JP3450109B2 - Silicon casting method - Google Patents
Silicon casting methodInfo
- Publication number
- JP3450109B2 JP3450109B2 JP34012595A JP34012595A JP3450109B2 JP 3450109 B2 JP3450109 B2 JP 3450109B2 JP 34012595 A JP34012595 A JP 34012595A JP 34012595 A JP34012595 A JP 34012595A JP 3450109 B2 JP3450109 B2 JP 3450109B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- mold
- release material
- silicon nitride
- silicon dioxide
- 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
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- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Recrystallisation Techniques (AREA)
Description
【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明はシリコンの鋳造法に
関し、特に太陽電池などを形成するための多結晶シリコ
ンの鋳造法に関する。
【０００２】
【従来の技術および発明が解決しようとする課題】従来
から太陽電池を形成するための半導体基板の一種として
多結晶シリコンが用いられている。このような多結晶シ
リコンは、通常、分割可能な黒鉛製鋳型の内表面に離型
材を塗布して、この鋳型内に高温度で加熱溶融させたシ
リコン融液を注湯して凝固させることによって形成した
り、鋳型内に入れたシリコン原料を一旦溶解した後、再
び凝固させることによって形成していた。
【０００３】このような離型材としては、シリコンの窒
化物である窒化シリコン（Ｓｉ3 Ｎ4 ）を用いることが
よく知られている（例えば、15th Photovoltaic Spesia
lists Conf. (1981), P576〜P580, "A NEW DIRECTIONAL
SOLIDIFICATION TECHNIQUEFOR POLYCRYSTALLINE SOLAR
GRADE SILICON"を参照）。
【０００４】ところが、窒化シリコンを黒鉛製鋳型の内
表面に塗布してシリコンを鋳造する場合、窒化シリコン
膜は脆弱であることから、シリコン融液を注湯する際
に、またその後の凝固の際に、窒化シリコン膜が破損し
て鋳型にシリコン融液が接触し、鋳型がシリコンの鋳塊
に付着して脱型する際にシリコンの鋳塊に欠けが発生す
るという問題があった。また、鋳型内に入れたシリコン
原料を溶解する際に、窒化シリコン膜が破損するという
問題があった。
【０００５】また、二酸化シリコン（ＳｉＯ2 ）を黒鉛
製鋳型の内表面に塗布してシリコンを鋳造することも提
案されているが、二酸化シリコンを離型材として用いる
場合、二酸化シリコンは黒鉛と付着性がよく、また二酸
化シリコンとシリコンの鋳塊も付着性がよいために、二
酸化シリコンが鋳型に付着して鋳型の再使用ができなく
なったり、鋳型が離型材を介してシリコンの鋳塊に付着
し、脱型するときにシリコンの鋳塊の一部に欠けが発生
するという問題があった。
【０００６】このような問題を解決するために、特開平
７−２０６４１９号公報では、一層目に二酸化シリコン
を塗布し、二層目に二酸化シリコンと窒化シリコンの混
合物を塗布し、さらに三層目に窒化シリコンを塗布する
ことが提案されている。
【０００７】ところが、このように離型材を三層構造に
塗布すると、それぞれの層に対応する離型材を調合して
塗布しなければならず、離型材の塗布と調合に手間が掛
かるという問題があった。
【０００８】本発明は、このような従来技術の問題点に
鑑みて為されたものであり、鋳型内にシリコン融液を注
湯する際、その後の凝固の際、或いは鋳型に入れたシリ
コン原料を溶解する際に、離型材が剥離したり、離型材
が鋳型に付着して鋳型が再使用できなくなったり、離型
材の混合と塗布に手間が掛かることを解消したシリコン
の鋳造法を提供することを目的とする。
【０００９】上記目的を達成するために、本発明に係る
シリコンの鋳造方法では、鋳型の内表面に離型材を塗布
してシリコン融液を凝固させるシリコンの鋳造法におい
て、前記離型材として窒化シリコンと二酸化シリコンを
２８：７２〜７５：２５の重量比率で混合したものを用
いると共に、窒化シリコンと二酸化シリコンを３８：６
２〜７５：２５の重量比率で混合したものを用いる場合
は、０．０３ｇ／ｃｍ２以上塗布し、窒化シリコンと二
酸化シリコンを２８：７２以上３８：６２未満で用いる
場合は、０．１３ｇ／ｃｍ２以上塗布することを特徴と
する。
【００１０】
【発明の実施の形態】以下、本発明を添付図面に基づき
詳細に説明する。図１は、本発明に係るシリコンの鋳造
法に用いられる鋳型の一例を示す図である。鋳型１は例
えば黒鉛などから成り、一つの底部材１ａと四つの側部
材１ｂを組み合わせた分割と組み立てが可能な分割型鋳
型などで構成される。なお、底部材１ａと側部材１ｂ
は、ボルト（不図示）などで固定することによって分割
可能に組み立てられたり、底部材１ａと側部材１ｂが丁
度嵌まる枠部材（不図示）で固定することによって分割
可能に組み立てられる。
【００１１】鋳型１の内表面には、底部材１ａや側部材
１ｂを何回も繰り返して使用することができるように離
型材２が塗布される。このような離型材２としては、窒
化シリコン（Ｓｉ3 Ｎ4 ）と二酸化シリコン（Ｓｉ
Ｏ2 ）を２８：７２〜７５：２５の重量比率で混合した
ものを用いる。窒化シリコンと二酸化シリコンの粉体を
ポリビニルアルコール水溶液で混ぜ合わせて鋳型１の内
面に塗布する。窒化シリコンと二酸化シリコンをポリビ
ニルアルコール水溶液などで混合することによって、粉
体である窒化シリコンと二酸化シリコンがスラリー状と
なり、黒鉛製鋳型１に塗布しやすくなる。
【００１２】窒化シリコンの粉体としては、０．４〜
０．６μｍ程度の平均粒径を有するものが用いられる。
また、二酸化シリコンの粉体としては、２０μｍ程度の
平均粒径を有するものが用いられる。このような窒化シ
リコンと二酸化シリコンを濃度が５〜１５重量％程度の
ポリビニルアルコール水溶液に混合してスラリー状と
し、へらや刷毛などで鋳型１の内表面に塗布する。その
状態で自然乾燥又はホットプレートに載せて乾燥させて
鋳型１内にシリコン融液を注湯する。
【００１３】離型材２中の窒化シリコンと二酸化シリコ
ンの比率は、重量比率で２８：７２〜７５：２５とす
る。窒化シリコンの重量比率が２８％よりも小さくなる
と離型材２が鋳型１に付着して剥がれなくなり、鋳型１
の底部材１ａや側部材１ｂを再使用できなくなる。ま
た、鋳型１が離型材２を介してシリコンの鋳塊に付着
し、シリコンの鋳塊から鋳型１の底部材１ａや側部材１
ｂを剥離するときに、シリコンの一部に欠けが発生す
る。また、窒化シリコンの重量比率が７５％より大きく
なると、離型材２を塗布して形成した皮膜が破損して鋳
型１がシリコンの鋳塊に付着し、シリコンの鋳塊から鋳
型の底部材１ａや側部材１ｂを剥離を剥離できなくな
る。
【００１４】シリコン融液の注湯と凝固は、例えば鋳型
の内面に離型材２を塗布して乾燥させた後に、鋳型１を
７．０〜９．０Ｔｏｒｒに減圧したアルゴン（Ａｒ）雰
囲気中に置き、鋳型１をシリコン融液と同程度か若干低
い温度で加熱してシリコン融液を注湯する。また鋳型内
にシリコン原料を入れ、直接溶解してもよい。しかる
後、鋳型１の底部から徐々に降温させてシリコン融液を
鋳型の底部から徐々に凝固させる。最後に鋳型を分割し
てシリコンのインゴットを取り出すことにより完成す
る。
【００１５】
【実施例】平均粒径０．５μｍの窒化シリコン粉末と平
均粒径２０μｍの二酸化シリコン粉末を秤量して８．７
％のポリビニルアルコール水溶液で攪拌混合してスラリ
ー状にした離型材を得た。その離型材を黒鉛製鋳型の内
表面に刷毛で塗布してホットプレートに載せて乾燥し
た。乾燥終了後、鋳型を８．０Ｔｏｒｒに減圧したアル
ゴン雰囲気中に置き、黒鉛ヒータを使って１０００℃に
加熱した状態で鋳型内にシリコン融液６８ｋｇを注湯し
て７時間かけて徐々に凝固させた。冷却後固化したシリ
コンの鋳塊を鋳型から取り出し、離型材と鋳型の付着の
有無、シリコンの鋳塊と鋳型の付着の有無について調べ
た。その結果を表１に示す。
【００１６】
【表１】
【００１７】表１から明らかなように、窒化シリコンの
重量比率が７％以下の場合、離型材と鋳型の付着及びシ
リコンの鋳塊と鋳型の付着が発生するが、窒化シリコン
の重量比率が２８％以上になると離型材と鋳型の付着は
無くなり、シリコンの鋳塊と鋳型の付着も殆ど無くな
る。特に、窒化シリコンの重量比率が２８％でも窒化シ
リコンと二酸化シリコンの塗布量が０．１３ｇ／ｃｍ2
以上の場合は、シリコンの鋳塊と鋳型の付着は無くな
る。一方、窒化シリコンの重量比率が８９％以上になる
と、離型材と鋳型の付着は無いものの、シリコンの鋳塊
と鋳型の付着が発生する。
【００１８】したがって、窒化シリコンと二酸化シリコ
ンの重量比率を２８：７２〜７５：２５に設定しなけれ
ばならない。また、鋳型の内表面に窒化シリコンと二酸
化シリコンを０．１３ｇ／ｃｍ2 以上塗布すると窒化シ
リコンの重量比率が２８％でも離型材と鋳型の付着やシ
リコンの鋳塊と鋳型の付着は無い。さらに、窒化シリコ
ンの重量比率が３８％になると、窒化シリコンと二酸化
シリコンの塗布量は０．０３ｇ／ｃｍ2 でも離型材と鋳
型の付着やシリコンと鋳型の付着はない。
【００１９】
【発明の効果】以上のように、本発明に係るシリコンの
鋳造法によれば、離型材として窒化シリコンと二酸化シ
リコンを２８：７２〜７５：２５の重量比率で混合した
ものを用いると共に、窒化シリコンと二酸化シリコンを
３８：６２〜７５：２５の重量比率で混合したものを用
いる場合は、０．０３ｇ／ｃｍ２以上塗布し、窒化シリ
コンと二酸化シリコンを２８：７２以上３８：６２未満
で用いる場合は、０．１３ｇ／ｃｍ２以上塗布すること
から、離型材を一回で鋳型の内表面に塗布することがで
きると共に、離型材が鋳型に付着したり、鋳型がシリコ
ンの鋳塊に付着することによって発生するシリコンの欠
けを防止することができる。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for casting silicon, and more particularly to a method for casting polycrystalline silicon for forming solar cells and the like. 2. Description of the Related Art Conventionally, polycrystalline silicon has been used as a kind of semiconductor substrate for forming a solar cell. Such polycrystalline silicon is usually formed by applying a mold release material to the inner surface of a splittable graphite mold, pouring a silicon melt heated and melted at a high temperature into the mold, and solidifying it. It is formed by dissolving the silicon raw material once formed or put in the mold and then solidifying it again. As such a release material, it is well known to use silicon nitride (Si 3 N 4 ), which is a nitride of silicon (for example, 15th Photovoltaic Spesia).
lists Conf. (1981), P576-P580, "A NEW DIRECTIONAL
SOLIDIFICATION TECHNIQUEFOR POLYCRYSTALLINE SOLAR
However, when silicon nitride is applied to the inner surface of a graphite mold to cast silicon, since the silicon nitride film is brittle, it is difficult to pour a silicon melt. In addition, during subsequent solidification, the silicon nitride film is damaged, the silicon melt contacts the mold, and the mold is attached to the silicon ingot and the silicon ingot is chipped when it is released from the mold. In addition, there is a problem that the silicon nitride film is broken when dissolving the silicon raw material put in the mold, and the inner surface of the graphite mold is made of silicon dioxide (SiO 2 ). It has also been proposed to cast silicon by coating on silicon, but when silicon dioxide is used as a mold release material, silicon dioxide has good adhesion to graphite, and ingots of silicon dioxide and silicon also have good adhesion. The silicon dioxide adheres to the mold, making it impossible to reuse the mold, or the mold adheres to the silicon ingot through the mold release material and forms a part of the silicon ingot when demolding. [0006] In order to solve such a problem, Japanese Patent Laid-Open No. 7-206419 discloses a method in which silicon dioxide is applied to a first layer, and silicon dioxide and silicon nitride are applied to a second layer. However, it has been proposed to apply a mixture of the following, and further apply silicon nitride on the third layer: However, when the release material is applied in a three-layer structure, the release material corresponding to each layer is formed. The present invention has been made in view of the above-mentioned problems of the prior art, because it requires time to apply and mix the release material. , Casting When pouring the silicon melt into the mold, during subsequent solidification, or when dissolving the silicon raw material in the mold, the mold release material peels off or the mold release material adheres to the mold and the mold can be reused. SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for casting silicon, which eliminates the problem of eliminating or eliminating the trouble of mixing and applying a release material. In a silicon casting method in which a release material is applied to the inner surface of a mold to solidify a silicon melt, a mixture of silicon nitride and silicon dioxide in a weight ratio of 28:72 to 75:25 is used as the release material. Together with silicon nitride and silicon dioxide 38: 6
When using a mixture of 2 to 75:25 by weight, apply 0.03 g / cm 2 or more, and when using silicon nitride and silicon dioxide at 28:72 or more and less than 38:62, apply 0.13 g / cm 2. cm 2 or more. The present invention will be described below in detail with reference to the accompanying drawings. FIG. 1 is a diagram showing an example of a mold used in the silicon casting method according to the present invention. The mold 1 is made of, for example, graphite or the like, and is composed of a split mold that can be divided and assembled by combining one bottom member 1a and four side members 1b. The bottom member 1a and the side member 1b
Can be divided and assembled by fixing with bolts (not shown) or the like, or can be divided and assembled by fixing with a frame member (not shown) where the bottom member 1a and the side member 1b just fit. A mold release material 2 is applied to the inner surface of the mold 1 so that the bottom member 1a and the side member 1b can be used repeatedly. As such a release material 2, silicon nitride (Si 3 N 4 ) and silicon dioxide (Si
The O 2) 28: 72~75: use a mixture in a weight ratio of 25. The powders of silicon nitride and silicon dioxide are mixed with an aqueous solution of polyvinyl alcohol and applied to the inner surface of the mold 1. By mixing silicon nitride and silicon dioxide with an aqueous solution of polyvinyl alcohol or the like, powdery silicon nitride and silicon dioxide are slurried, and can be easily applied to the graphite mold 1. [0012] As a powder of silicon nitride, 0.4 to
Those having an average particle size of about 0.6 μm are used.
As the silicon dioxide powder, a powder having an average particle size of about 20 μm is used. Such silicon nitride and silicon dioxide are mixed with an aqueous solution of polyvinyl alcohol having a concentration of about 5 to 15% by weight to form a slurry, and the slurry is applied to the inner surface of the mold 1 with a spatula or a brush. In this state, the silicon melt is poured into the mold 1 by air drying or drying on a hot plate. The ratio between silicon nitride and silicon dioxide in the release material 2 is 28:72 to 75:25 by weight. When the weight ratio of silicon nitride is less than 28%, the release material 2 adheres to the mold 1 and does not peel off.
The bottom member 1a and the side member 1b cannot be reused. Further, the mold 1 adheres to the silicon ingot through the mold release material 2, and the bottom member 1a and the side members 1 of the mold 1 are separated from the silicon ingot.
When peeling b, a part of silicon is chipped. If the weight ratio of silicon nitride is more than 75%, the film formed by applying the release material 2 is damaged, and the mold 1 adheres to the silicon ingot, and the silicon ingot is used to remove the mold bottom member 1a and the base member 1a. The side member 1b cannot be peeled off. For pouring and solidifying the silicon melt, for example, after releasing the mold release material 2 on the inner surface of the mold and drying the mold, the mold 1 is placed in an argon (Ar) atmosphere reduced to 7.0 to 9.0 Torr. Then, the mold 1 is heated at a temperature approximately equal to or slightly lower than the silicon melt, and the silicon melt is poured. Alternatively, a silicon raw material may be placed in a mold and directly dissolved. Thereafter, the temperature is gradually lowered from the bottom of the mold 1 to gradually solidify the silicon melt from the bottom of the mold. Finally, the mold is divided and the silicon ingot is taken out to complete the process. EXAMPLE A silicon nitride powder having an average particle diameter of 0.5 μm and a silicon dioxide powder having an average particle diameter of 20 μm were weighed to 8.7.
% Of a polyvinyl alcohol aqueous solution with stirring to obtain a release material in a slurry state. The release material was applied to the inner surface of a graphite mold with a brush and placed on a hot plate and dried. After the drying is completed, the mold is placed in an argon atmosphere depressurized to 8.0 Torr, and while being heated to 1000 ° C. using a graphite heater, 68 kg of the silicon melt is poured into the mold and gradually solidified over 7 hours. Was. The silicon ingot solidified after cooling was removed from the mold, and the presence or absence of adhesion between the release material and the mold and the presence or absence of adhesion of the silicon ingot and the mold were examined. Table 1 shows the results. [Table 1] As is clear from Table 1, when the weight ratio of silicon nitride is 7% or less, adhesion of the mold release material and the mold and adhesion of the silicon ingot and the mold occur, but the weight ratio of silicon nitride is 28%. %, The adhesion between the release material and the mold disappears, and the adhesion between the silicon ingot and the mold almost disappears. In particular, even when the weight ratio of silicon nitride is 28%, the coating amount of silicon nitride and silicon dioxide is 0.13 g / cm 2.
In the above case, the adhesion between the silicon ingot and the mold is eliminated. On the other hand, when the weight ratio of silicon nitride is 89% or more, there is no adhesion between the release material and the mold, but adhesion between the silicon ingot and the mold occurs. Therefore, the weight ratio of silicon nitride to silicon dioxide must be set between 28:72 and 75:25. Further, when 0.13 g / cm 2 or more of silicon nitride and silicon dioxide are applied to the inner surface of the mold, there is no adhesion between the mold release material and the mold, and no adhesion between the silicon ingot and the mold, even if the weight ratio of silicon nitride is 28%. Further, when the weight ratio of silicon nitride becomes 38%, even if the application amount of silicon nitride and silicon dioxide is 0.03 g / cm 2 , there is no adhesion between the release material and the mold or between the silicon and the mold. As described above, according to the silicon casting method of the present invention, a mixture of silicon nitride and silicon dioxide at a weight ratio of 28:72 to 75:25 is used as a mold release material. In the case where a mixture of silicon nitride and silicon dioxide at a weight ratio of 38:62 to 75:25 is used, 0.03 g / cm 2 or more is applied, and silicon nitride and silicon dioxide are 28:72 or more and 38:62. When used in less than 0.13 g / cm 2 or more, the release material can be applied to the inner surface of the mold at one time, and at the same time, the release material adheres to the mold or the mold is made of silicon. It is possible to prevent chipping of silicon caused by adhering to the lump.
【図面の簡単な説明】
【図１】本発明に係るシリコンの鋳造法に用いられる鋳
型の一例を示す図である。
【符号の説明】
１・・・鋳型、２・・・離型材BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a view showing an example of a mold used in a method for casting silicon according to the present invention. [Explanation of Signs] 1 ... mold, 2 ... release material
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C01B 33/02 C30B 1/00 - 35/00 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. 7 , DB name) C01B 33/02 C30B 1/00-35/00
Claims (1)
ン融液を凝固させるシリコンの鋳造法において、前記離
型材として窒化シリコンと二酸化シリコンを２８：７２
〜７５：２５の重量比率で混合したものを用いると共
に、窒化シリコンと二酸化シリコンを３８：６２〜７
５：２５の重量比率で混合したものを用いる場合は、
０．０３ｇ／ｃｍ ２ 以上塗布し、窒化シリコンと二酸化
シリコンを２８：７２以上３８：６２未満で用いる場合
は、０．１３ｇ／ｃｍ ２ 以上塗布することを特徴とする
シリコンの鋳造法。(57) [Claim 1] In a silicon casting method in which a mold release material is applied to an inner surface of a mold to solidify a silicon melt, silicon nitride and silicon dioxide are used as the mold release material in a ratio of 28:72.
75: Co Using a mixture in a weight ratio of 25
38: 62-7 silicon nitride and silicon dioxide
When using a mixture in a weight ratio of 5:25,
0.03 g / cm 2 or more, silicon nitride and dioxide
When silicon is used at 28:72 or more and less than 38:62
Is a method of casting silicon, characterized by applying 0.13 g / cm 2 or more .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34012595A JP3450109B2 (en) | 1995-12-27 | 1995-12-27 | Silicon casting method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34012595A JP3450109B2 (en) | 1995-12-27 | 1995-12-27 | Silicon casting method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09175809A JPH09175809A (en) | 1997-07-08 |
| JP3450109B2 true JP3450109B2 (en) | 2003-09-22 |
Family
ID=18333969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34012595A Expired - Fee Related JP3450109B2 (en) | 1995-12-27 | 1995-12-27 | Silicon casting method |
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| Country | Link |
|---|---|
| JP (1) | JP3450109B2 (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5058419B2 (en) * | 2001-09-26 | 2012-10-24 | コスモ石油株式会社 | Silicon manufacturing apparatus and method |
| WO2007010622A1 (en) * | 2005-07-22 | 2007-01-25 | Kyocera Corporation | Polycrystal silicon substrate, fabrication method thereof, photoelectric conversion element, and photoelectric conversion module |
| JP5153636B2 (en) * | 2006-08-30 | 2013-02-27 | 京セラ株式会社 | Method for forming mold for manufacturing silicon ingot, method for manufacturing substrate for solar cell element, and method for manufacturing solar cell element |
| JP4884150B2 (en) * | 2006-09-25 | 2012-02-29 | 京セラ株式会社 | Manufacturing method of mold for silicon casting |
| EP2116637A3 (en) | 2008-05-07 | 2012-03-21 | Covalent Materials Corporation | Crucible for melting silicon and release agent used to the same |
| SG191391A1 (en) * | 2010-12-28 | 2013-08-30 | Ube Industries | Polycrystalline silicon ingot casting mold and method for producing same, and silicon nitride powder for mold release material for polycrystalline silicon ingot casting mold and slurry containing same |
| JP5637220B2 (en) * | 2010-12-28 | 2014-12-10 | 宇部興産株式会社 | Polycrystalline silicon ingot casting mold, manufacturing method thereof, silicon nitride powder for mold release material of polycrystalline silicon ingot casting mold, and slurry containing the same |
| JP5762784B2 (en) * | 2011-03-25 | 2015-08-12 | 信越石英株式会社 | Square silica container for producing polycrystalline silicon ingot, porous silica plate and method for producing the same |
| JP5762777B2 (en) * | 2011-02-01 | 2015-08-12 | 信越石英株式会社 | Square silica container for producing polycrystalline silicon ingot, porous silica plate and method for producing the same |
| US8747538B2 (en) * | 2011-09-20 | 2014-06-10 | Chung-Hou Tony Hsiao | Photovoltaic ingot mold release |
| JP6096653B2 (en) * | 2012-12-28 | 2017-03-15 | 京セラ株式会社 | Silicon casting mold and manufacturing method thereof |
-
1995
- 1995-12-27 JP JP34012595A patent/JP3450109B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09175809A (en) | 1997-07-08 |
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