JPH0243830B2 - - Google Patents
Info
- Publication number
- JPH0243830B2 JPH0243830B2 JP58035530A JP3553083A JPH0243830B2 JP H0243830 B2 JPH0243830 B2 JP H0243830B2 JP 58035530 A JP58035530 A JP 58035530A JP 3553083 A JP3553083 A JP 3553083A JP H0243830 B2 JPH0243830 B2 JP H0243830B2
- Authority
- JP
- Japan
- Prior art keywords
- electrode
- exchange membrane
- ion exchange
- gas
- chemical plating
- 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.)
- Expired - Lifetime
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
-
- 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
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inert Electrodes (AREA)
Description
【発明の詳細な説明】
本発明は、イオン交換膜と電極とを一体にに接
合する方法に係り、特に電極がガス拡散電極の場
合に電極とイオン交換膜との接触抵抗を小ならし
めんとするにある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for integrally joining an ion exchange membrane and an electrode, and particularly to a method for reducing the contact resistance between the electrode and the ion exchange membrane when the electrode is a gas diffusion electrode. There it is.
近年、イオン交換膜、特にパーフルオロカーボ
ンを基体にしたカチオン交換膜に電極を一体に接
合したタイプの電気化学装置に関する技術が飛躍
的に進歩してきている。 In recent years, technology regarding electrochemical devices of the type in which an electrode is integrally bonded to an ion exchange membrane, particularly a cation exchange membrane based on perfluorocarbon, has been rapidly progressing.
このタイプの電気化学装置としては、水電解装
置、燃料電池、酸素濃縮装置、脱酸素装置、食塩
電解装置、塩化カリ電解装置、塩酸電解装置など
がある。 This type of electrochemical device includes a water electrolysis device, a fuel cell, an oxygen concentrator, a deoxygenation device, a salt electrolysis device, a potassium chloride electrolysis device, a hydrochloric acid electrolysis device, and the like.
これらの電気化学装置はガス電極から発生する
場合、ガスが電極に外部から供給される場合、あ
るいは一対の電極の一方からガスが発生し、他方
にはガスが供給される場合の３種類に分類でき
る。 These electrochemical devices are classified into three types: those in which the gas is generated from a gas electrode, those in which the gas is supplied to the electrode from the outside, or those in which the gas is generated from one of a pair of electrodes and the gas is supplied to the other. can.
ガスが一対の電極の双方から発生する電気化学
装置としては、水電解装置、食塩電解装置、塩化
カリ電解装置および塩酸電解装置がある。ガスが
陰極、陽極の双方に供給される電気化学装置は燃
料電池である。これに対して、陰極にガス、特に
空気が供給され、陽極からガスが発生する電気化
学装置としては、酸素濃縮装置、脱酸素装置があ
る。そして、塩酸電解装置を陰極に空気を供給
し、陽極から塩素だけを発生させるタイプのもの
にすれば、この最後の種類に分類することができ
る。 Electrochemical devices in which gas is generated from both of a pair of electrodes include water electrolyzers, salt electrolyzers, potassium chloride electrolyzers, and hydrochloric acid electrolyzers. An electrochemical device in which gas is supplied to both the cathode and the anode is a fuel cell. On the other hand, electrochemical devices in which gas, especially air, is supplied to the cathode and gas is generated from the anode include oxygen concentrators and deoxidizers. If the hydrochloric acid electrolyzer is of a type that supplies air to the cathode and generates only chlorine from the anode, it can be classified into this last type.
いずれにしても、電極だけについていうなら
ば、ガスが電極から発生するタイプの電極とガス
が外部から供給されるタイプの電極とに分類する
ことができ、前者はガス発生電極といわれ、後者
はガス拡散電極といわれる。 In any case, when it comes to electrodes alone, they can be classified into electrodes where gas is generated from the electrode and electrodes where gas is supplied from outside.The former is called a gas-generating electrode, and the latter is a gas-generating electrode. It is called a gas diffusion electrode.
本発明は後者のガス拡散電極を特に対象とした
場合のイオン交換膜と電極との接合法に関するも
のである。 The present invention relates to a method of bonding an ion exchange membrane and an electrode, particularly targeting the latter gas diffusion electrode.
従来、イオン交換膜に電極を一体に接合する方
法としては、例えば特開昭55−38934号に提案さ
れているように、イオン交換膜の片面に触媒金属
の化合物の塩の水溶液を接触させ、他面に還元剤
の水溶液を接触させることによつて、イオン交換
膜の片面に触媒金属を析出させ、この析出した触
媒金属を電極とする化学メツキ法がある。この化
学メツキ法によつて得られる電極は、ガス発生電
極としては好適であり、イオン交換膜と電極との
接触抵抗も小さいが、ガス拡散電極、特に酸素の
電解還元反応に与かるいわゆる酸素極としてはほ
とんど働かない。これはイオン交換膜がプロトン
伝導性を示すカチオン交換膜の場合には酸素極で
は、O2＋4H+＋4e-→2H2O
なる反応によつて、水が生成し、この水が電極の
細孔を満たして、酸素が反応サイトである電極と
イオン交換膜との界面まで到達するのを妨害する
からである。 Conventionally, as a method of integrally bonding an electrode to an ion exchange membrane, for example, as proposed in JP-A-55-38934, one side of the ion exchange membrane is brought into contact with an aqueous solution of a salt of a catalytic metal compound. There is a chemical plating method in which a catalytic metal is deposited on one side of an ion exchange membrane by contacting the other side with an aqueous solution of a reducing agent, and the precipitated catalytic metal is used as an electrode. The electrode obtained by this chemical plating method is suitable as a gas generation electrode and has low contact resistance between the ion exchange membrane and the electrode, but it is also suitable as a gas diffusion electrode, especially a so-called oxygen electrode that takes part in the electrolytic reduction reaction of oxygen. It hardly works as such. This is because when the ion exchange membrane is a cation exchange membrane that exhibits proton conductivity, water is generated at the oxygen electrode through the reaction O 2 +4H + +4e - →2H 2 O, and this water flows into the pores of the electrode. This is because it prevents oxygen from reaching the reaction site, which is the interface between the electrode and the ion exchange membrane.
一方、その他のイオン交換膜と電極との一体接
合法としては、例えば特開昭54−107493号に提案
されているように、イオン交換膜に触媒金属粉末
と撥水性結合剤との混合物を加熱圧着するという
加熱圧着法がある。この加熱圧着法によつて得ら
れる電極は、撥水性結着剤が電極細孔の水の充満
を阻止し、反応ガスの拡散がスムースにおこなわ
れるので、ガス拡散電極として良好に働く。しか
し一般に、イオン交換膜表面に、触媒金属粒子と
結着剤粒子との双方が接合するため、前述の化学
メツキ法に比較すると触媒金属粒子とイオン交換
膜との接触面積が相対的に小さくなるので、イオ
ン交換膜と電極との接触抵抗が相対的に大きくな
り、電気化学装置とした場合の電圧損失につなが
るという難点がみられた。 On the other hand, as another method of integrally bonding an ion exchange membrane and an electrode, for example, as proposed in JP-A-54-107493, a mixture of catalyst metal powder and water-repellent binder is heated on the ion exchange membrane. There is a heat compression bonding method called crimping. The electrode obtained by this heat-press bonding method works well as a gas diffusion electrode because the water-repellent binder prevents the electrode pores from being filled with water and the reaction gas is diffused smoothly. However, since both catalyst metal particles and binder particles are generally bonded to the ion exchange membrane surface, the contact area between the catalyst metal particles and the ion exchange membrane is relatively small compared to the chemical plating method described above. Therefore, the contact resistance between the ion-exchange membrane and the electrode becomes relatively large, which leads to voltage loss when used as an electrochemical device.
本発明は、化学メツキ法と加熱圧着法の双方の
組合わせによつてイオン交換膜と電極とを一体に
接合することにより、それぞれの方法の利点を生
かし、欠点を補なおうとするものである。 The present invention attempts to take advantage of the advantages of each method and compensate for their shortcomings by integrally bonding an ion exchange membrane and an electrode by a combination of both chemical plating and thermocompression bonding methods. .
すなわち、本発明は、あらかじめ化学メツキ法
により、イオン交換膜に触媒金属だけを接合し、
その上に加熱圧着法により、触媒金属と撥水性結
着剤との混合層を形成することにより接触抵抗が
小さく、かつ電極がガス拡散電極として良好に機
能するイオン交換膜−電極接合体を提供するもの
である。 That is, in the present invention, only a catalyst metal is bonded to an ion exchange membrane in advance by a chemical plating method,
By forming a mixed layer of a catalytic metal and a water-repellent binder thereon by a heat-pressing method, an ion exchange membrane-electrode assembly with low contact resistance and an electrode that functions well as a gas diffusion electrode is provided. It is something to do.
本発明のかかる化学メツキ法と加熱圧着法との
阜合法は一見、それぞれの方法の単なる組合わせ
のように見えるが、後述のように化学メツキ法お
よび加熱圧着法それぞれ単独の方法に比較して、
飛躍的な性能の向上がみられることとこの複合法
における化学メツキ工程でイオン交換膜に接合さ
るべき触媒金属の接合量が、化学メツキ法単独の
場合には望ましい性能が得られないほど少量にす
る必要があるという事実とから、全く新しい意義
をもつていると理解されるべきである。 At first glance, the chemical plating method and the thermocompression bonding method of the present invention seem to be a simple combination of the respective methods, but as will be described later, compared to the chemical plating method and the thermocompression bonding method alone, ,
A dramatic improvement in performance can be seen, and the amount of catalyst metal to be bonded to the ion-exchange membrane in the chemical plating process in this combined method is so small that the desired performance cannot be achieved with the chemical plating process alone. It should be understood that it takes on a completely new meaning due to the fact that it is necessary to do so.
本発明に用いられるイオン交換膜としては、パ
ーフルオロカーボンを基体にし、これにスルフオ
ン基、カルボキシル基あるいは両者を導入したも
のが適している。 Suitable ion exchange membranes used in the present invention include those having perfluorocarbon as a base and having sulfon groups, carboxyl groups, or both introduced therein.
化学メツキ工程でイオン交換膜に接合さるべき
触媒金属としては、白金がもつとも適している
が、ロジウム、パラジウムなどのその他の白金族
金属も使用できる。 Platinum is most suitable as the catalyst metal to be bonded to the ion exchange membrane in the chemical plating process, but other platinum group metals such as rhodium and palladium can also be used.
また、化学メツキ法単独で電極を形成する場合
には、触媒金属の担持量を５〜10mg／cm2にする必
要があるのに対し、本発明の複合法における化学
メツキ工程では、触媒金属の担持量を５mg／cm2以
下にすることが必須である。 In addition, when forming an electrode using the chemical plating method alone, the amount of catalyst metal supported must be 5 to 10 mg/ cm2 , whereas in the chemical plating step of the composite method of the present invention, the amount of catalyst metal supported is 5 to 10 mg/cm2. It is essential that the supported amount be 5 mg/cm 2 or less.
加熱圧着工程で使用される触媒粉末としては、
白金族金属、酸化イリジウム、酸化ルテニウム、
タングステンカーバイト、タングステンブロン
ズ、カーボンあるいはカーボンに白金族金属を担
持したものが適している。 Catalyst powder used in the heat compression process includes:
Platinum group metals, iridium oxide, ruthenium oxide,
Suitable materials include tungsten carbide, tungsten bronze, carbon, or carbon supporting a platinum group metal.
撥水性結着剤としては、ポリ４フツ化エチレ
ン、４フッ化エチレン−６フツ化プロピレンコポ
リマー、４フツ化エチレン−エチレンコポリマー
などが適している。 As the water-repellent binder, polytetrafluoroethylene, tetrafluoroethylene-hexafluoropropylene copolymer, tetrafluoroethylene-ethylene copolymer, etc. are suitable.
加熱圧着工程では、化学メツキ工程であらかじ
め触媒が接合されたイオン交換膜に、触媒粉末と
撥水性結着剤とを含む泥合物を吹き付け、一旦乾
燥したのち加熱しながらプレスする方法、あるい
は触媒粉末と撥水性結着剤との混合物から、あら
かじめ抄造法、フイルター法、ロールプレス法な
どの方法で、薄膜状にしたものを加熱圧着すると
いう方法が採用される。加熱温度としては、100
〜300℃の範囲、プレス圧としては、50〜300Kg／
cm2の範囲が適している。 In the heat-press bonding process, a slurry containing catalyst powder and a water-repellent binder is sprayed onto the ion exchange membrane to which the catalyst has been bonded in advance in the chemical plating process, and after drying, the mixture is pressed while heating, or the catalyst is bonded to the ion exchange membrane in advance. A method is adopted in which a mixture of powder and a water-repellent binder is made into a thin film by a method such as a papermaking method, a filter method, or a roll press method, and then heat-pressed. The heating temperature is 100
~300℃ range, press pressure is 50~300Kg/
A range of cm2 is suitable.
なお、加熱圧着工程では触媒粉末と撥水性結着
剤との混合層の上に、さらに多孔性ポリ４フツ化
エチレン膜あるいはフツ素樹脂とカーボン粉末と
の混合物からなり、しかもフツ素樹脂の配合割合
が触媒層と比較して相対的に多くした多孔性防水
層を形成することも効果的な場合がある。 In addition, in the heat-pressing process, on top of the mixed layer of catalyst powder and water-repellent binder, a porous polytetrafluoroethylene film or a mixture of fluororesin and carbon powder is formed, and furthermore, a mixture of fluororesin and carbon powder is added. It may also be effective to form a porous waterproof layer with a relatively higher proportion compared to the catalyst layer.
以下、本発明の一実施例について詳述する。 An embodiment of the present invention will be described in detail below.
実施例：
スルフオン基をイオン交換基とし、パーフルオ
ロカーボンを基体とするイオン交換膜の片面に、
塩化白金酸の水溶液を配し、他面に還元剤として
のヒドラジンを配することによつて、イオン交換
膜の片面に白金を析出させる。白金の析出量は、
２mg／cm2である。次に、同様にしてイオン交換膜
の他面にロジウムを７mg／cm2析出させる。Example: On one side of an ion exchange membrane with a sulfon group as the ion exchange group and a perfluorocarbon as the base,
Platinum is deposited on one side of the ion exchange membrane by disposing an aqueous solution of chloroplatinic acid and hydrazine as a reducing agent on the other side. The amount of platinum deposited is
It is 2mg/ cm2 . Next, 7 mg/cm 2 of rhodium is deposited on the other surface of the ion exchange membrane in the same manner.
一方、白金ブラック10ｇに対し、10c.c.のエチレ
ングリコールを加え、よく混合したものに60％の
ポリ４フツ化エチレン水懸濁液を５c.c.加えよく混
合した泥状物質をロールプレスして厚みが0.5mm
の白金−ポリ４フツ化エチレン混合物シートを製
作する。 On the other hand, add 10 c.c. of ethylene glycol to 10 g of platinum black, mix well, add 5 c.c. of 60% polytetrafluoroethylene aqueous suspension, and roll press the well-mixed slurry. and the thickness is 0.5mm
A platinum-polytetrafluoroethylene mixture sheet is manufactured.
次に、前述の白金とロジウムを化学メツキした
イオン交換膜の白金が接合された面に、上述の白
金−ポリ４フツ化エチレン混合物シートを載置
し、250℃の温度、100Kg／cm2の圧力で２分間加熱
プレスする。 Next, the platinum-polytetrafluoroethylene mixture sheet was placed on the platinum-bonded surface of the ion exchange membrane chemically plated with platinum and rhodium, and heated at 250℃ and 100Kg/cm 2 . Press under pressure for 2 minutes.
かくして電極とイオン交換膜とを一体に接合し
た電気化学セルが得られる。この電気化学セルは
脱酸素装置としてうまく機能する。つまり上述の
各電気化学セルの電流密度−電圧特性を求めたと
ころ、第１図に示すような効果が得られた。 In this way, an electrochemical cell in which the electrode and the ion exchange membrane are integrally joined is obtained. This electrochemical cell works well as an oxygen scavenger. That is, when the current density-voltage characteristics of each of the above-mentioned electrochemical cells were determined, the effects shown in FIG. 1 were obtained.
これらの結果から、化学メツキ法だけでイオン
交換膜に電極を接合した場合には、電気化学セル
の内部抵抗、換言すれば電極とイオン交換膜との
接触抵抗は小さいが、ガス拡散電極としては全く
機能せず、加熱圧着法単独の場合には、ガス拡散
電極としては機能するが、電極とイオン交換膜と
の接触抵抗が大きすぎるためには電気化学セルの
特性はかなり劣るのに対し、本発明にかゝる化学
メツキ法と加熱圧着法とを複合した場合には、電
極とイオン交換膜との接触抵抗は加熱圧着法に比
較して大幅に低下し、しかもガス拡散電極として
充分機能するばかりか、電気化学セルの特性も極
めてすぐれたものになることがわかる。 From these results, when the electrode is bonded to the ion exchange membrane using only the chemical plating method, the internal resistance of the electrochemical cell, in other words, the contact resistance between the electrode and the ion exchange membrane is small, but as a gas diffusion electrode it is It does not function at all, and when the heat-pressing method is used alone, it functions as a gas diffusion electrode, but because the contact resistance between the electrode and the ion exchange membrane is too high, the properties of the electrochemical cell are quite poor. When the chemical plating method and the heat pressure bonding method according to the present invention are combined, the contact resistance between the electrode and the ion exchange membrane is significantly lower than that in the heat pressure bonding method, and moreover, it functions well as a gas diffusion electrode. It can be seen that not only this, but also the properties of the electrochemical cell become extremely excellent.
以上詳述せる如く、本発明は、従来の化学メツ
キ法と加熱圧着法とを複合することによつて、飛
躍的にすぐれたイオン交換膜と電極とを一体に接
合する方法を提供するもので、その工業的価値極
めて大である。 As detailed above, the present invention provides a dramatically superior method of bonding an ion exchange membrane and an electrode together by combining the conventional chemical plating method and thermocompression bonding method. , its industrial value is extremely large.
なお、本発明における電極は、特にガス拡散電
極としてすぐれているが、ガス発生電極としても
機能する。 Note that the electrode in the present invention is particularly excellent as a gas diffusion electrode, but also functions as a gas generation electrode.
第１図は脱酸素装置用電気化学セルの電流密度
−電圧特性を示す。
Ａ……本発明例、Ｂ……従来例。
FIG. 1 shows the current density-voltage characteristics of an electrochemical cell for an oxygen absorber. A: Example of the present invention, B: Conventional example.
Claims (1)
溶液を配し、他面に還元剤溶液を配することによ
り、イオン交換膜に触媒金属を析出せしめ、その
上に触媒粉末単独か触媒粉末と導電性粉末との混
合物とフツ素樹脂結着剤との混合物を加熱圧着す
ることを特徴とするイオン交換膜と電極とを一体
に接合する方法。1. By placing an aqueous solution of a catalytic metal compound on one side of the ion exchange membrane and a reducing agent solution on the other side, the catalytic metal is deposited on the ion exchange membrane. 1. A method for integrally bonding an ion exchange membrane and an electrode, the method comprising heat-pressing a mixture of a fluorine-containing powder and a fluororesin binder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58035530A JPS59159991A (en) | 1983-03-03 | 1983-03-03 | Method for joining ion exchange membrane to electrode as one body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58035530A JPS59159991A (en) | 1983-03-03 | 1983-03-03 | Method for joining ion exchange membrane to electrode as one body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59159991A JPS59159991A (en) | 1984-09-10 |
| JPH0243830B2 true JPH0243830B2 (en) | 1990-10-01 |
Family
ID=12444285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58035530A Granted JPS59159991A (en) | 1983-03-03 | 1983-03-03 | Method for joining ion exchange membrane to electrode as one body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59159991A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1248564B (en) * | 1991-06-27 | 1995-01-19 | Permelec Spa Nora | ELECTROCHEMICAL DECOMPOSITION OF NEUTRAL SALTS WITHOUT HALOGEN OR ACID CO-PRODUCTION AND ELECTROLYSIS CELL SUITABLE FOR ITS REALIZATION. |
| ITFI20050002A1 (en) * | 2005-01-11 | 2006-07-12 | Acta Spa | ASSEMBLED MAMBRANA-ELECTRODES FOR FUEL CELLS, THEIR MANUFACTURE AND USE AND FUEL CELLS THAT COUNT |
| JP5065727B2 (en) * | 2007-03-27 | 2012-11-07 | 株式会社神鋼環境ソリューション | Method for manufacturing solid electrolyte membrane, solid electrolyte membrane, and water electrolysis device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5816082A (en) * | 1981-07-21 | 1983-01-29 | Permelec Electrode Ltd | Electrolytic device using ion exchange membrane and production thereof |
-
1983
- 1983-03-03 JP JP58035530A patent/JPS59159991A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59159991A (en) | 1984-09-10 |
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