JPH02117068A - Manufacture of gas diffusion electrode - Google Patents

Manufacture of gas diffusion electrode

Info

Publication number
JPH02117068A
JPH02117068A JP63270568A JP27056888A JPH02117068A JP H02117068 A JPH02117068 A JP H02117068A JP 63270568 A JP63270568 A JP 63270568A JP 27056888 A JP27056888 A JP 27056888A JP H02117068 A JPH02117068 A JP H02117068A
Authority
JP
Japan
Prior art keywords
powder
water
conductive carbon
gas diffusion
ptfe
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
Application number
JP63270568A
Other languages
Japanese (ja)
Inventor
Noriaki Hara
原 範明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tanaka Kikinzoku Kogyo KK
Original Assignee
Tanaka Kikinzoku Kogyo KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tanaka Kikinzoku Kogyo KK filed Critical Tanaka Kikinzoku Kogyo KK
Priority to JP63270568A priority Critical patent/JPH02117068A/en
Publication of JPH02117068A publication Critical patent/JPH02117068A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8817Treatment of supports before application of the catalytic active composition
    • H01M4/8821Wet proofing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8803Supports for the deposition of the catalytic active composition
    • H01M4/8807Gas diffusion layers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8825Methods for deposition of the catalytic active composition
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8878Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8896Pressing, rolling, calendering
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

Abstract

PURPOSE:To improve the electrode characteristic by attaching powder made up of catalyst supporting carbon powder and polytetrafluoroethylene-(PTFE) to one side of a gas diffusion layer made up of water-repellent-treated conductive carbon paper, pressure-sticking the powder thereto under cold pressing and further, hot-pressing or baking it. CONSTITUTION:A gas diffusion layer to be used is made by water-repellent-treating a conductive carbon paper with PTFE, and a powder made by mixing carbon powder, a powder made to support a catalyst such as platinum, etc., and PTFE is made to be dispersed in alcohol cont. demineralized water or distilled water to produce a mixed solution. This water-repellent-treated conductive carbon paper is closely attached to the filtration face of a unit of filtration under reduced pressure by use of the alcohol cont. demineralized water or distilled water in advance, and the mixed solution is added thereto under such a condition as the paper is slightly sucked. Successively, a suction of the paper is increased and then the catalyst supporting carbon powder and PTFE powder are made to be attached to one side of the conductive carbon paper. Next, the powder are pressure-attached under a cold press condition, and further, hot-pressed or baked. Thereby, it is possible to keep an electric potential stable for a long time.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、ガス拡散電極の製造方法の改良に関するもの
である。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an improvement in a method for manufacturing a gas diffusion electrode.

(従来技術とその問題点) 従来、燃料電池等に用いられているガス拡散電極の製法
として、ロール法、ミリング法、Drジブレード法があ
るが、それぞれ単位面積あたりの触媒量の調整が比較的
難しく、しかも、得られた電極の初期性能および寿命が
不充分である。
(Prior art and its problems) Conventionally, there are the roll method, milling method, and Dr. giblade method as methods for manufacturing gas diffusion electrodes used in fuel cells, etc., but each method is relatively difficult to adjust the amount of catalyst per unit area. It is difficult, and the initial performance and lifetime of the obtained electrodes are unsatisfactory.

そこで、電極性能を向上させるための改良については盛
んに行われているが、その主なものとして、触媒金属を
微粒子化してできる限り均一分散させるための方法、導
電性粒子の改質により触媒金属の分散性を良くし利用率
を高める方法等の触媒活性および有効利用に関するもの
等である。
Therefore, many improvements are being made to improve electrode performance, but the main ones include methods to make the catalytic metal into fine particles and disperse it as uniformly as possible, and methods to improve the catalytic metal by modifying conductive particles. These topics relate to catalytic activity and effective utilization, such as methods to improve the dispersibility of and increase the utilization rate.

上記の種々の研究から、ガス拡散電極の触媒層をできる
限り均一にする方法が検討されているが、例えばロール
法によるもので白金担持触媒を用いた電極では電極特性
として、燃料電池用半電池試験の電位が720mv、@
200mA/c++!程度で、ライフテストでは15m
v/100時間程度の電圧低下が生じてしまうという欠
点があり、他の方法でもほぼ同様の結果である。
Based on the various studies mentioned above, methods to make the catalyst layer of gas diffusion electrodes as uniform as possible are being considered. The test potential is 720 mv, @
200mA/c++! It is about 15m in the life test.
There is a drawback that a voltage drop of about v/100 hours occurs, and other methods have almost the same results.

(発明の目的) 本発明は、上記従来の欠点を解決するためになされたも
ので、ガス拡販電極の触媒層を均一にかつ、高い性能を
持った電極を形成することで触媒の分散性を高め、電極
特性を向上させるとともに、安定性のあるガス拡散層を
得る方法を提供するものである。
(Object of the Invention) The present invention has been made to solve the above-mentioned conventional drawbacks, and it improves the dispersibility of the catalyst by making the catalyst layer of the gas sales promotion electrode uniform and forming an electrode with high performance. The object of the present invention is to provide a method for obtaining a gas diffusion layer with high stability and improved electrode properties.

(問題点を解決するための手段) 本発明は、撥水処理された導電性カーボンペーパから成
るガス拡散層の片側面に、触媒担持カーボン粉末とポリ
テトラフルオロエチレン粉末とアルコールを含む脱イオ
ン水または蒸留水から成る混合溶液を攪拌下で、該撥水
処理された導電性カーボンペーパを濾過面に介して吸引
濾過して触媒担持カーボン粉末とポリテトラフルオロエ
チレンとから成る粉末を付着させ、次いで冷間プレスを
して圧着し、さらに熱間プレスまたは焼成することを特
徴とするガス拡散電極の製造方法である。
(Means for Solving the Problems) The present invention provides deionized water containing catalyst-supported carbon powder, polytetrafluoroethylene powder, and alcohol on one side of a gas diffusion layer made of water-repellent conductive carbon paper. Alternatively, a mixed solution of distilled water is suction-filtered through the water-repellent conductive carbon paper through the filtration surface while stirring to deposit a powder of catalyst-supported carbon powder and polytetrafluoroethylene, and then This is a method for manufacturing a gas diffusion electrode, which is characterized by cold pressing and crimping, followed by hot pressing or firing.

以下、本発明の詳細について説明する。The details of the present invention will be explained below.

ガス拡散電極のガス拡販層は導電性カーボン粉末をテト
ラフルオロエチレンで撥水処理を行ったものを用い、次
いで、カーボン粉末に白金等の触媒となる金属を担持さ
せた粉末(以下「触媒担持カーボン粉末」という。)と
テトラフルオロエチレン(以下rPTFE」という。〉
を40〜60%を混合した粉末をアルコールを含む脱イ
オン水または蒸留水中に攪拌して分散させ混合溶液とす
る。
The gas promotion layer of the gas diffusion electrode is made of conductive carbon powder treated with water repellent treatment with tetrafluoroethylene. ) and tetrafluoroethylene (hereinafter referred to as "rPTFE").
A mixed solution of 40 to 60% of the powder is stirred and dispersed in deionized water or distilled water containing alcohol to form a mixed solution.

上記の撥水処理された導電性カーボンペーパを吸引濾過
装置の濾過面にまえもってアルコールを含む脱イオン水
または蒸留水を用いて密着させておき、僅かに吸引させ
た状態で該混合溶液を加える。
The above-mentioned water-repellent conductive carbon paper is brought into close contact with the filtration surface of the suction filtration device using deionized water or distilled water containing alcohol in advance, and the mixed solution is added under slight suction.

次いで、吸引量を高めて触媒担持カーボン粉末とPTF
Eの粉末を撥水処理された導電性カーボンペーパの片側
面に付着させる。
Next, increase the amount of suction to remove the catalyst-supported carbon powder and PTF.
Powder E is attached to one side of a water-repellent conductive carbon paper.

この際吸引中は該混合溶液を適度の速度で攪拌を続けて
おく。
At this time, the mixed solution is continued to be stirred at an appropriate speed during suction.

アルコールは親水性で表面張力の小さいものがよく、メ
チルアルコール、エチルアルコール、プロピルアルコー
ル等である。
The alcohol is preferably hydrophilic and has a low surface tension, such as methyl alcohol, ethyl alcohol, propyl alcohol, etc.

また、アルコールの加える割合は脱イオン水または蒸留
水に対して5%程度であることが好ましく、撥水処理さ
れた導電性カーボンペーパを吸引濾過装置の濾過面にま
えもって密着させておくために用いる、アルコールを含
む脱イオン水または蒸留水も同じ割合のものがよい。
In addition, the ratio of alcohol added is preferably about 5% to deionized water or distilled water, and is used to make the water-repellent conductive carbon paper adhere to the filtration surface of the suction filtration device in advance. , deionized water or distilled water containing alcohol should also be used in the same proportions.

アルコールを用いる理由は、PTFE粉末の表面を僅か
に親水性とし脱イオン水または蒸留水中で均一分散させ
るためであり、アルコールの割合が多くなるとPTFE
の持つ特性が失われるばかりでなく、撥水処理された導
電性カーボンペーパの撥水性をもそこなうので好ましく
ない。
The reason for using alcohol is to make the surface of the PTFE powder slightly hydrophilic so that it can be uniformly dispersed in deionized water or distilled water.
This is not preferable because it not only loses its properties but also impairs the water repellency of the water-repellent treated conductive carbon paper.

また、触媒担持カーボン粉末とPTFEの粉末の川は任
意とする触媒層の厚みから求めればよいが、該触媒担持
カーボン粉末とPTFEの粉末の慴がアルコールを含む
脱イオン水または蒸留水に対する割合は0.3重量%以
下であることが好ましい。
In addition, the amount of catalyst-supported carbon powder and PTFE powder can be determined from the thickness of an arbitrary catalyst layer, but the ratio of the catalyst-supported carbon powder and PTFE powder to deionized water or distilled water containing alcohol is It is preferably 0.3% by weight or less.

次いで、触媒担持カーボン粉末とPTFEの粉末を田水
処理された導電性カーボンペーパの片側面に付着させた
ものを、吸引濾過装置の吸引を止めたのらに取り出し、
まず、冷間プレスする、圧力は50kg/cn程度で1
5秒間を4回行う。
Next, the catalyst-supported carbon powder and PTFE powder adhered to one side of the rice-treated conductive carbon paper were taken out after the suction of the suction filtration device was stopped.
First, cold press at a pressure of about 50 kg/cn.
Do 4 times for 5 seconds.

該圧力と時間は触媒層の厚みにより多少の変化をさせる
ことは言うまでもない。
It goes without saying that the pressure and time will vary somewhat depending on the thickness of the catalyst layer.

上記冷間圧着させる理由は、吸引濾過により均一に触媒
担持カーボン粉末とPTFEの粉末を付着させた状態を
維持させて撥水処理された導電性カーボンペーパの片側
面圧着させるためである。
The reason for the above-mentioned cold press bonding is to keep the catalyst-supporting carbon powder and PTFE powder uniformly adhered by suction filtration and press the water-repellent conductive carbon paper on one side thereof.

次いで、熱間プレスを温度350℃前後で圧力は50k
g/cI+!程度とし時間は5秒程度で行うことで目的
とするガス拡散電極が得られる。
Next, hot press at a temperature of around 350°C and a pressure of 50k.
g/cI+! The desired gas diffusion electrode can be obtained by performing the process for about 5 seconds.

あるいは、不活性ガス中で、350℃前後で10分間程
度焼成しても目的とするガス拡散電極が得られる。
Alternatively, the desired gas diffusion electrode can be obtained by baking in an inert gas at around 350° C. for about 10 minutes.

本発明の方法によれば、電極特性として例えば白金担持
触媒での結果では750mv、 200mA / cn
fが得られ、しかもライフテストでは5mv/1000
時間という安定した電極である。
According to the method of the present invention, the electrode characteristics are, for example, 750 mV and 200 mA/cn for a platinum supported catalyst.
f is obtained, and the life test is 5mv/1000
Time is a stable electrode.

以下、本発明の実施例について記載するが、該実施例は
本発明を限定するものではない。
Examples of the present invention will be described below, but the examples do not limit the present invention.

(実施例) 白金触媒(60重量%)とPTFE(40重量%)の混
合粉末425+++gにエチルアルコール20−を加え
て攪拌しながら蒸留水400mfを加えた混合粉末溶液
を攪拌し続けておき、撥水処理された導電性カーボンペ
ーパ(50caf)を吸引濾過装置の濾過面にエチルア
ルコール20mj!と蒸留水400−を混合した溶液で
密着させておいたところへ、該混合粉末溶液を注入して
攪拌しながら吸引して撥水処理された導電性カーボンペ
ーパ上に付着させた。
(Example) A mixed powder solution of 425+++g of mixed powder of platinum catalyst (60% by weight) and PTFE (40% by weight) was added with 20-g of ethyl alcohol, and while stirring, 400mf of distilled water was added to the mixed powder solution. Water-treated conductive carbon paper (50 caf) was placed on the filter surface of the suction filtration device with 20 mj of ethyl alcohol! The mixed powder solution was injected into the area that had been brought into close contact with a mixed solution of 400% of distilled water and 400% of distilled water, and was suctioned while stirring to adhere to the water-repellent conductive carbon paper.

次いで、室温で50kg/cdの圧力で15秒間を4回
プレスしたのち、350℃、5 kg / cd、5秒
で熱間プレスして白金0.5mg/cmのガス拡散電極
を得た。
Next, it was pressed four times for 15 seconds at a pressure of 50 kg/cd at room temperature, and then hot pressed at 350° C. and 5 kg/cd for 5 seconds to obtain a gas diffusion electrode with platinum of 0.5 mg/cm.

この電極を燃料電池用半電池試験をしたところ200m
A/cfflにて、750mvの電位が得られ、耐久試
験では5mv/1000時間の変化であった。
When this electrode was subjected to a half-cell test for fuel cells, the distance was 200 m.
A potential of 750 mv was obtained at A/cffl, and the change was 5 mv/1000 hours in the durability test.

(従来例) 白金触媒(60重量%)とPTFE(40重量%)の混
合粉末850mgにソルベントナフサ1.5−を加えて
充分にねりあわせてローラにてO,l mmの厚さにし
、200℃で1時間乾燥したのち、撥水処理された導電
性カーボンペーパ(50cnf)上に合わせて、350
℃、50 kg/cm、5秒で熱間プレスして圧着した
のち撥水処理された導電性カーボンペーパ(50crd
)より出ている部分をカットして白金0.5mg/cn
fのガス拡散電極を得た。
(Conventional Example) Add 1.5-mg of solvent naphtha to 850 mg of mixed powder of platinum catalyst (60% by weight) and PTFE (40% by weight), knead thoroughly, and roll to a thickness of 0.1 mm using a roller. After drying at ℃ for 1 hour, a total of 350
℃, 50 kg/cm, 5 seconds, conductive carbon paper (50 crd
) Cut the part sticking out and add 0.5mg/cn of platinum.
A gas diffusion electrode of f was obtained.

この電極を燃料電池用半電池試験をしたところ200 
m A/c++fにて、?20mvの電位が得られ、耐
久試験では15mv/100時間の変化であった。
When this electrode was subjected to a half-cell test for fuel cells, the result was 200.
At m A/c++f? A potential of 20 mv was obtained, and in the durability test, the change was 15 mv/100 hours.

(発明の効果) 本発明は、従来の欠点を解決するために、ガス拡散電極
の触媒層をアルコールを含む蒸留水を用い吸引濾過する
ことや、冷間プレスすること等で均一なものにすること
ができ、電極特性の優れたガス拡散電極を得ることがで
き、従来法では得られなかった電位と長時間安定した電
位を保つという効果があり、ガス拡販電極の利用拡大に
大きく貢献するものである。
(Effects of the Invention) In order to solve the conventional drawbacks, the present invention makes the catalyst layer of the gas diffusion electrode uniform by suction filtration using distilled water containing alcohol, cold pressing, etc. It is possible to obtain a gas diffusion electrode with excellent electrode properties, and it has the effect of maintaining a stable potential for a long time, which is a potential that could not be obtained with conventional methods, and will greatly contribute to the expansion of the use of gas sales electrodes. It is.

Claims (1)

【特許請求の範囲】[Claims] 1、撥水処理された導電性カーボンペーパから成るガス
拡散層の片側面に、触媒担持カーボン粉末とポリテトラ
フルオロエチレン粉末とアルコールを含む脱イオン水ま
たは蒸留水から成る混合溶液を攪拌下で、該撥水処理さ
れた導電性カーボンペーパを濾過面に介して吸引濾過し
て触媒担持カーボン粉末とポリテトラフルオロエチレン
とから成る粉末を付着させ、次いで冷間プレスをして圧
着し、さらに熱間プレスまたは焼成することを特徴とす
るガス拡散電極の製造方法。
1. On one side of a gas diffusion layer made of water-repellent conductive carbon paper, a mixed solution of catalyst-supported carbon powder, polytetrafluoroethylene powder, and deionized or distilled water containing alcohol is stirred. The water-repellent conductive carbon paper is suction-filtered through the filtration surface to adhere powder consisting of catalyst-supported carbon powder and polytetrafluoroethylene, then cold-pressed to bond, and then hot-pressed. A method for producing a gas diffusion electrode, the method comprising pressing or firing.
JP63270568A 1988-10-26 1988-10-26 Manufacture of gas diffusion electrode Pending JPH02117068A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63270568A JPH02117068A (en) 1988-10-26 1988-10-26 Manufacture of gas diffusion electrode

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63270568A JPH02117068A (en) 1988-10-26 1988-10-26 Manufacture of gas diffusion electrode

Publications (1)

Publication Number Publication Date
JPH02117068A true JPH02117068A (en) 1990-05-01

Family

ID=17487969

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63270568A Pending JPH02117068A (en) 1988-10-26 1988-10-26 Manufacture of gas diffusion electrode

Country Status (1)

Country Link
JP (1) JPH02117068A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10151134B4 (en) * 2000-10-17 2012-07-05 Toyota Jidosha K.K. Diffusion layer for a fuel cell and a method for producing the same
JP2017117584A (en) * 2015-12-22 2017-06-29 パナソニック株式会社 Electrode manufacturing method and method of manufacturing film electrode assembly
WO2021070652A1 (en) * 2019-10-10 2021-04-15 東レ株式会社 Carbon fiber sheet and method for producing same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10151134B4 (en) * 2000-10-17 2012-07-05 Toyota Jidosha K.K. Diffusion layer for a fuel cell and a method for producing the same
JP2017117584A (en) * 2015-12-22 2017-06-29 パナソニック株式会社 Electrode manufacturing method and method of manufacturing film electrode assembly
WO2021070652A1 (en) * 2019-10-10 2021-04-15 東レ株式会社 Carbon fiber sheet and method for producing same

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