JPH044973B2 - - Google Patents
Info
- Publication number
- JPH044973B2 JPH044973B2 JP58012305A JP1230583A JPH044973B2 JP H044973 B2 JPH044973 B2 JP H044973B2 JP 58012305 A JP58012305 A JP 58012305A JP 1230583 A JP1230583 A JP 1230583A JP H044973 B2 JPH044973 B2 JP H044973B2
- Authority
- JP
- Japan
- Prior art keywords
- solid electrolyte
- lead
- lead iodide
- iodide
- reaction
- 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
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 44
- 239000007784 solid electrolyte Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- -1 alkali metal salt Chemical class 0.000 claims description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 229940071870 hydroiodic acid Drugs 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 21
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 7
- 239000007774 positive electrode material Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
- Y02E60/10—Energy storage using batteries
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Description
【発明の詳細な説明】
本発明は固体電解質電池用の正極活物質として
有用なヨウ化鉛の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing lead iodide useful as a positive electrode active material for solid electrolyte batteries.
従来から、この種のヨウ化鉛の製造法の一例と
して、硝酸鉛とヨウ化カリウムとを水中で反応さ
せる方法が知られている。この反応はつぎの反応
式
Pb（NO3）2＋2KI→PbI2＋2KNO3
で表わされるが、硝酸鉛の使用量は、鉛塩を有効
利用し、かつ反応後の液中に有害な鉛塩を残存さ
せたくないという観点から、従来はヨウ化カリウ
ムに対して理論モル比（１／２）ないしそれ以下
の割合とされていた。しかるに、かかる方法で得
られるヨウ化鉛を正極活物質とした固体電解質電
池は、その放電容量がバラツキやすく、また全体
に低くなる欠点があつた。 Conventionally, as an example of a method for producing this type of lead iodide, a method in which lead nitrate and potassium iodide are reacted in water has been known. This reaction is expressed by the following reaction formula: Pb(NO 3 ) 2 +2KI→PbI 2 +2KNO 3.The amount of lead nitrate used is determined by making effective use of the lead salt and ensuring that harmful lead salts remain in the solution after the reaction. Conventionally, from the viewpoint of preventing this from occurring, the ratio was set at a theoretical molar ratio (1/2) or less to potassium iodide. However, solid electrolyte batteries using lead iodide as a positive electrode active material obtained by such a method have the disadvantage that their discharge capacities tend to vary and are generally low.
そのため、本発明者らは固体電解質電池の正極
活物質として有用なヨウ化鉛を得るため種々検討
を重ね、前記反応における硝酸鉛を使用量を従来
に比べて多くすることにより、高くかつ安定した
放電容量を有するヨウ化鉛が得られることを見出
し、それについて既に特許出願をした（特願昭57
−118840号）。 Therefore, the present inventors conducted various studies in order to obtain lead iodide useful as a positive electrode active material for solid electrolyte batteries, and by increasing the amount of lead nitrate used in the reaction compared to the conventional method, we achieved high and stable lead iodide. He discovered that lead iodide with a high discharge capacity could be obtained, and had already filed a patent application for it (patent application filed in 1983).
−118840).
本発明者らは、そのような知見に基づき、さら
に研究を重ねた結果、生成したヨウ化鉛を空気に
触れさせないで乾燥するときは、放電特性がさら
に良好なヨウ化鉛が得られることを見出し、それ
に基づいて本発明を完成するにいたつた。 Based on such knowledge, the present inventors conducted further research and found that when the produced lead iodide is dried without exposing it to air, lead iodide with even better discharge characteristics can be obtained. Based on this finding, we have completed the present invention.
すなわち、本発明は水溶性鉛塩とヨウ化水素酸
またはそのアルカリ金属塩とを反応させ、生成し
たヨウ化鉛を空気が存在しない雰囲気中で乾燥す
ることを特徴とする固体電解質電池用ヨウ化鉛の
製造法に関する。 That is, the present invention provides an iodide for solid electrolyte batteries characterized by reacting a water-soluble lead salt with hydroiodic acid or an alkali metal salt thereof and drying the produced lead iodide in an air-free atmosphere. Concerning the manufacturing method of lead.
本発明において用いる水溶性鉛塩の代表的なも
のは前記例示の硝酸鉛であるが、それ以外に例え
ば酢酸鉛、Pb（SO3NH2）2、PbSiF6などを用いる
ことができる。またヨウ化水素酸またはそのアル
カリ金属塩としては、例えばヨウ化水素、ヨウ化
カリウム、ヨウ化ナトリウムなどが用いられる。 A typical water-soluble lead salt used in the present invention is the above-mentioned lead nitrate, but other materials such as lead acetate, Pb(SO 3 NH 2 ) 2 , PbSiF 6 and the like can also be used. Further, as the hydroiodic acid or its alkali metal salt, for example, hydrogen iodide, potassium iodide, sodium iodide, etc. are used.
上記水溶性鉛塩はヨウ化水素酸またはそのアル
カリ金属塩に対して理論反応モル比より多く、通
常２／２〜20／２の割合、特に好適には８／２〜
９／２の割合となるように使用するのが好まし
い。 The above-mentioned water-soluble lead salt is used in a ratio higher than the theoretical reaction molar ratio to hydroiodic acid or its alkali metal salt, usually in a ratio of 2/2 to 20/2, particularly preferably 8/2 to 20/2.
It is preferable to use a ratio of 9/2.
反応は一般に水溶性鉛塩の水溶液とヨウ化水素
酸またはそのアルカリ金属塩の水溶液とを混合す
ることによつてすみやかに進行する。その際の反
応温度は15℃以下、特に５℃以下で、反応後の凝
固点近くにするのが、放電特性の良好なヨウ化鉛
を得る観点から好ましい。 The reaction generally proceeds rapidly by mixing an aqueous solution of a water-soluble lead salt with an aqueous solution of hydriodic acid or its alkali metal salt. The reaction temperature at that time is preferably 15° C. or lower, particularly 5° C. or lower, close to the freezing point after the reaction, from the viewpoint of obtaining lead iodide with good discharge characteristics.
そして、生成したヨウ化鉛の乾燥は空気が存在
しない雰囲気中で行なわれる。具体的には例えば
生成したヨウ化鉛をただちに真空乾燥器に入れそ
のまま乾燥するか、あるいはアルゴン、ヘリウム
などの不活性気流下電気炉で乾燥することによつ
て行なわれる。乾燥温度や時間としては通常200
℃で24時間が採用される。そして、そのようにし
て乾燥したヨウ化鉛は使用直前まで不活性ガス中
で保存するのが好ましい。 The produced lead iodide is then dried in an air-free atmosphere. Specifically, for example, the produced lead iodide is immediately put into a vacuum dryer and dried as is, or it is dried in an electric furnace under an inert atmosphere of argon, helium, or the like. The drying temperature and time are usually 200
24 hours at °C is employed. The thus dried lead iodide is preferably stored in an inert gas until immediately before use.
本発明におけるように、生成したヨウ化鉛の乾
燥条件が放電性能に影響を与えるなどというよう
なことは従来はまつたく意識されず、本発明者ら
も従来は生成したヨウ化鉛を大気中で風乾した
り、60℃のインキユベーターでの乾燥など種々の
方法で乾燥していた。 As in the present invention, the fact that the drying conditions of the generated lead iodide affect the discharge performance has not been consciously known in the past, and the present inventors have also Various methods were used for drying, including air-drying at 60°C and drying in an incubator at 60°C.
ところが、前記のように水溶性鉛塩をヨウ化水
素酸またはそのアルカリ金属塩に対する理論反応
モル比より多く使用することによつて放電特性の
良好なヨウ化鉛が安定して得られるようになり、
その結果、乾燥条件がヨウ化鉛の放電性能に影響
を及ぼすことが見出され、本発明が完成されたの
である。すなわち、同じ合成条件下で合成したも
のでも乾燥時の条件が異なると放電特性にバラツ
キがあらわれることより、本発明者らは、その原
因の解明と防止対策を見出すべく鋭意研究を重
ね、空気との接触が放電性能に悪影響を及ぼすこ
と、そして、それを防止するためには不活性ガス
気流中または真空中で乾燥するなど、空気の存在
しない雰囲気中で乾燥する必要があることを見出
したのである。 However, as mentioned above, by using more water-soluble lead salt than the theoretical reaction molar ratio to hydroiodic acid or its alkali metal salt, lead iodide with good discharge characteristics can be stably obtained. ,
As a result, it was discovered that drying conditions affect the discharge performance of lead iodide, and the present invention was completed. In other words, even if the products are synthesized under the same synthesis conditions, variations in discharge characteristics will occur if the drying conditions are different.The inventors of the present invention have conducted intensive research to elucidate the cause of this phenomenon and find ways to prevent it. It was discovered that contact with the material adversely affects discharge performance, and that to prevent this, it is necessary to dry in an atmosphere free of air, such as in an inert gas stream or in a vacuum. be.
空気中の酸素のみが放電特性に悪影響を及ぼす
のか、あるいは他の成分も悪影響を及ぼすのか現
在のところ明らかではないが、酸素のみならず、
二酸化炭素も悪影響を及ぼすように考えられる。 It is currently unclear whether only oxygen in the air has a negative effect on discharge characteristics, or whether other components also have a negative effect, but not only oxygen but also
Carbon dioxide also appears to have a negative effect.
つぎに実施例おび試験例をあげて本発明を説明
する。 Next, the present invention will be explained with reference to Examples and Test Examples.
実施例
硝酸塩80ｇをイオン交換水200ｇに溶解してな
る水溶液に、この水溶液を激しく撹拌しながら、
ヨウ化カリウム20ｇをイオン交換水200ｇに溶解
してなる水溶液を一気に注ぎ込み、硝酸鉛とヨウ
化カリウムとを反応させた。反応の間、反応温度
を５℃に保つた。Example: Adding 80g of nitrate to 200g of ion-exchanged water, stirring vigorously,
An aqueous solution prepared by dissolving 20 g of potassium iodide in 200 g of ion-exchanged water was poured all at once to cause lead nitrate and potassium iodide to react. The reaction temperature was kept at 5°C during the reaction.
反応終了後、反応液を８分間静止したのち、
過し、沈澱物を別し、大量のイオン交換水でよ
く洗浄した。洗浄後、ただちに、生成したヨウ化
鉛をアルゴンで置換した電気炉に移しアルゴン気
流下に200℃で24時間乾燥して本発明の固体電解
質電池用のヨウ化鉛を得た。 After the reaction was completed, the reaction solution was allowed to stand still for 8 minutes, and then
The precipitate was separated and thoroughly washed with a large amount of ion-exchanged water. Immediately after washing, the produced lead iodide was transferred to an electric furnace purged with argon and dried at 200° C. for 24 hours under an argon stream to obtain lead iodide for the solid electrolyte battery of the present invention.
なお、上記反応におけるヨウ化カリウムに対す
る硝酸鉛の使用モル比は８／２であつた。 The molar ratio of lead nitrate to potassium iodide in the above reaction was 8/2.
比較例
実施例と同様にして硝酸鉛とヨウ化カリウムを
反応させ、反応液より沈澱物を別し、イオン交
換水で洗浄したのち、空気中、常温で48時間風乾
してヨウ化鉛を得た。Comparative Example Lead nitrate and potassium iodide were reacted in the same manner as in the example, and the precipitate was separated from the reaction solution, washed with ion-exchanged water, and then air-dried in the air at room temperature for 48 hours to obtain lead iodide. Ta.
試験例
0.88Li3N−0.12LiI化合物からなる固体電解質
50mgを内径10mm金型中で1t／cm2の加圧力で仮成形
したのち、この上に前記実施例および比較例で得
たヨウ化鉛３ｇとカルボニルニツケル１ｇとから
なる混合物150mgを充填し、7t／cm2で加圧成形し
た。得られた２層ペレツトの固体電解質側に厚さ
0.21mm、直径８mmのリチウムホイルを押し付けて
圧着し、以下、常法に準じ第１図に示すような固
体電解質電池を作製した。Test example Solid electrolyte consisting of 0.88Li 3 N−0.12LiI compound
After temporarily molding 50 mg in a mold with an inner diameter of 10 mm at a pressure of 1 t/cm 2 , 150 mg of the mixture consisting of 3 g of lead iodide and 1 g of carbonyl nickel obtained in the above examples and comparative examples was filled on top of the mold. Pressure molded at 7t/ cm2 . The thickness of the solid electrolyte side of the resulting two-layer pellet is
A lithium foil with a diameter of 0.21 mm and a diameter of 8 mm was pressed and bonded, and a solid electrolyte battery as shown in FIG. 1 was produced in accordance with a conventional method.
第１図中、１はリチウムよりなる負極、２はヨ
ウ化鉛を正極活物質とする正極、３は固体電解質
層、４は負極板、５は正極板、６はセラミツク製
リングよりなる絶縁体で、ロウ材７によつて負極
板４と正極板５に固着されている。 In Figure 1, 1 is a negative electrode made of lithium, 2 is a positive electrode made of lead iodide as a positive electrode active material, 3 is a solid electrolyte layer, 4 is a negative electrode plate, 5 is a positive electrode plate, and 6 is an insulator made of a ceramic ring. The negative electrode plate 4 and the positive electrode plate 5 are fixed to each other by a brazing material 7.
これらの固体電解質電池を20℃、30μAの定電
流で終止電圧1.4Vまで放電させたときの放電容
量を第２図に示す。 Figure 2 shows the discharge capacity of these solid electrolyte batteries when they were discharged to a final voltage of 1.4V at 20°C and a constant current of 30μA.
第２図に示すように、本発明の方法で得られた
ヨウ化鉛を用いた電池Ａは、乾燥を空気中で行な
つたヨウ化鉛を用いた電池Ｂに比べて放電容量が
大きく、乾燥を空気が存在しない雰囲気中で行な
う本発明の効果を明らかにしている。 As shown in FIG. 2, battery A using lead iodide obtained by the method of the present invention has a larger discharge capacity than battery B using lead iodide that was dried in air. The effect of the present invention in which drying is performed in an atmosphere without air is clarified.
第１図は本発明の方法で得られたヨウ化鉛を正
極活物質として用いた固体電解質電池の一例を示
す断面図であり、第２図は本発明の方法で得られ
たヨウ化鉛を正極活物質として用いた固体電解質
電池と従来法にしたがい乾燥を空気中で行なつた
ヨウ化鉛を正極活物質として用いた固体電解質電
池の放電特性図である。
２……正極、３……固体電解質層。
Figure 1 is a cross-sectional view showing an example of a solid electrolyte battery using lead iodide obtained by the method of the present invention as a positive electrode active material, and Figure 2 is a cross-sectional view showing an example of a solid electrolyte battery using lead iodide obtained by the method of the present invention. FIG. 2 is a discharge characteristic diagram of a solid electrolyte battery used as a positive electrode active material and a solid electrolyte battery using lead iodide dried in air according to a conventional method as a positive electrode active material. 2...Positive electrode, 3...Solid electrolyte layer.
Claims (1)
リ金属塩とを反応させ、生成したヨウ化鉛を空気
が存在しない雰囲気中で乾燥することを特徴とす
る固体電解質電池用ヨウ化鉛の製造法。 ２ 乾燥を不活性ガス気流中で行なう特許請求の
範囲第１項記載の固体電解質電池用ヨウ化鉛の製
造法。 ３ 乾燥を真空中で行なう特許請求の範囲第１項
記載の固体電解質電池用ヨウ化鉛の製造法。 ４ ヨウ化水素酸またはそのアルカリ金属塩に対
する水溶性鉛塩の反応モル比をその理論モル比
（１／２）より大きくした特許請求の範囲第１項、
第２項または第３項記載の固体電解質電池用ヨウ
化鉛の製造法。 ５ ヨウ化水素酸またはそのアルカリ金属塩に対
する水溶性鉛塩の反応モル比が２／２〜20／２で
ある特許請求の範囲第１項、第２項または第３項
記載の固体電解質電池用ヨウ化鉛の製造法。 ６ 反応を15℃以下で行なう特許請求の範囲第１
項、第２項、第３項、第４項または第５項記載の
固体電解質電池用ヨウ化鉛の製造法。 ７ 反応を５℃以下で行なう特許請求の範囲第１
項、第２項、第３項、第４項または第５項記載の
固体電解質電池用ヨウ化鉛の製造法。[Claims] 1. A solid electrolyte battery characterized by reacting a water-soluble lead salt with hydroiodic acid or an alkali metal salt thereof and drying the produced lead iodide in an air-free atmosphere. Manufacturing method of lead iodide. 2. A method for producing lead iodide for solid electrolyte batteries according to claim 1, wherein drying is carried out in an inert gas stream. 3. A method for producing lead iodide for solid electrolyte batteries according to claim 1, wherein drying is carried out in a vacuum. 4 Claim 1, in which the reaction molar ratio of water-soluble lead salt to hydroiodic acid or its alkali metal salt is greater than its theoretical molar ratio (1/2);
The method for producing lead iodide for solid electrolyte batteries according to item 2 or 3. 5. Solid electrolyte battery according to claim 1, 2 or 3, wherein the reaction molar ratio of water-soluble lead salt to hydroiodic acid or its alkali metal salt is from 2/2 to 20/2. Manufacturing method of lead iodide. 6 Claim 1 in which the reaction is carried out at 15°C or lower
The method for producing lead iodide for solid electrolyte batteries according to item 1, 2, 3, 4, or 5. 7 Claim 1 in which the reaction is carried out at 5°C or lower
The method for producing lead iodide for solid electrolyte batteries according to item 1, 2, 3, 4, or 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58012305A JPS59141423A (en) | 1983-01-28 | 1983-01-28 | Preparation of lead iodide for solid electrolyte cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58012305A JPS59141423A (en) | 1983-01-28 | 1983-01-28 | Preparation of lead iodide for solid electrolyte cell |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59141423A JPS59141423A (en) | 1984-08-14 |
| JPH044973B2 true JPH044973B2 (en) | 1992-01-30 |
Family
ID=11801604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58012305A Granted JPS59141423A (en) | 1983-01-28 | 1983-01-28 | Preparation of lead iodide for solid electrolyte cell |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59141423A (en) |
-
1983
- 1983-01-28 JP JP58012305A patent/JPS59141423A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59141423A (en) | 1984-08-14 |
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