JPH0660883A - Porous electrode and manufacture thereof - Google Patents
Porous electrode and manufacture thereofInfo
- Publication number
- JPH0660883A JPH0660883A JP4209125A JP20912592A JPH0660883A JP H0660883 A JPH0660883 A JP H0660883A JP 4209125 A JP4209125 A JP 4209125A JP 20912592 A JP20912592 A JP 20912592A JP H0660883 A JPH0660883 A JP H0660883A
- Authority
- JP
- Japan
- Prior art keywords
- electrode
- porous electrode
- air
- holes
- porous
- 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
Links
Classifications
-
- 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
- Measuring Oxygen Concentration In Cells (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
- Inert Electrodes (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ガスセンサ、温度セン
サ及び燃料電池等に用いられる多孔質電極及びその製造
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a porous electrode used for gas sensors, temperature sensors, fuel cells and the like, and a method for manufacturing the same.
【０００２】[0002]
【従来の技術と課題】一般に多孔質電極は、集電性能の
他に、ガスを透過させる性能が要求される。従来、多孔
質電極を作製する場合は、カーボン等の可燃性材料粉末
を電極材料のセラミック原料に混合して焼成する方法が
採用されていた。この方法は、可燃性材料の粉末が、セ
ラミック原料の焼成中に燃焼して飛散することを利用し
て可燃性材料の粉末跡に気孔を形成するものである。2. Description of the Related Art Generally, a porous electrode is required to have gas permeation performance in addition to current collection performance. Conventionally, in the case of producing a porous electrode, a method has been adopted in which flammable material powder such as carbon is mixed with a ceramic raw material of an electrode material and fired. This method utilizes the fact that the powder of the flammable material burns and scatters during firing of the ceramic raw material to form pores in the traces of the powder of the flammable material.
【０００３】しかしながら、従来の方法は多孔質電極の
内部に閉気孔が発生するため、通気性が劣っていた。そ
こで、本発明の課題は、導電性及び通気性が優れた多孔
質電極及びその製造方法を提供することにある。However, the conventional method is inferior in air permeability because closed pores are formed inside the porous electrode. Then, the subject of this invention is providing the porous electrode excellent in electroconductivity and air permeability, and its manufacturing method.
【０００４】[0004]
【課題を解決するための手段と作用】以上の課題を解決
するため、本発明に係る多孔質電極は、酸化物を主成分
とする、抵抗率が１０Ωｃｍ以下のセラミック材料から
なり、かつ、電極の厚み方向に電極の表面から裏面まで
貫通する孔を複数個設けたことを特徴とする。また、こ
の多孔質電極を形成するには、酸化物を主成分とする抵
抗率が１０Ωｃｍ以下のセラミック材料からなる電極部
の表面にフォトレジスト膜を形成し、該電極部に形成さ
れる孔のパターンが描かれたマスクでレジスト膜を覆
い、露光処理を行った後に溶剤で処理してレジスト膜に
エッチング用の窓を開け、エッチング液を用いて窓の部
分の電極部をエッチングし電極部に孔を開ければよい。In order to solve the above-mentioned problems, the porous electrode according to the present invention is made of a ceramic material containing oxide as a main component and having a resistivity of 10 Ωcm or less. Is provided with a plurality of holes penetrating from the front surface to the back surface of the electrode. Further, in order to form this porous electrode, a photoresist film is formed on the surface of an electrode portion made of a ceramic material containing oxide as a main component and having a resistivity of 10 Ωcm or less, and a hole formed in the electrode portion is formed. Cover the resist film with a mask with a pattern drawn on it, and after exposing it to light, treat it with a solvent to open a window for etching in the resist film, and then use an etching solution to etch the electrode part of the window part to the electrode part. Just make a hole.
【０００５】以上の構成からなる多孔質電極において、
多孔質電極に設けられた貫通孔はガスの透過通路とな
る。一方、多孔質電極の導電性については、貫通孔の孔
径や個数を適当に設定することにより、貫通孔を設けな
い多孔質電極と殆んど変わらない導電性が確保される。In the porous electrode having the above structure,
The through hole provided in the porous electrode serves as a gas passage. On the other hand, regarding the conductivity of the porous electrode, by setting the hole diameter and the number of the through holes appropriately, it is possible to secure the conductivity which is almost the same as that of the porous electrode having no through holes.
【０００６】[0006]
【実施例】以下、本発明に係る多孔質電極の一実施例を
その製造方法と共に説明する。実施例として、固体電解
質型燃料電池の空気側電極に適用した場合について説明
する。図１は空気側電極２及び燃料側電極３を設けた固
体電解質１の構成図である。固体電解質１にはイットリ
ウム安定化ジルコニア、空気側電極２には酸化物導電体
であるランタンマンガナイト、燃料側電極３には白金が
用いられている。空気側電極２には、図２に示すよう
に、孔２ａが設けられている。空気はこの孔２ａを通っ
て固体電解質１に達することになる。EXAMPLES An example of the porous electrode according to the present invention will be described below together with its manufacturing method. As an example, the case of application to the air side electrode of a solid oxide fuel cell will be described. FIG. 1 is a configuration diagram of a solid electrolyte 1 provided with an air side electrode 2 and a fuel side electrode 3. Yttrium-stabilized zirconia is used for the solid electrolyte 1, lanthanum manganite that is an oxide conductor is used for the air-side electrode 2, and platinum is used for the fuel-side electrode 3. As shown in FIG. 2, the air side electrode 2 is provided with a hole 2a. Air reaches the solid electrolyte 1 through the holes 2a.
【０００７】固体電解質１の原料として、Ｙ2Ｏ3を８モ
ル％添加したＺｒＯ2の粉末（純度が９９％以上、平均
粒径が０．７μｍの粉末）を準備した。この粉末１００
ｇに対して、焼結助剤としてＭｎＣＯ3を１ｇ、さらに
溶剤（エタノール／トルエン＝２／８：重量比）を１０
０ｃｃ、ポリビニルブチラール系バインダを６ｇ、可塑
剤（ジオクチルブタレート系）を２ｇ、分散剤（ソルビ
タン脂肪酸エステル系）を１ｇ添加してスラリー化し、
ドクターブレード法によって厚み５０μｍの固体電解質
グリーンシートを作製した。As a raw material of the solid electrolyte 1, a ZrO 2 powder (purity of 99% or more and an average particle size of 0.7 μm) containing 8 mol% of Y 2 O 3 was prepared. 100 of this powder
With respect to g, 1 g of MnCO 3 as a sintering aid, and 10% of solvent (ethanol / toluene = 2/8: weight ratio)
0 cc, 6 g of polyvinyl butyral type binder, 2 g of plasticizer (dioctyl butyrate type) and 1 g of dispersant (sorbitan fatty acid ester type) were added to form a slurry,
A solid electrolyte green sheet having a thickness of 50 μm was produced by the doctor blade method.
【０００８】空気側電極２の原料として、（Ｌａ0.7Ｓ
ｒ0.3）Ｍｎ1.1Ｏ3の粉末（純度が９９％以上、平均粒
径が１．０μｍの粉末）を準備した。この粉末１００ｇ
に対して、焼結助剤としてＳｉＯ2を１ｇ、さらに溶剤
（エタノール／トルエン＝２／８：重量比）を７０ｃ
ｃ、ポリビニルブチラール系バインダを９ｇ、可塑剤
（ジオクチルブタレート系）を２ｇ、分散剤（ソルビタ
ン脂肪酸エステル系）を１ｇ添加してスラリー化し、ド
クターブレード法によって厚み５０μｍの空気側電極グ
リーンシートを作製した。As a raw material for the air side electrode 2, (La 0.7 S
A powder of r 0.3 ) Mn 1.1 O 3 (a powder having a purity of 99% or more and an average particle size of 1.0 μm) was prepared. 100g of this powder
On the other hand, 1 g of SiO 2 as a sintering aid and 70 c of a solvent (ethanol / toluene = 2/8: weight ratio) were used.
c, polyvinyl butyral-based binder 9 g, plasticizer (dioctyl butarate-based) 2 g, dispersant (sorbitan fatty acid ester-based) 1 g were added to form a slurry, and an air-side electrode green sheet having a thickness of 50 μm was prepared by a doctor blade method. did.
【０００９】作製された固体電解質グリーンシートを８
枚積み重ね、さらにその上に空気側電極グリーンシート
を２枚積み重ねた後、温度７０℃の条件下で圧力２トン
の静水圧成型を行い、圧着体とした。この圧着体を所定
の大きさに裁断した後、空気中で１３００℃まで昇温
し、この温度下で２時間焼成した。こうして、一辺の長
さが５０ｍｍ、厚さが０．３５ｍｍの短形状焼結体を得
た。The prepared solid electrolyte green sheet is
After stacking one sheet and further stacking two air-side electrode green sheets thereon, hydrostatic molding with a pressure of 2 tons was carried out at a temperature of 70 ° C. to obtain a pressure-bonded body. After this pressure-bonded body was cut into a predetermined size, the temperature was raised to 1300 ° C. in the air, and firing was performed at this temperature for 2 hours. Thus, a short shaped sintered body having a side length of 50 mm and a thickness of 0.35 mm was obtained.
【００１０】次に、焼結体の空気側電極２に貫通孔２ａ
を形成する方法について説明する。焼結体の表裏面にス
ピナーを用いてフォトリソグラフ用レジスト膜を塗布し
た。次に、図３に示されている一辺の長さが４５ｍｍの
矩形状フォトマスク４を配置し、空気側電極２の表面に
塗布されたレジスト膜を全面にわたって露光した。フォ
トマスク４には、一辺の長さが０．０５ｍｍの矩形状パ
ターン５を有する基本部分４ａが縦横に配列されてい
る。この矩形状パターン５の部分のみが光を透過し、他
の部分は光を透過しない。そして、この光を透過した部
分のレジスト膜が現像の際に除去され、その部分に空気
側電極２の一部が露出することになる。そして、この露
出している空気側電極２の部分を、規定濃度が１０の塩
酸をエッチング液として用いてエッチングし、孔２ａを
形成した。その後、溶剤にて残っているレジスト膜を除
去した。Next, a through hole 2a is formed in the air side electrode 2 of the sintered body.
A method of forming the will be described. A resist film for photolithography was applied to the front and back surfaces of the sintered body using a spinner. Next, a rectangular photomask 4 having a side length of 45 mm shown in FIG. 3 was arranged, and the resist film applied on the surface of the air-side electrode 2 was exposed over the entire surface. In the photomask 4, basic portions 4a having a rectangular pattern 5 having a side length of 0.05 mm are arranged vertically and horizontally. Only the portion of the rectangular pattern 5 transmits light, and the other portions do not transmit light. Then, the resist film in the portion that transmits the light is removed during development, and a part of the air-side electrode 2 is exposed in that portion. Then, the exposed portion of the air-side electrode 2 was etched using hydrochloric acid having a prescribed concentration of 10 as an etching solution to form a hole 2a. Then, the remaining resist film was removed with a solvent.
【００１１】さらに、固体電解質１の他方の面に、白金
からなる多孔質電極を燃料側電極３として形成する。こ
うして得られた実施例品の発電能力及び抵抗率について
評価した。評価結果を表１に示す。比較のために、従来
の空気側電極を備えた比較例品の評価結果も合わせて示
す。この比較例品の空気側電極は、その原料として、
（Ｌａ0.7Ｓｒ0 .3）Ｍｎ1.1Ｏ3の粉末（純度が９９％以
上、平均粒径が１．０μｍの粉末）が準備され、この粉
末１００ｇに対して、焼結助剤としてＳｉＯ2を１ｇ、
気孔形成剤として粒径２０μｍのアビセル（球状のセル
ロース系樹脂）を２０ｇ、さらに溶剤（エタノール／ト
ルエン＝２／８：重量比）を８０ｃｃ、ポリビニルブチ
ラール系バインダを１０ｇ、可塑剤（ジオクチルブタレ
ート系）を２ｇ、分散剤（ソルビタン脂肪酸エステル
系）を１ｇ添加してスラリー化し、ドクターブレード法
によって厚み５０μｍの空気側電極グリーンシートを作
製した。この空気極電極グリーンシートと前述の固体電
解質グリーンシート及び白金を用いて実施例品と同様の
方法で比較例品を作製した。Further, a porous electrode made of platinum is formed as the fuel side electrode 3 on the other surface of the solid electrolyte 1. The power generation capacity and resistivity of the thus obtained example products were evaluated. The evaluation results are shown in Table 1. For comparison, the evaluation result of the comparative example product including the conventional air-side electrode is also shown. The air-side electrode of this comparative example product, as its raw material,
(La 0.7 Sr 0 .3) Mn 1.1 O 3 powder (purity 99%, average particle size powder of 1.0 .mu.m) is ready, Powder 100 g, SiO 2 as sintering aids 1g,
20 g of Avicel (spherical cellulose-based resin) having a particle size of 20 μm as a pore-forming agent, 80 cc of solvent (ethanol / toluene = 2/8: weight ratio), 10 g of polyvinyl butyral-based binder, plasticizer (dioctyl butarate-based) 2 g) and 1 g of a dispersant (sorbitan fatty acid ester type) were added to form a slurry, and an air side electrode green sheet having a thickness of 50 μm was prepared by a doctor blade method. Using this air electrode electrode green sheet, the above-mentioned solid electrolyte green sheet and platinum, a comparative example product was produced in the same manner as the example product.
【００１２】[0012]
【表１】 [Table 1]
【００１３】発電能力は以下に説明する測定回路を用い
て評価した。図４に示すように、電極２，３にそれぞれ
空気供給管７ａ、燃料ガス供給管７ｂを取り付けて燃料
電池を作製した。この燃料電池を測定回路１９に接続
し、発電能力を測定した。すなわち、燃料電池を１００
０℃の温度に保持しながら、空気と燃料である水素ガス
をそれぞれ電極２，３に供給し、固体電解質１を介して
電極反応を起こさせ、かつ、電流計１１にて観察しなが
ら単位電極面積当たり０．３Ａ／ｃｍ2の電流が流れる
状態下の燃料電池に発生する電圧値を電圧計１０で測定
した。なお、８ａ，８ｂは白金線、９は可変抵抗器であ
る。この電圧値が大きいほど電極の導電性及びガス透過
性が優れ、かつ、電池としての性能も優れていることに
なる。表１には、実施例品と比較例品の抵抗率が略等し
いにもかかわらず、電圧に大きな違いが生じていること
が示されている。従って、両者のガス透過性には違いが
あり、実施例品は比較例品より優れていることがわか
る。The power generation capacity was evaluated using the measuring circuit described below. As shown in FIG. 4, an air supply pipe 7a and a fuel gas supply pipe 7b were attached to the electrodes 2 and 3, respectively, to fabricate a fuel cell. This fuel cell was connected to the measurement circuit 19 and the power generation capacity was measured. That is, 100 fuel cells
While maintaining the temperature at 0 ° C., air and hydrogen gas, which are fuels, are supplied to the electrodes 2 and 3, respectively, to cause an electrode reaction through the solid electrolyte 1, and while observing with the ammeter 11, the unit electrode The voltage value generated in the fuel cell under the condition that a current of 0.3 A / cm 2 per area flows was measured by the voltmeter 10. In addition, 8a and 8b are platinum wires, and 9 is a variable resistor. The higher the voltage value, the better the conductivity and gas permeability of the electrode, and the better the battery performance. Table 1 shows that there is a large difference in voltage even though the resistivity of the example product and the resistivity of the comparative example product are substantially equal. Therefore, there is a difference in gas permeability between the two, and it is understood that the example product is superior to the comparative product.
【００１４】なお、本発明に係る多孔質電極及びその製
造方法は前記実施例に限定するものではなく、その要旨
の範囲内で種々に変形することができる。多孔質電極に
設けられる貫通孔は、必ずしも前記実施例のように、離
散して配置する必要はなく、直線状に連続的に接近させ
て溝状に配置させてもよい。また、前記実施例では固体
電解質型燃料電池の空気側電極に適用した場合を説明し
たが、これ以外に、例えばガスセンサや湿度センサの多
孔質電極に適用してもよい。The porous electrode and the method for producing the same according to the present invention are not limited to the above-mentioned embodiment, but can be variously modified within the scope of the gist thereof. The through holes provided in the porous electrode do not necessarily have to be arranged discretely as in the above-mentioned embodiment, and may be arranged linearly and continuously so as to be arranged in a groove shape. Further, in the above-mentioned embodiment, the case where the present invention is applied to the air side electrode of the solid oxide fuel cell has been described, but other than this, it may be applied to the porous electrode of, for example, a gas sensor or a humidity sensor.
【００１５】[0015]
【発明の効果】以上の説明で明らかなように、本発明に
係る多孔質電極によれば、電極に複数の貫通孔を設けて
多孔質構造としたので、ガスはこの貫通孔を介してスム
ースに電極を透過できる。一方、電極の導電性について
は、抵抗率が１０Ωｃｍ以下のセラミック材料を電極材
料として用い、また、貫通孔の孔径や個数を適当に設定
することにより、貫通孔を設けない多孔質電極と殆ど変
わらない導電性が確保できる。従って、導電性及び通気
性が優れた多孔質電極を得ることができる。この結果、
ガスセンサ、温度センサ及び燃料電池等の性能を向上さ
せることが可能になる。As is apparent from the above description, according to the porous electrode of the present invention, a plurality of through holes are provided in the electrode to form a porous structure, so that the gas smoothly passes through the through holes. Can pass through the electrode. On the other hand, the conductivity of the electrode is almost the same as that of the porous electrode having no through hole by using a ceramic material having a resistivity of 10 Ωcm or less as the electrode material and appropriately setting the hole diameter and the number of through holes. There is no conductivity. Therefore, a porous electrode having excellent conductivity and air permeability can be obtained. As a result,
It is possible to improve the performance of the gas sensor, the temperature sensor, the fuel cell and the like.
【００１６】さらに、本発明に係る製造方法によれば、
導電性及び通気性が優れた前記多孔質電極を容易に得る
ことができる。Further, according to the manufacturing method of the present invention,
The porous electrode having excellent conductivity and air permeability can be easily obtained.
【図１】本発明に係る多孔質電極の一実施例を表面に設
けた固体電解質の斜視図。FIG. 1 is a perspective view of a solid electrolyte provided on the surface of an embodiment of a porous electrode according to the present invention.
【図２】図１に示した多孔質電極を表面に設けた固体電
解質の一部拡大断面図。FIG. 2 is a partially enlarged cross-sectional view of a solid electrolyte having a surface on which the porous electrode shown in FIG. 1 is provided.
【図３】図１に示した多孔質電極を形成する際に用いら
れるマスクの平面図。FIG. 3 is a plan view of a mask used when forming the porous electrode shown in FIG.
【図４】図１に示した多孔質電極を備えた燃料電池の発
電能力を測定するための測定回路を示す電気回路図。FIG. 4 is an electric circuit diagram showing a measuring circuit for measuring the power generation capacity of the fuel cell provided with the porous electrode shown in FIG.
２…空気側電極 ２ａ…貫通孔 2 ... Air side electrode 2a ... Through hole
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｂ 1/20 Ｚ 7244−5Ｇ Ｈ０１Ｍ 4/88 Ｔ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI Technical display location H01B 1/20 Z 7244-5G H01M 4/88 T
Claims (2)
ｃｍ以下のセラミック材料からなり、かつ、電極の厚み
方向に電極の表面から裏面まで貫通する孔を複数個設け
たことを特徴とする多孔質電極。1. A resistivity of 10 Ω, which is mainly composed of an oxide.
A porous electrode, which is made of a ceramic material having a size of 1 cm or less and has a plurality of holes penetrating from the front surface to the back surface of the electrode in the thickness direction of the electrode.
ｍ以下のセラミック材料からなる電極部の表面にフォト
レジスト膜を形成し、該電極部に形成される孔のパター
ンが描かれたマスクでレジスト膜を覆い、露光処理を行
った後に溶剤で処理してレジスト膜にエッチング用の窓
を開け、エッチング液を用いて窓の部分の電極部をエッ
チングし電極部に孔を開けることを特徴とする多孔質電
極の製造方法。2. The oxide-based resistivity is 10 Ωc.
A photoresist film is formed on the surface of the electrode portion made of a ceramic material of m or less, and the resist film is covered with a mask in which a pattern of holes formed in the electrode portion is drawn. A method for manufacturing a porous electrode, characterized in that a window for etching is opened in the resist film, and an electrode portion of the window portion is etched by using an etching solution to form a hole in the electrode portion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4209125A JPH0660883A (en) | 1992-08-05 | 1992-08-05 | Porous electrode and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4209125A JPH0660883A (en) | 1992-08-05 | 1992-08-05 | Porous electrode and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0660883A true JPH0660883A (en) | 1994-03-04 |
Family
ID=16567703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4209125A Pending JPH0660883A (en) | 1992-08-05 | 1992-08-05 | Porous electrode and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0660883A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002286680A (en) * | 2001-03-27 | 2002-10-03 | Ngk Spark Plug Co Ltd | Lamination type gas sensor element and its manufacturing method |
| JP2006173091A (en) * | 2004-12-16 | 2006-06-29 | General Electric Co <Ge> | High-performance fuel cell electrode and its manufacturing method |
| JP2006344486A (en) * | 2005-06-08 | 2006-12-21 | Japan Fine Ceramics Center | Solid oxide fuel cell and its manufacturing method |
| JP2008004423A (en) * | 2006-06-23 | 2008-01-10 | Japan Fine Ceramics Center | Solid oxide fuel cell, and its manufacturing method |
-
1992
- 1992-08-05 JP JP4209125A patent/JPH0660883A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002286680A (en) * | 2001-03-27 | 2002-10-03 | Ngk Spark Plug Co Ltd | Lamination type gas sensor element and its manufacturing method |
| JP4730722B2 (en) * | 2001-03-27 | 2011-07-20 | 日本特殊陶業株式会社 | Method for manufacturing laminated gas sensor element and laminated gas sensor element |
| JP2006173091A (en) * | 2004-12-16 | 2006-06-29 | General Electric Co <Ge> | High-performance fuel cell electrode and its manufacturing method |
| JP2006344486A (en) * | 2005-06-08 | 2006-12-21 | Japan Fine Ceramics Center | Solid oxide fuel cell and its manufacturing method |
| JP2008004423A (en) * | 2006-06-23 | 2008-01-10 | Japan Fine Ceramics Center | Solid oxide fuel cell, and its manufacturing method |
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