JP4919166B2 - Method for producing membrane / electrode assembly - Google Patents
Method for producing membrane / electrode assembly Download PDFInfo
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- JP4919166B2 JP4919166B2 JP2007170216A JP2007170216A JP4919166B2 JP 4919166 B2 JP4919166 B2 JP 4919166B2 JP 2007170216 A JP2007170216 A JP 2007170216A JP 2007170216 A JP2007170216 A JP 2007170216A JP 4919166 B2 JP4919166 B2 JP 4919166B2
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- 239000012528 membrane Substances 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000003054 catalyst Substances 0.000 claims description 57
- 239000003014 ion exchange membrane Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 34
- 238000009423 ventilation Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000009792 diffusion process Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 229920000557 Nafion® Polymers 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- 239000002759 woven fabric Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims 2
- 238000005342 ion exchange Methods 0.000 claims 1
- 208000021668 chronic eosinophilic leukemia Diseases 0.000 description 23
- 239000010410 layer Substances 0.000 description 18
- 238000010586 diagram Methods 0.000 description 16
- 238000002347 injection Methods 0.000 description 15
- 239000007924 injection Substances 0.000 description 15
- 238000000465 moulding Methods 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- 210000000170 cell membrane Anatomy 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
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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
- 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
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- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Description
本発明は、膜／電極接合体の作製方法に関し、特に、イオン交換膜（Ｐｒｏｔｏｎ Ｅｘｃｈａｎｇｅ Ｍｅｍｂｒａｎｅ、ＰＥＭ）の両面に、それぞれ、平らの触媒電極層（Ｃａｔａｌｙｓｔ Ｅｌｅｃｔｒｏｄｅ Ｌａｙｅｒ、ＣＥＬ）が形成され、また、膜／電極接合体（Ｍｅｍｂｒａｎｅ Ｅｌｅｃｔｒｏｄｅ Ａｓｓｅｍｂｌｙ、ＭＥＡ）の形成厚さを制御できるものに関する。 The present invention relates to a method for producing a membrane / electrode assembly, and in particular, a flat catalyst electrode layer (Catalyst Electrode Layer, CEL) is formed on each side of an ion exchange membrane (Proton Exchange Membrane, PEM). The present invention relates to a film / electrode assembly (Mebrane Electrode Assembly, MEA) capable of controlling the formation thickness.
一般の従来のものは、例えば、中華民国専利公報第０９３１０１２９６号に掲示された「印刷工程により燃料電池膜電極セットを作製する製造方法」があり、それは；（ａ）イオン交換膜と陽極触媒剤及び陰極触媒剤溶液を用意するステップと；（ｂ）適当な面積に切られたイオン交換膜を薄板ベースにセットし、また、該薄板ベースをスクリーン印刷テーブルにセットするステップと；（ｃ）選別した印刷板材を該スクリーン印刷テーブルのスクリーン板固定具に固定するステップと；（ｄ）へらで、用意した触媒剤を均一的に印刷板材パターンに塗布し、そして、印刷板材のパターンの触媒剤を薄板ベース上のイオン交換膜にセットし；（ｅ）該スクリーン印刷を終了した後、該イオン交換膜を加熱板上にセットして加熱し；（ｆ）該イオン交換膜が平らに回復すると、該イオン交換膜上に、均一な触媒層が形成される。 As a general conventional one, for example, there is a “manufacturing method for producing a fuel cell membrane electrode set by a printing process” published in the Chinese Patent Publication No. 0931101296, which includes: (a) an ion exchange membrane and an anode catalyst agent And (b) setting an ion exchange membrane cut to an appropriate area on a thin plate base, and setting the thin plate base on a screen printing table; and (c) sorting. Fixing the prepared printing plate material to the screen plate fixing tool of the screen printing table; (d) applying the prepared catalyst agent uniformly to the printing plate material pattern with a spatula, and applying the catalyst agent of the pattern of the printing plate material; (E) after completion of the screen printing, the ion exchange membrane is set on a heating plate and heated; (f) the ion exchange membrane on the thin plate base; When-exchange membrane flat restored, on the ion-exchange membrane, uniform catalyst layer is formed.
上記の従来の「印刷工程で燃料電池膜電極セットを作製する製造方法」は、イオン交換膜上に、陽極や陰極の触媒層を形成するが、該イオン交換膜が、陽極触媒剤や陰極触媒剤溶液に接触すると、容易にしわが発生し、触媒層が形成されると同時に、襞が形成される場合があり、平らの触媒塗布膜層が得られないため、通常に、余計に襞を除去する工程を増やして、襞を消去し、また、肉厚の触媒塗布層を形成する時、多数回の塗布と皺除去工程を繰り返すことが必要であるため、工程が複雑になり、実用的ではない。
本発明の主な目的は、ＰＥＭの両面上に、それぞれ、平らのＣＥＬを形成でき、また、ＭＥＡの肉厚を制御できる膜／電極接合体の作製方法を提供する。 The main object of the present invention is to provide a method for producing a membrane / electrode assembly capable of forming a flat CEL on both sides of a PEM and controlling the thickness of the MEA.
本発明は、上記の目的を達成するため、少なくとも、一次注入と一次成型、逆転、二次注入及び二次成型等のステップが備えられ、作製する時、加熱温度制御可能や加熱できない真空固定装置を用意し、真空固定装置に、通気平面を設置し、真空作用により、該通気平面上にＰＥＭを固定し、また、ＰＥＭ上に貫通穴を有するフォルマをセットし、触媒スラリーをフォルマの貫通穴に注入し、同時に、該真空固定装置を、該触媒スラリーと該ＰＥＭとの調和温度（常温調和であれば、加熱しない）まで加熱し、また、押え板の突出部を該フォルマの貫通穴に押し入れることにより、該ＰＥＭの一面に第１のＣＥＬが形成され、冷却の後、該ＰＥＭを逆転して、同様的に、該触媒スラリーを注入して調和温度まで加熱した後、押え板を該フォルマの貫通穴に押し入れることにより、該ＰＥＭのもう一面上に、第２のＣＥＬ’が形成される。これにより、該ＰＥＭの両面上に、それぞれ、平らのＣＥＬが形成されてＣＥＬ＋ＰＥＭ＋ＣＥＬ’の三層式ＭＥＡ（ＭＥＡ−３−ｌａｙｅｒ）が得られ、ＭＥＡの肉厚を制御できる効果が得られる。また、２回の押え板を押し入れる前、それぞれ、気体拡散層（Ｇａｓ Ｄｉｆｆｕｓｉｏｎ Ｌａｙｅｒ、ＧＤＬ）を追加すると、ＧＤＬ＋ＣＥＬ＋ＰＥＭ＋ＣＥＬ’＋ＧＤＬ’の五層式ＭＥＡ（ＭＥＡ−５−ｌａｙｅｒ）が得られる膜／電極接合体の作製方法である。 In order to achieve the above object, the present invention is provided with at least steps of primary injection, primary molding, reverse rotation, secondary injection, secondary molding, and the like. Prepare a ventilation plane in the vacuum fixing device, fix the PEM on the ventilation plane by vacuum action, set a forma with a through hole on the PEM, and put the catalyst slurry into the through hole of the forma At the same time, the vacuum fixing device is heated to a harmonious temperature between the catalyst slurry and the PEM (if it is conditioned at normal temperature, it is not heated), and the protrusion of the presser plate is inserted into the through hole of the forma. The first CEL is formed on one side of the PEM by pushing it in. After cooling, the PEM is reversed, and similarly, the catalyst slurry is injected and heated to a harmonized temperature. The fol By pushing the through hole, on another side of the PEM, the second CEL 'is formed. Thereby, a flat CEL is formed on both sides of the PEM to obtain a three-layer MEA (MEA-3-layer) of CEL + PEM + CEL ′, and the effect of controlling the thickness of the MEA is obtained. In addition, when a gas diffusion layer (Gas Diffusion Layer, GDL) is added before each presser plate is pushed in twice, a membrane / electrode that provides a five-layer MEA (MEA-5-layer) of GDL + CEL + PEM + CEL ′ + GDL ′ This is a method for manufacturing a joined body.
図１は、本発明の流れ概念図である。図のように、本発明は、膜／電極接合体（Ｍｅｍｂｒａｎｅ Ｅｌｅｃｔｒｏｄｅ Ａｓｓｅｍｂｌｙ、ＭＥＡ）の作製方法で、少なくとも、用意ステップ１と一次注入２、一次成型３、逆転４、二次注入５及び二次成型６等のステップから構成され、イオン交換膜（Ｐｒｏｔｏｎ Ｅｘｃｈａｎｇｅ Ｍｅｍｂｒａｎｅ、ＰＥＭ）の両面上に、それぞれ、平らの触媒電極層（Ｃａｔａｌｙｓｔ Ｅｌｅｃｔｒｏｄｅ Ｌａｙｅｒ、ＣＥＬ）が形成され、ＣＥＬの肉厚を制御できる効果が得られる。上記の構造により、新規の膜／電極接合体の作製方法が構成される。 FIG. 1 is a conceptual flow diagram of the present invention. As shown in the figure, the present invention is a method for producing a membrane / electrode assembly (MEB), and includes at least a preparation step 1, a primary injection 2, a primary molding 3, a reverse 4, a secondary injection 5, and a secondary. It consists of steps such as molding 6, etc., and a flat catalyst electrode layer (Catalyst Electrode Layer, CEL) is formed on both sides of the ion exchange membrane (Proton Exchange Membrane, PEM), and the thickness of the CEL can be controlled. Is obtained. The above structure constitutes a method for producing a novel membrane / electrode assembly.
図２〜図８は、それぞれ、本発明の製造概念図と本発明の一次注入概念図、本発明の一次成型概念図、本発明の逆転概念図、本発明の二次注入概念図、本発明の二次成型概念図及び本発明の成品概念図である。図のように、本発明は、次の作製ステップが含有される。 2 to 8 are respectively a manufacturing conceptual diagram of the present invention, a primary injection conceptual diagram of the present invention, a primary molding conceptual diagram of the present invention, a reverse conceptual diagram of the present invention, a secondary injection conceptual diagram of the present invention, and a present invention. It is a secondary molding conceptual diagram of this and the product conceptual diagram of this invention. As shown, the present invention includes the following fabrication steps.
（ａ）用意ステップ１であり、熱温制御可能や加熱できない真空固定装置７１を用意し、該真空固定装置７１に通気平面７２を設置し、通気平面７２上にＰＥＭ７３をセットし、真空作用により、ＰＥＭ７３を平らに該通気平面７２に固定し、その後、更に、該ＰＥＭ７３上に、貫通穴７４１を有するフォルマ７４をセットする。該通気平面は、燒結材やオリフィス板、マトリックス板、網状層或いは上記の一部や全部の任意の組み合せからなり、また、上端や外端に、通気可能の平面が形成される。 (A) In preparation step 1, a vacuum fixing device 71 that can control the heat temperature and cannot be heated is prepared, a ventilation plane 72 is installed in the vacuum fixing device 71, a PEM 73 is set on the ventilation plane 72, and a vacuum action is performed. , PEM 73 is fixed flatly to the ventilation plane 72, and then a form 74 having a through hole 741 is set on the PEM 73. The ventilation plane is composed of a sintered material, an orifice plate, a matrix plate, a mesh layer, or any combination of part or all of the above, and a ventable plane is formed at the upper end and the outer end.
（ｂ）一次注入２であり、陽極触媒スラリー８や陰極触媒スラリー８ａを、該膜／電極接合体キャビティー７の該フォルマ７４の貫通穴７４１に注入し、同時に、該真空固定装置７１内の温度制御加熱素子７２１を駆動して、温度を緩やかに該陽極触媒スラリー８や陰極触媒スラリー８ａとＰＥＭとの調和温度（常温調和であれば、加熱を駆動しない）まで加熱する。 (B) In the primary injection 2, the anode catalyst slurry 8 and the cathode catalyst slurry 8a are injected into the through hole 741 of the form 74 of the membrane / electrode assembly cavity 7, and at the same time, in the vacuum fixing device 71 The temperature control heating element 721 is driven, and the temperature is gradually heated to the harmonized temperature of the anode catalyst slurry 8 or the cathode catalyst slurry 8a and the PEM (if the temperature is harmonized, heating is not driven).
（ｃ）一次成型３であり、真空固定装置７１の温度を、該調和温度に保持しながら、突出部７５１を有する押え板７５を、該フォルマ７４の貫通穴７４１に押し入れることにより、ＰＥＭ７３の一面上に第１のＣＥＬ８１が形成される。 (C) It is the primary molding 3, and the press plate 75 having the projecting portion 751 is pushed into the through hole 741 of the form 74 while maintaining the temperature of the vacuum fixing device 71 at the harmonized temperature. A first CEL 81 is formed on one surface.
（ｄ）逆転４であり、ＰＥＭ７３の一面に該第１のＣＥＬ８１が形成された後、冷却して、真空固定装置７１の真空作用と加熱を中止し、フォルマ７４を取り出して、該ＰＥＭ７３を逆転してから、真空固定装置７１の真空作用により、ＰＥＭ７３を、平らに通気平面７２上に固定し、その後、ＰＥＭ７３上に、上記のフォルマ７４をセットする。 (D) Reversal 4, after the first CEL 81 is formed on one surface of the PEM 73, the cooling is performed, the vacuum action and heating of the vacuum fixing device 71 are stopped, the form 74 is taken out, and the PEM 73 is reversed. Then, the PEM 73 is flatly fixed on the ventilation plane 72 by the vacuum action of the vacuum fixing device 71, and then the above-described form 74 is set on the PEM 73.
（ｅ）二次注入５であり、陽極触媒スラリー８や陰極触媒スラリー８ａを、該固定装置７内にある該フォルマ７４の貫通穴７４１に注入し、同時に、真空固定装置７１内の温度制御加熱素子７２１を駆動して、温度を緩やかに陽極触媒スラリー８や陰極触媒スラリー８ａとＰＥＭとの調和温度（常温調和であれば加熱を駆動しない）まで加熱する。 (E) Secondary injection 5, in which the anode catalyst slurry 8 and the cathode catalyst slurry 8a are injected into the through hole 741 of the form 74 in the fixing device 7 and at the same time, the temperature controlled heating in the vacuum fixing device 71 The element 721 is driven, and the temperature is gradually heated to the harmonious temperature of the anode catalyst slurry 8 or the cathode catalyst slurry 8a and the PEM (the heating is not driven if the room temperature is harmonized).
（ｆ）二次成型６であり、真空固定装置７１の温度を該調和温度に保持しながら、押え板７５の突出部７５１を該フォルマ７４の貫通穴７４１に押し入れることにより、ＰＥＭ７３のもう一面上に、第２のＣＥＬ’８２が形成され、これにより、組み合せがＣＥＬ８１＋ＰＥＭ７３＋ＣＥＬ’８２である三層式ＭＥＡ（ＭＥＡ−３−ｌａｙｅｒ）が得られる。 (F) The secondary molding 6, and the other side of the PEM 73 is formed by pressing the protrusion 751 of the press plate 75 into the through hole 741 of the form 74 while maintaining the temperature of the vacuum fixing device 71 at the harmonized temperature. On top, a second CEL'82 is formed, thereby obtaining a three-layer MEA (MEA-3-layer) with the combination CEL81 + PEM73 + CEL'82.
２回の押え板を押し入れる前、それぞれ、気体拡散層（Ｇａｓ Ｄｉｆｆｕｓｉｏｎ Ｌａｙｅｒ、ＧＤＬ）を追加すると、組み合せがＧＤＬ＋ＣＥＬ８１＋ＰＥＭ７３＋ＣＥＬ’８２＋ＧＤＬ’である五層式ＭＥＡ（ＭＥＡ−５−ｌａｙｅｒ）が得られる。該ＧＤＬ気体拡散層は、導電炭材を含む織布や不織布、或いはカーボン紙の通気性材料である。 Before the presser plate is pushed in twice, a gas diffusion layer (Gas Diffusion Layer, GDL) is added to obtain a five-layer MEA (MEA-5-layer) whose combination is GDL + CEL81 + PEM73 + CEL'82 + GDL '. The GDL gas diffusion layer is a breathable material such as a woven or non-woven fabric containing conductive carbon material, or carbon paper.
作製において、ＰＥＭ７３両面上の第１のＣＥＬ８１や第２のＣＥＬ’８２は、一次注入２と二次注入５の時において、陽極や陰極触媒スラリー８、８ａが注入されることにより、陽極や陰極に決められ、第１のＣＥＬ８１や第２のＣＥＬ’８２を陽極とする時、Ｐｔ／Ｒｕ／ＣキャリアとＮａｆｉｏｎ溶液が混合された陽極触媒スラリー８を使用し、また、第１のＣＥＬ８１や第２のＣＥＬ’８２を陰極とする時、Ｐｔ／ＣキャリアとＮａｆｉｏｎ溶液が混合された陰極触媒スラリー８ａを使用する。 In the production, the first CEL 81 and the second CEL ′ 82 on both sides of the PEM 73 are injected into the anode and cathode catalyst slurry 8 and 8a at the time of the primary injection 2 and the secondary injection 5, so that the anode and cathode When the first CEL 81 or the second CEL '82 is used as an anode, the anode catalyst slurry 8 in which a Pt / Ru / C carrier and a Nafion solution are mixed is used. When the second CEL'82 is used as a cathode, a cathode catalyst slurry 8a in which a Pt / C carrier and a Nafion solution are mixed is used.
また、ＰＥＭ７３両面上の第１、２のＣＥＬ、ＣＥＬ’８１、８２を、必要とする肉厚に作製する時、一次成型３と二次成型６の時、押え板７５の突出部７５１をフォルマ７４の貫通穴７４１に押し入れる深さを制御することにより、それぞれ、ＰＥＭ７３の両面上に形成された第１、２のＣＥＬ、ＣＥＬ’８１、８２の肉厚を制御できる。 In addition, when the first and second CELs and CEL'81 and 82 on both sides of the PEM 73 are manufactured to have the required thickness, the protrusion 751 of the presser plate 75 is formed in the former in the primary molding 3 and the secondary molding 6. By controlling the depth to be pushed into the 74 through holes 741, the thicknesses of the first and second CELs and CEL ′ 81 and 82 formed on both sides of the PEM 73 can be controlled.
以上のように、本発明に係わる膜／電極接合体の作製方法は、有効に従来の諸欠点を解消でき、ＰＥＭの両面上に、それぞれ、平らの触媒電極であるＭＥＡが形成でき、また、触媒電極の組み合せ肉厚を制御できる効果が得られるため、本発明は、より進歩的かつより実用的で、法に従って特許請求を出願する。 As described above, the method for producing a membrane / electrode assembly according to the present invention can effectively eliminate the conventional drawbacks, and can form MEAs that are flat catalyst electrodes on both sides of the PEM, Because of the effect of controlling the combined thickness of the catalyst electrodes, the present invention is more progressive and more practical, and claims are filed according to law.
以上は、ただ、本発明のより良い実施例であり、本発明は、それによって制限されることが無く、本発明に係わる特許請求の範囲や明細書の内容に基づいて行った等価の変更や修正は、全てが、本発明の特許請求の範囲内に含まれる。 The above is merely a better embodiment of the present invention, and the present invention is not limited thereby, and equivalent changes made based on the scope of the claims and the description of the present invention. All modifications are within the scope of the claims of the present invention.
１ 用意ステップ
２ 一次注入
３ 一次成型
４ 逆転
５ 二次注入
６ 二次成型
７ 膜／電極接合体キャビティー
７１ 真空固定装置
７２ 通気平面
７２１ 温度制御加熱素子
７３ イオン交換膜
７４ フォルマ
７４１ 貫通穴
７５ 押え板
７５１ 突出部
８ 触媒スラリー
８ａ 触媒スラリー
８１ 第１の触媒電極層
８２ 第２の触媒電極層
1 Preparatory Step 2 Primary Injection 3 Primary Molding 4 Reverse Injection 5 Secondary Injection 6 Secondary Molding 7 Membrane / Electrode Assembly Cavity 71 Vacuum Fixing Device 72 Ventilation Plane 721 Temperature Control Heating Element 73 Ion Exchange Membrane 74 Form 741 Through Hole 75 Presser Plate 751 Projection 8 Catalyst slurry 8a Catalyst slurry 81 First catalyst electrode layer 82 Second catalyst electrode layer
Claims (9)
6. The method for producing a membrane / electrode assembly according to claim 5, wherein the gas diffusion layer is a breathable material such as a woven fabric, a nonwoven fabric, or carbon paper containing a conductive carbon material.
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| JP2007170216A JP4919166B2 (en) | 2007-06-28 | 2007-06-28 | Method for producing membrane / electrode assembly |
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| JP4919166B2 true JP4919166B2 (en) | 2012-04-18 |
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