JPS61105847A - Method for cleaning substrate surface - Google Patents
Method for cleaning substrate surfaceInfo
- Publication number
- JPS61105847A JPS61105847A JP22752984A JP22752984A JPS61105847A JP S61105847 A JPS61105847 A JP S61105847A JP 22752984 A JP22752984 A JP 22752984A JP 22752984 A JP22752984 A JP 22752984A JP S61105847 A JPS61105847 A JP S61105847A
- Authority
- JP
- Japan
- Prior art keywords
- water
- wafer
- sulfuric acid
- hydrogen peroxide
- mixed
- 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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
Abstract
Description
【発明の詳細な説明】
（１）発明の技術分野
本発明は半導体基板表面洗浄方法、例えば半導体集積回
路（ＩＣ）の製造工程においてシリコンウェハの表面を
洗浄する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (1) Technical Field of the Invention The present invention relates to a method for cleaning the surface of a semiconductor substrate, for example, a method for cleaning the surface of a silicon wafer in the manufacturing process of a semiconductor integrated circuit (IC).
（２）技術の背景
ＩＣの製造過程ではシリコン基板に不純物が入ることを
防止するため、シリコンウェハの洗浄が頻繁に行われる
。一般的な工程においては、先ずウェハを洗浄し、熱酸
化によりウェハ表面に酸化膜を形成し、マスクを用いレ
ジストを塗布して各種の処理を行い、レジスト除去後に
洗浄を行い、次いで熱処理などを行いその後に洗浄をな
すという具合に、工程のきわめて多くの段階で洗浄がな
される。レジストが残存していたりその他の有機系の不
純物が基板表面に付着したままで熱処理を行うと不純物
が基板内にしみ込み製造されるＩＣの特性に悪影響を及
ぼすから、ウェハの洗浄はきわめて重要である。(2) Background of the Technology In the process of manufacturing ICs, silicon wafers are frequently cleaned to prevent impurities from entering the silicon substrate. In a typical process, the wafer is first cleaned, an oxide film is formed on the wafer surface by thermal oxidation, resist is applied using a mask and various treatments are performed, the resist is removed and then cleaned, and then heat treatment etc. Cleaning is performed at numerous stages of the process, such as cleaning and subsequent cleaning. Cleaning the wafer is extremely important because if heat treatment is performed with resist remaining or other organic impurities still attached to the substrate surface, the impurities will seep into the substrate and adversely affect the characteristics of the IC being manufactured. be.
ウェハの洗浄には種々の薬液が用いられるが、硫酸（Ｈ
２ＳＯ４）と過酸化水素（ＩＩ２０２）の混液を１００
°Ｃ程度に昇温し、先ずそれを用いてレジスト除去を含
めてウェハを洗浄し、次いで純水で再度洗浄する。それ
には模式的に第１図（ａ）に示されるディップ方式と同
図（ｂ）に示される噴霧方式とがあり、図において、１
はシリコンウェハ、２は石英製の加熱槽、３は混液供給
管、４はヒータを示す。Various chemical solutions are used to clean wafers, but sulfuric acid (H
2SO4) and hydrogen peroxide (II202) at 100%
The temperature is raised to about .degree. C., and the wafer is first cleaned, including resist removal, and then cleaned again with pure water. There are two types of methods: the dip method schematically shown in FIG. 1(a) and the spray method shown in FIG. 1(b).
2 is a silicon wafer, 2 is a quartz heating tank, 3 is a mixed liquid supply pipe, and 4 is a heater.
ディップ方式では前記Ｈ２ＳＯ４＋Ｉ１．Ｌ０２の混液
５を充たした槽２内にウェハ１を浸漬し、槽の下方のヒ
ータ４で混液を１００°Ｃ程度に加温する。In the dip method, the H2SO4+I1. The wafer 1 is immersed in a tank 2 filled with a mixed liquid 5 of L02, and the mixed liquid is heated to about 100° C. by a heater 4 located below the tank.
噴霧方式では、１００’Ｃに加温した混液を供給管３か
ら霧状に噴出させてウェハ１を洗浄する。In the spray method, the wafer 1 is cleaned by spraying a mixed liquid heated to 100'C from the supply pipe 3 in the form of mist.
（３）従来技術と問題点
従来のディップ方式ではヒータを設けた加熱槽が必要で
、また噴霧方式では予め加熱した混液を噴射させる必要
があり、いずれの方式においても装置と配管の材料、そ
れの加工、および操作における安全上の問題があった。(3) Prior art and problems The conventional dip method requires a heating tank equipped with a heater, and the spray method requires spraying a preheated mixture. There were safety issues during processing and operation.
１００°Ｃに加熱された混液は加熱槽や混液供給管それ
自体を侵すものであって、洗浄に用いる混液に装置や配
管材料が混入することがあり、そうなると完全な洗浄が
なされないから、装置の製作、運営がきわめて難しくな
り、他方ヒータを用いたり混液を１００℃にまで加熱す
るについては、電力の消費の問題もある。The mixed liquid heated to 100°C will corrode the heating tank and the mixed liquid supply pipe itself, and equipment and piping materials may get mixed into the mixed liquid used for cleaning, and if this happens, complete cleaning will not be possible. It becomes extremely difficult to manufacture and operate the system, and on the other hand, there is also the problem of power consumption when using a heater or heating the mixed liquid up to 100°C.
（４）発明の目的
本発明は上記従来の問題に浴み、加熱ヒータまたは混液
加熱の必要がなく、装置、配管材等の設計自由度があり
安全性が高められた基板表面洗浄方法を提供することを
目的とする。(4) Purpose of the Invention The present invention addresses the above-mentioned conventional problems and provides a substrate surface cleaning method that does not require a heater or mixed liquid heating, has a degree of freedom in designing equipment, piping materials, etc., and has improved safety. The purpose is to
（５）発明の構成
そしてこの目的は本発明によれば、硫酸と無水硫酸との
混液（以下オリラムと称す。）を洗浄すべき基板表面に
隣接する位置で水と混合させ、かくして得られた混合液
と過酸化水素とを混合して基板表面上に供給することを
特徴とする基板表面洗浄方法、および前記硫酸と無水硫
酸との混液、過酸化水素および水をそれぞれ供給する管
の出口を基板表面に隣接して配置し、噴霧状に基板表面
に向けて供給し、基板表面上に混合発熱領域を形成する
ことを特徴とする基板表面洗浄方法を提供することによ
って達成される。(5) Structure and object of the invention According to the present invention, a mixture of sulfuric acid and sulfuric anhydride (hereinafter referred to as Orilum) is mixed with water at a position adjacent to the surface of the substrate to be cleaned, and the thus obtained A substrate surface cleaning method characterized by mixing a mixed solution and hydrogen peroxide and supplying the mixture onto the substrate surface, and an outlet of a pipe that supplies the mixed solution of sulfuric acid and sulfuric anhydride, hydrogen peroxide, and water, respectively. This is achieved by providing a method for cleaning a substrate surface, characterized in that the method is disposed adjacent to the substrate surface and is supplied in the form of a spray toward the substrate surface to form a mixed heating region on the substrate surface.
（６）発明の実施例 以下本発明の実施例を図面によって詳述する。(6) Examples of the invention Embodiments of the present invention will be described in detail below with reference to the drawings.
本発明はオリラムに水を加えると、オリラム中の無水硫
酸（Ｓ０３）と水が反応し硫酸を生じ、しかも大きな反
応熱により昇温した熱濃硫酸が得られる事実を利用する
ものである。The present invention utilizes the fact that when water is added to orylum, the sulfuric anhydride (S03) in orylum reacts with water to produce sulfuric acid, and hot concentrated sulfuric acid whose temperature is raised due to the large heat of reaction is obtained.
ＳＯ３＋ ０２０ −→ＩＩ２．Ｓｏ＋＋ ２１ Ｋｃ
ａｌ／ｍｇそしてオリラム中の無水硫酸の濃度と加える
水の量およびそのときの発熱量、ならびに硫酸の濃度（
洗浄の度合は硫酸濃度に正比例する）について実験をな
した。SO3+ 020 −→II2. So++ 21 Kc
al/mg, the concentration of sulfuric anhydride in orilum, the amount of water added and the calorific value at that time, and the concentration of sulfuric acid (
The degree of cleaning is directly proportional to the sulfuric acid concentration).
この実験においては第２図に断面図で示す装置を用い、
同図において、１１は４つロフラスコ（容量５００ｍβ
）、１２は断熱材１３を充填した槽、１４は圧抜き口、
１５はオリラムと硫酸混液役人容器、１６は６４ｒ、ｐ
、ｍ、の攪拌モータ、１７は温度計、１８は水（Ｈ２Ｏ
）を示す。かかる装置を用いた実験によって次のデータ
か（Ｍられた。In this experiment, we used the device shown in cross section in Figure 2.
In the same figure, 11 indicates four Lof flasks (capacity 500 mβ).
), 12 is a tank filled with heat insulating material 13, 14 is a pressure release port,
15 is an official container containing orilum and sulfuric acid mixture, 16 is 64r, p
, m, stirring motor, 17 is a thermometer, 18 is water (H2O
) is shown. The following data were obtained from experiments using such an apparatus.
オ リ ウ ム ＩＩ、Ｏｌｌ
２Ｓｏ。Ollium II
2So.
濃度 仕込量 仕込時間 仕込量 温度 濃度（％）（
ｇ）（秒） （ｇ） （”Ｃ）（％）０
５００ ３１．４ １０ ４２ ９７．７５
５００ ３１．４ １６ ６０ ９７．８７
５００ ３１．４ １８ ７５ ９７．４
Ｂ ５００ ３１．４ １９ ８０ ９７
．９１０ ５００ ３＋、／Ｉ ２１．５
９０ ９７．６１０ ５００ ３Ｌ、１ ２１
．５ ９０ ９８．０２０ ５００ ３１．４
２１．５ ９０ ９８．０２５ ５００ ３２．
２ ３９．０ １４５ ９７．７上記データで、オ
リラム濃度０ば硫酸のみの場合を、また５％、７％４．
、は硫酸中に無水硫酸が５％、７％１０．混入されたこ
とを示す。このデータから、オリラム濃度が５％から２
５％までの間で硫酸温度は６０°Ｃ〜１４５°Ｃ１硫酸
濃度は９７．４％〜９８．０％であり実用可能な熱濃硫
酸が得られることが判明した。Concentration Preparation amount Preparation time Preparation amount Temperature Concentration (%) (
g) (seconds) (g) (”C) (%)0
500 31.4 10 42 97.75
500 31.4 16 60 97.87
500 31.4 18 75 97.4
B 500 31.4 19 80 97
．． 910 500 3+, /I 21.5
90 97.610 500 3L, 1 21
．． 5 90 98.020 500 31.4
21.5 90 98.025 500 32.
2 39.0 145 97.7 Based on the above data, if the concentration of orilum is 0, the case with sulfuric acid only, 5%, 7%, 4.
, sulfuric acid anhydride in sulfuric acid is 5%, 7%10. Indicates that it has been mixed. From this data, the concentration of orilum ranges from 5% to 2.
It has been found that when the sulfuric acid temperature is 60° C. to 145° C. and the sulfuric acid concentration is 97.4% to 98.0%, a practically usable hot concentrated sulfuric acid can be obtained.
本発明の第１実施例は第３図に断面図で示され、同図に
おいて、２１は槽、２２はウェハ、２３は真空回転チャ
ック、２４はオリラム供給管、２５は水供給管、２６は
過酸化水素水溶液供給管を示し、供給管２４と２５とは
第１供給管２７につながり、第１供給管２７と過酸化水
素水供給管２６とは合体して第２供給管２Ｂとなる。A first embodiment of the present invention is shown in cross section in FIG. 3, in which 21 is a tank, 22 is a wafer, 23 is a vacuum rotating chuck, 24 is an orilum supply pipe, 25 is a water supply pipe, and 26 is a A hydrogen peroxide aqueous solution supply pipe is shown, supply pipes 24 and 25 are connected to a first supply pipe 27, and the first supply pipe 27 and hydrogen peroxide water supply pipe 26 are combined to form a second supply pipe 2B.
操作のシーフェンスは第４図の線図に従うもので、この
線図において時間経過は矢印ｔの方向に進み、■〜■の
各線はそれぞれ水、過酸化水素水、オリラムの供給状態
を表し、各線で高いレベルはオン（供給）、低いレベル
はオフ（供給停止）の状態を示す。The operational sea fence follows the diagram in Figure 4. In this diagram, the passage of time progresses in the direction of arrow t, and each line from ■ to ■ represents the supply status of water, hydrogen peroxide, and orilum, respectively. In each line, a high level indicates an on (supply) state, and a low level indicates an off (supply stopped) state.
先ず、線■に示す如く水供給管２５をオンにして１１□
０を供給し、ウェハ２２の前洗浄を行う。First, turn on the water supply pipe 25 as shown by the line □
0 is supplied, and the wafer 22 is pre-cleaned.
次いで、線■に示す如く過酸化水素水を管２６から供給
し、水と過酸化水素水をウェハ上に滴下する。Next, hydrogen peroxide solution is supplied from the pipe 26 as shown by line (2), and the water and hydrogen peroxide solution are dropped onto the wafer.
次に線■に示す如くオリラムを管２４から供給し、３者
の混合液をウェハ上に滴下する。Next, as shown by line (3), orilum is supplied from the tube 24, and a mixed solution of the three components is dropped onto the wafer.
一方、チャック２３ば同図の線（４）に示す如く水供給
と同時に回転している（Ｒｏｔ、）から、ウェハのクリ
ーニングは、■のオン状態の間に行われる。On the other hand, since the chuck 23 is rotating simultaneously with water supply (Rot) as shown by line (4) in the figure, wafer cleaning is performed during the ON state (2).
クリーニングが終り■がオフセットになった後で過酸化
水素水の供給を止め、次いで水のみで後洗浄を行い、し
かる後にチャックの回転（Ｒｏｔ、）を停止する。そし
て各ウェハ毎に上記の操作を繰り返す。After the cleaning is completed and the mark ① becomes offset, the supply of hydrogen peroxide solution is stopped, and then post-cleaning is performed using only water, and then the rotation of the chuck (Rot) is stopped. The above operation is then repeated for each wafer.
第３図に示される装置において、オリラム供給管は同混
液が未だ発熱していないから、従来形の管を用いてよい
。第１供給管２７では前記した如（に１００°Ｃ程度に
発熱するから第１供給管は耐熱性材料例えば石英、セラ
ミック等を用いて形成し、第１供給管で発生する熱が管
２４．２５に伝達しないように断熱材２９を用いて管２
４．２５を管２７から遮蔽する。第２供給管２８も管２
７と同様耐熱性材料で作る。In the apparatus shown in FIG. 3, a conventional type of pipe may be used as the orilum supply pipe since the mixed liquid has not yet generated heat. As described above, the first supply pipe 27 generates heat of about 100°C, so the first supply pipe is made of a heat-resistant material such as quartz or ceramic, and the heat generated in the first supply pipe is transferred to the pipe 24. pipe 2 using insulation material 29 to prevent transmission to 25
4.25 from tube 27. The second supply pipe 28 is also the pipe 2
Like 7, it is made of heat-resistant material.
本発明の第２実施例は第５図の模式的断面図に示される
如く噴霧式装置を用いるものであり、同図において、３
１はウェハ、３２はオリラム供給管、３３は過酸化水素
水供給管、３４は水供給管を示し、これらの液の供給順
序は第４図に示す場合と同様であるが、Ｎ、ガスを加え
て噴霧状に供給する。かくすることにより、混合発熱は
図に点線３５で示す空間に発生して１００°Ｃ程度の熱
濃硫酸でウェハ３１の表面の洗浄が行われる。The second embodiment of the present invention uses a spraying device as shown in the schematic cross-sectional view of FIG.
1 is a wafer, 32 is an orilum supply pipe, 33 is a hydrogen peroxide water supply pipe, and 34 is a water supply pipe, and the order of supplying these liquids is the same as that shown in Fig. 4, except that N and gas are In addition, it is supplied in a spray form. As a result, heat generated by the mixture is generated in the space indicated by the dotted line 35 in the figure, and the surface of the wafer 31 is cleaned with hot concentrated sulfuric acid at about 100°C.
いずれの実施例においても１００°Ｃの発熱が得られな
いときは図示しない予備ヒータを用いて加熱する。ヒー
タは抵抗加熱に限らず、ランプ加熱等も考えられる。ま
たいずれの場合にも最後には純水を用いて最終的洗浄を
行う。なお本発明の適用範囲は上記のウェハ洗浄の場合
に限定されるものでない。In any of the examples, if heat generation of 100°C cannot be obtained, heating is performed using a preliminary heater (not shown). The heater is not limited to resistance heating, but lamp heating or the like may also be used. In either case, final cleaning is performed using pure water. Note that the scope of application of the present invention is not limited to the above-mentioned wafer cleaning.
（７）発明の効果
以」二詳細に説明した如く本発明によれば、加熱ヒータ
を省くことができ、また予備的加熱ヒータが必要な場合
でも加熱エネルギーを節約することができ（従来は全加
熱であった）、また配管出口以降での加熱であるから、
配管材等の設計自由度と安全性が高まり、半導体装置製
造における歩留りの向上に効果大である。(7) Effects of the Invention As explained in detail in 2, according to the present invention, the heater can be omitted, and even if a preliminary heater is required, heating energy can be saved (conventionally, all ), and since the heating occurred after the pipe exit,
This increases the degree of freedom and safety in designing piping materials, etc., and is highly effective in improving yields in semiconductor device manufacturing.
第１図は従来のシリコンウェハを洗浄する装置の模式的
断面図、第２図は本発明のための実験に用いた装置の断
面図、第３図は本発明の第１の実施例に用いる装置の断
面図、第４図は第３図の装置の運転シーフェンスを示す
線図、第５図は本発明の第２の実施例に用いる装置の模
式的断面図である。
２１一槽、２２．３１− シリコンウェハ、２３−真空
チャック、
２４、３２−−−オリラム供給管、
２５、３４−−一純水供給管、FIG. 1 is a schematic cross-sectional view of a conventional silicon wafer cleaning device, FIG. 2 is a cross-sectional view of the device used in experiments for the present invention, and FIG. 3 is a cross-sectional view of the device used in the first embodiment of the present invention. FIG. 4 is a diagram showing the operational sea fence of the device shown in FIG. 3, and FIG. 5 is a schematic sectional view of the device used in the second embodiment of the present invention. 21 one tank, 22. 31- silicon wafer, 23- vacuum chuck, 24, 32-- orilum supply pipe, 25, 34-- one pure water supply pipe,
Claims (4)
洗浄すべき基板表面に隣接する位置で混合し、基板表面
上に供給することを特徴とする基板表面洗浄方法。(1) A mixture of sulfuric acid and sulfuric anhydride, water and hydrogen peroxide,
A method for cleaning a substrate surface, characterized in that the mixture is mixed at a position adjacent to the surface of the substrate to be cleaned, and the mixture is supplied onto the surface of the substrate.
隣接する位置で水と混合させ、かくして得られた混合液
と過酸化水素とを混合して基板表面上に供給することを
特徴とする特許請求の範囲第１項記載の基板表面洗浄方
法。(2) A mixture of sulfuric acid and sulfuric anhydride is mixed with water at a position adjacent to the surface of the substrate to be cleaned, and the mixture thus obtained is mixed with hydrogen peroxide and the mixture is supplied onto the surface of the substrate. A substrate surface cleaning method according to claim 1.
水をそれぞれ供給する管の出口を基板表面に隣接して配
置し、噴霧状に基板表面に向けて供給し、基板表面上に
混合発熱領域を形成することを特徴とする特許請求の範
囲第１項記載の基板表面洗浄方法。(3) The outlets of the tubes that supply the mixture of sulfuric acid and sulfuric anhydride, hydrogen peroxide, and water, respectively, are arranged adjacent to the substrate surface, and the mixture is supplied in the form of a spray toward the substrate surface, and mixed on the substrate surface. 2. The substrate surface cleaning method according to claim 1, further comprising forming a heat generating region.
囲内にあることを特徴とする特許請求の範囲第１項また
は第２項記載の基板表面洗浄方法。(4) The substrate surface cleaning method according to claim 1 or 2, wherein the mixing ratio of sulfuric anhydride in the sulfuric acid is within the range of 5% to 25%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59227529A JPH0715895B2 (en) | 1984-10-29 | 1984-10-29 | Substrate surface cleaning method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59227529A JPH0715895B2 (en) | 1984-10-29 | 1984-10-29 | Substrate surface cleaning method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61105847A true JPS61105847A (en) | 1986-05-23 |
| JPH0715895B2 JPH0715895B2 (en) | 1995-02-22 |
Family
ID=16862329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59227529A Expired - Lifetime JPH0715895B2 (en) | 1984-10-29 | 1984-10-29 | Substrate surface cleaning method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0715895B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01114043A (en) * | 1987-10-28 | 1989-05-02 | Teru Kyushu Kk | Cleaning method |
| EP0390134A2 (en) * | 1989-03-30 | 1990-10-03 | Kabushiki Kaisha Toshiba | Method and apparatus for cleaning semiconductor devices |
| JP2001319849A (en) * | 2000-05-08 | 2001-11-16 | Tokyo Electron Ltd | Liquid processing device and liquid processing method |
| US9966282B2 (en) | 2014-09-30 | 2018-05-08 | Shibaura Mechatronics Corporation | Substrate processing apparatus and substrate processing method |
| TWI629115B (en) * | 2014-09-30 | 2018-07-11 | 芝浦機械電子裝置股份有限公司 | Substrate processing device and substrate processing method |
| US11810796B2 (en) | 2018-09-18 | 2023-11-07 | Lam Research Ag | Wafer cleaning method and apparatus therefore |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53101975A (en) * | 1977-02-18 | 1978-09-05 | Toshiba Corp | Treating method of semiconductor substrates |
-
1984
- 1984-10-29 JP JP59227529A patent/JPH0715895B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53101975A (en) * | 1977-02-18 | 1978-09-05 | Toshiba Corp | Treating method of semiconductor substrates |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01114043A (en) * | 1987-10-28 | 1989-05-02 | Teru Kyushu Kk | Cleaning method |
| EP0390134A2 (en) * | 1989-03-30 | 1990-10-03 | Kabushiki Kaisha Toshiba | Method and apparatus for cleaning semiconductor devices |
| JPH02257632A (en) * | 1989-03-30 | 1990-10-18 | Toshiba Corp | Method and apparatus for cleaning of semiconductor device |
| JP2001319849A (en) * | 2000-05-08 | 2001-11-16 | Tokyo Electron Ltd | Liquid processing device and liquid processing method |
| US9966282B2 (en) | 2014-09-30 | 2018-05-08 | Shibaura Mechatronics Corporation | Substrate processing apparatus and substrate processing method |
| TWI629115B (en) * | 2014-09-30 | 2018-07-11 | 芝浦機械電子裝置股份有限公司 | Substrate processing device and substrate processing method |
| US11810796B2 (en) | 2018-09-18 | 2023-11-07 | Lam Research Ag | Wafer cleaning method and apparatus therefore |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0715895B2 (en) | 1995-02-22 |
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