JPH04126373A - Secondary battery - Google Patents
Secondary batteryInfo
- Publication number
- JPH04126373A JPH04126373A JP2249495A JP24949590A JPH04126373A JP H04126373 A JPH04126373 A JP H04126373A JP 2249495 A JP2249495 A JP 2249495A JP 24949590 A JP24949590 A JP 24949590A JP H04126373 A JPH04126373 A JP H04126373A
- Authority
- JP
- Japan
- Prior art keywords
- battery
- carbon material
- negative electrode
- sulfur element
- cation
- 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
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 21
- 239000011593 sulfur Substances 0.000 claims abstract description 21
- 150000001768 cations Chemical class 0.000 claims abstract description 11
- 239000011255 nonaqueous electrolyte Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 4
- 239000000571 coke Substances 0.000 abstract description 3
- 239000006230 acetylene black Substances 0.000 abstract description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 229920002239 polyacrylonitrile Polymers 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- 229910052744 lithium Inorganic materials 0.000 description 9
- 238000006477 desulfuration reaction Methods 0.000 description 8
- 230000023556 desulfurization Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000002006 petroleum coke Substances 0.000 description 6
- 239000011335 coal coke Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- -1 aluminum Chemical compound 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 2
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000003466 welding 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
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
【発明の詳細な説明】 （イ） 産業上の利用分野 本発明は、非水電解液を用いた二次電池に関する。[Detailed description of the invention] (b) Industrial application fields The present invention relates to a secondary battery using a non-aqueous electrolyte.
（ロ） 従来の技術
リチウムを負極活物質とした二次電池は、そのエネルギ
ー密度が大きく、特に研究が盛んである。この種、二次
電池は、そのリチウムの充放電効率が低いために、サイ
クル特性に問題がある。(b) Conventional technology Secondary batteries using lithium as a negative electrode active material have a high energy density, and are currently being actively researched. This type of secondary battery has a problem with cycle characteristics because its lithium charging and discharging efficiency is low.
これを解決するために、リチウムと合金化する金属、た
とえばアルミニウムを用いてリチウム−アルミニウム合
金を形成して、これを負極とする方法や、Ｌ ＩＡ ｓ
Ｆ ａ系の電解液を用いてリチウムの充放電効率を向
上させ、サイクル特性の向上を計る方法が提案されてい
る。In order to solve this problem, there is a method of forming a lithium-aluminum alloy using a metal that alloys with lithium, such as aluminum, and using this as a negative electrode, and a method of using LIAs as a negative electrode.
A method has been proposed for improving lithium charging and discharging efficiency using an F a -based electrolyte to improve cycle characteristics.
しかし、前者の方法では作動電圧が低下するという欠点
があり、後者の方法では電解液が有毒であり安全性の面
で問題が生じる。However, the former method has the disadvantage that the operating voltage is reduced, and the latter method has a toxic electrolyte, which poses a safety problem.
これらの問題点を改善するために、カーボン系の物質を
負極基材として用い、ここにリチウムを吸蔵、放出させ
て負極を構成する方法が提案されている。この場合は、
前記せるような作動電圧の低下や毒性はなく、エネルギ
ー密度も大きい。In order to improve these problems, a method has been proposed in which a carbon-based material is used as a negative electrode base material, and lithium is intercalated and released therein to form a negative electrode. in this case,
There is no drop in operating voltage or toxicity as mentioned above, and the energy density is high.
然し乍ら、不純物、特にコークス等の原料に含まれてい
る硫黄成分が、カチオンであるリチウムと反応し、保存
特性が低下するという問題がある。However, there is a problem in that impurities, particularly sulfur components contained in raw materials such as coke, react with lithium, which is a cation, and the storage properties deteriorate.
（ハ） 発明が解決しようとする課題
本発明は前記問題点に鑑みて成されたものであって、炭
素材料中の硫黄成分と、カチオン例えばリチウムとの反
応を抑制することによって、サイクル特性が高く、且つ
保存特性に優れた二次電池を提供しようとするものであ
る。(c) Problems to be Solved by the Invention The present invention has been made in view of the above-mentioned problems, and improves the cycle characteristics by suppressing the reaction between the sulfur component in the carbon material and a cation such as lithium. The aim is to provide a secondary battery that is high in cost and has excellent storage characteristics.
（ニ） 課題を解決するための手段
本発明は、正極と、カチオンを吸蔵、放出する炭素材料
よりなる負極と、非水電解液とを有する電池であって、
前記炭素材料が、硫黄成分が抑制されたものであること
を特徴とする。(d) Means for Solving the Problems The present invention is a battery having a positive electrode, a negative electrode made of a carbon material that occludes and releases cations, and a non-aqueous electrolyte, comprising:
The carbon material is characterized in that a sulfur component is suppressed.
ここで前記硫黄成分としては、５％以下とするのが、電
池の保存特性上、好ましい。Here, the sulfur component is preferably 5% or less from the viewpoint of storage characteristics of the battery.
また、前記カチオンとしては、リチウムイオンやナトリ
ウムイオン等のアルカリ金属イオン、カリウムイオンや
マグネシウムイオン等のアルカリ土類金属イオン、アル
ミニウムイオン等が挙げられる。Examples of the cations include alkali metal ions such as lithium ions and sodium ions, alkaline earth metal ions such as potassium ions and magnesium ions, and aluminum ions.
（ホ）作用
負極を構成する炭素材料は、カチオン、例えばリチウム
イオンを吸蔵、放出することができるが、従来の炭素材
料では硫黄成分が多く、これと吸蔵したカチオンが反応
して、電池の自己放電反応を生じていた。(e) The carbon material constituting the working negative electrode can absorb and release cations, such as lithium ions, but conventional carbon materials have a large sulfur component, and the absorbed cations react with this, causing the battery to self-isolate. A discharge reaction was occurring.
しかし、本発明では負極に硫黄成分が抑制された炭素材
料を用いているため、自己放電反応がほとんど生じない
。このために保存特性が向上する。However, in the present invention, since a carbon material with a suppressed sulfur component is used for the negative electrode, almost no self-discharge reaction occurs. This improves storage properties.
ここで用いる炭素材料としては、ポリアクリロニトリル
などの高分子を焼成した熱処理炭素、各種コークス、黒
鉛、更にはアセチレンブラック等の無定形炭素等があげ
られる。Examples of the carbon material used here include heat-treated carbon obtained by firing a polymer such as polyacrylonitrile, various types of coke, graphite, and amorphous carbon such as acetylene black.
（へ） 実施例 以下に、実施例を示し、本発明を具体的に説明する。(f) Examples EXAMPLES Below, the present invention will be specifically explained with reference to Examples.
［実施例１コ
石油コークスを粉砕し、４００メツシユパスした後、反
応温度３００℃、反応圧力５０ｋｇ／ｍ”、水素循環量
１００ｍ”／ｋＪ＋にて、石油コークスを水素化精製す
ることで脱硫を行った。この脱硫後の硫黄成分は０．５
％であった。尚、ここで石油コークスを脱硫するために
、水素を使用しているが、酸素を用いても同様の脱硫を
行うことができる。そして、このように脱硫した炭素材
料である石油コークスを、金属リチウム粉末と混合、プ
レスして、負極を作製した。[Example 1] After pulverizing petroleum coke and passing it through 400 meshes, desulfurization was carried out by hydrorefining the petroleum coke at a reaction temperature of 300°C, a reaction pressure of 50 kg/m", and a hydrogen circulation rate of 100 m"/kJ+. Ta. The sulfur component after this desulfurization is 0.5
%Met. Note that although hydrogen is used here to desulfurize the petroleum coke, similar desulfurization can be performed using oxygen. Then, petroleum coke, which is a carbon material desulfurized in this way, was mixed with metallic lithium powder and pressed to produce a negative electrode.
一方、正極としては二酸化マンガンを用い、過塩素酸リ
チウム／プロピレンカーボネート溶液を電解液として、
第１図に示す本発明電池Ａを組み立てた。On the other hand, manganese dioxide was used as the positive electrode, and lithium perchlorate/propylene carbonate solution was used as the electrolyte.
The battery A of the present invention shown in FIG. 1 was assembled.
第１図は、本発明電池の縦断面図である。第１図中、１
は正極外装体、２は負極外装体であり、絶縁性の樹脂か
ら成る絶縁バッキング３で、絶縁されている。また、４
は正極、５は負極であり、セパレータ６によって隔離さ
れている。また、前記正極外装体１の内底面には正極集
電体７が、前記負極外装体２の内底面には負極集電体８
が、それぞれ溶接固定されている。FIG. 1 is a longitudinal sectional view of the battery of the present invention. In Figure 1, 1
2 is a positive electrode housing, and 2 is a negative electrode housing, which are insulated with an insulating backing 3 made of an insulating resin. Also, 4
is a positive electrode, and 5 is a negative electrode, which are separated by a separator 6. Further, a positive electrode current collector 7 is disposed on the inner bottom surface of the positive electrode outer casing 1, and a negative electrode current collector 8 is disposed on the inner bottom surface of the negative electrode casing 2.
are fixed by welding.
［比較例１］
負極に脱硫処理を行わない石油コークスを炭素材料とし
て用いた以外は、前記実施例１と同様の炭素材料を使用
して、比較電池Ｘを組み立てた。[Comparative Example 1] Comparative battery X was assembled using the same carbon material as in Example 1, except that petroleum coke, which was not subjected to desulfurization treatment, was used as the carbon material for the negative electrode.
尚、この脱硫処理を施していない石油コークスの硫黄成
分は１０％であった。Note that the sulfur component of the petroleum coke that was not subjected to the desulfurization treatment was 10%.
これらの電池Ａ、Ｘを用い、電池の保存特性を比較した
。この時の実験条件は、１０ｍＡｈで１０回充放電した
後、１０ｍＡｈ充電し、６０℃で保存し、電池の放電容
量を測定するというものである。Using these batteries A and X, the storage characteristics of the batteries were compared. The experimental conditions at this time were to charge and discharge at 10 mAh 10 times, then charge at 10 mAh, store at 60° C., and measure the discharge capacity of the battery.
第２図に、この結果を示す。第２図は、電池の保存特性
図である。これより、本発明電池Ａは３０日経過しても
容量残存率が９５％あるのに対し、比較電池Ｘは７０％
しか容量残存率がない。Figure 2 shows the results. FIG. 2 is a diagram showing the storage characteristics of the battery. From this, battery A according to the invention has a remaining capacity rate of 95% even after 30 days, while comparative battery X has a remaining capacity rate of 70%.
However, there is no remaining capacity.
このように本発明電池Ａは、保存特性において優れたも
のであることが分かる。Thus, it can be seen that the battery A of the present invention has excellent storage characteristics.
［実施例２コ
石炭コークスを粉砕し、４００メツシユパスした後、反
応温度３００℃、反応圧力５０ｋｇ／が、水素循環量１
００ｍ”／Ｖにて、石炭コークスを水素化精製すること
で脱硫した。この脱硫後の硫黄成分は０．９％であった
。このように脱硫した炭素材料である石炭コークスを、
金属リチウム粉末と混合、プレスすることにより、負極
を作製した。[Example 2] After pulverizing coal coke and passing it through 400 meshes, the reaction temperature was 300°C, the reaction pressure was 50 kg/, and the amount of hydrogen circulation was 1.
Coal coke was desulfurized by hydrorefining at 00 m"/V. The sulfur content after desulfurization was 0.9%. Coal coke, which is a carbon material desulfurized in this way,
A negative electrode was produced by mixing with metal lithium powder and pressing.
一方、正極として二酸化マンガンを用いて、過塩素酸リ
チウム／プロピレンカーボネート溶液を電解液として、
前記第１図に示す構造と同一構造を有する、本発明電池
Ｂを組み立てた。On the other hand, using manganese dioxide as the positive electrode and lithium perchlorate/propylene carbonate solution as the electrolyte,
A battery B of the present invention having the same structure as shown in FIG. 1 was assembled.
［比較例２コ
負極に脱硫処理を行わない石炭コークスを炭素材料とし
て用いた以外は、前記実施例２と同様の炭素材料を使用
して、比較電池Ｙを組み立てた。Comparative Example 2 A comparative battery Y was assembled using the same carbon material as in Example 2, except that coal coke without desulfurization treatment was used as the carbon material for the negative electrode.
尚、この脱硫処理を施していない石炭コークスの硫黄成
分は１０％であった。Incidentally, the sulfur content of the coal coke that was not subjected to this desulfurization treatment was 10%.
これらの電池Ｂ、Ｙを用い、電池の保存特性を比較した
。この時の実験条件は、１０ｍＡｈで１０回充放電した
後、１０ ｍ Ａ ｈ充電し、６０℃で保存し、電池の
放電容量を測定するというものである。Using these batteries B and Y, the storage characteristics of the batteries were compared. The experimental conditions at this time were to charge and discharge at 10 mAh 10 times, then charge at 10 mAh, store at 60° C., and measure the discharge capacity of the battery.
第３図に、この結果を示す。第３図は、電池の保存特性
図である。これより、本発明電池Ｂは３０日経過しても
容量残存率が９５％あるのに対し、比較電池Ｙは５０％
しか容量残存率がない。Figure 3 shows the results. FIG. 3 is a diagram showing the storage characteristics of the battery. From this, inventive battery B has a remaining capacity rate of 95% even after 30 days, while comparative battery Y has a remaining capacity rate of 50%.
However, there is no remaining capacity.
このように本発明電池Ｂは、保存特性において優れたも
のであることが理解される。It is thus understood that the battery B of the present invention has excellent storage characteristics.
次に、負極を構成する炭素材料中の硫黄の濃度と、電池
の自己放電率との関係を調べた。Next, we investigated the relationship between the concentration of sulfur in the carbon material constituting the negative electrode and the self-discharge rate of the battery.
この結果を、第４図に示す。第４図は、硫黄の濃度と、
電池の自己放電率との関係を示す図である。これより、
炭素材料中における硫黄の濃度を５％以下とするのが、
電池の保存特性上、好ましいことが分かる。The results are shown in FIG. Figure 4 shows the concentration of sulfur and
FIG. 3 is a diagram showing the relationship with the self-discharge rate of a battery. Than this,
Setting the concentration of sulfur in the carbon material to 5% or less is
It can be seen that this is preferable in terms of storage characteristics of the battery.
（ト）発明の効果
以上述べた如く、本発明によれば、電池の保存特性を向
上させることが可能となり、その工業的価値は極めて大
きい。(G) Effects of the Invention As described above, according to the present invention, it is possible to improve the storage characteristics of a battery, and its industrial value is extremely large.
第１図は本発明電池の縦断面図、第２図及び第３図は電
池の保存特性図、第４図は硫黄の濃度と電池の自己放電
率の関係を示す図である。
１・・・・・正極外装体、２・・・ 負極外装体、３・
・絶縁バッキング、４ ・ ・正極、５・・・・負極、
６・・・・・セパレータ、７ ・・・・・・・・負極集
電体、
Ａ、Ｂ・・・・本発明電池、
Ｘ、Ｙ・・・・比較電池。
正極集電体、FIG. 1 is a longitudinal sectional view of the battery of the present invention, FIGS. 2 and 3 are storage characteristic diagrams of the battery, and FIG. 4 is a diagram showing the relationship between the sulfur concentration and the self-discharge rate of the battery. 1... Positive electrode exterior body, 2... Negative electrode exterior body, 3.
・Insulating backing, 4...Positive electrode, 5...Negative electrode,
6...Separator, 7...Negative electrode current collector, A, B...Battery of the present invention, X, Y...Comparative battery. positive electrode current collector,
Claims (2)
なる負極と、非水電解液とを有する電池であって、 前記炭素材料が、硫黄成分が抑制されたものであること
を特徴とする二次電池。(1) A battery comprising a positive electrode, a negative electrode made of a carbon material that occludes and releases cations, and a non-aqueous electrolyte, characterized in that the carbon material has a suppressed sulfur component. Secondary battery.
る請求項１記載の二次電池。(2) The secondary battery according to claim 1, wherein the sulfur component is 5% or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP02249495A JP3133317B2 (en) | 1990-09-18 | 1990-09-18 | Rechargeable battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP02249495A JP3133317B2 (en) | 1990-09-18 | 1990-09-18 | Rechargeable battery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04126373A true JPH04126373A (en) | 1992-04-27 |
| JP3133317B2 JP3133317B2 (en) | 2001-02-05 |
Family
ID=17193821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP02249495A Expired - Fee Related JP3133317B2 (en) | 1990-09-18 | 1990-09-18 | Rechargeable battery |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3133317B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0810680A2 (en) * | 1996-05-27 | 1997-12-03 | SANYO ELECTRIC Co., Ltd. | Non-aqueous electrolyte battery with carbon electrode |
| CN102399339A (en) * | 2010-09-08 | 2012-04-04 | 清华大学 | Preparation method of sulfurized polyacrylonitrile |
-
1990
- 1990-09-18 JP JP02249495A patent/JP3133317B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0810680A2 (en) * | 1996-05-27 | 1997-12-03 | SANYO ELECTRIC Co., Ltd. | Non-aqueous electrolyte battery with carbon electrode |
| EP0810680A3 (en) * | 1996-05-27 | 1998-08-05 | SANYO ELECTRIC Co., Ltd. | Non-aqueous electrolyte battery with carbon electrode |
| US5888671A (en) * | 1996-05-27 | 1999-03-30 | Sanyo Electric Co., Ltd. | Non-aqueous electrolyte battery |
| CN102399339A (en) * | 2010-09-08 | 2012-04-04 | 清华大学 | Preparation method of sulfurized polyacrylonitrile |
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|---|---|
| JP3133317B2 (en) | 2001-02-05 |
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