JP2005044815A - Manufacturing method of solid polymer electrolyte fuel cell - Google Patents

Manufacturing method of solid polymer electrolyte fuel cell Download PDF

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JP2005044815A
JP2005044815A JP2004292617A JP2004292617A JP2005044815A JP 2005044815 A JP2005044815 A JP 2005044815A JP 2004292617 A JP2004292617 A JP 2004292617A JP 2004292617 A JP2004292617 A JP 2004292617A JP 2005044815 A JP2005044815 A JP 2005044815A
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fuel cell
sulfonic acid
polymer electrolyte
solid polymer
electrolyte fuel
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JP3675473B2 (en
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Masayuki Tamura
正之 田村
Kiyoshige Jitsukata
清成 實方
Haruhisa Miyake
晴久 三宅
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AGC Inc
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    • 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
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    • 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
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a solid polymer electrolyte fuel cell with a small energy loss and high performance. <P>SOLUTION: In a manufacturing method of a solid polymer electrolyte fuel cell having a positive ion exchange membrane made of perfluorocarbon polymer containing a sulfonic acid group as a solid polymer electrolyte, on the surface of which, a gas diffusion electrode is adhered, the gas diffusion electrode is produced by molding the mixture obtained after mixing a liquid solution of the perfluorocarbon polymer which is a dry resin having the sulfonic acid group, of which, the ion exchange capacity is 0.95-1.6 milli-equivalent/g, in an electrode material. Thereby, the fuel cell is manufactured. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は固体高分子電解質型の燃料電池に関するものである。   The present invention relates to a solid polymer electrolyte fuel cell.

近年プロトン伝導性の高分子膜を電解質として用いる燃料電池（固体高分子電解質型燃料電池）の研究が進んでいる。固体高分子電解質型燃料電池は、低温で作動し出力密度が高く小型化が可能であるという特徴を有し、車載用電源等の用途に対し有望視されている。   In recent years, research on fuel cells (solid polymer electrolyte fuel cells) using proton conductive polymer membranes as electrolytes has been progressing. The solid polymer electrolyte fuel cell has a feature that it operates at a low temperature, has a high output density, and can be miniaturized, and is promising for uses such as an in-vehicle power source.

本用途に用いられる高分子膜は、通常厚さ１００〜２００μｍのプロトン伝導性イオン交換膜が用いられ、特にスルホン酸基を有するパーフルオロカーボン重合体からなる陽イオン交換膜が基本特性に優れるため広く検討されている。
陽イオン交換膜の表面に密着されるガス拡散電極中の組成については、燃料電池特性に大きく影響することが知られているが、必ずしも十分に検討されていない。 As the polymer membrane used in this application, a proton conductive ion exchange membrane having a thickness of 100 to 200 μm is usually used. In particular, a cation exchange membrane made of a perfluorocarbon polymer having a sulfonic acid group is excellent in basic characteristics, so that it is widely used. It is being considered.
The composition in the gas diffusion electrode that is in close contact with the surface of the cation exchange membrane is known to greatly affect the fuel cell characteristics, but has not been fully studied.

特許文献１、特許文献２には米国デュポン社製のスルホン酸基を有するパーフルオロカーボン重合体系イオン交換ポリマー：ナフィオンを用いた検討を行っているが、燃料電池特性を十分に改善するには至っていない。   In Patent Document 1 and Patent Document 2, a study using Nafion, a perfluorocarbon polymer-based ion exchange polymer having a sulfonic acid group manufactured by DuPont in the United States, has not been made to sufficiently improve the fuel cell characteristics. .

特開平３−２９５１７２号公報JP-A-3-295172 特開平４−１６２３６５号公報JP-A-4-162365

そこで本発明は、前述の問題点を解決することを目的とする。   Therefore, an object of the present invention is to solve the above-described problems.

本発明は、スルホン酸基を有するパーフルオロカーボン重合体からなる陽イオン交換膜を固体高分子電解質とし、前記陽イオン交換膜の表面にガス拡散電極が密着される固体高分子電解質型燃料電池の製造方法において、イオン交換容量が０．９５〜１．６ミリ当量／ｇ乾燥樹脂でありスルホン酸基を有するパーフルオロカーボン重合体の溶液を電極材料に混合した後、得られた混合物を成形することによりガス拡散電極を作製することを特徴とする固体高分子電解質型燃料電池の製造方法を提供する。   The present invention provides a solid polymer electrolyte fuel cell in which a cation exchange membrane comprising a perfluorocarbon polymer having a sulfonic acid group is used as a solid polymer electrolyte, and a gas diffusion electrode is in close contact with the surface of the cation exchange membrane. In the method, by mixing a solution of a perfluorocarbon polymer having an ion exchange capacity of 0.95 to 1.6 meq / g dry resin and having a sulfonic acid group into an electrode material, the resulting mixture is molded. A method for producing a solid polymer electrolyte fuel cell, characterized by producing a gas diffusion electrode.

本発明で良好な効果が達成される機構は必ずしも明らかではないが、電極中に陽イオン交換膜と同等の特性を有するスルホン酸型パーフルオロカーボン重合体を分散し含有させることにより、電極との接触を確実にして電極反応の効率が高められると考えられる。   Although the mechanism by which a good effect is achieved in the present invention is not necessarily clear, contact with the electrode can be achieved by dispersing and containing a sulfonic acid type perfluorocarbon polymer having the same characteristics as a cation exchange membrane in the electrode. It is considered that the efficiency of the electrode reaction is improved by ensuring the above.

本発明におけるガス拡散電極中に分散し含有されるスルホン酸基を有するパーフルオロカーボン重合体（以下、スルホン酸型パーフルオロカーボン重合体という。）のイオン交換容量は０．９５〜１．６ミリ当量／ｇ乾燥樹脂であり、好ましくは１．０〜１．５ミリ当量／ｇ乾燥樹脂である。   The ion exchange capacity of the perfluorocarbon polymer having sulfonic acid groups dispersed and contained in the gas diffusion electrode in the present invention (hereinafter referred to as sulfonic acid type perfluorocarbon polymer) is 0.95 to 1.6 meq / g dry resin, preferably 1.0 to 1.5 meq / g dry resin.

スルホン酸型パーフルオロカーボン重合体は、ポリマー自体の粉末がガス拡散電極中に分散し含有されること、又は白金などの触媒微粒子等を担持させたカーボンブラックなどの炭素粉末に予めコーティングさせてガス拡散電極中に分散し含有されること、のいずれも採用可能である。更には、場合によって使用される、ポリプロピレン、ポリスチレン、ポリメタクリル酸メチル、フェノール樹脂、ポリスルホン等の有機系高分子の微粒子や、ＳｉＯ２、ＴｉＯ２、ＺｒＯ２等の無機化合物の微粒子に予めコーティングし、ガス拡散電極中に分散し含有されることも採用可能である。 In the sulfonic acid type perfluorocarbon polymer, the powder of the polymer itself is dispersed and contained in the gas diffusion electrode, or the carbon powder such as carbon black supporting the catalyst fine particles such as platinum is coated in advance to diffuse the gas. Any of being dispersed and contained in the electrode can be employed. Furthermore, it may be coated in advance with fine particles of organic polymer such as polypropylene, polystyrene, polymethyl methacrylate, phenol resin, polysulfone and inorganic compounds such as SiO 2 , TiO 2 , ZrO 2, etc. It is also possible to adopt a dispersion and inclusion in the gas diffusion electrode.

スルホン酸型パーフルオロカーボン重合体をガス拡散電極中に、分散含有させる方法としては、ロールプレス等により多孔質体でシート状のガス拡散電極を得る前に、スルホン酸型パーフルオロカーボン重合体の粉末又は溶液を電極材料に混合する方法や、シート状のガス拡散電極を得た後に電極をスルホン酸型パーフルオロカーボン重合体の溶液中に浸漬する方法、のいずれも採用可能である。本発明では、スルホン酸型パーフルオロカーボン重合体の溶液を電極材料に混合する方法を採用している。   As a method of dispersing and containing the sulfonic acid type perfluorocarbon polymer in the gas diffusion electrode, before obtaining the sheet-like gas diffusion electrode with a porous material by a roll press or the like, the sulfonic acid type perfluorocarbon polymer powder or Either a method of mixing a solution with an electrode material or a method of immersing an electrode in a sulfonic acid type perfluorocarbon polymer solution after obtaining a sheet-like gas diffusion electrode can be employed. In the present invention, a method of mixing a solution of a sulfonic acid type perfluorocarbon polymer with an electrode material is employed.

本発明でガス拡散電極中に分散し含有されるスルホン酸型パーフルオロカーボン重合体の量としては、電極作製に用いるカーボンブラックに対し５〜３０重量％、特には８〜２０重量％であることが好ましい。上記範囲より少ない場合には、スルホン酸型パーフルオロカーボン重合体を含有させた効果が小さく、一方上限値より多い場合は、カーボンブラックが塊状になりやすく電極作製における操作性が低下する。   The amount of the sulfonic acid type perfluorocarbon polymer dispersed and contained in the gas diffusion electrode in the present invention is 5 to 30% by weight, particularly 8 to 20% by weight, based on the carbon black used for electrode preparation. preferable. When the amount is less than the above range, the effect of containing the sulfonic acid-type perfluorocarbon polymer is small. On the other hand, when the amount is more than the upper limit, the carbon black tends to be agglomerated and the operability in electrode preparation is lowered.

本発明でガス拡散電極に含有されるスルホン酸型パーフルオロカーボン重合体としては、テトラフルオロエチレンとＣＦ２＝ＣＦ−（ＯＣＦ２ＣＦＸ）ｍ−Ｏｑ−（ＣＦ２）ｎ−Ａ（式中ｍは０〜３、ｎは０〜１２、ｑは０又は１、ＸはＦ又はＣＦ３、Ａはスルホン酸基。）で表されるフルオロビニル化合物との共重合体が好ましく採用可能である。
上記フルオロビニル化合物の好ましい例としては、下記のものなどが挙げられる。ただし、ｒ、ｓは１〜８であり、ｔは０〜８であり、ｕは１〜３である。 As the sulfonic acid type perfluorocarbon polymer contained in the gas diffusion electrode in the present invention, tetrafluoroethylene and CF 2 ═CF— (OCF 2 CFX) m —O q — (CF 2 ) n —A (where m 0 to 3, n is 0 to 12, q is 0 or 1, X is F or CF 3 , and A is a sulfonic acid group.) A copolymer with a fluorovinyl compound is preferably used.
Preferable examples of the fluorovinyl compound include the following. However, r and s are 1-8, t is 0-8, u is 1-3.

Figure 2005044815
Figure 2005044815

なお、スルホン酸型パーフルオロカーボン重合体を構成するためのコモノマーである上記テトラフルオロエチレンの代わりにヘキサフルオロプロピレンの如きパーフルオロオレフィン、パーフルオロ（アルキルビニルエーテル）等を用いることも可能である。   In addition, it is also possible to use a perfluoroolefin such as hexafluoropropylene, perfluoro (alkyl vinyl ether) or the like in place of the tetrafluoroethylene which is a comonomer for constituting the sulfonic acid type perfluorocarbon polymer.

本発明の、イオン交換容量が０．９５〜１．６ミリ当量／ｇ乾燥樹脂のスルホン酸型パーフルオロカーボン重合体が分散し含有されるガス拡散電極は、通常の既知の手法に従ってその表面に陽イオン交換膜を加熱プレス法等により密着させ、次いで集電体を取り付け、燃料電池として組み立てられる。   The gas diffusion electrode of the present invention, in which a sulfonic acid type perfluorocarbon polymer having an ion exchange capacity of 0.95 to 1.6 meq / g dry resin is dispersed and contained, is positively applied to the surface in accordance with an ordinary known method. The ion exchange membrane is brought into close contact by a hot press method or the like, and then a current collector is attached to assemble the fuel cell.

スルホン酸型パーフルオロカーボン重合体からなる陽イオン交換膜は、フィブリル状、織布状、又は不織布状のパーフルオロカーボン重合体で補強することもできる。   The cation exchange membrane made of a sulfonic acid type perfluorocarbon polymer can be reinforced with a fibril-like, woven fabric, or non-woven fabric perfluorocarbon polymer.

集電体には燃料ガス又は酸化剤ガスの通路となる溝が形成された導電性カーボン板等が用いられる。   As the current collector, a conductive carbon plate or the like in which grooves serving as fuel gas or oxidant gas passages are formed is used.

［実施例１］
特開平２−８８６４５号公報に記載されている方法に準拠し、ＣＦ２＝ＣＦ２とＣＦ２＝ＣＦＯ（ＣＦ２ＣＦ（ＣＦ３））Ｏ（ＣＦ２）２ＳＯ２Ｆとの共重合体からなるイオン交換容量１．１ミリ当量／ｇ乾燥樹脂の共重合体を得た。この共重合体の一部を２２０℃で押し出し製膜し、厚さ１００μｍのフィルムを得た。 [Example 1]
Copolymer of CF 2 ═CF 2 and CF 2 ═CFO (CF 2 CF (CF 3 )) O (CF 2 ) 2 SO 2 F in accordance with the method described in JP-A-2-88645 A copolymer having an ion exchange capacity of 1.1 meq / g dry resin was obtained. A part of this copolymer was extruded at 220 ° C. to obtain a film having a thickness of 100 μm.

上記の共重合体フィルムを、ジメチルスルホキシド３０重量％と苛性カリ１５重量％とを含む水溶液中で加水分解を行い、水洗した後１Ｎの塩酸中に浸漬した。次に膜を水洗し、膜の四辺を専用治具で拘束した後６０℃、１時間乾燥し陽イオン交換膜を製造した。   The copolymer film was hydrolyzed in an aqueous solution containing 30% by weight of dimethyl sulfoxide and 15% by weight of caustic potash, washed with water, and then immersed in 1N hydrochloric acid. Next, the membrane was washed with water, the four sides of the membrane were restrained with a dedicated jig, and then dried at 60 ° C. for 1 hour to produce a cation exchange membrane.

上で得られたイオン交換容量１．１ミリ当量／ｇ乾燥樹脂の粉体を上記と同様な処理を施し酸型のポリマーを得た。通常の既知の手法に従って、水とエタノールとが重量比で１：１の混合溶媒を用いてスルホン酸型パーフルオロカーボン重合体溶液を得た。   The ion exchange capacity 1.1 meq / g dry resin powder obtained above was treated in the same manner as above to obtain an acid type polymer. A sulfonic acid type perfluorocarbon polymer solution was obtained using a mixed solvent of water and ethanol in a weight ratio of 1: 1 according to a usual known method.

白金触媒微粒子を担持させたカーボンブラックに、スルホン酸型パーフルオロカーボン重合体溶液を混合した後、乾燥し、スルホン酸型パーフルオロカーボン重合体でコーティングされた白金触媒担持のカーボンブラックを得た。スルホン酸型パーフルオロカーボン重合体はカーボンブラックに対し１０重量％混合したことになる。   A carbon black carrying platinum catalyst fine particles was mixed with a sulfonic acid type perfluorocarbon polymer solution and then dried to obtain a platinum black supported on a platinum catalyst coated with a sulfonic acid type perfluorocarbon polymer. The sulfonic acid type perfluorocarbon polymer was mixed with carbon black at 10% by weight.

上記のカーボンブラック粉末にポリテトラフルオロエチレン（以下、ＰＴＦＥという。）を混合し、ロールプレスを用いて厚さ２５０μｍのシート状のガス拡散電極を作製した。このガス拡散電極２枚の間に、上記陽イオン交換膜を挿入し平板熱プレス機を用いて積層することにより膜電極接合体を作製した。膜電極接合体の白金触媒量は膜面積１ｃｍ２当たり１ｍｇであった。 Polytetrafluoroethylene (hereinafter referred to as PTFE) was mixed with the carbon black powder, and a sheet-like gas diffusion electrode having a thickness of 250 μm was produced using a roll press. A membrane electrode assembly was prepared by inserting the cation exchange membrane between the two gas diffusion electrodes and laminating them using a flat plate heat press. The amount of platinum catalyst in the membrane / electrode assembly was 1 mg per 1 cm 2 of membrane area.

次に、膜電極接合体をチタン製の集電体、ＰＴＦＥ製のガス供給室、ヒーターの順番で両側からはさみ、有効膜面積９ｃｍ２の燃料電池を組み立てた。セルの温度を６０℃に保ち、正極に酸素、負極に水素をそれぞれ１気圧で供給したときの電流密度に対する端子電圧を測定したところ、電流密度０．４Ａ／ｃｍ２でセル電圧０．７０Ｖであった。 Next, the membrane electrode assembly was sandwiched from both sides in the order of a titanium current collector, a PTFE gas supply chamber, and a heater, and a fuel cell having an effective membrane area of 9 cm 2 was assembled. When the cell voltage was maintained at 60 ° C. and the terminal voltage was measured against the current density when oxygen was supplied to the positive electrode and hydrogen was supplied to the negative electrode at 1 atm, the cell voltage was 0.70 V at a current density of 0.4 A / cm 2. there were.

［比較例１］
特開平２−８８６４５号公報に記載されている方法に準拠し、ＣＦ２＝ＣＦ２とＣＦ２＝ＣＦＯ（ＣＦ２ＣＦ（ＣＦ３））Ｏ（ＣＦ２）２ＳＯ２Ｆとの共重合体からなるイオン交換容量０．９ミリ当量／ｇ乾燥樹脂の共重合体を得た。この共重合体に実施例１と同様な処理を施し酸型のポリマーを得た。次に通常の既知の手法に従って、水とエタノールとが重量比で１：１の混合溶媒を用いてスルホン酸型パーフルオロカーボン重合体溶液を得た。 [Comparative Example 1]
Copolymer of CF 2 ═CF 2 and CF 2 ═CFO (CF 2 CF (CF 3 )) O (CF 2 ) 2 SO 2 F in accordance with the method described in JP-A-2-88645 A copolymer having an ion exchange capacity of 0.9 meq / g dry resin was obtained. This copolymer was treated in the same manner as in Example 1 to obtain an acid type polymer. Next, a sulfonic acid type perfluorocarbon polymer solution was obtained by using a mixed solvent of water and ethanol in a weight ratio of 1: 1 according to an ordinary known method.

実施例１において、白金触媒担持のカーボンブラックに上記のスルホン酸型パーフルオロカーボン重合体溶液で処理することを除いて、同様の手法により厚さ２５０μｍのシート状のガス拡散電極を作製した。   In Example 1, a sheet-like gas diffusion electrode having a thickness of 250 μm was produced in the same manner except that the platinum catalyst-supported carbon black was treated with the sulfonic acid-type perfluorocarbon polymer solution.

実施例１と同一なイオン交換容量１．１ミリ当量／ｇ乾燥樹脂の陽イオン交換膜を用い、同様な方法により膜電極接合体を作製し燃料電池を組み立てた後、同様な条件下で電流密度に対する端子電圧を測定したところ、電流密度０．４Ａ／ｃｍ２でセル電圧０．６５Ｖであった。 Using the same ion exchange capacity 1.1 milliequivalent / g dry resin cation exchange membrane as in Example 1, a membrane electrode assembly was prepared by the same method and a fuel cell was assembled. When the terminal voltage with respect to the density was measured, the cell voltage was 0.65 V at a current density of 0.4 A / cm 2 .

上記の結果からわかるように、実施例１のガス拡散電極は比較例１の電極に比べ、燃料電池を組み上げたときのエネルギー損失が小さい。   As can be seen from the above results, the gas diffusion electrode of Example 1 has less energy loss when the fuel cell is assembled than the electrode of Comparative Example 1.

ガス拡散電極中に、スルホン酸型パーフルオロカーボン重合体を分散、含有させることにより、エネルギー損失が小さい高性能の固体高分子電解質型燃料電池が提供できる。   By dispersing and containing a sulfonic acid type perfluorocarbon polymer in the gas diffusion electrode, a high performance solid polymer electrolyte fuel cell with low energy loss can be provided.

Claims (3)

スルホン酸基を有するパーフルオロカーボン重合体からなる陽イオン交換膜を固体高分子電解質とし、前記陽イオン交換膜の表面にガス拡散電極が密着される固体高分子電解質型燃料電池の製造方法において、イオン交換容量が０．９５〜１．６ミリ当量／ｇ乾燥樹脂でありスルホン酸基を有するパーフルオロカーボン重合体の溶液を電極材料に混合した後、得られた混合物を成形することによりガス拡散電極を作製することを特徴とする固体高分子電解質型燃料電池の製造方法。   In a method for producing a solid polymer electrolyte fuel cell, a cation exchange membrane comprising a perfluorocarbon polymer having a sulfonic acid group is used as a solid polymer electrolyte, and a gas diffusion electrode is in close contact with the surface of the cation exchange membrane. After mixing a solution of a perfluorocarbon polymer having an exchange capacity of 0.95 to 1.6 meq / g dry resin and having a sulfonic acid group with an electrode material, the resulting mixture is molded to form a gas diffusion electrode. A method for producing a solid polymer electrolyte fuel cell, characterized by comprising: 前記電極材料には、触媒微粒子を担持させた炭素粉末が含まれる請求項１に記載の固体高分子電解質型燃料電池の製造方法。   2. The method for producing a solid polymer electrolyte fuel cell according to claim 1, wherein the electrode material includes carbon powder supporting catalyst fine particles. 前記パーフルオロカーボン重合体が、ＣＦ２＝ＣＦ２とＣＦ２＝ＣＦ−（ＯＣＦ２ＣＦＸ）ｍ−Ｏｑ−（ＣＦ２）ｎ−Ａ（式中ｍは０〜３、ｎは０〜１２、ｑは０又は１、ＸはＦ又はＣＦ３、Ａはスルホン酸基。）との共重合体である請求項１又は２に記載の固体高分子電解質型燃料電池の製造方法。
The perfluorocarbon polymer, CF 2 = CF 2 and CF 2 = CF- (OCF 2 CFX ) m -O q - (CF 2) n -A ( wherein m is 0 to 3, n is 0 to 12, The method for producing a solid polymer electrolyte fuel cell according to claim 1 or 2, wherein q is a copolymer with 0 or 1, X is F or CF 3 , and A is a sulfonic acid group.
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JPS6167786A (en) * 1984-09-10 1986-04-07 Japan Storage Battery Co Ltd Production of joined body of ion exchange resin film and electrode
JPS6167789A (en) * 1984-09-10 1986-04-07 Japan Storage Battery Co Ltd Production of joined body of ion exchange resin film and electrode
JPS62288616A (en) * 1986-06-06 1987-12-15 Asahi Glass Co Ltd Production of perfluorocarbon polymer having sulfonic acid type functional group
JPS6337134A (en) * 1986-08-01 1988-02-17 Tokuyama Soda Co Ltd Fluorine-containing ion exchange membrane
JPH0536418A (en) * 1991-03-13 1993-02-12 Fuji Electric Co Ltd Solid polymer electrolytic fuel cell and manufacture of the same
JPH06150937A (en) * 1992-11-09 1994-05-31 Asahi Chem Ind Co Ltd Solid high polymer type fuel cell
JPH06203840A (en) * 1993-01-08 1994-07-22 Asahi Chem Ind Co Ltd Solid polyelectrolyte fuel cell
JPH06295729A (en) * 1993-02-09 1994-10-21 Asahi Chem Ind Co Ltd High performance high polymer electrolyte type fuel cell

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56127782A (en) * 1980-02-11 1981-10-06 Ppg Industries Inc Solid polymer electrolyte and method
JPS6167786A (en) * 1984-09-10 1986-04-07 Japan Storage Battery Co Ltd Production of joined body of ion exchange resin film and electrode
JPS6167789A (en) * 1984-09-10 1986-04-07 Japan Storage Battery Co Ltd Production of joined body of ion exchange resin film and electrode
JPS62288616A (en) * 1986-06-06 1987-12-15 Asahi Glass Co Ltd Production of perfluorocarbon polymer having sulfonic acid type functional group
JPS6337134A (en) * 1986-08-01 1988-02-17 Tokuyama Soda Co Ltd Fluorine-containing ion exchange membrane
JPH0536418A (en) * 1991-03-13 1993-02-12 Fuji Electric Co Ltd Solid polymer electrolytic fuel cell and manufacture of the same
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JPH06203840A (en) * 1993-01-08 1994-07-22 Asahi Chem Ind Co Ltd Solid polyelectrolyte fuel cell
JPH06295729A (en) * 1993-02-09 1994-10-21 Asahi Chem Ind Co Ltd High performance high polymer electrolyte type fuel cell

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