JPH07211329A - Method for manufacturing gas diffusion electrode - Google Patents
Method for manufacturing gas diffusion electrodeInfo
- Publication number
- JPH07211329A JPH07211329A JP6015797A JP1579794A JPH07211329A JP H07211329 A JPH07211329 A JP H07211329A JP 6015797 A JP6015797 A JP 6015797A JP 1579794 A JP1579794 A JP 1579794A JP H07211329 A JPH07211329 A JP H07211329A
- Authority
- JP
- Japan
- Prior art keywords
- gas diffusion
- reaction layer
- hydrophilic
- diffusion electrode
- layer sheet
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Inert Electrodes (AREA)
Abstract
(57)【要約】
【目的】 反応層の表面を改質することにより、触媒担
持を容易とし、かつ電解液の反応層への侵入を容易とし
得、ひいては電極性能を高め得るガス拡散電極の製造方
法を提供する。
【構成】 ガス拡散層シート、集電網、ガス拡散層シー
ト及び反応層シートを重ねてホットプレス後に反応層表
面を親水化処理することにより、反応層表面を完全に親
水性にする。
(57) [Summary] [Objective] By modifying the surface of a reaction layer, catalyst loading can be facilitated, and electrolyte can easily penetrate into the reaction layer. A manufacturing method is provided. [Structure] A gas diffusion layer sheet, a current collecting network, a gas diffusion layer sheet, and a reaction layer sheet are superposed, and the reaction layer surface is hydrophilized after hot pressing to make the reaction layer surface completely hydrophilic.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、燃料電池等の電極とし
て用いられるガス拡散電極の製造方法にかんする。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a gas diffusion electrode used as an electrode of a fuel cell or the like.
【０００２】[0002]
【従来の技術】従来、この種のガス拡散電極は、撥水性
カーボンブラックとＰＴＦＥ（ポリテットラフルオロエ
チレン）等のフッ素樹脂からなるガス拡散層シート、ニ
ッケル網からなる集電網、上記のものと同様のガス拡散
層シート、及び親水性カーボンブラックと撥水性カーボ
ンブラックとＰＴＦＥ等のフッ素樹脂からなる反応層シ
ートを順に積み重ねてホットプレスした後、反応層に白
金等の触媒を塗布法により担持させて製造されている。
又、触媒を担持した親水性カーボンブラックとＰＴＦＥ
等のフッ素樹脂からなる反応層シートを用い、ガス拡散
層シート及び集電網と共に上述したようにホットプレス
して製造することも行なわれている。2. Description of the Related Art Heretofore, a gas diffusion electrode of this type has a gas diffusion layer sheet made of a water repellent carbon black and a fluororesin such as PTFE (polytetrafluoroethylene), a current collection network made of a nickel net, A similar gas diffusion layer sheet and a reaction layer sheet composed of hydrophilic carbon black, water repellent carbon black and fluororesin such as PTFE were sequentially stacked and hot pressed, and then a catalyst such as platinum was supported on the reaction layer by a coating method. Are manufactured.
Also, hydrophilic carbon black carrying a catalyst and PTFE
It is also practiced to use a reaction layer sheet made of a fluororesin such as the above, and hot press it together with the gas diffusion layer sheet and the current collector as described above.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、従来の
ガス拡散電極の製造方法では、 300℃以上の温度でプレ
ス時間を30秒以上長くすると、反応層内部のＰＴＦＥ等
のフッ素樹脂が反応層表面に滲み出し、表面の撥水性が
強固になっていた。このため、触媒担持を塗布法により
行なう場合、触媒溶液が反応層表面から内部に浸透せ
ず、触媒が表面にのみ付着して有効に使用できないの
で、電極性能が著しく悪くなる不具合がある。又、触媒
担持の親水性カーボンブラックを用いたガス拡散電極で
は、使用時に電極液の反応層への侵入がなく、触媒と電
解液が接触しないので、同様に電極性能が悪くなる不具
合がある。However, in the conventional method for manufacturing a gas diffusion electrode, when the pressing time is extended for 30 seconds or longer at a temperature of 300 ° C. or higher, the fluororesin such as PTFE inside the reaction layer is not formed on the surface of the reaction layer. Exudation and surface water repellency were strong. For this reason, when the catalyst is supported by the coating method, the catalyst solution does not penetrate from the surface of the reaction layer to the inside, and the catalyst adheres only to the surface and cannot be effectively used. Further, in the gas diffusion electrode using the hydrophilic carbon black supporting the catalyst, there is no invasion of the electrode solution into the reaction layer at the time of use, and the catalyst and the electrolytic solution do not come into contact with each other.
【０００４】かかる不具合に対処するため、図４に示す
ように、集電網21を介在したガス拡散層22に反応層23を
接合し、かつ反応層23の上に親水層24を設けることも勘
案されるているが、結着剤であるＰＴＦＥ等のフッ素樹
脂の量が少なくなるので、親水層24の強度が小さく剥離
し易いと共に、電解液の移動が妨げられるので電極性能
が低下する。又、触媒を塗布法で担持する場合、触媒が
親水層にのみ担持され、必要とする反応層に担持できな
いという欠点があった。そこで、本発明は、反応層の表
面を改質することにより、触媒担持を容易とし、かつ電
解液の反応層への侵入を容易とし得、ひいては電極性能
を高め得るガス拡散電極の製造方法を提供することを目
的とする。In order to deal with such a problem, as shown in FIG. 4, it is also considered that the reaction layer 23 is joined to the gas diffusion layer 22 with the current collecting network 21 interposed and the hydrophilic layer 24 is provided on the reaction layer 23. However, since the amount of the fluororesin such as PTFE as the binder is small, the hydrophilic layer 24 has low strength and is easily peeled off, and the movement of the electrolytic solution is hindered, so that the electrode performance is deteriorated. Further, when the catalyst is supported by the coating method, there is a drawback that the catalyst is supported only on the hydrophilic layer and cannot be supported on the required reaction layer. Therefore, the present invention provides a method for producing a gas diffusion electrode, which can facilitate catalyst loading by modifying the surface of the reaction layer and facilitate invasion of the electrolytic solution into the reaction layer, and thus enhance electrode performance. The purpose is to provide.
【０００５】[0005]
【課題を解決するための手段】前記課題を解決するた
め、本発明のガス拡散電極の製造方法は、ガス拡散層シ
ート、集電網、ガス拡散層シート及び反応層シートを重
ねてホットプレスするガス拡散電極の製造方法におい
て、前記ホットプレス後に反応層表面を水との接触角が
90°未満となるよう、親水化処理することを特徴とす
る。前記親水化処理を、親水性微粒子のスプレーとする
ことが好ましい。前記親水化処理を、親水性微粒子の擦
り込みとしてもよい。又、前記親水化処理を、ブラズマ
処理としてもよい。更に、ガス拡散層シート、集電網、
ガス拡散層シート及び反応層シートを重ねてホットプレ
スするガス拡散電極の製造方法において、前記ホットプ
レス時に反応層シートと接する治具表面に予め親水性微
粒子をスプレーしておくことを特徴とする。なお、ここ
で言う親水性微粒子としては、シリカ、アルミナ、及び
表面に−ＣＯＯＨ等の水と親和性のある活性基を持つ親
水性カーボンブラック等の微粒子が用いられる。In order to solve the above problems, a method for producing a gas diffusion electrode according to the present invention is a gas for hot pressing a gas diffusion layer sheet, a current collecting network, a gas diffusion layer sheet and a reaction layer sheet in a stacked manner. In the method for manufacturing a diffusion electrode, the contact angle with water on the surface of the reaction layer is
It is characterized in that it is subjected to a hydrophilic treatment so that it becomes less than 90 °. The hydrophilic treatment is preferably a spray of hydrophilic fine particles. The hydrophilic treatment may be rubbing of hydrophilic fine particles. The hydrophilic treatment may be plasma treatment. Furthermore, a gas diffusion layer sheet, a current collector,
In the method for producing a gas diffusion electrode in which a gas diffusion layer sheet and a reaction layer sheet are stacked and hot pressed, hydrophilic fine particles are sprayed in advance on the surface of a jig that is in contact with the reaction layer sheet during the hot pressing. As the hydrophilic fine particles, fine particles such as silica, alumina, and hydrophilic carbon black having an active group having an affinity for water such as —COOH on the surface thereof are used.
【０００６】[0006]
【作用】本発明のガス拡散電極の製造方法においては、
反応層の表面が完全に親水性となる。In the method of manufacturing the gas diffusion electrode of the present invention,
The surface of the reaction layer becomes completely hydrophilic.
【０００７】[0007]
【実施例】以下、本発明の実施例について詳細に説明す
る。なお、以下の実施例においても親水性カーボンブラ
ックは表面に−ＣＯＯＨ等の水と親和性のある活性基を
持つもので、水に分散する性質を有し、撥水性カーボン
ブラックはグラファイト化が進行しており、水と親和性
のある活性基を持たず、そのままでは水に分散しないも
のを使用する。EXAMPLES Examples of the present invention will be described in detail below. Also in the following examples, the hydrophilic carbon black has an active group having an affinity for water such as -COOH on the surface and has a property of dispersing in water, and the water-repellent carbon black undergoes graphitization. Therefore, those that do not have active groups having an affinity for water and that do not disperse in water as they are are used.
【０００８】[0008]
【実施例１】治具内に、撥水性カーボンブラックとＰＴ
ＦＥからなる厚さ 0.2mmのガス拡散層シート、集電網と
なるニッケル網、上記のものと同様のガス拡散層シー
ト、及び親水性カーボンブラックと撥水性カーボンブラ
ックとＰＴＦＥかなる厚さ 0.2mmの反応層シートを順に
積み重ね、50kgf/cm2 の圧力、 380℃の温度、10分間の
プレス時間でホットプレスした。得られた反応層１の表
面には、図１に示すように、親水性カーボンブラック２
の粒子間に存在するＰＴＦＥ３が滲み出し、その撥水性
が強固であった。ついで、反応層１の表面を指等で擦る
ことによって、図２に示すように、滲み出したＰＴＦＥ
３が擦り落とされ、表面が親水性となった。そして、反
応層２の表面に、図３に示すように、親水性カーボンブ
ラック、シリカ、アルミナ等の親水性微粒子４を擦り込
んで、表面を完全に親水性とした後、塗布法により反応
層１に白金を触媒として担持させてガス拡散電極を得
た。[Example 1] Water-repellent carbon black and PT were placed in a jig.
A gas diffusion layer sheet made of FE and having a thickness of 0.2 mm, a nickel mesh serving as a current collecting network, a gas diffusion layer sheet similar to the above, and a 0.2 mm thick layer made of hydrophilic carbon black, water repellent carbon black and PTFE. The reaction layer sheets were stacked in order and hot pressed at a pressure of 50 kgf / cm 2 , a temperature of 380 ° C. and a pressing time of 10 minutes. As shown in FIG. 1, hydrophilic carbon black 2 is formed on the surface of the obtained reaction layer 1.
The PTFE 3 existing between the particles was exuded, and its water repellency was strong. Then, by rubbing the surface of the reaction layer 1 with a finger or the like, as shown in FIG.
3 was rubbed off and the surface became hydrophilic. Then, as shown in FIG. 3, hydrophilic fine particles 4 such as hydrophilic carbon black, silica, or alumina are rubbed on the surface of the reaction layer 2 to make the surface completely hydrophilic, and then the reaction layer is applied by a coating method. Platinum was supported on 1 as a catalyst to obtain a gas diffusion electrode.
【０００９】得られたガス拡散電極を、20％のＫＯＨを
電解液とする水素−酸素燃料電池の電極として用いて電
極性能を測定したところ、電池出力は、電圧 0.6Ｖで電
流密度 0.5A/cm2 以上となり、親水化処理をしなかった
従来のもの（電力 0.6Ｖで電流密度0.04A/cm2 ）の12倍
以上であった。The obtained gas diffusion electrode was used as an electrode of a hydrogen-oxygen fuel cell using 20% KOH as an electrolyte, and the electrode performance was measured. The cell output was 0.6 V at a current density of 0.5 A / becomes cm 2 or more, were those of conventional did not hydrophilic treatment (power 0.6V at a current density of 0.04 a / cm 2) of 12 times or more.
【００１０】[0010]
【実施例２】実施例１と同様に反応層の表面のＰＴＦＥ
を擦り落とした後、反応層の表面にＬＢ（Ｌａｎｇｍｕ
ｉｒ Ｂｌｏｄｇｅｔｔ）膜を形成して完全に親水性と
した。ついで、実施例１と同様に塗布法により反応層に
白金を触媒として担持させてガス拡散電極を得、実施例
１と同様にして電極性能を測定したところ、同様の性能
をしめした。Example 2 Similar to Example 1, PTFE on the surface of the reaction layer was used.
After scraping off, LB (Langmu
An ir Bloodgett) film was formed to make it completely hydrophilic. Then, in the same manner as in Example 1, platinum was loaded on the reaction layer as a catalyst by a coating method to obtain a gas diffusion electrode, and the electrode performance was measured in the same manner as in Example 1, and the same performance was shown.
【００１１】[0011]
【実施例３】実施例１と同様にホットプレスした後、反
応層表面をプラズマ処理することにより完全に親水性と
した。ついで、実施例１と同様に塗布法により反応層に
白金を触媒として担持させてガス拡散電極を得、実施例
１と同様にして電極性能を測定したところ、同様の性能
を示した。Example 3 After hot pressing in the same manner as in Example 1, the surface of the reaction layer was treated with plasma to make it completely hydrophilic. Then, in the same manner as in Example 1, platinum was supported as a catalyst on the reaction layer by a coating method to obtain a gas diffusion electrode, and the electrode performance was measured in the same manner as in Example 1, and the same performance was shown.
【００１２】[0012]
【実施例４】実施例１と同様にホットプレスした後、反
応層表面にスプレーで親水性カーボンブラック、シリ
カ、アルミナ等の親水性微粒子を吹き付けて乾燥させて
から、高級アルコール、界面活性剤を小量吹き付けるこ
とにより、完全に親水性とした。界面活性剤は、固体で
内部に浸透しないものが好ましく、かつ加熱時に脱離す
ることが望ましい。ついで、実施例１と同様に塗布法に
より反応層に白金を触媒として担持させてガス拡散電極
を得、実施例１と同様にして電極性能を測定したとこ
ろ、同様の性能を示した。Example 4 After hot pressing in the same manner as in Example 1, the reaction layer surface was sprayed with hydrophilic fine particles of hydrophilic carbon black, silica, alumina, etc. and dried, and then a higher alcohol and a surfactant were added. It was made completely hydrophilic by spraying a small amount. The surfactant is preferably solid and does not penetrate inside, and is preferably desorbed when heated. Then, in the same manner as in Example 1, platinum was supported as a catalyst on the reaction layer by a coating method to obtain a gas diffusion electrode, and the electrode performance was measured in the same manner as in Example 1, and the same performance was shown.
【００１３】[0013]
【実施例５】治具の表面にスプレーで親水性カーボンブ
ラック、シリカ、アルミナ等の親水性微粒子を吹き付け
乾燥させた後、その上に反応層シート、ガス拡散層シー
ト、集電網、及びガス拡散層シートを順に積み重ね、実
施例１と同様の条件でホットプレスし、余分を親水性微
粒子を除いた。ついで、実施例１と同様に塗布法により
反応層に白金を触媒として担持させてガス拡散電極を
得、実施例１と同様にして電極性能を測定したところ、
同様の性能を示した。なお、上記実施例において白金触
媒を反応層に前もって担持しておいてからホットプレス
しても、上記と同様の結果がえられた。[Example 5] After spraying hydrophilic fine particles of hydrophilic carbon black, silica, alumina, etc. onto the surface of the jig by spraying and drying, a reaction layer sheet, a gas diffusion layer sheet, a current collecting network, and a gas diffusion layer were formed on the surface. The layered sheets were stacked in order and hot pressed under the same conditions as in Example 1 to remove the excess hydrophilic fine particles. Then, in the same manner as in Example 1, platinum was supported on the reaction layer as a catalyst by a coating method to obtain a gas diffusion electrode, and the electrode performance was measured in the same manner as in Example 1,
It showed similar performance. In addition, the same results as above were obtained by hot pressing after loading the platinum catalyst on the reaction layer in the above-mentioned example.
【００１４】[0014]
【発明の効果】以上説明したように、本発明のガス拡散
電極の製造方法によれば、反応層の表面が水との接触角
90°未満の親水性となるので、塗布法による反応層に対
する触媒担持を容易に行なうことができると共に、触媒
担持の親水性カーボンブラックを用いたものでも、反応
層に対する電解液の侵入を容易とすることができ、ひい
ては電極性能を高くすることができる。As described above, according to the method for producing a gas diffusion electrode of the present invention, the surface of the reaction layer has a contact angle with water.
Since it has a hydrophilicity of less than 90 °, it is possible to easily carry the catalyst to the reaction layer by the coating method, and even if the catalyst-supporting hydrophilic carbon black is used, the penetration of the electrolytic solution into the reaction layer is facilitated. It is possible to improve the electrode performance.
【図１】本発明のガス拡散電極の製造方法の一実施例を
示す各工程の断面説明図である。FIG. 1 is a cross-sectional explanatory view of each step showing an embodiment of a method for manufacturing a gas diffusion electrode of the present invention.
【図２】本発明のガス拡散電極の製造方法の一実施例を
示す各工程の断面説明図である。FIG. 2 is a cross-sectional explanatory diagram of each step showing one embodiment of the method for manufacturing a gas diffusion electrode of the present invention.
【図３】本発明のガス拡散電極の製造方法の一実施例を
示す各工程の断面説明図である。FIG. 3 is a cross-sectional explanatory diagram of each step showing one embodiment of the method for manufacturing the gas diffusion electrode of the present invention.
【図４】従来の方法によるガス拡散電極の断面図であ
る。FIG. 4 is a cross-sectional view of a gas diffusion electrode according to a conventional method.
１ 反応層 ２ 親水性カーボンブラック ３ ＰＴＦＥ ４ 親水性微粒子 1 Reaction Layer 2 Hydrophilic Carbon Black 3 PTFE 4 Hydrophilic Fine Particles
Claims (5)
ート及び反応層シートを重ねてホットプレスするガス拡
散電極の製造方法において、前記ホットプレス後に反応
層表面を水との接触角が90°未満となるよう親水化処理
することを特徴とするガス拡散電極の製造方法。1. A method for producing a gas diffusion electrode in which a gas diffusion layer sheet, a current collecting network, a gas diffusion sheet and a reaction layer sheet are stacked and hot-pressed, and the contact angle of the reaction layer surface with water after hot-pressing is 90 °. A method for producing a gas diffusion electrode, which is characterized in that a hydrophilic treatment is performed so that the amount becomes less than the above.
レーとすることを特徴とする請求項１記載のガス拡散電
極の製造方法。2. The method for producing a gas diffusion electrode according to claim 1, wherein the hydrophilic treatment is spraying of hydrophilic fine particles.
込みとすることを特徴とする請求項１記載のガス拡散電
極の製造方法。3. The method for producing a gas diffusion electrode according to claim 1, wherein the hydrophilic treatment is rubbing of hydrophilic fine particles.
ことを特徴とする請求項１記載のガス拡散電極の製造方
法。4. The method for producing a gas diffusion electrode according to claim 1, wherein the hydrophilic treatment is a plasma treatment.
シート及び反応層シートを重ねてホットプレスするガス
拡散電極の製造方法において、前記ホットプレス時に反
応層シートを接する治具表面に予め親水性微粒子をスプ
レーしておくことを特徴とするガス拡散電極の製造方
法。5. A method for manufacturing a gas diffusion electrode, comprising stacking a gas diffusion layer sheet, a current collecting net, a gas diffusion layer sheet and a reaction layer sheet and hot-pressing them, wherein the jig surface which is in contact with the reaction layer sheet at the time of hot pressing is previously hydrophilic. A method for producing a gas diffusion electrode, which comprises spraying fine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6015797A JPH07211329A (en) | 1994-01-14 | 1994-01-14 | Method for manufacturing gas diffusion electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6015797A JPH07211329A (en) | 1994-01-14 | 1994-01-14 | Method for manufacturing gas diffusion electrode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07211329A true JPH07211329A (en) | 1995-08-11 |
Family
ID=11898839
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6015797A Pending JPH07211329A (en) | 1994-01-14 | 1994-01-14 | Method for manufacturing gas diffusion electrode |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07211329A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003059506A (en) * | 2001-08-16 | 2003-02-28 | Mitsubishi Electric Corp | Electrochemical element and electrochemical element device |
| JP2004031326A (en) * | 2002-04-12 | 2004-01-29 | Sgl Carbon Ag | Carbon fiber electrode substrate for electrochemical cells |
| JP2007506250A (en) * | 2003-09-18 | 2007-03-15 | スリーエム イノベイティブ プロパティズ カンパニー | Fuel cell gas diffusion layer |
| KR101107076B1 (en) * | 2006-03-03 | 2012-01-20 | 삼성에스디아이 주식회사 | Membrane-electrode assembly for fuel cell and fuel cell system comprising same |
| JP2022521156A (en) * | 2019-02-13 | 2022-04-06 | フラウンホーファー－ゲゼルシャフト ツァー フェルデルング デア アンゲヴァンテン フォーシャング アインゲトラーゲナー フェアアイン | A method for hydrophilizing a semi-finished device and an electrode element, bipolar element, or heat exchange element manufactured from the semi-finished device. |
-
1994
- 1994-01-14 JP JP6015797A patent/JPH07211329A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003059506A (en) * | 2001-08-16 | 2003-02-28 | Mitsubishi Electric Corp | Electrochemical element and electrochemical element device |
| JP2004031326A (en) * | 2002-04-12 | 2004-01-29 | Sgl Carbon Ag | Carbon fiber electrode substrate for electrochemical cells |
| JP2007506250A (en) * | 2003-09-18 | 2007-03-15 | スリーエム イノベイティブ プロパティズ カンパニー | Fuel cell gas diffusion layer |
| JP2012212686A (en) * | 2003-09-18 | 2012-11-01 | Three M Innovative Properties Co | Fuel cell gas diffusion layer |
| EP1668729B1 (en) * | 2003-09-18 | 2018-04-25 | 3M Innovative Properties Company | Fuel cell gas diffusion layer |
| KR101107076B1 (en) * | 2006-03-03 | 2012-01-20 | 삼성에스디아이 주식회사 | Membrane-electrode assembly for fuel cell and fuel cell system comprising same |
| JP2022521156A (en) * | 2019-02-13 | 2022-04-06 | フラウンホーファー－ゲゼルシャフト ツァー フェルデルング デア アンゲヴァンテン フォーシャング アインゲトラーゲナー フェアアイン | A method for hydrophilizing a semi-finished device and an electrode element, bipolar element, or heat exchange element manufactured from the semi-finished device. |
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