JPH0326910B2 - - Google Patents
Info
- Publication number
- JPH0326910B2 JPH0326910B2 JP59153190A JP15319084A JPH0326910B2 JP H0326910 B2 JPH0326910 B2 JP H0326910B2 JP 59153190 A JP59153190 A JP 59153190A JP 15319084 A JP15319084 A JP 15319084A JP H0326910 B2 JPH0326910 B2 JP H0326910B2
- Authority
- JP
- Japan
- Prior art keywords
- activated carbon
- water
- fine particles
- gas diffusion
- repellent
- 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
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 83
- 239000005871 repellent Substances 0.000 claims description 25
- 238000009792 diffusion process Methods 0.000 claims description 15
- 239000010419 fine particle Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000007789 gas Substances 0.000 description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 description 14
- 230000002940 repellent Effects 0.000 description 13
- 238000003860 storage Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8817—Treatment of supports before application of the catalytic active composition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8896—Pressing, rolling, calendering
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
-
- 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
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Inert Electrodes (AREA)
Description
［産業上の利用分野］
本発明は長寿命で、かつ電気抵抗の小さなガス
拡散電極の製造法に関するものである。
［従来の技術］
従来は特開昭48−55333のように、炭素粉末の
分散液と撥水性を有する結着剤の分散液とを混合
して、炭素粉に決着剤の粒子を付着せしめ、アル
カリ処理、熱処理を施して炭素粉末と決着剤と触
媒物質を一体に結合するガス電極の製造法があつ
た。また、特開昭49−41830のように、結着剤と
撥水剤とを兼ねて、ポリテトラフルオロエチレン
（PTFE）粉末を用いるものであつた。さらに、
液体もしくは固体撥水剤を溶剤、例えば灯油に溶
かして活性炭に含浸させ、溶剤を蒸発させる製造
法もあつた。
［発明が解決しようとする問題点］
空気電池等は貯蔵特性、高温高湿下での放電等
において、ガス拡散電極の撥水性が重要なポイン
トであつた。PTFEの量を多くすると、ガス拡散
電極のガス透過性が悪くなり作動電圧が低下し、
さらに長期貯蔵性が良好でなかつた。また、撥水
剤を溶剤に溶かして活性炭に含浸させ、溶剤を蒸
発させる方法は、撥水剤が活性炭の全表面を覆つ
てしまい、ガス拡散電極の電気抵抗が大きくなる
ため、作動電圧が低くなつた。また撥水剤の量を
少なくすると、充分な撥水効果が得られない問題
点があつた。
本発明は撥水性の微粒子を部分的に活性炭表面
に強固かつ安定な状態で溶着させことにより、ガ
ス拡散電極の電気抵抗、接触能力を劣化せしめず
撥水性を持たせ、長期貯蔵特性を向上させるもの
である。
［問題点を解決するための手段］
本発明の製造法を説明する。
まず、活性炭もしくは触媒を吸着した活性炭を
水に分散せしめる。また撥水性の微粒子も同様に
水に分散せしめる。次に活性炭分散液を撹拌しな
がら、撥水性の微粒子分散液を滴下する。この量
は使用する活性炭の種類により適宜調節して用い
る。次に、この混合溶液に20KHz〜100KHzの間
の超音波を照射しながら撹拌混合し、または混合
後照射して、活性炭と撥水性の微粒子の表面に吸
着した気泡を除去しながら、活性炭に撥水性の微
粒子を含浸させ、次に過乾燥する。さらに該微
粒子の融点以上の温度で加熱し、活性炭表面に撥
水性の微粒子を融着せしめる。融着は活性炭全面
を覆うのではないので、部分的に撥水化される。
このようにして撥水処理した活性炭に撥水性の微
粒子とを混合し、ローラーによりシート化し、ニ
ツケルネツトに圧着し、さらに撥水性フイルムを
圧着してガス拡散電極を製造するものである。
［作用］
本発明は活性炭表面に吸着している気泡を超音
波で除去し、撥水性微粒子を活性炭表面に部分的
に付着させ該微粒子の融点以上の温度に加熱する
ため強固に融着でき、また活性炭の全面を覆うの
でなく部分的に撥水化し酸素を還元する表面は充
分残している。このため大電流で使用でき、電池
の振動、温度シヨツク等に対して強くなり、長期
貯蔵性が向上するものである。
［実施例］
本発明のガス拡散電極の実施例を用いた空気電
池を説明する。
まず、活性炭もしくは触媒を吸着した活性炭
100ｇを水１に分散せしめ、次に径0.01〜50μの
PTFEの60重量％の水性分散液を、水で10倍にう
すめる。活性炭分散液を撹拌しながらPTFE分散
液を100ml滴下する。この滴下量はPTFE固形分
と活性炭との重量比が、活性炭を100とすると、
0.1：100〜40：100の間で良好な結果が得られる。
使用する活性炭の種類によつて上記範囲内で適宜
調節して用いる。次に、上記混合液を20KHzの発
振器と100KHzの発振器を同時に使用して同時マ
ルチ周波の超音波を照射しながら10分間撹拌混合
して、活性炭とPTFE表面の微細な吸着気泡を除
去しながら、活性炭表面にPTFEの微粒子を含浸
させ、ついでこの活性炭を過し乾燥する。さら
に、PTFEの融点以上の温度380℃〜400℃で30分
加熱し、活性炭表面にPTFE粒の一部を融着させ
る。該微粒子の融着は活性炭の全面を覆うのでな
く、活性炭表面に部分的に融着し撥水化させる。
超音波処理によりPTFEは活性炭と部分的に強固
に一体化されるため、酸素還元触媒の作用する表
面は充分残している。このようにして撥水処理し
た活性炭80重量％とPTFE粉20重量％とを混合
し、ローラーによりシート化し、ニツケルネツト
を圧着し、さらにPTFEフイルムを圧着して、ガ
ス拡散電極を製造する。
次に、本発明のガス拡散電極を使用したPR44
型の空気合鉛電池〔Ａ〕と、灯油により撥水処理
をした活性炭よりなる従来法によるガス拡散電極
を用いた同型の従来電池〔Ｂ〕とを試作し、初度
の電池内部抵抗、0.9Vまでの放電容量、60％放
電時の放電作動電圧を表１に、温度45℃、湿度60
％中で、空気孔を開放して１ケ月間貯蔵した後、
電池の放電容量と、放電作動電圧とを表２に、電
池〔Ａ〕、〔Ｂ〕とを比較して示した。
[Industrial Application Field] The present invention relates to a method for manufacturing a gas diffusion electrode that has a long life and low electrical resistance. [Prior art] Conventionally, as in JP-A-48-55333, a dispersion of carbon powder and a dispersion of a water-repellent binder are mixed, and particles of the binder are attached to the carbon powder. There has been a method for manufacturing gas electrodes in which carbon powder, a fixing agent, and a catalyst material are combined into one body through alkali treatment and heat treatment. Further, as in JP-A-49-41830, polytetrafluoroethylene (PTFE) powder was used as both a binder and a water repellent. moreover,
Another manufacturing method involved dissolving a liquid or solid water repellent in a solvent, such as kerosene, impregnating activated carbon and then evaporating the solvent. [Problems to be Solved by the Invention] Water repellency of gas diffusion electrodes is an important point in air batteries and the like in terms of storage characteristics, discharge under high temperature and high humidity, and the like. If the amount of PTFE is increased, the gas permeability of the gas diffusion electrode will deteriorate and the operating voltage will decrease.
Furthermore, the long-term storage property was not good. In addition, in the method of dissolving a water repellent in a solvent and impregnating it into activated carbon, and then evaporating the solvent, the water repellent covers the entire surface of the activated carbon, increasing the electrical resistance of the gas diffusion electrode, resulting in a low operating voltage. Summer. Furthermore, when the amount of water repellent is reduced, there is a problem that a sufficient water repellent effect cannot be obtained. The present invention allows water-repellent particles to be partially welded onto the activated carbon surface in a strong and stable state, thereby imparting water-repellency to the gas diffusion electrode without deteriorating its electrical resistance or contact ability, and improving long-term storage characteristics. It is something. [Means for Solving the Problems] The manufacturing method of the present invention will be explained. First, activated carbon or activated carbon that has adsorbed a catalyst is dispersed in water. Water-repellent fine particles are also similarly dispersed in water. Next, while stirring the activated carbon dispersion, a water-repellent fine particle dispersion is added dropwise. This amount is adjusted as appropriate depending on the type of activated carbon used. Next, this mixed solution is stirred and mixed while being irradiated with ultrasonic waves between 20 KHz and 100 KHz, or is irradiated after mixing to remove air bubbles adsorbed to the surface of the activated carbon and water-repellent particles, while repelling the activated carbon. Impregnate with aqueous microparticles and then overdry. Further, the activated carbon is heated at a temperature higher than its melting point to fuse the water-repellent particles to the surface of the activated carbon. Since the fusion does not cover the entire activated carbon, it becomes partially water repellent.
A gas diffusion electrode is produced by mixing the water-repellent activated carbon with water-repellent fine particles, forming it into a sheet using a roller, pressing it onto a nickel net, and then pressing a water-repellent film onto it. [Function] The present invention uses ultrasonic waves to remove air bubbles adsorbed on the activated carbon surface, and allows water-repellent fine particles to be partially attached to the activated carbon surface and heated to a temperature higher than the melting point of the fine particles, so that they can be firmly fused. Furthermore, rather than covering the entire surface of the activated carbon, sufficient surface area is left to partially make it water repellent and reduce oxygen. Therefore, it can be used with a large current, is resistant to battery vibration, temperature shock, etc., and has improved long-term storage performance. [Example] An air battery using an example of the gas diffusion electrode of the present invention will be described. First, activated carbon or activated carbon that has adsorbed a catalyst
Disperse 100g in 1 part of water, then add a
A 60% by weight aqueous dispersion of PTFE is diluted 10 times with water. Drop 100 ml of the PTFE dispersion into the activated carbon dispersion while stirring. The amount of this dripping is based on the weight ratio of PTFE solid content to activated carbon, assuming that activated carbon is 100.
Good results are obtained between 0.1:100 and 40:100.
The amount is appropriately adjusted within the above range depending on the type of activated carbon used. Next, the above mixture was stirred and mixed for 10 minutes while irradiating simultaneous multi-frequency ultrasound using a 20KHz oscillator and a 100KHz oscillator to remove fine adsorption bubbles on the activated carbon and PTFE surfaces. The activated carbon surface is impregnated with PTFE particles, and then the activated carbon is filtered and dried. Furthermore, it is heated for 30 minutes at a temperature of 380°C to 400°C, which is higher than the melting point of PTFE, to fuse some of the PTFE grains to the surface of the activated carbon. The fine particles do not cover the entire surface of the activated carbon, but are partially fused to the surface of the activated carbon to make it water repellent.
Because the PTFE is partially firmly integrated with the activated carbon by ultrasonic treatment, a sufficient surface area is left for the action of the oxygen reduction catalyst. A gas diffusion electrode is produced by mixing 80% by weight of the activated carbon treated to be water repellent in this manner and 20% by weight of PTFE powder, forming it into a sheet using a roller, pressing a nickel net, and then pressing a PTFE film. Next, PR44 using the gas diffusion electrode of the present invention
We prototyped an air lead-acid battery [A] of the same type and a conventional battery of the same type [B] using a conventional gas diffusion electrode made of activated carbon treated with kerosene to make it water repellent.The initial internal resistance of the battery was 0.9V. Table 1 shows the discharge capacity up to and the discharge operating voltage at 60% discharge at a temperature of 45℃ and a humidity of 60℃.
After storing for one month in % with the air holes open,
Table 2 shows the discharge capacity and discharge operating voltage of the batteries for comparison between batteries [A] and [B].
【表】【table】
【表】
表１、２の結果から、本発明品〔Ａ〕は、撥水
剤が部分的に融着していて活性炭表面が残つてい
るため接着抵抗が小さく、このため電池の内部抵
抗が小さい。また、貯蔵後の放電容量と放電作動
電圧共に従来品〔Ｂ〕より優れていることがわか
る。
上記実施例では撥水性としてポリテトラフルオ
ロエチレンを用いたガス拡散電極について記した
が、この他に４フツ化エチレンと６フツ化プロピ
レンとの共重合体等のフツ素樹脂の撥水性微粒子
を用いても、同様な効果があることを実験により
確認した。
また、本発明は超音波の周波数を、20KHz〜
100KHzの範囲に限定したが、20KHz未満だと照
射時間が数時間となり効率が悪く、100KHzを越
えると、活性炭自体の破砕、あるいは活性炭に吸
着している酸素還元触媒の活性炭よりの離脱が起
り始めるので、都合が悪いものである。
［発明の効果］
以上のように、本発明のガス拡散電極を用いた
空気電池は、電池内部抵抗が小さく、また貯蔵後
の放電特性が優れている。[Table] From the results in Tables 1 and 2, the product [A] of the present invention has a low adhesion resistance because the water repellent is partially fused and the activated carbon surface remains, and therefore the internal resistance of the battery is low. small. Further, it can be seen that both the discharge capacity after storage and the discharge operating voltage are superior to the conventional product [B]. In the above example, a gas diffusion electrode using polytetrafluoroethylene for water repellency was described, but in addition, water repellent fine particles of fluororesin such as a copolymer of tetrafluoroethylene and hexafluoropropylene were used. It was confirmed through experiments that similar effects can be obtained. In addition, the present invention allows the frequency of ultrasonic waves to be adjusted from 20KHz to
We limited the range to 100KHz, but if it is less than 20KHz, the irradiation time will take several hours and the efficiency will be poor, and if it exceeds 100KHz, the activated carbon itself will be crushed, or the oxygen reduction catalyst adsorbed on the activated carbon will begin to separate from the activated carbon. Therefore, it is inconvenient. [Effects of the Invention] As described above, the air battery using the gas diffusion electrode of the present invention has low internal battery resistance and excellent discharge characteristics after storage.
Claims (1)
水性の微粒子との分散液に、2KHz〜100KHzの超
音波を照射しながら撹拌し、該微粒子を活性炭表
面に含浸付着させ、後乾燥し、次に、該微粒子の
融点以上の温度で加熱し、撥水性の微粒子を部分
的に活性炭表面に融着せしめることを特徴とする
ガス拡散電極の製造法。 ２ 該微粒子が、フツ素系樹脂であることを特徴
とする特許請求の範囲第１項記載のガス拡散電極
の製造法。 ３ 該超音波が、20KHz〜100KHzの範囲内同時
発振させた同時マルチ周波であることを特徴とす
る特許請求の範囲第１項記載のガス拡散電極の製
造法。[Claims] 1. A dispersion of activated carbon or activated carbon adsorbing a catalyst and water-repellent fine particles is stirred while irradiating ultrasonic waves of 2 KHz to 100 KHz to impregnate and adhere the fine particles to the surface of the activated carbon. A method for producing a gas diffusion electrode, which comprises drying and then heating at a temperature higher than the melting point of the fine particles to partially fuse the water-repellent fine particles to the surface of the activated carbon. 2. The method for producing a gas diffusion electrode according to claim 1, wherein the fine particles are a fluororesin. 3. The method for manufacturing a gas diffusion electrode according to claim 1, wherein the ultrasonic waves are simultaneous multi-frequency waves oscillated within a range of 20 KHz to 100 KHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59153190A JPS6158167A (en) | 1984-07-25 | 1984-07-25 | Manufacture of gas diffusion electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59153190A JPS6158167A (en) | 1984-07-25 | 1984-07-25 | Manufacture of gas diffusion electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6158167A JPS6158167A (en) | 1986-03-25 |
| JPH0326910B2 true JPH0326910B2 (en) | 1991-04-12 |
Family
ID=15557012
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59153190A Granted JPS6158167A (en) | 1984-07-25 | 1984-07-25 | Manufacture of gas diffusion electrode |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6158167A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302985C (en) * | 2002-01-11 | 2007-03-07 | 御国色素株式会社 | Carbonaceous materials and dispersions containing carbonaceous materials |
-
1984
- 1984-07-25 JP JP59153190A patent/JPS6158167A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6158167A (en) | 1986-03-25 |
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