 Application number: 85301213.6 Date of filing: 22.02.85 Oxygen permeable membrane. Priority: 24.02.84 JP 33589/84 Proprietor: KABUSHIKI KAISHA TOSHIBA 24.02.84 JP 33593/84 72, Horikawa-cho Saiwai-ku Kawasaki-shi Kanagawa-ken 210 (JP) Date of publication of application: 11.09.85 Bulletin 85/37 Inventor: Susuki, Nobukazu c/o Patent Division Kabushiki Kaisha Toshiba 1-1 Shibaura 1-chome Minato-ku Tokyo (JP) Publication of the grant of the patent: Inventor: Tsuruta, Shinji c/o Patent Division 04.10.89 Bulletin 89/40 Kabushiki Kaisha Toshiba 1-1 Shibaura 1-chome Minato-ku Tokyo (JP) Designated Contracting States: DEFRGB Representative: Eyles, Christopher Thomas et al BATCHELLOR, KIRK & EYLES 2 Pear Tree Court Farringdon Road References cited: London, EC1R0DS(GB) EP-A-0097 770 US-A-3972 732 US-A-4018943 CD GO <O in Note: Within nine months from the publication of the mention of the grant of the European patent, any person may shall give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition been filed until the opposition fee has been 0. be filed in a written reasoned statement. It shall not be deemed to have ) convention). UJ paid. (Art. 99(1 European patent Courier Press, Leamington Spa, England. EP 0 154 468 B1 Description This invention relates to an oxygen permeable membrane which permits oxygen gas to pass through while substantially blocking other gases. The present invention has application in hydrogen-oxygen 5 electric fuel cells, metal-air battery cells and oxygen sensing devices. In the prior art, gas diffusion electrodes have been used for air electrodes in various fuel cells, air-metal cells, such as air-zinc cells, and Galvanic oxygen sensors. Thick porous electrodes having distributed pores with a uniform diameter were used as the gas diffusion electrode. In recent years, however, electrodes having a two-layer structure have been used. The electrode comprised a porous electrode body with an 10 electrochemical reduction function for oxygen gas (a function for ionising oxygen) and a current collector function. The electrode also had a thin water repellent layer deposited integrally on the gas-side surface of the electrode body. In such electrodes, the electrode body may be formed by a conductive powder, a porous metallic body, a porous carbon body or a non-woven carbon fabric material. This may be accomplished by the use of a 15 binder such as polytetrafluoroethylene. Such conductive powders may be selected from among active carbon powders carrying a nickel tungstate with a low reduction overvoltage to oxygen gas, a tungsten carbide coated with palladium, cobalt, nickel, silver, platinum or palladium. US — A — 3972732 describes a catalytic electrode which comprises a metallic oxide and a carbonaceous material. 20 The aforementioned water repellent layer, which is deposited integrally on the gas-side surface of the electrode body, is a porous thin membrane which comprises a fluorine-containing resin such as polytetrafluoroethylene, tetrafluoroethylene-hexafluoropropylene copolymer or ethylene-tetrafluoro- ethylene copolymer. The membrane may also be comprised of a resin, such as polypropylene, in the form of a porous material including, for example, a sintered powder material having a particle size of from 0.2 to 25 40 urn; a paper-like non-woven fabric material prepared by heat treatment of fibres comprising polypropylene resin or a similar woven fabric material; a powder material wherein the polypropylene resin is partially replaced by a fluorinated graphite; a film material prepared by rolling fine powder together with a pore-increasing agent or a lubricant oil followed by heat treatment or a film material prepared by rolling without being followed by heat treatment. Such materials are disclosed in Japanese Patent Publication No. 30 44978/1973. In an air electrode having the structure as described above, however, the water repellent layer deposited on the gas-side surface of the electrode body is impervious to electrolyte but is not impervious to air and water vapour in the air. For this reaosn, water vapour in the air may penetrate the electrode body through the water repellent layer and dilute the electrolyte or the water in the electrode may otherwise 35 dissipate through the water repellent layer, therby increasing electrolyte concentration. As a result, the concentration of the electrolyte will fluctuate and it will thus be impossible to maintain stable discharge characteristics over a long period of time. When carbon dioxide gas in the air penetrates the electrode body through the water repellent layer and is absorbed by an active site (a porous portion of the electrode body), the electrochemical reducing 40 function of the active site to oxygen gas is reduced at the point of absorption. Thus, the heavy-load discharge capability of the cell is adversely affected. Moreover, when an alkaline electrolyte is used, there will be a change in the properties of the electrolyte, a reduction in the concentration of the electrolyte and, if the cathode is zinc, passivation of the zinc cathode. Furthermore, heavy-load discharge may be hindered because the area of electrochemical reduction is reduced by the production of carbonate in the active site 45 which blocks the pores. These factors lead to a decline in the performance of the cell from its design rating after the cell is stored or used for a long period of time. In order to overcome the aforementioned disadvantages, there has been proposed a cell in which a water repellent layer for the air electrode is provided on the gas side (air side) thereof with a layer comprising a water-absorbing agent, such as calcium chloride, or a carbon dioxide gas-absorbing gent, so such as a hydroxide of an alkaline earth metal. Such a cell is disclosed in Japanese Patent Publication No. 841 1/1 973. This type of cell can prevent the above-mentioned problems to some extent. However, when the absorbing agent has been saturated with water or carbon dioxide gas, it becomes wholly ineffective. There have also been attempts to laminate an oxygen permeable membrane on the above-mentioned water repellent layer. Such a membrane is disclosed in Japanese Patent Publication No. 26896/1973. 55 However, a sufficiently effective oxygen gas permeable membrane has not been developed thus far. The present invention accordingly seeks to provide a selectively permeable composite membrane, and an air electrode being made therefrom, which is permeable to oxygen gas while at the same time being impervious to water vapour in air. It also seeks to provide an air electrode comprising an oxygen gas permeable membrane which eo enables a heavy-load discharge to be maintained over a long period of time. According to a first aspect of this invention, there is provided a composite membrane for passing oxygen gas, said membrane comprising a metallic oxide and and a carbonaceous material characterised in that the membrane comprises: a porous membrane having micropores the diameter of which is equal to or less than 1 um; and 65 a thin layer affixed to at least one surface of said porous membrane and having a thickness in the range EP 0154 468 B1 said metallic oxide being of 0.01 to 1 |im, said thin layer containing a metallic oxide in a carbon matrix, barium oxide, selected from among the group consisting of tin dioxide, zinc oxide, strontium oxide, titanium dioxide, silicon dioxide, cuprous oxide, manganese monoxide, nickel oxide, tricobalt tetroxide, vanadium dioxide, molybdenum dioxide, tungsten dioxide, ruthenium dioxide, niobium dioxide, dioxide and platinum 5 chromium dioxide, rhenium dioxide, osmium dioxide, rhodium dioxide, iridium dioxide.. The invention thus provides a selectively permeable composite membrane having a two-layer construction. The membrane comprises a porous membrane layer having micropores and a thin layer the containing, in a carbon matrix, a water-containable or wettable metallic oxide, a metal oxide having The thin is 10 capability of absorbing oxygen or a metal oxide having a rutile-type crystal structure. layer laminated integrally on to one or both surfaces of the porous membrane layer. According to the second aspect of this invention, there is provided an air electrode for a cell comprising a metallic oxide and a carbonaceous material characterised in that it comprises: with a main electrode body having the capability of electro-chemical reduction of oxygen gas a is laminated 15 collector function; and the composite membrane according to the invention. The thin layer membrane integrally on the gas side surface of the main body of the electrode with a porous layer between. The metallic oxide which is contained in the carbon matrix is a water-containable or wettable metallic oxide or has the ability of absorbing oxygen or has a rutile-type crystal structure. The water- containable or wettable metallic oxide used in this invention is a material having the ability to absorb water absorbed 20 and having properties for permitting water absorbed to exist as chemically and physically water. The water-containable (wettable) properties means that a metallic oxide exists in combination with water molecules or in a state having an interaction with water molecules. Examples of the above mentioned metallic oxides include tin dioxide (SnO2), zinc oxide (ZnO), aluminium oxide (AI2O3), magnesium oxide silicon (MgO), calcium oxide (CaO), strontium oxide (SrO), barium oxide (BaO), titanium dioxide (TiO2) and of 25 dioxide (SiO2). These oxides may be used alone or in the form of a composite comprising a combination two or more types thereof.
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