JP3126349B2 - Manufacturing method of gas diffusion electrode - Google Patents
Manufacturing method of gas diffusion electrodeInfo
- Publication number
- JP3126349B2 JP3126349B2 JP11102914A JP10291499A JP3126349B2 JP 3126349 B2 JP3126349 B2 JP 3126349B2 JP 11102914 A JP11102914 A JP 11102914A JP 10291499 A JP10291499 A JP 10291499A JP 3126349 B2 JP3126349 B2 JP 3126349B2
- Authority
- JP
- Japan
- Prior art keywords
- mixer
- dispersion
- gas diffusion
- diffusion electrode
- dispersion liquid
- 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.)
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Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【発明の属する技術分野】本発明は、燃料電池、食塩電
解の酸素陰極等に用いるガス拡散電極の製造方法に関
し、特にガス供給層と反応層とを連続して製造すること
ができるガス拡散電極の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a gas diffusion electrode used for a fuel cell, an oxygen cathode for salt electrolysis, etc., and more particularly to a gas diffusion electrode capable of continuously manufacturing a gas supply layer and a reaction layer. And a method for producing the same.
【０００２】[0002]
【従来の技術】ガス拡散電極は、通常、反応層とガス供
給層とが積層してなる。ガス拡散電極の反応層、ガス供
給層は、その製造にあたりポリテトラフルオロエチレン
（ＰＴＦＥ）を含むそれぞれの原料分散液をアルコール
で自己組織化させ、それを濾過して塗布するという工程
で製膜していた。2. Description of the Related Art Generally, a gas diffusion electrode is formed by laminating a reaction layer and a gas supply layer. The reaction layer and gas supply layer of the gas diffusion electrode are formed by self-organizing each raw material dispersion containing polytetrafluoroethylene (PTFE) with alcohol in the production thereof, filtering and coating the dispersion. I was
【０００３】[0003]
【発明が解決しようとする課題】アルコールで自己組織
化させた場合、ＰＴＦＥは凝集力が大きいので分散液は
餅状になりやすい。餅状の分散液はヘラで塗りつけない
と製膜できない。そのため、従来は、アルコールで自己
組織化させて濾過し、餅状の濾過物を所定の基体上にへ
らでこしりつけて製膜する。この製膜法は工程が複雑で
熟練を要するという欠点があった。このため製造法の簡
略化が求められていた。そこで本発明は、工程が簡単で
ほとんど熟練を要しないガス拡散電極の製造方法を提供
することを目的とする。When self-assembled with alcohol, PTFE has a large cohesive force, so that the dispersion liquid tends to be rice cake-like. A mochi-like dispersion cannot be formed unless it is applied with a spatula. For this reason, conventionally, self-assembly with alcohol is performed, followed by filtration. This film forming method has the drawback that the process is complicated and requires skill. Therefore, simplification of the manufacturing method has been required. Therefore, an object of the present invention is to provide a method for manufacturing a gas diffusion electrode that has a simple process and requires little skill.
【０００４】[0004]
【課題を解決するための手段】本発明は、以下の手段に
より上記の課題を解決した。 （１）親水部分散液と疎水部分散液とを、供給量を制御
しながら混合器に送り込み、混合器から出た混合液をス
プレーし、ガス供給層と反応層とをどちらか一方を先に
して両者を順次製膜することを特徴とするガス拡散電極
の製造方法。 （２）親水部分散液と疎水部分散液とを供給量を制御し
ながら第一混合器に送り込み、得られた第一段の混合液
と自己組織化剤とを第二混合器に送り込み、第二混合器
から出た混合液をスプレーして製膜することを特徴とす
るガス拡散電極の製造方法。 （３）該スプレーは、被スプレー基体の温度を８０℃以
上３００℃以下に加熱した処に行う前記（１）又は
（２）に記載のガス拡散電極の製造方法。The present invention has solved the above-mentioned problems by the following means. (1) The hydrophilic part dispersion liquid and the hydrophobic part dispersion liquid are fed into a mixer while controlling the supply amounts, and the mixture liquid discharged from the mixer is sprayed, and one of the gas supply layer and the reaction layer is placed first. A method for producing a gas diffusion electrode, comprising: (2) The hydrophilic part dispersion liquid and the hydrophobic part dispersion liquid are fed into the first mixer while controlling the supply amounts, and the obtained first-stage liquid mixture and the self-organizing agent are fed into the second mixer, A method for producing a gas diffusion electrode, comprising spraying a liquid mixture discharged from a second mixer to form a film . (3) The method for producing a gas diffusion electrode according to (1) or (2), wherein the spraying is performed at a temperature where the temperature of the substrate to be sprayed is heated to 80 ° C or more and 300 ° C or less.
【０００５】上記の手段では、ガス拡散電極の疎水部分
散液及び親水部分散液とを混合器にそれぞれの供給量を
制御しながら送り込み、スプレーすることで、反応層、
ガス供給層を連続的に製膜する。更に自己組織化剤との
混合器を付ければ、自己組織化した反応層材料、ガス供
給層材料を霧化することで連続して製膜できる。こうし
た方法は、必要があれば、例えば疎水部分散液の供給量
を徐々に減らし、同時に親水部分散液の供給量を徐々に
増加させるようにして、反応層の親水部、疎水部の組成
を傾斜組成にすることもできる。[0005] In the above means, the hydrophobic part dispersion liquid and the hydrophilic part dispersion liquid of the gas diffusion electrode are fed into the mixer while controlling the respective supply amounts, and sprayed, so that the reaction layer,
The gas supply layer is formed continuously. Furthermore, if a mixer with a self-organizing agent is attached, the film can be continuously formed by atomizing the self-assembled reaction layer material and gas supply layer material. Such a method, if necessary, for example, gradually reduces the supply amount of the hydrophobic part dispersion, and at the same time, gradually increases the supply amount of the hydrophilic part dispersion, thereby changing the composition of the hydrophilic part and the hydrophobic part of the reaction layer. A gradient composition can also be used.
【０００６】[0006]
【発明の実施の形態】親水部分散液は、銀等の触媒を担
持した親水性カーボンブラックをトライトン（界面活性
剤）で分散させ、さらにＰＴＦＥディスパージョンを加
える。また、銀微粒子とＰＴＦＥディスパージョンとの
混合物等の液体状となる分散液でも良い。疎水部分散液
は、疎水性カーボンブラックをトライトンで分散させ、
ＰＴＦＥディスパーションを加えて作る。これらの分散
液を、例えばローラーポンプでそれぞれの供給量を制御
しながら混合器に導入する。混合器から出た混合液を直
ちにスプレーする。必要なら無機塩水溶液を自己組織化
剤として用いてもよい。スプレーする方法としてはエア
スプレー法、エアレススプレー法、エア霧化静電法、回
転霧化静電法など使用できる。スプレー時、被スプレー
物の温度を制御する事で塗膜の状態を変えることが出来
る。また、自己組織化剤と混合した後、スプレーするた
めに新たに混合器を増設しても良い。混合器の温度を上
下することで自己組織化状態を制御することもできる。
スプレーガスの温度を上げると製膜速度を上げることが
できる。BEST MODE FOR CARRYING OUT THE INVENTION A hydrophilic part dispersion is prepared by dispersing a hydrophilic carbon black carrying a catalyst such as silver with Triton (a surfactant), and further adding a PTFE dispersion. Also, a liquid dispersion such as a mixture of silver fine particles and PTFE dispersion may be used. Hydrophobic part dispersion liquid disperses hydrophobic carbon black with Triton,
Make by adding PTFE dispersion. These dispersions are introduced into a mixer while controlling the respective supply amounts by, for example, a roller pump. Spray the mixture from the mixer immediately. If necessary, an inorganic salt aqueous solution may be used as a self-organizing agent. As a method of spraying, an air spray method, an airless spray method, an air atomization electrostatic method, a rotary atomization electrostatic method, or the like can be used. During spraying, the state of the coating film can be changed by controlling the temperature of the object to be sprayed. After mixing with the self-organizing agent, a new mixer may be additionally provided for spraying. The self-assembled state can be controlled by raising and lowering the temperature of the mixer.
Increasing the temperature of the spray gas can increase the film forming speed.
【０００７】図１は、本発明の方法を実施した際の概念
図である。この場合は、第一混合器と第二混合器を使用
して自己組織化液をも混合するものである。吸入口２と
吸入口３を有する第一混合器１を設け、吸入口２は親水
部分散液槽（図示しない）に通じ、別の吸入口３は疎水
部分散液槽（図示しない）に通じてある。第一混合器１
の吐出口は、別の第二混合器４の吸入口５に通じ、第二
混合器４の吸入口６はイソプロピルアルコール槽に通じ
ている。第二混合器４の吐出口７は、その吐出方向に直
角の方向に噴出方向を有する高圧ガスノズル８の噴出口
と互いの口をつき合わせている。FIG. 1 is a conceptual diagram when the method of the present invention is performed. In this case, the self-organizing liquid is also mixed using the first mixer and the second mixer. A first mixer 1 having a suction port 2 and a suction port 3 is provided. The suction port 2 communicates with a hydrophilic part dispersion tank (not shown), and another suction port 3 communicates with a hydrophobic part dispersion tank (not shown). It is. First mixer 1
Is connected to a suction port 5 of another second mixer 4, and a suction port 6 of the second mixer 4 is connected to an isopropyl alcohol tank. The discharge port 7 of the second mixer 4 is in contact with the discharge port of the high-pressure gas nozzle 8 having a discharge direction perpendicular to the discharge direction.
【０００８】[0008]
【実施例】以下、実施例により本発明を具体的に説明す
る。ただし本発明はこれらの実施例のみに限定されるも
のではない。The present invention will be described below in detail with reference to examples. However, the present invention is not limited to only these examples.
【０００９】実施例１ 平均粒径０．１５ミクロンのジルコニア微粒子２０ｇを
１リットル水溶液中に分散させ、硝酸銀３５ｇ、ホルマ
リン、苛性ソーダを加えることで銀をジルコニア微粒子
に担持した。銀を担持したジルコニア微粒子４部（重
量、以下同様）にトライトン（界面活性剤）を１部，水
９部を加え、超音波分散機で前記ジルコニア微粒子を分
散させる。次いでこれにＰＴＦＥディスパージョンＤ−
１（ダイキン工業社製）１部を加え、撹拌混合し、親水
部分散液を作製する。疎水性カーボンブラック（Ｎｏ．
６、平均粒径５００Å、試作品、電気化学工業社製）６
部に濃度２％のトライトン水溶液を２００部とＰＴＦＥ
ディスパージョン（Ｄ−１（ダイキン工業社製）４部と
を分散させ、疎水部分散液を作った。Example 1 20 g of zirconia fine particles having an average particle diameter of 0.15 μm were dispersed in a 1-liter aqueous solution, and silver was carried on the zirconia fine particles by adding 35 g of silver nitrate, formalin and caustic soda. One part of Triton (surfactant) and 9 parts of water are added to 4 parts (weight, the same applies hereinafter) of zirconia fine particles carrying silver, and the zirconia fine particles are dispersed by an ultrasonic dispersing machine. Next, PTFE dispersion D-
1 part (manufactured by Daikin Industries, Ltd.) is added and stirred and mixed to prepare a hydrophilic part dispersion liquid. Hydrophobic carbon black (No.
6, average particle size 500 mm, prototype, manufactured by Denki Kagaku Kogyo)
200 parts of 2% aqueous triton solution and PTFE
4 parts of the dispersion (D-1 (manufactured by Daikin Industries, Ltd.)) was dispersed to prepare a hydrophobic part dispersion liquid.
【００１０】このようにして得られた親水部分散液と疎
水部分散液とをそれぞれローラーポンプを介して混合器
に接続させ、混合器の出口はスプレーに接続した。始め
に親水部分散液のみを混合器に送り込み、所定の基体上
に薄膜を形成した後、疎水部分散液も混合器に送り込
み、スプレーすることで反応層を形成する。徐々に疎水
部分散液の割合を多くして、反応層の組成を傾斜させ
る。最後に親水部分散液の送りを止め、疎水部分散液の
みをスプレーしてガス供給層を形成させた。スプレーす
る速度は基体上に液だれしない程度とする。基体は加熱
しているとスプレー速度を速めることが出来る。スプレ
ー後、形成された膜を８０℃で乾燥し、ロールをかけて
圧縮した後、エタノール抽出器で界面活性剤を除去す
る。８０℃で３時間乾燥し、銀網と共にプレスする。プ
レス温度３５０℃、プレス圧４０ｋｇ／ｃｍ2 、３０秒
間プレスする事でガス拡散電極を得た。得られたこの電
極の酸素還元性能を測定したところ、電流密度３０Ａ／
ｄｍ2で０．８３Ｖ（ｖｓ．ＲＨＥ）の高い性能が得ら
れた。The thus obtained dispersion of hydrophilic part and dispersion of hydrophobic part were each connected to a mixer via a roller pump, and the outlet of the mixer was connected to a spray. First, only the hydrophilic part dispersion is sent to the mixer to form a thin film on a predetermined substrate, and then the hydrophobic part dispersion is also sent to the mixer and sprayed to form a reaction layer. The composition of the reaction layer is inclined by gradually increasing the ratio of the hydrophobic part dispersion liquid. Finally, the supply of the hydrophilic part dispersion liquid was stopped, and only the hydrophobic part dispersion liquid was sprayed to form a gas supply layer. The spray speed is such that it does not drip onto the substrate. When the substrate is heated, the spray speed can be increased. After spraying, the formed membrane is dried at 80 ° C., rolled and compressed, and then the surfactant is removed with an ethanol extractor. Dry at 80 ° C. for 3 hours and press with silver screen. A gas diffusion electrode was obtained by pressing at a pressing temperature of 350 ° C. and a pressing pressure of 40 kg / cm 2 for 30 seconds. When the oxygen reduction performance of the obtained electrode was measured, the current density was 30 A /
A high performance of 0.83 V (vs. RHE) was obtained at dm 2 .
【００１１】実施例２ 粒径０．１ミクロンの銀コロイド（田中貴金属社製、試
作品）を２０％濃度で含む水溶液２５部に、２０％濃度
のトライトン水溶液３部とＰＴＦＥディスパージョン
（Ｄ−１，ダイキン工業社製）１部とを分散させ、親水
部分散液を作った。別に、疎水性カーボンブラック（Ｎ
ｏ．６、平均粒径５００Å、試作品、電気化学工業社
製）２部に２％濃度のトライトン水溶液を５０部とＰＴ
ＦＥディスパージョン（Ｄ−１，ダイキン工業社製）
１．３部とを分散させて疎水部分散液を作った。Example 2 In 25 parts of an aqueous solution containing a 20% concentration of a silver colloid (produced by Tanaka Kikinzoku Co., Ltd.) having a particle size of 0.1 micron, 3 parts of a 20% concentration triton aqueous solution and PTFE dispersion (D- 1 (manufactured by Daikin Industries, Ltd.) to obtain a hydrophilic part dispersion. Separately, hydrophobic carbon black (N
o. 6, average particle size 500 mm, prototype, manufactured by Denki Kagaku Kogyo Co., Ltd.)
FE dispersion (D-1, manufactured by Daikin Industries, Ltd.)
1.3 parts were dispersed to prepare a hydrophobic part dispersion liquid.
【００１２】図１に示す混合器を用いて、親水部分散液
と疎水部分散液をスプレーした。親水部分散液と疎水部
分散液をローラーポンプでそれぞれ第一混合器１に供給
量を制御しながら送り込む。混合された分散液を更に別
の第二混合器４に入れ、イソプロピルアルコールと合流
させ自己組織化させ、自己組織化した分散液をスプレー
する。スプレーは次のようにする。まず、１２０℃に加
熱した熱板上にアルミ箔を敷き、このアルミ箔上に親水
部分散夜のみを薄くスプレーする。次に親水部分散夜と
疎水部分散夜が９：１（厚さ１０ミクロン）、７：３
（１２０ミクロン）、３：７（２０ミクロン）、０：１
０（３００ミクロン）と比率を変えてスプレーした。ス
プレー中に熱板の温度を上下し、堆積物が平滑になるよ
うに膜厚を制御した。The dispersion of the hydrophilic part and the dispersion of the hydrophobic part were sprayed using the mixer shown in FIG. The hydrophilic part dispersion liquid and the hydrophobic part dispersion liquid are fed into the first mixer 1 by a roller pump while controlling the supply amounts. The mixed dispersion is put into another second mixer 4, combined with isopropyl alcohol, self-organized, and the self-organized dispersion is sprayed. Spray as follows. First, an aluminum foil is laid on a hot plate heated to 120 ° C., and only the hydrophilic portion dispersed night is sprayed thinly on the aluminum foil. Next, the hydrophilic part dispersion night and the hydrophobic part dispersion night were 9: 1 (thickness 10 microns), 7: 3.
(120 microns), 3: 7 (20 microns), 0: 1
Spraying was performed at a different ratio of 0 (300 microns). During spraying, the temperature of the hot plate was raised and lowered, and the film thickness was controlled so that the deposits became smooth.
【００１３】熱板の温度が高いと凹凸面になるのでロー
ラ等で平滑化する必要がある。しかし、親水部と疎水部
の入り組んだ構造にするときには好都合である。スプレ
ー後、８０℃で乾燥し、得られたシートに常温下、４０
ｋｇ／ｃｍ2 の圧力を加えてプレスして形状を固めた
後、エタノール抽出器で界面活性剤を除去する。８０℃
で３時間乾燥し、銀網と共に３５０℃、４０ｋｇ／ｃｍ
2 圧力下、３０秒間プレスする事でガス拡散電極を得
た。この電極の酸素還元性能を測定したところ、電流密
度３０Ａ／ｄｍ2 で電解電圧０．８３Ｖ（ｖｓ，ＲＨ
Ｅ）という高い性能が得られた。If the temperature of the hot plate is high, the surface becomes uneven, so it is necessary to smooth it with a roller or the like. However, it is convenient to make the structure in which the hydrophilic part and the hydrophobic part are complicated. After spraying, it was dried at 80 ° C.
After applying a pressure of kg / cm 2 and pressing to harden the shape, the surfactant is removed with an ethanol extractor. 80 ℃
At 350 ° C, 40 kg / cm with silver screen
A gas diffusion electrode was obtained by pressing under 2 pressures for 30 seconds. When the oxygen reduction performance of this electrode was measured, the electrolysis voltage was 0.83 V (vs, RH) at a current density of 30 A / dm 2.
High performance E) was obtained.
【００１４】[0014]
【発明の効果】本発明によれば、工程が簡単で、ほとん
ど熟練を要しない手段によりガス拡散電極の製造方法を
提供することができる。親水部分散液と疎水部分散液の
供給量を制御する事で反応層とガス供給層を連続して製
膜することにより、親水部と疎水部の組成が傾斜組成と
なった層を形成することができる。電極の製作工程が簡
略化され、生産性が増大した。これにより、初期性能と
寿命の両立した電極が作製できる。According to the present invention, it is possible to provide a method for manufacturing a gas diffusion electrode by means which has a simple process and requires little skill. By controlling the supply amounts of the hydrophilic part dispersion liquid and the hydrophobic part dispersion liquid, the reaction layer and the gas supply layer are continuously formed to form a layer in which the composition of the hydrophilic part and the hydrophobic part has a gradient composition. be able to. The manufacturing process of the electrode was simplified, and the productivity was increased. Thereby, an electrode having both initial performance and lifetime can be manufactured.
【図１】ガス拡散電極を製造する混合器の例を示す概念
図である。FIG. 1 is a conceptual diagram showing an example of a mixer for producing a gas diffusion electrode.
１ 第一混合器 ２ 吸入口 ３ 吸入口 ４ 第二混合器 ５ 吸入口 ６ 吸入口 ７ 吐出口 ８ 高圧ガスノズル DESCRIPTION OF SYMBOLS 1 First mixer 2 Suction port 3 Suction port 4 Second mixer 5 Suction port 6 Suction port 7 Discharge port 8 High pressure gas nozzle
───────────────────────────────────────────────────── フロントページの続き (72)発明者 古屋 長一 山梨県甲府市中村町２−14 (56)参考文献 特開 平６−316784（ＪＰ，Ａ) 特開 平11−80985（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C25B 1/00 - 15/08 ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Choichi Furiya 2-14 Nakamura-cho, Kofu City, Yamanashi Prefecture (56) References JP-A-6-316784 (JP, A) JP-A-11-80985 (JP, A) (58) Fields surveyed (Int. Cl. 7 , DB name) C25B 1/00-15/08
Claims (3)
量を制御しながら混合器に送り込み、混合器から出た混
合液をスプレーし、ガス供給層と反応層とをどちらか一
方を先にして両者を順次製膜することを特徴とするガス
拡散電極の製造方法。1. A dispersion of a hydrophilic part and a dispersion of a hydrophobic part are fed into a mixer while controlling the supply amounts, and the mixture discharged from the mixer is sprayed, and one of the gas supply layer and the reaction layer is separated. A method for producing a gas diffusion electrode, characterized in that both are sequentially formed into a film.
を制御しながら第一混合器に送り込み、得られた第一段
の混合液と自己組織化剤とを第二混合器に送り込み、第
二混合器から出た混合液をスプレーして製膜することを
特徴とするガス拡散電極の製造方法。2. The hydrophilic part dispersion liquid and the hydrophobic part dispersion liquid are fed into the first mixer while controlling the supply amounts, and the obtained first-stage mixture and the self-organizing agent are added to the second mixer. A method for producing a gas diffusion electrode, comprising: forming a film by spraying a mixed solution that has been fed and discharged from a second mixer.
８０℃以上３００℃以下に加熱した処に行う請求項１又
は請求項２に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 spraying is performed at a temperature where the temperature of the substrate to be sprayed is heated to 80 ° C. or more and 300 ° C. or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11102914A JP3126349B2 (en) | 1999-04-09 | 1999-04-09 | Manufacturing method of gas diffusion electrode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11102914A JP3126349B2 (en) | 1999-04-09 | 1999-04-09 | Manufacturing method of gas diffusion electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000297394A JP2000297394A (en) | 2000-10-24 |
| JP3126349B2 true JP3126349B2 (en) | 2001-01-22 |
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| DE102010024053A1 (en) * | 2010-06-16 | 2011-12-22 | Bayer Materialscience Ag | Oxygenating electrode and process for its preparation |
| JP5548296B1 (en) * | 2013-09-06 | 2014-07-16 | ペルメレック電極株式会社 | Method for producing electrode for electrolysis |
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