JPH0680592B2 - Electrolyte matrix for molten carbonate fuel cell - Google Patents
Electrolyte matrix for molten carbonate fuel cellInfo
- Publication number
- JPH0680592B2 JPH0680592B2 JP60181382A JP18138285A JPH0680592B2 JP H0680592 B2 JPH0680592 B2 JP H0680592B2 JP 60181382 A JP60181382 A JP 60181382A JP 18138285 A JP18138285 A JP 18138285A JP H0680592 B2 JPH0680592 B2 JP H0680592B2
- Authority
- JP
- Japan
- Prior art keywords
- electrolyte
- fiber
- molten carbonate
- zro
- electrolyte matrix
- 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 - Fee Related
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0289—Means for holding the electrolyte
- H01M8/0295—Matrices for immobilising electrolyte melts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/14—Fuel cells with fused electrolytes
- H01M8/141—Fuel cells with fused electrolytes the anode and the cathode being gas-permeable electrodes or electrode layers
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fuel Cell (AREA)
Description
【発明の詳細な説明】 〔発明の技術分野〕 本発明は溶融炭酸塩を電解質として用いる燃料電池の電
解質マトリックスの改良に関する。Description: TECHNICAL FIELD OF THE INVENTION The present invention relates to improvement of an electrolyte matrix of a fuel cell using a molten carbonate as an electrolyte.
従来、水素のように酸化され易いガスと、酸素のように
酸化力のあるガスとを電気化学的反応プロセスを経て反
応させることにより直流電力を得るようにした燃料電池
が広く知られている。この燃料電池は、使用する電解質
によってリン酸型、溶融炭酸塩型、固体電解質型等に大
別される。2. Description of the Related Art Conventionally, there is widely known a fuel cell in which a DC power is obtained by reacting a gas such as hydrogen which is easily oxidized with a gas having an oxidizing power such as oxygen through an electrochemical reaction process. This fuel cell is roughly classified into a phosphoric acid type, a molten carbonate type, a solid electrolyte type, etc. depending on the electrolyte used.
ところで、上記のような燃料電池のうち、溶融炭酸塩型
の燃料電池は、650℃近辺の温度で動作させるようにし
たものであり、その主要部は、通常、炭酸リチウム、炭
酸カリウム等の炭酸塩の電解質と、リチウムアルニネー
ト等のセラミックス系保持材とを平板状に一体化してな
る電解質マトリックスの両面にニッケル合金等のガス拡
散極を当接して単位電池を構成し、この単位電池を複数
個、相互間に双極性隔離板を介在させて積層した積層体
に構成されている。By the way, among the fuel cells as described above, the molten carbonate type fuel cell is designed to be operated at a temperature around 650 ° C., and its main part is usually a carbonate such as lithium carbonate or potassium carbonate. A unit battery is constructed by abutting gas diffusion electrodes such as nickel alloys on both sides of an electrolyte matrix formed by integrating a salt electrolyte and a ceramic-based holding material such as lithium aluminate in a flat plate shape. It is configured as a laminated body in which a bipolar separator is interposed between the individual pieces.
しかしながら、上記のように構成された従来の電解質マ
トリックスにあっては、電解質保持材と溶融温度以下の
固相状態の電解質との熱膨張率差及び電解質マトリック
スと電極、セルハウジングとの熱膨張率差に起因して、
熱サイクルを与えると降温時に電解質マトリックスに貫
通割れの発生することが往々にしてあった。However, in the conventional electrolyte matrix configured as described above, the difference in the coefficient of thermal expansion between the electrolyte holding material and the electrolyte in the solid state below the melting temperature and the coefficient of thermal expansion between the electrolyte matrix, the electrode, and the cell housing. Due to the difference,
When a heat cycle was applied, penetration cracking often occurred in the electrolyte matrix when the temperature was lowered.
そこで、このような不具合を解消するために、カンタル
線やアルミナ（Al2O3）繊維等を補強繊維として混入
し、これらによって貫通割れに至るまでの強度を向上さ
せることが考えられている。Therefore, in order to eliminate such a problem, it has been considered to mix kanthal wire, alumina (Al 2 O 3 ) fiber or the like as a reinforcing fiber to improve the strength up to a through crack.
しかし、補強繊維として用いられるカンタル線やアルミ
ナ繊維は電解質と化学反応を起すため、長期にわたって
補強の役割を果たさないという問題点があった。このた
め、熱サイクルを与えることにより電解質マトリックス
に一旦微小な割れが発生すると、この割れに応力が集中
して大きな割れに発展することには変わりがなかった。However, the kanthal wire and the alumina fiber used as the reinforcing fiber cause a chemical reaction with the electrolyte, so that there is a problem that they do not play a reinforcing role for a long time. Therefore, once a minute crack is generated in the electrolyte matrix by applying the heat cycle, the stress is concentrated on this crack, and the crack still develops.
一方、溶融炭酸塩に対して比較的安定な物質としてジル
コニア（ZrO2）が知られており、特にY2O3、CaO等の添
加により安定化あるいは部分安定化されたものに関して
は、溶融炭酸塩に対する長期間にわたる安定性が立証さ
れている。また、ジルコニアは酸化物セラミックスとし
ては容易に繊維状物質（通常、径が８μｍ程度、長さ数
mm）が得られる材料である。したがって、これらの観点
のみから判断すれば、ジルコニア繊維は電解質マトリッ
クスの補強繊維の用途に適しているといえる。On the other hand, zirconia (ZrO 2 ) is known as a substance that is relatively stable to molten carbonates, and especially those that have been stabilized or partially stabilized by the addition of Y 2 O 3 , CaO, etc. Long-term stability to salt has been demonstrated. Zirconia is a fibrous substance (usually having a diameter of about 8 μm and a number of lengths) as an oxide ceramic.
mm) is the material that can be obtained. Therefore, judging from only these viewpoints, it can be said that the zirconia fiber is suitable for use as the reinforcing fiber of the electrolyte matrix.
ただし、ジルコニア繊維は溶融炭酸塩に対するぬれ性に
乏しいため、電解質マトリックスに１重量％程度混入さ
せても電解質の保持性が著しく低下する。そして、混入
量を多くすると、電解質マトリックスのスランプ特性の
劣化を引起こす原因となる。このため、補強繊維として
ジルコニア繊維を用いる場合には、スランプ特性の劣化
が起らないような表面処理が必要となるという問題があ
った。However, since the zirconia fiber has a poor wettability with respect to the molten carbonate, even if it is mixed in the electrolyte matrix in an amount of about 1% by weight, the retention of the electrolyte is significantly reduced. Then, increasing the amount of mixing causes deterioration of the slump characteristics of the electrolyte matrix. Therefore, when zirconia fibers are used as the reinforcing fibers, there is a problem in that surface treatment is required so that deterioration of slump characteristics does not occur.
本発明は上記事情を考慮してなされたものであり、スラ
ンプ特性の劣化等を招くことなく、熱サイクルを受けて
も長期にわたって貫通割れを防止できる等、高強度を有
する溶融炭酸塩型燃料電池用電解質マトリックスを提供
しようとするものである。The present invention has been made in consideration of the above circumstances, and has a high strength such as a molten carbonate fuel cell that can prevent penetration cracking for a long period of time even when subjected to a thermal cycle without causing deterioration of slump characteristics and the like. It is intended to provide an electrolyte matrix for use.
本発明の溶融炭酸塩型燃料電池用電解質マトリックス
は、溶融状態で電解質として用いられる炭酸塩及び溶融
炭酸塩を保持するセラミックス保持材に、１〜20重量％
のLi2ZrO3繊維を混入したことを特徴とするものであ
る。The electrolyte matrix for a molten carbonate fuel cell of the present invention contains 1 to 20% by weight of a carbonate used as an electrolyte in a molten state and a ceramic holding material that holds the molten carbonate.
It is characterized by containing Li 2 ZrO 3 fiber of.
本発明において補強繊維として用いられるLi2ZrO3繊維
は、ジルコニア繊維とLiを含む溶融炭酸塩とを800℃以
上の高温で反応させることにより得られる。この反応温
度は通常の溶融炭酸塩型燃料電池の動作温度よりも高温
であることから、Li2ZrO3繊維は電池の動作温度程度の
溶融炭酸塩中では長期にわたって化学的に安定である。
また、Li2ZrO3繊維は溶融炭酸塩に対するぬれ性が良好
であるので、電解質マトリックスに多量に混入させても
電解質の保持性を低下させることがなく、スランプ特性
の劣化を招くことがない。更に、従来の電解質マトリッ
クスでは降温に伴う溶融炭酸塩の固化時において気孔が
発生し、これが凝集して粗大化することが熱サイクル後
の強度低下、更には割れの要因となっていると考えられ
ているが、Li2ZrO3繊維が混入されている電解質マトリ
ックスでは、降温に伴う溶融炭酸塩の固化時の気孔の発
生及び流動が繊維によって抑制されて気孔が細かく分散
するので、熱サイクルを受けても強度低下を防止するこ
とができる。The Li 2 ZrO 3 fiber used as the reinforcing fiber in the present invention is obtained by reacting zirconia fiber and a molten carbonate containing Li at a high temperature of 800 ° C. or higher. Since this reaction temperature is higher than the operating temperature of a normal molten carbonate fuel cell, the Li 2 ZrO 3 fiber is chemically stable for a long period of time in a molten carbonate at about the operating temperature of the cell.
Further, since the Li 2 ZrO 3 fiber has a good wettability with respect to the molten carbonate, even if a large amount of Li 2 ZrO 3 fiber is mixed in the electrolyte matrix, the electrolyte retention is not deteriorated and the slump characteristics are not deteriorated. Further, in the conventional electrolyte matrix, it is considered that pores are generated at the time of solidification of the molten carbonate accompanying the temperature decrease, and that the aggregation and coarsening of the pores cause the strength decrease after the thermal cycle and further the cracking. However, in the electrolyte matrix mixed with Li 2 ZrO 3 fibers, the generation and flow of pores during the solidification of the molten carbonate due to the temperature decrease are suppressed by the fibers and the pores are finely dispersed. However, it is possible to prevent the strength from decreasing.
なお、上述したようにジルコニア繊維を溶融炭酸塩に浸
漬してLi2ZrO3繊維を製造する場合、中心層にジルコニ
アが残存し、表面層がLi2ZrO3となった繊維が得られる
が、この表面層が溶融炭酸塩に対する化学的安定性及び
ぬれ性を発揮するので、上記のような本発明の効果を得
ることができる。Incidentally, as described above, when the zirconia fiber is immersed in a molten carbonate to produce a Li 2 ZrO 3 fiber, zirconia remains in the center layer, and a fiber having a surface layer of Li 2 ZrO 3 is obtained, Since this surface layer exhibits chemical stability and wettability with respect to molten carbonate, the effects of the present invention as described above can be obtained.
また、本発明において、電解質マトリックスを構成する
各要素の配合割合は、電解質55〜70重量％、保持材25〜
45重量％、Li2ZrO3繊維１〜20重量％であることが望ま
しい。上記配合割合は保持材の材質等によっても変動す
るが、Li2ZrO3繊維の配合割合については以下のような
理由による。すなわち、Li2ZrO3繊維が１重量％未満で
は本発明の効果を得ることができず、一方20重量％を超
えると所定の機械的強度を得るためには電解質の量を減
少させなければならず、電池反応時の内部抵抗の増大に
より電池特性の劣化を生じるためである。より好ましい
範囲は５〜15重量％である。また、電解質及び保持材の
配合割合については、使用される保持材の比表面積にも
よるが、例えば比表面積25m2/gのもので、保持材１重量
部に対し電解質３重量部以下でなければ、電解質を保持
することができない。このように電解質及び保持材の配
合割合は保持材により電解質を保持し得るという要件を
満たしたうえで、機械的強度と電池特性とを考慮して上
記範囲内で適宜設定される。Further, in the present invention, the mixing ratio of each element constituting the electrolyte matrix is 55 to 70% by weight of electrolyte, the holding material 25 to
45% by weight and 1 to 20% by weight of Li 2 ZrO 3 fiber are desirable. The above blending ratio varies depending on the material of the holding material and the like, but the blending ratio of the Li 2 ZrO 3 fiber is as follows. That is, if the Li 2 ZrO 3 fiber content is less than 1% by weight, the effect of the present invention cannot be obtained. On the other hand, if it exceeds 20% by weight, the amount of electrolyte must be reduced in order to obtain a desired mechanical strength. This is because the battery characteristics deteriorate due to an increase in internal resistance during the battery reaction. A more preferred range is 5 to 15% by weight. The mixing ratio of the electrolyte and the holding material depends on the specific surface area of the holding material used. For example, the specific surface area is 25 m 2 / g, and the amount of the electrolyte should be 3 parts by weight or less relative to 1 part by weight of the holding material. For example, the electrolyte cannot be retained. As described above, the mixing ratio of the electrolyte and the holding material satisfies the requirement that the holding material can hold the electrolyte, and is appropriately set within the above range in consideration of mechanical strength and battery characteristics.
以下、本発明の実施例を説明する。 Examples of the present invention will be described below.
まず、ジルコニア繊維を800℃の溶融炭酸塩（Li2CO3とK
2CO3との混合溶融炭酸塩）に浸漬して反応させ、Li2ZrO
3繊維を得た。このLi2ZrO3繊維は径が約10μｍ、長さが
約70μｍの短繊維であった。次に、Li2ZrO3繊維、炭酸
塩（Li2CO3とK2CO3）及び保持材（γ−LiAlO2）を下記
表に示す配合割合で総量が100gとなるように配合し、そ
れぞれアルミナボールとともにアルミナポットに入れ、
アセトンを溶媒として20時間湿式混合を行なった。つづ
いて、混合後の粉末を乾燥・分級した後、それぞれ60g
を採取し、10cm角の金型に均一充填した。次いで、460
℃で300kg/cm2の圧力を15分間かけてプレス成形を行な
い、厚み約2.4mmで10cm角の電解質マトリックスを作製
した。なお、下記表中、比較例１はLi2ZrO3繊維を全く
混入させていないもの、比較例２はLi4ZrO4繊維を10wt
％混入させたものである。First, the zirconia fiber was melted at 800 ° C (Li 2 CO 3 and K
2 CO 3 mixed molten carbonate) and reacted to form Li 2 ZrO
3 fibers were obtained. The Li 2 ZrO 3 fiber was a short fiber having a diameter of about 10 μm and a length of about 70 μm. Next, Li 2 ZrO 3 fiber, carbonate (Li 2 CO 3 and K 2 CO 3 ) and holding material (γ-LiAlO 2 ) were compounded at the compounding ratios shown in the table below so that the total amount would be 100 g. Put it in an alumina pot with alumina balls,
Wet mixing was performed for 20 hours using acetone as a solvent. Next, dry and classify the mixed powder, then 60g each
Was sampled and uniformly filled in a 10 cm square mold. Then 460
Press molding was performed at 300 ° C. for 15 minutes under a pressure of 300 kg / cm 2 to prepare a 10 cm square electrolyte matrix having a thickness of about 2.4 mm. In the following table, Comparative Example 1 contains no Li 2 ZrO 3 fiber, and Comparative Example 2 contains 10 wt% of Li 4 ZrO 4 fiber.
% Mixed.
以上のようにして得られた各電解質マトリックスから炭
酸ガスレーザーにより4cm角の熱サイクル試験片を切出
した。これら各試験片の上下をそれぞれアノード及びカ
ソードで挟み、炭酸ガス雰囲気中で1kg/cm2の圧力をか
け、650℃で１時間保持した後、降温した。From each electrolyte matrix obtained as described above, a 4 cm square thermal cycle test piece was cut out by a carbon dioxide gas laser. The upper and lower sides of each of these test pieces were sandwiched by an anode and a cathode, a pressure of 1 kg / cm 2 was applied in a carbon dioxide gas atmosphere, the temperature was kept at 650 ° C. for 1 hour, and then the temperature was lowered.
各電解質マトリックスについて、熱サイクル試験を行な
っていないものと、熱サイクル試験を行なったものとか
らそれぞれ2cm×4cmの曲げ試験片を切出し、３点曲げ試
験を行なった。この結果を下記表に併記する。For each electrolyte matrix, a 2 cm × 4 cm bending test piece was cut out from each of the non-heat cycled test sample and the heat cycled test sample, and a 3-point bending test was performed. The results are also shown in the table below.
また、試験後の構成相の安定性を評価するため、構成相
の割合をＸ線回折から算出し、単斜晶ZrO2への相変化率
を求めた。その結果を下記表に併記する。Further, in order to evaluate the stability of the constituent phase after the test, the proportion of the constituent phase was calculated from X-ray diffraction, and the phase change rate to monoclinic ZrO 2 was obtained. The results are also shown in the table below.
上記表から明らかなように、比較例１の電解質マトリッ
クスでは熱サイクル後に微細な割れが生じたため、熱サ
イクル後の曲げ強度が熱サイクル前と比べると大幅に低
下している。これに対し、実施例１〜５の電解質マトリ
ックスはいずれも熱サイクルを受けても割れが生じず熱
サイクル後の曲げ強度は比較例１の電解質マトリックス
と比べて向上している。また、実施例１〜５の電解質マ
トリックスではLi2ZrO3繊維の配合割合が多くなるにつ
れ、熱サイクル後の曲げ強度が向上している。一方、比
較例２では試験後に単斜晶ZrO2へ相変化する割合が非常
に大きくなっている。 As is clear from the above table, since the electrolyte matrix of Comparative Example 1 had fine cracks after the heat cycle, the bending strength after the heat cycle was significantly reduced as compared with that before the heat cycle. On the other hand, the electrolyte matrices of Examples 1 to 5 did not crack even when subjected to a heat cycle, and the bending strength after the heat cycle was improved as compared with the electrolyte matrix of Comparative Example 1. Further, in the electrolyte matrices of Examples 1 to 5, the bending strength after the heat cycle was improved as the blending ratio of Li 2 ZrO 3 fiber was increased. On the other hand, in Comparative Example 2, the rate of phase change to monoclinic ZrO 2 after the test is very large.
なお、上記実施例では保持材（γ−LiAlO2）の配合割合
を40重量％に固定し、電解質（K2CO3及びLi2CO3）とLi2
ZrO3繊維との和を一定としている。この場合、Li2ZrO3
繊維を20重量％以上混入すると、電解質が40重量％以下
となり、電池反応時の内部抵抗の増大により電池特性が
劣化するため、Li2ZrO3繊維を20重量％以上混入するこ
とは好ましくない。In the above examples, the holding material (γ-LiAlO 2 ) content was fixed to 40% by weight, and the electrolyte (K 2 CO 3 and Li 2 CO 3 ) and Li 2
The sum with ZrO 3 fiber is constant. In this case, Li 2 ZrO 3
If the fibers are mixed in an amount of 20% by weight or more, the electrolyte becomes 40% by weight or less, and the battery characteristics are deteriorated due to an increase in internal resistance during the battery reaction. Therefore, it is not preferable to mix 20% by weight or more of Li 2 ZrO 3 fibers.
更に、実施例３の電解質マトリックスについて、熱サイ
クルを与えた試験片の抗折破面を走査型電子顕微鏡によ
り観察したところ、気孔が細かく分散していることが確
認された。Further, with respect to the electrolyte matrix of Example 3, the fracture surface of the test piece subjected to the heat cycle was observed by a scanning electron microscope, and it was confirmed that the pores were finely dispersed.
以上詳述した如く本発明によれば、スランプ特性の劣化
等を招くことなく、熱サイクルを受けても長期にわたっ
て貫通割れを防止できる等高強度を有する溶融炭酸塩型
燃料電池用電解質マトリックスを提供できるものであ
る。As described in detail above, according to the present invention, there is provided an electrolyte matrix for a molten carbonate fuel cell, which has high strength such that penetration cracking can be prevented for a long period of time even when subjected to a thermal cycle without causing deterioration of slump characteristics. It is possible.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 柘植 章彦 神奈川県川崎市幸区小向東芝町１番地 株 式会社東芝総合研究所内 (56)参考文献 特開 昭56−82583（ＪＰ，Ａ) 特開 昭60−101876（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Akihiko Tsuge No. 1 Komukai Toshiba-cho, Kouki-ku, Kawasaki-shi, Kanagawa Inside the Toshiba Research Institute Co., Ltd. (56) Reference JP-A-56-82583 (JP, A) Kaisho 60-101876 (JP, A)
Claims (1)
及び溶融炭酸塩を保持するセラミックス保持材に、１〜
20重量％のLi2ZrO3繊維を混入したことを特徴とする溶
融炭酸塩型燃料電池用電解質マトリックス。1. A carbonate holding material used as an electrolyte in a molten state and a ceramic holding material holding a molten carbonate,
An electrolyte matrix for a molten carbonate fuel cell, characterized in that it contains 20% by weight of Li 2 ZrO 3 fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60181382A JPH0680592B2 (en) | 1985-08-19 | 1985-08-19 | Electrolyte matrix for molten carbonate fuel cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60181382A JPH0680592B2 (en) | 1985-08-19 | 1985-08-19 | Electrolyte matrix for molten carbonate fuel cell |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6243074A JPS6243074A (en) | 1987-02-25 |
| JPH0680592B2 true JPH0680592B2 (en) | 1994-10-12 |
Family
ID=16099752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60181382A Expired - Fee Related JPH0680592B2 (en) | 1985-08-19 | 1985-08-19 | Electrolyte matrix for molten carbonate fuel cell |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0680592B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3492709B2 (en) * | 1991-04-08 | 2004-02-03 | 株式会社東芝 | Molten carbonate fuel cell |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5682583A (en) * | 1979-12-10 | 1981-07-06 | Hitachi Ltd | Fuel cell |
| JPS60101876A (en) * | 1983-11-08 | 1985-06-05 | Agency Of Ind Science & Technol | Manufacture method of fused carbonate salts type fuel cell |
-
1985
- 1985-08-19 JP JP60181382A patent/JPH0680592B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6243074A (en) | 1987-02-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |