JPH02277706A - Method for preparing noble metal fine particles - Google Patents
Method for preparing noble metal fine particlesInfo
- Publication number
- JPH02277706A JPH02277706A JP9976789A JP9976789A JPH02277706A JP H02277706 A JPH02277706 A JP H02277706A JP 9976789 A JP9976789 A JP 9976789A JP 9976789 A JP9976789 A JP 9976789A JP H02277706 A JPH02277706 A JP H02277706A
- Authority
- JP
- Japan
- Prior art keywords
- noble metal
- fine particles
- organic
- metal compound
- metal fine
- 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
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 54
- 239000010419 fine particle Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 13
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 claims abstract description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims abstract description 8
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 229940117955 isoamyl acetate Drugs 0.000 claims abstract description 4
- 239000008096 xylene Substances 0.000 claims abstract description 4
- 229910052737 gold Inorganic materials 0.000 claims abstract description 3
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 3
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 3
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 3
- 229910052709 silver Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 8
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000007983 Tris buffer Substances 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- -1 acetate compound Chemical class 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 19
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 1
- 150000002894 organic compounds Chemical class 0.000 abstract 1
- 239000010970 precious metal Substances 0.000 description 9
- 238000007796 conventional method Methods 0.000 description 4
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、触媒、各種ペースト、プリントの材料、その
地雷気材料分野に利用される貴金属微粒子を球状の単分
散した状態で貴金属微粒子の粒径を調製する方法に関す
るものである。Detailed Description of the Invention (Industrial Field of Application) The present invention is a method of manufacturing precious metal fine particles in a spherical monodispersed state, which is used in the field of catalysts, various pastes, printing materials, and mine materials. This invention relates to a method for adjusting the diameter.
（従来技術とその問題点）
従来貴金属微粒子の利用として、貴金属を含有するペー
スト、インキの原料や、触媒、機能膜等に貴金属を担持
、あるいは被膜を形成する等、その利用範囲は多く、し
かも高価な貴金属を有効に活用するため、粒子径が用途
に合った大きさで、粒子径の揃ったもので、サブミクロ
ン以下のものの開発が強く望まれている。(Prior art and its problems) Conventionally, precious metal fine particles have been used in many ways, such as as raw materials for pastes and inks containing precious metals, as supporting precious metals on catalysts, functional films, etc., or as forming coatings. In order to make effective use of expensive precious metals, there is a strong desire to develop particles with uniform particle sizes, submicron or smaller, that suit the application.
しかし、従来法は貴金属塩化物が多く用いられ、該塩化
物を水に溶解し高分子の界面活性剤等を加えて貴金属を
還元して貴金属微粒子を得る方法が用いられている。However, in the conventional method, a noble metal chloride is often used, and a method is used in which the chloride is dissolved in water, and a polymeric surfactant or the like is added to reduce the noble metal to obtain noble metal fine particles.
上記、従来法の欠点は粒子径が０．３μ程度が限界であ
り、しかも、貴金属微粒子を高分子の界面活性剤等の不
純物と分離するのが極めてむずかしく、微粒子が洗浄中
に凝集したりして粒子径の分布範囲が広くなりやすくな
るという欠点があった。The disadvantage of the conventional method mentioned above is that the particle size is limited to about 0.3μ, and it is extremely difficult to separate precious metal fine particles from impurities such as polymeric surfactants, and the fine particles may aggregate during cleaning. This has the disadvantage that the particle size distribution range tends to become wider.
（発明の目的）
本発明は、上記従来法の欠点を解決するためになされた
もので、貴金属微粒子の粒子径が０．０５〜０．３μの
ものを任意に調製し、しかも球状で粒径分布の範囲が狭
い貴金属微粒子を調製する方法を提供するものである。(Object of the invention) The present invention was made to solve the above-mentioned drawbacks of the conventional method. The present invention provides a method for preparing noble metal fine particles having a narrow distribution range.
（問題点を解決するための手段）
本発明は、有機貴金属化合物を有機溶媒に溶解した溶液
を加熱分解して球状の単分散した貴金属微粒子を調製す
ることを特徴とする貴金属微粒子の調製方法であり、有
機貴金属化合物の貴金属は金、銀、白金、パラジウム、
ロジウム、イリジウム、ルテニウムで、有機貴金属化合
物がトリスまたはビス（アセチルアセトアト）貴金属化
合物、貴金属酢酸化合物、アセチルアセトン貴金属化合
物、および貴金属樹脂酸塩より選択した１種または２種
以上からなり、有機溶媒がキシレン、ブロモベンゼン、
メチルイソブチルケトン、酢酸イソアミル、ジメチルス
ルフオキシドより選択した１種または２種以上から成る
ことと、加熱分解が還流器付き反応容器内で攪拌下溶液
の沸点で行われることを特徴とする貴金属微粒子の調製
方法である。(Means for Solving the Problems) The present invention provides a method for preparing noble metal fine particles, which comprises preparing spherical monodisperse noble metal fine particles by thermally decomposing a solution of an organic noble metal compound dissolved in an organic solvent. Yes, the noble metals of organic noble metal compounds include gold, silver, platinum, palladium,
Rhodium, iridium, and ruthenium, the organic noble metal compound is one or more selected from tris or bis(acetylacetoato) noble metal compound, noble metal acetate compound, acetylacetone noble metal compound, and noble metal resinate, and the organic solvent is xylene, bromobenzene,
Precious metal fine particles comprising one or more selected from methyl isobutyl ketone, isoamyl acetate, and dimethyl sulfoxide, and thermal decomposition is carried out at the boiling point of the solution under stirring in a reaction vessel equipped with a reflux device. This is a preparation method.
以下、本発明の詳細について説明する。The details of the present invention will be explained below.
本発明に用いる有機貴金属化合物として、トリスまたは
ビス（アセチルアセトアト）貴金属化合物、貴金属酢酸
塩、アセチルアセトン貴金属化合物、貴金属樹脂酸塩は
、人手しやすいと共に合成するのも比較的簡単にでき、
一般的な有機溶媒に溶解するもので、低い温度で分解し
て金属となるものであり、貴金属以外の元素が限られた
組成であるため貴金属微粒子と分離がしやすいからであ
る。As the organic noble metal compounds used in the present invention, tris or bis(acetylacetoato) noble metal compounds, noble metal acetates, acetylacetone noble metal compounds, and noble metal resinates are easy to handle and relatively easy to synthesize.
This is because it dissolves in common organic solvents and decomposes into metal at low temperatures, and because it has a composition with a limited number of elements other than noble metals, it is easy to separate it from noble metal fine particles.
有機溶媒としては、キシレン、ブロモベンゼン、メチル
イソブチルケトン（ＭＩＢＫ）、酢酸イソアミル、ジメ
チルスルフオキシドより選択した１種または２種以上を
用いるのは上記有機貴金属化合物を溶解するものを用い
て均一な溶液とすることができ、さらに有機貴金属化合
物を分解するための温度や貴金属微粒子が凝集しないた
めの適度の粘性を持たせるためである。As the organic solvent, one or more selected from xylene, bromobenzene, methyl isobutyl ketone (MIBK), isoamyl acetate, and dimethyl sulfoxide are used to dissolve the above-mentioned organic noble metal compounds and to obtain a uniform solution. This is because it can be made into a solution and has a temperature sufficient to decompose the organic noble metal compound and an appropriate viscosity to prevent noble metal fine particles from agglomerating.
該有機貴金属化合物を有機溶媒に溶解した溶液を加熱分
解する方法は、還流器付きの反応容器を用いて有機貴金
属化合物を有機溶媒に溶解した溶液の沸点で還流すると
貴金属微粒子が生成し、貴金属微粒子の粒子径を調製す
るのは、上記溶液の沸点で還流する時間で調節すること
ができる。In the method of thermally decomposing a solution of an organic noble metal compound dissolved in an organic solvent, noble metal fine particles are generated by refluxing the solution of the organic noble metal compound dissolved in an organic solvent at the boiling point using a reaction vessel equipped with a reflux device. The particle size of the solution can be adjusted by adjusting the time for refluxing the solution at its boiling point.
但し、有機貴金属化合物の有機溶媒中の濃度は１ミリモ
ル〜５ミリモルの範囲が好ましい。However, the concentration of the organic noble metal compound in the organic solvent is preferably in the range of 1 mmol to 5 mmol.
上記の条件で還流すると貴金属微粒子の粒子径は０．０
５〜０．３μのものが得られ、その粒子径の大きさは還
流時間に比例しており、２０分間程度を過ぎると変化せ
ずに一定の粒子径を保つようになり、その微粒子は単分
散したものである。When refluxed under the above conditions, the particle diameter of precious metal fine particles is 0.0.
5 to 0.3 μm are obtained, and the particle size is proportional to the reflux time, and after about 20 minutes, the particle size remains constant without changing. It is dispersed.
以下、本発明の実施例を記載するが該実施例は本発明を
限定するものではない。Examples of the present invention will be described below, but the examples are not intended to limit the present invention.
（実施例１）
酢酸パラジウムをメチルイソブチルケトンに溶解して、
２ミリモルの溶液とし、これを攪拌しながら、還流器付
きフラスコ内で溶液の沸点で１時間還流したところ、平
均粒径０．２７μの球状の単分散したパラジウムの微粒
子が得られた。(Example 1) Palladium acetate was dissolved in methyl isobutyl ketone,
A 2 mmol solution was prepared, and this was refluxed for 1 hour at the boiling point of the solution in a flask equipped with a reflux device while stirring, to obtain spherical monodispersed fine palladium particles with an average particle size of 0.27 μm.
（実施例２）
酢酸パラジウムをメチルイソブチルケトンに溶解して、
２ミリモルの溶液とし、これを攪拌しながら、還流器付
きフラスコ内で溶液の沸点で還流時間を２分、５分、１
０分、１５分、２０分、３０分、４０分の７段階に分け
て行ったところ、平均粒径は、２分では０．０５μ、５
分では０．１μ、１０分では０．１５μ、１５分では０
．２１μ、２０分では０．２７μ、３０分では０．２６
μ、４０分では０．２７μで、それぞれ球状の単分散し
たパラジウムの微粒子が得られた。(Example 2) Palladium acetate was dissolved in methyl isobutyl ketone,
A 2 mmol solution was prepared, and while stirring, the solution was refluxed for 2 minutes, 5 minutes, and 1 minute at the boiling point of the solution in a flask equipped with a reflux device.
When the test was carried out in 7 stages: 0 minutes, 15 minutes, 20 minutes, 30 minutes, and 40 minutes, the average particle size was 0.05 μ at 2 minutes, 5 μ
0.1μ for minutes, 0.15μ for 10 minutes, 0 for 15 minutes
．． 21μ, 0.27μ for 20 minutes, 0.26 for 30 minutes
After 40 minutes, spherical and monodispersed palladium fine particles were obtained.
（実施例３）
酢酸パラジウムを有機溶媒として、メチルイソブチルケ
トンを用いて０．５〜４．ＧミｌＪモル／βの濃度で段
階的に溶解した溶液を実施例１と同様に沸点でそれぞれ
４０分間還流して生成したパラジウムの微粒子の粒子径
を測定したところ下記の表−１のような結果であった。(Example 3) Using palladium acetate as an organic solvent and using methyl isobutyl ketone, 0.5 to 4. The particle size of the palladium fine particles produced by refluxing the solution in steps at a concentration of G mil J mol/β for 40 minutes at the boiling point as in Example 1 was measured, and the results were as shown in Table 1 below. It was the result.
酢酸パラジウムを有機溶媒として、ブロモベンゼン、オ
ルトキシレン、ジメチルスルフオキシドを用いて０．１
〜３．０ミＩＪモル／ｉの濃度で段階的に溶解した溶液
を実施例１と同様に沸点でそれぞれ４０分間還流して生
成したパラジウムの微粒子の粒子径を測定したところ下
記の表−２、表−３、表−４のような結果であった。0.1 using palladium acetate as an organic solvent, bromobenzene, ortho-xylene, and dimethyl sulfoxide.
The particle size of the fine palladium particles produced by refluxing the solution in stages at a concentration of ~3.0 mmIJmol/i for 40 minutes at the boiling point in the same manner as in Example 1 was measured, and the results are shown in Table 2 below. The results were as shown in Table 3 and Table 4.
〔結果１−有機溶媒ブロモベンゼン〕 （以下余白） （実施例４） 貴金属化合物を使用するようにしてもよいものである。[Result 1-Organic solvent bromobenzene] (Margin below) (Example 4) A noble metal compound may also be used.
（発明の効果）
本発明は、従来法では得られなかったサブミクロン以下
の貴金属微粒子を任意の粒子径に調製することができ、
しかも単分散して球状の粒径分布の幅の狭い安定したも
のを調製することが可能となり、触媒、ペースト、薄膜
形成材料等、化学工業、電気工業、電子工業等に於ける
貴金属微粒子の利用分野の拡大に貢献できるものである
。(Effects of the Invention) The present invention can prepare noble metal fine particles of submicron or less, which could not be obtained by conventional methods, to any particle size.
Furthermore, it has become possible to prepare stable monodispersed spherical particles with a narrow particle size distribution, making it possible to use precious metal fine particles in catalysts, pastes, thin film forming materials, etc. in the chemical industry, electrical industry, electronic industry, etc. It can contribute to the expansion of the field.
出願人 田中貴金属工業株式会社 目黒謙次部 江角邦男Applicant: Tanaka Kikinzoku Kogyo Co., Ltd. Kenjibe Meguro Kunio Esumi
Claims (5)
熱分解して球状の単分散した貴金属微粒子を調製するこ
とを特徴とする貴金属微粒子の調製方法。(1) A method for preparing noble metal fine particles, which comprises preparing spherical monodispersed noble metal fine particles by thermally decomposing a solution of an organic noble metal compound dissolved in an organic solvent.
ジウム、ロジウム、イリジウム、ルテニウムであること
を特徴とする請求項１の貴金属微粒子の調製方法。(2) The method for preparing noble metal fine particles according to claim 1, wherein the noble metal of the organic noble metal compound is gold, silver, platinum, palladium, rhodium, iridium, or ruthenium.
アセトアト）貴金属化合物、貴金属酢酸化合物、アセチ
ルアセトン貴金属化合物、貴金属樹脂酸塩であることを
特徴とする請求項１または２の貴金属微粒子の調製方法
。(3) The method for preparing noble metal fine particles according to claim 1 or 2, wherein the organic noble metal compound is a tris or bis(acetylacetoato) noble metal compound, a noble metal acetate compound, an acetylacetone noble metal compound, or a noble metal resinate.
ソブチルケトン、酢酸イソアミル、ジメチルスルフォキ
シドより選択した１種または２種以上から成ることを特
徴とする請求項１の貴金属微粒子の調製方法。(4) The method for preparing noble metal fine particles according to claim 1, wherein the organic solvent comprises one or more selected from xylene, bromobenzene, methyl isobutyl ketone, isoamyl acetate, and dimethyl sulfoxide.
沸点で行われることを特徴とする請求項１の貴金属微粒
子の調製方法。(5) The method for preparing noble metal fine particles according to claim 1, wherein the thermal decomposition is carried out at the boiling point of the solution under stirring in a reaction vessel equipped with a reflux device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1099767A JP2749863B2 (en) | 1989-04-19 | 1989-04-19 | Preparation method of noble metal fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1099767A JP2749863B2 (en) | 1989-04-19 | 1989-04-19 | Preparation method of noble metal fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02277706A true JPH02277706A (en) | 1990-11-14 |
| JP2749863B2 JP2749863B2 (en) | 1998-05-13 |
Family
ID=14256123
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1099767A Expired - Lifetime JP2749863B2 (en) | 1989-04-19 | 1989-04-19 | Preparation method of noble metal fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2749863B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5250101A (en) * | 1991-04-08 | 1993-10-05 | Mitsubishi Gas Chemical Company, Inc. | Process for the production of fine powder |
| CN112771186A (en) * | 2019-07-18 | 2021-05-07 | 斯沃奇集团研究和开发有限公司 | Method for producing an alloy of noble metals and alloy of noble metals thus obtained |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS505996A (en) * | 1973-05-21 | 1975-01-22 | ||
| JPS61107937A (en) * | 1984-11-01 | 1986-05-26 | Agency Of Ind Science & Technol | Preparation of noble metal organosol |
| JPS62121640A (en) * | 1985-11-21 | 1987-06-02 | Agency Of Ind Science & Technol | Preparation of noble metal organosol |
-
1989
- 1989-04-19 JP JP1099767A patent/JP2749863B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS505996A (en) * | 1973-05-21 | 1975-01-22 | ||
| JPS61107937A (en) * | 1984-11-01 | 1986-05-26 | Agency Of Ind Science & Technol | Preparation of noble metal organosol |
| JPS62121640A (en) * | 1985-11-21 | 1987-06-02 | Agency Of Ind Science & Technol | Preparation of noble metal organosol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5250101A (en) * | 1991-04-08 | 1993-10-05 | Mitsubishi Gas Chemical Company, Inc. | Process for the production of fine powder |
| CN112771186A (en) * | 2019-07-18 | 2021-05-07 | 斯沃奇集团研究和开发有限公司 | Method for producing an alloy of noble metals and alloy of noble metals thus obtained |
| CN112771186B (en) * | 2019-07-18 | 2022-04-19 | 斯沃奇集团研究和开发有限公司 | Method for producing an alloy of noble metals and alloy of noble metals thus obtained |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2749863B2 (en) | 1998-05-13 |
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