JPS6348753A - Manufacture of electrode catalyst layer for fuel cell - Google Patents
Manufacture of electrode catalyst layer for fuel cellInfo
- Publication number
- JPS6348753A JPS6348753A JP61190858A JP19085886A JPS6348753A JP S6348753 A JPS6348753 A JP S6348753A JP 61190858 A JP61190858 A JP 61190858A JP 19085886 A JP19085886 A JP 19085886A JP S6348753 A JPS6348753 A JP S6348753A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- fine
- catalyst
- fine particles
- dispersion
- 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.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 63
- 239000000446 fuel Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims abstract description 50
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 abstract description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052697 platinum Inorganic materials 0.000 abstract description 4
- 239000010409 thin film Substances 0.000 abstract description 2
- 230000015271 coagulation Effects 0.000 abstract 3
- 238000005345 coagulation Methods 0.000 abstract 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 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
- H01M4/8878—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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8864—Extrusion
-
- 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
Abstract
Description
【発明の詳細な説明】
〔発明の、属する技術分野〕
このくを明（ズ１１ンｒ夛・￥−で、；料電池用寛（夕
触媒層の調造方法にじ！１する。[Detailed Description of the Invention] [Technical field to which the invention pertains] This article describes a method for preparing a catalyst layer for a fuel cell.
燃料１ｆｆ：池は燃料のもつ化学エネルキ７？万接電気
エネルギに＾換する装置であり、その構成は、リン酸よ
りなる電解液層（図示せず）をはさんで第２図に示すよ
うな電極６（カーボン゛ｍＷ基材４の上に電極触媒層５
を融着させたもの）を対口して配置し、外部のガス供給
系より前記各［ｆｆｌへ燃料ガスおよび酸化剤ガスを併
給し、各電極の触媒微粒子７の上で酸化剤カスと燃料ガ
スを個別に電気化学的に反応させ、その結果として系外
に電気エネルギをとり出すことができる。Fuel 1ff: Pond is the chemical energy of fuel 7? It is a device that converts electrical energy into electrical energy, and its configuration consists of an electrode 6 (on a carbon substrate 4) as shown in Fig. 2 with an electrolyte layer (not shown) made of phosphoric acid in between. electrode catalyst layer 5
The fuel gas and oxidizer gas are supplied together from an external gas supply system to each [ffl, and the oxidizer scum and fuel are fused onto the catalyst fine particles 7 of each electrode. Gases can be reacted individually electrochemically, and as a result, electrical energy can be extracted outside the system.
触媒微粒子７としてはカーボンブラックなどの触媒担体
２の上に白金などの旦金属微粒子１を担持シたものが用
いられ、この七好微粒子７がホｌｌテトラフロロエチレ
ン（ＰＴＦＥ）からなる弗素樹脂の微粒子３により結着
され電猛触媒層５が形成される。The catalyst fine particles 7 used are those in which metal fine particles 1 such as platinum are supported on a catalyst carrier 2 such as carbon black, and these Shichiyoshi fine particles 7 are made of a fluororesin made of solid tetrafluoroethylene (PTFE). The particles 3 are bound together to form an electrolytic catalyst layer 5.
この、ような電柩触啄層５にあっては弗素樹脂の微粒子
３は触媒微粒子７を結着する作目のほかその撥水効果に
より電極触媒層５に対し＋１ン酸よりなるｖＬ電解液対
する適度のぬれ性を生じさせ電極触媒７Ｍ ５の内部に
電気化学反応に必要なガス（燃料あるいは酸化剤ガス）
と固体（触媒微粒子７）と液体（１１ン酸型電解液）よ
りなる３相界面を形成させる、
従来電極触媒、ｍ ５は触媒微粒子７を界面活性剤の水
溶液に分散させたのち揮発性の少ない有機溶媒を加えて
よく混合し、これにＰＴＦＥからなる弗素樹脂のディス
パージョンを加え、得られたペーストを底膜して電極触
媒、（ト）５を伜でいた。In the electrode catalyst layer 5, the fluororesin fine particles 3 serve to bind the catalyst fine particles 7, and due to their water-repellent effect, the vL electrolyte consisting of +1 phosphoric acid is applied to the electrode catalyst layer 5. The gas (fuel or oxidant gas) necessary for electrochemical reaction is generated inside the electrode catalyst 7M5.
A conventional electrode catalyst, M5, forms a three-phase interface consisting of a solid (catalyst fine particles 7) and a liquid (11-phosphate electrolyte), after dispersing catalyst fine particles 7 in an aqueous solution of a surfactant. A small amount of organic solvent was added and mixed well, a fluororesin dispersion made of PTFE was added thereto, the resulting paste was used as a bottom layer, and the electrode catalyst (g) 5 was added.
しかしながらこのような方法で電極触媒ＪＶ１５を調製
すると、第２図に示すように触媒微粒子７も弗素樹脂の
微粒子３も凝集により大きな集落を形成し、そのために
触媒微粒子７と弗素樹脂の微粒子３の均一混合体を得る
ことができず、その結果この電極触媒層を燃料電池用電
極として用いた場合、その電池の特性劣化がはやく寿命
が短いという問題かあった。However, when the electrode catalyst JV15 is prepared by such a method, as shown in FIG. A homogeneous mixture could not be obtained, and as a result, when this electrode catalyst layer was used as an electrode for a fuel cell, there was a problem that the characteristics of the cell deteriorated quickly and its lifespan was shortened.
〔発ｑ］の目的〕
この発明は上記の点に鑑みてなされたものでありその目
的とするところは、触媒微粒子と弗素樹脂の微粒子とが
均一によく混合されて電池寿命の長い燃料電池用電極触
媒層の製造方法を提倶するにある。[Purpose of Development Q] This invention has been made in view of the above points, and its purpose is to provide a fuel cell with a long battery life in which fine catalyst particles and fine fluororesin particles are uniformly and well mixed. A method for manufacturing an electrode catalyst layer is provided.
この発明は
（イ１触媒微粒子を界面活性剤の水溶液に分散させて触
媒微粒子の分散液を調製する工程。This invention comprises (1) a step of dispersing catalyst fine particles in an aqueous solution of a surfactant to prepare a dispersion of catalyst fine particles;
（ロ）上記分散液に弗素仲浦のディスパージョンを加え
て触媒微粒子と弗素樹脂の微粒子の混合分散液を調製す
る工程、
嘘上記混合分散液に揮発性の少ない有機溶媒を加えて触
媒微粒子と弗素樹脂の微粒子を凝集させる工程。(b) A step of adding a fluorine Nakaura dispersion to the above dispersion to prepare a mixed dispersion of fine catalyst particles and fine particles of a fluororesin; A process of agglomerating resin particles.
とにより燃料電池用電極触媒層を調装するのでその目的
を達する。The purpose is achieved by preparing an electrode catalyst layer for a fuel cell.
すなわち工程（イ）、（ロ）により得らｆｌだ触媒微粒
子と弗素樹脂の微粒子の混合分散液に揮発性の少ない有
機溶媒を加えよく混合された触媒微粒子と弗素樹脂の微
粒子の相互のブロッキング作用によりそれぞれの微粒子
を小さくかつ均一な混合状態において凝集させるように
したものである。That is, a less volatile organic solvent is added to the mixed dispersion of the catalyst fine particles and the fluororesin fine particles obtained in steps (a) and (b), and the mutual blocking effect of the well-mixed catalyst fine particles and the fluororesin fine particles occurs. This allows the fine particles to be aggregated in a small and uniformly mixed state.
次にこの発明の実施例を図面にも七づいて説明する。第
１ｒｇＪはこの発明の実施例を示すもので、電極触媒層
５においては、触媒微粒子７．およびＰＴＦＥの微粒子
３は第２図に示す従来の”を極触媒層に比し凝集のサイ
ズが小さくかつそれぞれの凝集された微粒子が均一に混
合している状態を示す。Next, embodiments of the present invention will be described with reference to the drawings. The first rgJ shows an embodiment of the present invention, and in the electrode catalyst layer 5, catalyst fine particles 7. The PTFE fine particles 3 have a smaller agglomerated size than the conventional "polar catalyst layer" shown in FIG. 2, and each agglomerated fine particle is uniformly mixed.
このようなｔ甑触媒１層は次のようにしてＤ４競するこ
とができる。約２５Ａの白金微粒子１を数１０００λの
カーボンブラック裂触媒担体２に担持した触媒微粒子７
を１００７とり、これを界面活性剤の水溶液２００ ｍ
ｌないし５００ ｍｌに分散させる。触媒微粒子７の分
散液にＰ Ｔ Ｆ Ｅのディスパージョン（ｍＷω重量
％、比重１．５）を触媒微粒子７の１惜１００に対し閣
ないし６０重量のＰＴＦＥ微粒子が混合さハ、るよう調
整して加える。よく混和させてから、エチレンジ１１コ
ール等の揮発性の少ない有機溶媒を数１００ｍ１加えて
触媒微粒子７とＰＴＦＥの微粒子３のそれぞれを凝集さ
せる。このとき、各微粒子はよく混合されているので相
互に相手方のＷ ％を阻１′する。One layer of such a T-catalyst can be subjected to D4 competition as follows. Catalyst fine particles 7 in which platinum fine particles 1 of about 25A are supported on a carbon black cracked catalyst carrier 2 of several thousand λ
Take 1007 and add it to 200 m of an aqueous solution of surfactant.
1 to 500 ml. A dispersion of PTFE (mWω weight %, specific gravity 1.5) was added to the dispersion of catalyst fine particles 7 so that 1 to 60 weight of PTFE fine particles were mixed for every 100 weight of catalyst fine particles 7. Add. After mixing well, several hundred milliliters of a less volatile organic solvent such as ethylene di-11 alcohol is added to coagulate each of the catalyst fine particles 7 and the PTFE fine particles 3. At this time, since the fine particles are well mixed, they mutually inhibit the W % of the other.
そのため各微粒子の凝集は大きく進み得す凝集のサイズ
は小さい。しかも各微粒子の凝集は、相互によく混合さ
れた状態において進行する。このようにして得られた粘
稠なペーストをニーダを用いてよ（混線し押出成型し、
カレンダロールにてｌｏＯないし２００μｍの厚さに展
延して電極触媒層の薄模を形成する。この薄膜状電極触
媒層５を乾燥し、カーボン電極基材４の上に載置して）
’ １’ Ｆ Ｅの溶融する温度（３５０”Ｃ）で加圧
し、′に、極触媒層５をカーボン屯（至）基材４に融着
するとともに融媒微粒子７をＰＴＦＥの微粒子３で結着
させた。Therefore, the aggregation of each fine particle can proceed greatly, but the size of the aggregation is small. Moreover, the aggregation of each fine particle proceeds in a state where they are well mixed with each other. The viscous paste obtained in this way is mixed and extruded using a kneader.
A thin pattern of the electrode catalyst layer is formed by rolling it out to a thickness of loO to 200 μm using a calender roll. This thin film electrode catalyst layer 5 is dried and placed on the carbon electrode base material 4)
'1' FE is pressurized at the melting temperature (350"C), and in ', the polar catalyst layer 5 is fused to the carbon base material 4, and the melting medium fine particles 7 are condensed with the PTFE fine particles 3. I made him wear it.
先に述べたように本発明の製法による電極触媒層５にお
いては、触媒微粒子７と）’ Ｔ Ｆ’ Ｅの微粒子３
はそれぞれ小さな凝集体の状態で相互によく均一に混合
されているため、多数のガス拡散通路網が形成されて３
相γ四面が安定化するものと推定される、そのためこの
電極層をリン酸型燃料電池に組込み温度１９０ ”Ｃ、
電流密度２００ｍＡ／ｉ、ガス圧力４．０ Ｋ９／Ｃ１
ｔｆの条件で運転したところ、その特注劣化率を従来の
ものに比して約へ以下に減らすことができる。As mentioned above, in the electrode catalyst layer 5 according to the manufacturing method of the present invention, the catalyst fine particles 7 and the )' T F' E fine particles 3
are mixed well and uniformly with each other in the state of small aggregates, forming a large number of gas diffusion channel networks.
It is presumed that the four phase γ planes are stabilized. Therefore, this electrode layer was incorporated into a phosphoric acid fuel cell at a temperature of 190 ''C.
Current density 200mA/i, gas pressure 4.0 K9/C1
When operated under the conditions of tf, the custom-made deterioration rate can be reduced to less than about 100% compared to the conventional one.
この発明によれば
イ）触媒微粒子を界面活性剤の水溶液１こ分散させて触
媒微粒子の分散液を調製する工程。According to this invention, a) a step of preparing a dispersion of catalyst fine particles by dispersing catalyst fine particles in an aqueous solution of a surfactant;
（ロ）上記分散＠ｉｒ弗素樹脂のディスパージョンを加
えて触媒微粒子と、弗素ｚｑｈの微粒子の混合分散液を
調時する工程。(b) A step of adding the dispersion of the above-mentioned dispersion@ir fluororesin to prepare a mixed dispersion of fine catalyst particles and fine particles of fluorine zqh.
（−”ｉ上記混合分散液に揮発性の少ない有機溶媒を加
える工程。(-"i) A step of adding a less volatile organic solvent to the above mixed dispersion.
により燃料電池用の′ｇｔ極触媒層を人造することとし
たので、工程［＋ 、 ｉｏ＋で得られた触媒微粒子と
弗素樹脂の微粒子の混合分散液に揮発性の少ない有機溶
媒を加えると触媒微粒子と弗素樹脂の微粒子は、それぞ
れ相互に相手方を阻害しながら、小さく、かつ均一に混
合状態で凝集することになる。Since we decided to artificially produce a 'gt electrode catalyst layer for fuel cells, we added a less volatile organic solvent to the mixed dispersion of the catalyst fine particles and fluororesin fine particles obtained in the steps [+ and io+] to form catalyst fine particles. The fine particles of the fluororesin and the fluororesin coagulate in a small and uniformly mixed state, each inhibiting the other.
その結果このようにして得られたペーストを成膜し、て
得た電極触媒層は寿命が長く高い信頼性をもつことが実
証された。As a result, it was demonstrated that the electrode catalyst layer obtained by forming the paste thus obtained had a long life and high reliability.
第１図はこの発明の電極触媒層を示す断面図、笛２図は
従来の電極触媒層の断面図である。
■・・・白金微粒子、２・・・触媒担体、３・・・Ｐ
ＴＦ Ｅの微粒子、４・・・カーボン電極基材、５・・
・電極触媒層。
６・・・を極、７・・・触媒微粒子。
′ゾ人井ｊ２；山口 息
１ 白金★ｑＬ子
第 １ 刺
Ｉ−ｖ套爲依狼δ
茶 ｚＩ′２１FIG. 1 is a sectional view showing an electrode catalyst layer of the present invention, and FIG. 2 is a sectional view of a conventional electrode catalyst layer. ■...Platinum fine particles, 2...Catalyst carrier, 3...P
TF E fine particles, 4... carbon electrode base material, 5...
・Electrode catalyst layer. 6... is a pole, 7... is a catalyst fine particle. 'zojinj2; Yamaguchi Breath 1 Shirokane★qL child 1st bite I-v mantle δ Brown zI'21
Claims (1)
て触媒微粒子の分散液を調製する工程、 （ロ）上記分散液に弗素樹脂のディスパージョンを加え
て触媒微粒子と弗素樹脂の微粒子の 混合分散液を調製する工程、 （ハ）上記混合分散液に揮発性の少ない有機溶媒を加え
て触媒微粒子と弗素樹脂の微粒子を 凝集させる工程、 を備えることを特徴とする燃料電池用電極触媒層の製造
方法。[Claims] 1) (a) A step of dispersing catalyst fine particles in an aqueous solution of a surfactant to prepare a dispersion of catalyst fine particles, (b) Adding a fluororesin dispersion to the above dispersion to prepare catalyst fine particles. and (c) adding a less volatile organic solvent to the mixed dispersion to agglomerate the catalyst fine particles and the fluororesin fine particles. A method for producing an electrode catalyst layer for a fuel cell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61190858A JPS6348753A (en) | 1986-08-14 | 1986-08-14 | Manufacture of electrode catalyst layer for fuel cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61190858A JPS6348753A (en) | 1986-08-14 | 1986-08-14 | Manufacture of electrode catalyst layer for fuel cell |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6348753A true JPS6348753A (en) | 1988-03-01 |
| JPH0563906B2 JPH0563906B2 (en) | 1993-09-13 |
Family
ID=16264943
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61190858A Granted JPS6348753A (en) | 1986-08-14 | 1986-08-14 | Manufacture of electrode catalyst layer for fuel cell |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6348753A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03256625A (en) * | 1990-03-05 | 1991-11-15 | Honda Motor Co Ltd | Method and device for feeding cover member for vehicle |
| WO2001071830A3 (en) * | 2000-03-23 | 2002-01-10 | Gillette Co | Method of making a cathode comprising a catalyst |
-
1986
- 1986-08-14 JP JP61190858A patent/JPS6348753A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03256625A (en) * | 1990-03-05 | 1991-11-15 | Honda Motor Co Ltd | Method and device for feeding cover member for vehicle |
| WO2001071830A3 (en) * | 2000-03-23 | 2002-01-10 | Gillette Co | Method of making a cathode comprising a catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0563906B2 (en) | 1993-09-13 |
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