JPH09274922A - Manufacture of solid electrolyte fuel cell - Google Patents
Manufacture of solid electrolyte fuel cellInfo
- Publication number
- JPH09274922A JPH09274922A JP8080229A JP8022996A JPH09274922A JP H09274922 A JPH09274922 A JP H09274922A JP 8080229 A JP8080229 A JP 8080229A JP 8022996 A JP8022996 A JP 8022996A JP H09274922 A JPH09274922 A JP H09274922A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- solvent
- film
- solid electrolyte
- cathode
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は固体電解質型燃料
電池（以下ＳＯＦＣと略記する）の製造方法に係り、特
に燃料電極の成膜方法の中で、表面改質粉末を利用した
製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a solid oxide fuel cell (hereinafter abbreviated as SOFC), and more particularly to a method for forming a fuel electrode using a surface-modified powder.
【０００２】[0002]
【従来の技術】ＳＯＦＣは電解質として固体のジルコニ
アを用い、１０００℃程度の高温で作動させる燃料電池
であり、電解質の支持や腐食の問題がなく作動中の活性
化過電圧を下げる触媒が不要であるなどの優れた特徴が
あり活発に研究されている。2. Description of the Related Art SOFC is a fuel cell which uses solid zirconia as an electrolyte and operates at a high temperature of about 1000 ° C., and there is no problem of electrolyte support or corrosion and a catalyst for lowering the activation overvoltage during operation is unnecessary. It has excellent features such as and is being actively researched.
【０００３】図４は従来のＳＯＦＣを示す分解斜視図で
ある。ＳＯＦＣは、酸素イオンの透過性を有する物質を
電解質層３とし、これを挟んで酸化剤極である空気電極
４と燃料電極２を配して構成され、燃料電極２は水素の
還元性雰囲気に強い材料を、一般的には多孔性ニッケル
あるいはニッケルと安定化ジルコニアのサーメットが使
用され、空気電極４は酸化性雰囲気で安定な材料を、一
般的にはランタンコバルトネート（ＬａＣｏＯ3 ）やラ
ンタンマンガネート（ＬａＭｎＯ3 ）を母体としたペロ
ブスカイト型酸化物が使用され、実際の使用にあたって
はＬａの一部をＣａあるいはＳｒで置換した固溶体とし
て電子導電性が高められている、電解質層３は酸素イオ
ンの透過性に優れイットリア安定化ジルコニア（ＹＳ
Ｚ）が使用されている。FIG. 4 is an exploded perspective view showing a conventional SOFC. The SOFC is composed of an electrolyte layer 3 made of a material having oxygen ion permeability, and an air electrode 4 and a fuel electrode 2 which are oxidant electrodes sandwiching the electrolyte layer 3, and the fuel electrode 2 is placed in a reducing atmosphere of hydrogen. A strong material, generally cermet of porous nickel or nickel and stabilized zirconia, is used, and the air electrode 4 is made of a material stable in an oxidizing atmosphere, typically lanthanum cobaltate (LaCoO 3 ) or lanthanum manganate. A perovskite type oxide having a base material (LaMnO 3 ) as a matrix is used, and in actual use, electronic conductivity is enhanced as a solid solution in which a part of La is replaced with Ca or Sr. The electrolyte layer 3 is an oxygen ion. Yttria-stabilized zirconia (YS
Z) is used.
【０００４】そうして、電解質層はガスの透過を防ぎ酸
素イオンのみを通すような緻密な膜であることが要求さ
れ、二つの電極についてはガスが内部まで入りこみ易い
ように多孔質であることが要求される。Thus, the electrolyte layer is required to be a dense membrane that prevents gas permeation and allows only oxygen ions to pass through, and the two electrodes must be porous so that gas can easily enter the inside. Is required.
【０００５】上記のＳＯＦＣの単位セル１をセパレータ
５を介して積層して構成される。セパレータは酸化にも
還元にも強く、しかも電子電導性が良好でイオン伝導性
のない材料が要求され、一般的にＬａＣｒＯ3 系に電子
電導性、焼結性の改善のため、ＬａやＣｒの一部をアル
カリ土類金属（Ｓｒ，Ｍｇ，Ｃａ等）で置換した酸化
物、あるいはＮｉ−Ａｌ合金やＮｉ−Ｃｒ合金等が使用
される。The SOFC unit cells 1 are laminated with a separator 5 in between. The separator is required to be a material that is strong against oxidation and reduction, has good electron conductivity, and does not have ionic conductivity. Generally, the LaCrO 3 system is used for improving La electron conductivity and sinterability. Oxides partially substituted with alkaline earth metals (Sr, Mg, Ca, etc.), Ni-Al alloys, Ni-Cr alloys, etc. are used.
【０００６】従来燃料電極板の製造方法は金属ニッケ
ル、酸化ニッケル等とジルコニアの粉体を溶剤に分散し
てスラリを調整し次いでこのスラリを金属多孔質体に塗
布し且つ含浸し、これを乾燥して還元雰囲気中で焼成し
て製造していた。Conventionally, a method of manufacturing a fuel electrode plate is such that powders of metallic nickel, nickel oxide and the like and zirconia are dispersed in a solvent to prepare a slurry, and then the slurry is applied and impregnated on a porous metal body and dried. It was manufactured by firing in a reducing atmosphere.
【０００７】表面改質粉では上記の粉体が、例えば金属
ニッケル粒子のまわりをイットリア安定化ジルコニア
（ＹＳＺ）がとり囲んだ構造である。In the surface-modified powder, the above-mentioned powder has a structure in which, for example, metal nickel particles are surrounded by yttria-stabilized zirconia (YSZ).
【０００８】また、プラズマ溶射法によって作製するこ
とが可能である。この場合には、イットリア安定化ジル
コニア（ＹＳＺ）およびニッケル粉末または酸化ニッケ
ル粉末を溶射装置の粉体供給部からプラズマジェット中
に供給して行う。Further, it can be manufactured by a plasma spraying method. In this case, yttria-stabilized zirconia (YSZ) and nickel powder or nickel oxide powder are supplied into the plasma jet from the powder supply unit of the thermal spraying device.
【０００９】[0009]
【発明が解決しようとする課題】従来のスラリ法やプラ
ズマ溶射法による製造では、例えば電解質ＹＳＺ部に微
細クラックが存在していたとき、スラリを塗布してもこ
の微細クラックは埋まらず、高活性な界面が形成できな
い。In the conventional manufacturing by the slurry method or the plasma spraying method, for example, when fine cracks exist in the electrolyte YSZ portion, the fine cracks are not filled even if the slurry is applied, and high activity is obtained. Interface cannot be formed.
【００１０】この発明は上記の点に鑑みてなされたもの
であり、その目的は、高活性な燃料極及び燃料極／電解
質界面を有するＳＯＦＣを提供することにある。The present invention has been made in view of the above points, and an object thereof is to provide an SOFC having a highly active fuel electrode and a fuel electrode / electrolyte interface.
【００１１】[0011]
【課題を解決するための手段】この発明の請求項１の手
段は、金属ニッケル、酸化ニッケル、ニッケルカルボニ
ル、炭酸ニッケルの群から選ばれた少なくとも一つを母
粒子としてその周りの全周または一部を安定化ジルコニ
ア粉末がとり囲んでなる表面改質粉体を溶媒に懸濁さ
せ、該溶媒中に、表面に固体電解質が成膜されている空
気極を陰極として設け、一方銅板を陽極として設け、前
記陰極と前記陽極に通電し、前記固体電解質上に前記表
面改質粉体を電着させて成膜することを特徴とする。According to a first aspect of the present invention, at least one selected from the group consisting of metallic nickel, nickel oxide, nickel carbonyl, and nickel carbonate is used as a mother particle, and the entire circumference or one circumference thereof is formed. The surface-modified powder in which the stabilized zirconia powder surrounds a part is suspended in a solvent, and an air electrode having a solid electrolyte film formed on the surface is provided as a cathode in the solvent, while a copper plate serves as an anode. It is characterized in that the cathode and the anode are energized, and the surface-modified powder is electrodeposited on the solid electrolyte to form a film.
【００１２】この発明の請求項２の手段は、ＳＯＦＣの
燃料極の成膜方法であって、最初に請求項１記載の方法
により所定厚さまで成膜したのち、その上に重ねて前記
表面改質粉体を溶剤に分散して調整してなるスラリを塗
布することにより成膜することを特徴とする。A second aspect of the present invention is a method of forming a film on a fuel electrode of an SOFC, which comprises first forming a film to a predetermined thickness by the method according to the first aspect, and then superimposing the film on the surface to modify the surface. It is characterized by forming a film by applying a slurry prepared by dispersing a fine powder in a solvent.
【００１３】この発明の請求項３の手段は、ＳＯＦＣの
燃料極の成膜方法であって、最初に請求項１記載の方法
により所定厚さまで成膜したのち、その上に重ねて安定
化ジルコニア粉末と、金属ニッケル、酸化ニッケル、ニ
ッケルカルボニル、炭酸ニッケルの群から選ばれた少な
くとも一つの物質の粉末とをプラズマ溶射することによ
り成膜することを特徴とする。According to a third aspect of the present invention, there is provided a method for forming a film of a SOFC fuel electrode, which comprises first forming a film to a predetermined thickness by the method according to the first aspect, and then superimposing the film on the stabilized zirconia. A film is formed by plasma spraying a powder and a powder of at least one substance selected from the group of metallic nickel, nickel oxide, nickel carbonyl, and nickel carbonate.
【００１４】この発明の請求項４の手段は、安定化ジル
コニア粉体を溶媒に懸濁させ、該溶媒中に、表面に固体
電解質が成膜されている空気極を陰極として設け、一方
銅板を陽極として設け、前記陰極と前記陽極に通電し、
前記固体電解質上に前記安定化ジルコニア粉体を電着さ
せて前記固体電解質の封孔をすることを特徴とする。According to a fourth aspect of the present invention, the stabilized zirconia powder is suspended in a solvent, and an air electrode having a solid electrolyte film formed on the surface thereof is provided as a cathode in the solvent, while a copper plate is provided. Provided as an anode, energizing the cathode and the anode,
The stabilized zirconia powder is electrodeposited on the solid electrolyte to seal the solid electrolyte.
【００１５】上記の電気泳動電着法により、選択的に導
電性の高いところ、すなわち、固体電解質の微細なクラ
ックや厚さの薄い部分に表面改質粉末を付着させること
ができ、これを焼成することにより電解質層に良質なＹ
ＳＺ膜が形成できると同時に高活性な燃料極との界面を
形成することができる。また、ＹＳＺ単独の粉末を付着
させて固体電解質の封孔をすることによりガスの透過を
防ぎ酸素イオンのみを通す緻密な固体電解質を形成する
ことができる。By the above-mentioned electrophoretic electrodeposition method, the surface-modified powder can be selectively adhered to a place having high conductivity, that is, a fine crack or a thin portion of the solid electrolyte, and this is baked. By doing so, good quality Y can be obtained in the electrolyte layer.
An SZ film can be formed and at the same time an interface with a highly active fuel electrode can be formed. Further, by adhering the powder of YSZ alone and sealing the solid electrolyte, it is possible to form a dense solid electrolyte that prevents gas permeation and allows only oxygen ions to pass.
【００１６】[0016]
【発明の実施の形態】この発明の実施の形態を図面に基
づいて説明する。Embodiments of the present invention will be described with reference to the drawings.
【００１７】図１はこの発明に係る電気泳動電着装置の
概略説明図である。図において、電気泳動用セル１０の
内部には溶媒１７が満たされ、溶媒１７に浸漬された電
極１９，２１が設けられている。そうして陰極１９には
ＳＯＦＣの空気極１１を装着する。空気極１１の表面に
は固体電解質（ＹＳＺ）１３が成膜されている。一方陽
極２１には銅板１５を装着する。溶媒１７としてはアル
コール類とメチル基含有ケトン類及びニトロセルロース
からなる混合溶媒を用いる。FIG. 1 is a schematic explanatory view of an electrophoretic electrodeposition apparatus according to the present invention. In the figure, the electrophoretic cell 10 is filled with a solvent 17, and electrodes 19 and 21 immersed in the solvent 17 are provided. Then, the SOFC air electrode 11 is attached to the cathode 19. A solid electrolyte (YSZ) 13 is formed on the surface of the air electrode 11. On the other hand, the copper plate 15 is attached to the anode 21. As the solvent 17, a mixed solvent composed of alcohols, methyl group-containing ketones and nitrocellulose is used.
【００１８】この発明は、溶媒１７中に、例えば、金属
ニッケルを母粒子としてその周りをＹＳＺ粉末がとり囲
んでなる表面改質粉体２３を懸濁させ、前記陰陽両極１
９，２１に通電し、陰極端子に接続した空気極１１上の
固体電解質１３の表面に上記の表面改質粉体２３を電着
させる。According to the present invention, the surface-modified powder 23, for example, having metallic nickel as the mother particles and surrounded by YSZ powder, is suspended in the solvent 17, and the positive and negative electrodes 1 are
9 and 21 are energized, and the surface-modified powder 23 is electrodeposited on the surface of the solid electrolyte 13 on the air electrode 11 connected to the cathode terminal.
【００１９】なお、表面改質粉体２３は、例えば高速回
転ボールミルによってニッケル粉末の周りにＹＳＺ粉末
を機械的に付着させることによって得られる。The surface-modified powder 23 is obtained, for example, by mechanically adhering YSZ powder around nickel powder with a high-speed rotating ball mill.
【００２０】上述の電気泳動電着により、拡大図に示す
ように、固体電解質１３に微細クラック２５が存在して
いた場合にはその部分に選択的に表面改質粉体２３を付
着させることができる。これらの制御は陰陽両極１９，
２１間にかける電圧と電流及び時間で行う。By the above-mentioned electrophoretic deposition, as shown in an enlarged view, when the fine cracks 25 exist in the solid electrolyte 13, the surface-modified powder 23 can be selectively adhered to the portion. it can. These controls are Yin and Yang 19,
The voltage, current, and time applied between 21 are used.
【００２１】また、上述の電気泳動電着法により、上記
の表面改質粉体の替りにＹＳＺ単独の粉末を用いること
によって固体電解質の封孔を実施する。Further, by the above-mentioned electrophoretic electrodeposition method, the solid electrolyte is sealed by using the powder of YSZ alone instead of the above-mentioned surface-modified powder.
【００２２】次にこの発明の請求項２に係る実施の形態
について説明する。Next, an embodiment according to claim 2 of the present invention will be described.
【００２３】上述の電気泳動電着法により電解質１３上
に厚さ１０μｍ程度の成膜を得たのち、空気極１１及び
電解質１３を電気泳動用セル１０から引き上げ焼成した
のち、図２のフローチャートに示すように、その上に重
ねて表面改質粉体をバインダ及び溶剤に分散して調整し
たスラリを塗布し、乾燥し、次いで焼成することによっ
てＳＯＦＣの燃料極板を形成する。After a film having a thickness of about 10 μm is formed on the electrolyte 13 by the above-mentioned electrophoretic electrodeposition method, the air electrode 11 and the electrolyte 13 are pulled out from the electrophoretic cell 10 and baked, and then the flow chart of FIG. As shown, an SOFC fuel electrode plate is formed by applying a slurry prepared by dispersing the surface-modified powder in a binder and a solvent on top of it, drying, and then firing.
【００２４】更に、この発明の請求項３に係る実施の形
態について説明する。Further, an embodiment according to claim 3 of the present invention will be described.
【００２５】上述の電気泳動電着法により電解質１３上
に厚さ１０μｍ程度の成膜を得たのち、空気極１１及び
電解質１３を電気泳動用セル１０から引き上げ焼成した
のち、図３のフローチャートに示すように、その上に重
ねてＹＳＺおよびニッケル粉末をプラズマ溶射装置の粉
体供給部からプラズマジェット中に供給して成膜を得
る。次いで焼成することによってＳＯＦＣの燃料極板を
形成する。After a film having a thickness of about 10 μm is formed on the electrolyte 13 by the above-mentioned electrophoretic electrodeposition method, the air electrode 11 and the electrolyte 13 are pulled out from the electrophoretic cell 10 and baked, and then the flow chart of FIG. As shown in the drawing, YSZ and nickel powder are superposed thereon and supplied into the plasma jet from the powder supply portion of the plasma spraying apparatus to obtain a film. Then, firing is performed to form an SOFC fuel electrode plate.
【００２６】[0026]
【発明の効果】この発明によれば、表面改質粉体を用い
電気泳動電着により、良質なＹＳＺ膜及び高活性な燃料
極および燃料極／電解質層界面を形成することができる
と共に、電気泳動法とスラリー法または溶射法の成膜方
法を併用することにより、緻密性が要求される電解質層
と多孔性が要求される燃料極を効率的に形成することが
できる。According to the present invention, a good quality YSZ film, a highly active fuel electrode, and a fuel electrode / electrolyte layer interface can be formed by electrophoretic electrodeposition using a surface-modified powder, and at the same time, an electrolysis By using the electrophoretic method and the film forming method such as the slurry method or the thermal spraying method in combination, it is possible to efficiently form an electrolyte layer that requires denseness and a fuel electrode that requires porosity.
【図１】この発明に係る電気泳動電着装置の概略説明
図。FIG. 1 is a schematic explanatory view of an electrophoretic electrodeposition apparatus according to the present invention.
【図２】この発明に係るＳＯＦＣの製造工程を示すフロ
ーチャート。FIG. 2 is a flowchart showing SOFC manufacturing steps according to the present invention.
【図３】この発明に係るＳＯＦＣの他の製造工程を示す
フローチャート。FIG. 3 is a flowchart showing another manufacturing process of the SOFC according to the present invention.
【図４】ＳＯＦＣの単電池を示す分解斜視図。FIG. 4 is an exploded perspective view showing an SOFC unit cell.
１０ 電気泳動用セル １１ ＳＯＦＣ空気極 １３ ＳＯＦＣ電解質 １５ 銅板 １７ 溶媒 １９ 陰極 ２１ 陽極 ２３ 表面改質粉体 ２５ 微細クラック 10 Electrophoresis Cell 11 SOFC Air Electrode 13 SOFC Electrolyte 15 Copper Plate 17 Solvent 19 Cathode 21 Anode 23 Surface Modified Powder 25 Fine Cracks
───────────────────────────────────────────────────── フロントページの続き (72)発明者 岩澤 力 東京都江東区木場１−５−１ 株式会社フ ジクラ内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Riki Iwasawa Fujikura Co., Ltd. 1-5-1 Kiba, Koto-ku, Tokyo
Claims (4)
カルボニル、炭酸ニッケルの群から選ばれた少なくとも
一つを母粒子としてその周りの全周または一部を安定化
ジルコニア粉末がとり囲んでなる表面改質粉体を溶媒に
懸濁させ、該溶媒中に、表面に固体電解質が成膜されて
いる空気極を陰極として設け、一方銅板を陽極として設
け、前記陰極と前記陽極に通電し、前記固体電解質上に
前記表面改質粉体を電着させて成膜することを特徴とす
る固体電解質型燃料電池の製造方法。1. A surface modification in which at least one selected from the group consisting of metallic nickel, nickel oxide, nickel carbonyl, and nickel carbonate is used as a mother particle, and the entire circumference or a part thereof is surrounded by a stabilized zirconia powder. The powder is suspended in a solvent, and in the solvent, an air electrode having a solid electrolyte film formed on its surface is provided as a cathode, while a copper plate is provided as an anode, and the cathode and the anode are energized to obtain the solid electrolyte. A method for producing a solid oxide fuel cell, characterized in that the surface-modified powder is electrodeposited thereon to form a film.
法であって、最初に請求項１記載の方法により所定厚さ
まで成膜したのち、その上に重ねて前記表面改質粉体を
溶剤に分散して調整してなるスラリを塗布することによ
り成膜することを特徴とする固体電解質型燃料電池の製
造方法。2. A method for forming a film on a fuel electrode of a solid oxide fuel cell, which comprises first forming a film to a predetermined thickness by the method according to claim 1, and then stacking the surface-modified powder on the film. A method for producing a solid oxide fuel cell, which comprises forming a film by applying a slurry prepared by dispersing in a solvent.
法であって、最初に請求項１記載の方法により所定厚さ
まで成膜したのち、その上に重ねて安定化ジルコニア粉
末と、金属ニッケル、酸化ニッケル、ニッケルカルボニ
ル、炭酸ニッケルの群から選ばれた少なくとも一つの物
質の粉末とをプラズマ溶射することにより成膜すること
を特徴とする固体電解質型燃料電池の製造方法。3. A method for forming a film on a fuel electrode of a solid oxide fuel cell, which comprises first forming a film to a predetermined thickness by the method according to claim 1, and then stacking the stabilized zirconia powder and metal. A method for producing a solid oxide fuel cell, comprising forming a film by plasma spraying powder of at least one substance selected from the group of nickel, nickel oxide, nickel carbonyl, and nickel carbonate.
せ、該溶媒中に、表面に固体電解質が成膜されている空
気極を陰極として設け、一方銅板を陽極として設け、前
記陰極と前記陽極に通電し、前記固体電解質上に前記安
定化ジルコニア粉体を電着させて前記固体電解質の封孔
をすることを特徴とする固体電解質型燃料電池の製造方
法。4. Stabilized zirconia powder is suspended in a solvent, and an air electrode having a solid electrolyte film formed on the surface thereof is provided as a cathode in the solvent, while a copper plate is provided as an anode, and the cathode and the A method for producing a solid oxide fuel cell, comprising energizing an anode and electrodepositing the stabilized zirconia powder on the solid electrolyte to seal the solid electrolyte.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8080229A JPH09274922A (en) | 1996-04-02 | 1996-04-02 | Manufacture of solid electrolyte fuel cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8080229A JPH09274922A (en) | 1996-04-02 | 1996-04-02 | Manufacture of solid electrolyte fuel cell |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09274922A true JPH09274922A (en) | 1997-10-21 |
Family
ID=13712530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8080229A Pending JPH09274922A (en) | 1996-04-02 | 1996-04-02 | Manufacture of solid electrolyte fuel cell |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09274922A (en) |
-
1996
- 1996-04-02 JP JP8080229A patent/JPH09274922A/en active Pending
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