JPH09175809A - Casting method for silicon - Google Patents
Casting method for siliconInfo
- Publication number
- JPH09175809A JPH09175809A JP34012595A JP34012595A JPH09175809A JP H09175809 A JPH09175809 A JP H09175809A JP 34012595 A JP34012595 A JP 34012595A JP 34012595 A JP34012595 A JP 34012595A JP H09175809 A JPH09175809 A JP H09175809A
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- mold
- silicon nitride
- release material
- casting
- 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
Landscapes
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Recrystallisation Techniques (AREA)
Abstract
Description
【０００１】[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。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.
【０００２】[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。2. Description of the Related Art Polycrystalline silicon has been used as a kind of semiconductor substrate for forming solar cells. Such polycrystalline silicon is usually prepared by applying a mold release material to the inner surface of a divisible graphite mold, and pouring and solidifying the silicon melt heated and melted at high temperature into the mold. It was formed by once forming or melting the silicon raw material put in the mold and then solidifying again.
【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）。It is well known that silicon nitride (Si 3 N 4 ) which is a nitride of silicon is used as such a release material (for example, 15th Photovoltaic Spesia).
lists Conf. (1981), P576 ~ P580, "A NEW DIRECTIONAL
SOLIDIFICATION TECHNIQUE FOR POLYCRYSTALLINE SOLAR
GRADE SILICON ").
【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。However, when silicon nitride is applied to the inner surface of a graphite mold to cast silicon, the silicon nitride film is fragile, so when the silicon melt is poured and during the subsequent solidification. In addition, there is a problem that the silicon nitride film is damaged and the silicon melt contacts the mold, and when the mold adheres to the silicon ingot and is released from the mold, the silicon ingot is chipped. Further, there is a problem that the silicon nitride film is damaged when the silicon raw material put in the mold is dissolved.
【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。It has also been proposed to apply silicon dioxide (SiO 2 ) to the inner surface of a graphite mold to cast silicon, but when silicon dioxide is used as a mold release material, silicon dioxide adheres to graphite. In addition, since the ingot of silicon dioxide and silicon also has good adhesion, silicon dioxide adheres to the mold and the mold cannot be reused, or the mold adheres to the ingot of silicon through the release material. However, there is a problem that a part of the silicon ingot is chipped when the mold is removed.
【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。In order to solve such a problem, in JP-A-7-206419, silicon dioxide is applied to the first layer, a mixture of silicon dioxide and silicon nitride is applied to the second layer, and then the third layer is applied. It has been proposed to apply silicon nitride to.
【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。However, when the release agent is applied to the three-layer structure as described above, the release agent corresponding to each layer must be prepared and applied, which causes a problem that it takes time to apply and prepare the release agent. there were.
【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。The present invention has been made in view of the above-mentioned problems of the prior art. When pouring a silicon melt into a mold, at the time of subsequent solidification, or in a mold, a silicon raw material is placed. Provide a casting method of silicon that eliminates the need for separating the release material, the release material adhering to the mold to prevent the mold from being reused, and the trouble of mixing and applying the release material. The purpose is to
【０００９】[0009]
【課題を解決するための手段】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注湯するシリコン
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。In order to achieve the above object, in the method for casting silicon according to the present invention, a method for casting silicon in which a mold release material is applied to the inner surface of a mold to pour a silicon melt As the release material, a mixture of silicon nitride and silicon dioxide in a weight ratio of 28:72 to 75:25 is used.
【００１０】[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。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. FIG. 1 is a diagram showing an example of a mold used in the method for casting silicon 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. In addition, the bottom member 1a and the side member 1b
Can be separably assembled by fixing with bolts (not shown) or the like, or separable by fixing with a frame member (not shown) in which the bottom member 1a and the side member 1b are just fitted.
【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。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 repeatedly used many times. Such a release material 2 includes silicon nitride (Si 3 N 4 ) and silicon dioxide (Si).
A mixture of O 2 ) in a weight ratio of 28:72 to 75:25 is used. Powders of silicon nitride and silicon dioxide are mixed with a polyvinyl alcohol aqueous solution 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 made into a slurry form, which can be easily applied to the graphite mold 1.
【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。As the silicon nitride powder, 0.4 to
A material having an average particle diameter of about 0.6 μm is used.
As the silicon dioxide powder, one having an average particle size of about 20 μm is used. Such silicon nitride and silicon dioxide are mixed into a polyvinyl alcohol aqueous solution having a concentration of about 5 to 15% by weight to form a slurry, which is applied to the inner surface of the mold 1 with a spatula or a brush. In that state, it is naturally dried or placed on a hot plate to be dried, and the silicon melt is poured into the mold 1.
【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。The weight ratio of silicon nitride to silicon dioxide in the release material 2 is 28:72 to 75:25. When the weight ratio of silicon nitride is less than 28%, the mold release material 2 adheres to the mold 1 and is not peeled off.
The bottom member 1a and side member 1b cannot be reused. Further, the mold 1 adheres to the ingot of silicon through the mold release material 2, and the bottom member 1a and the side member 1 of the mold 1 are attached from the ingot of silicon.
When b is peeled off, a part of silicon is chipped. When the weight ratio of silicon nitride is more than 75%, the coating formed by applying the mold release material 2 is damaged and the mold 1 adheres to the ingot of silicon, and the bottom member 1a of the mold and the mold from the ingot of silicon. The side member 1b cannot be peeled off.
【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。For pouring and solidifying the silicon melt, for example, the mold release material 2 is applied to the inner surface of the mold and dried, and then the mold 1 is depressurized to 7.0 to 9.0 Torr in an argon (Ar) atmosphere. Then, the mold 1 is heated at the same temperature as or slightly lower than the temperature of the silicon melt to pour the silicon melt. Alternatively, the silicon raw material may be put into the mold and directly melted. After that, 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.
【００１５】[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。EXAMPLE A silicon nitride powder having an average particle size of 0.5 μm and a silicon dioxide powder having an average particle size of 20 μm were weighed and then measured at 8.7.
% Polyvinyl alcohol aqueous solution with stirring to obtain a release material in the form of a slurry. The mold release material was applied to the inner surface of the graphite mold with a brush, placed on a hot plate and dried. After completion of the drying, the mold was placed in an argon atmosphere depressurized to 8.0 Torr, 68 kg of silicon melt was poured into the mold while being heated to 1000 ° C. using a graphite heater, and gradually solidified over 7 hours. It was The ingot of silicon which was solidified after cooling was taken out from the mold, and the presence or absence of adhesion of the mold release material and the mold, and the presence or absence of adhesion of the silicon ingot and mold were examined. Table 1 shows the results.
【００１６】[0016]
【表１】 [Table 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。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 mold release material and the mold is eliminated, and the adhesion between the silicon ingot and the mold is almost eliminated. In particular, even if the weight ratio of silicon nitride is 28%, the applied amount of silicon nitride and silicon dioxide is 0.13 g / cm 2.
In the above case, the silicon ingot and the mold are not attached. On the other hand, when the weight ratio of silicon nitride is 89% or more, the mold release material and the mold do not adhere to each other, but the silicon ingot and the mold adhere to each other.
【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。Therefore, the weight ratio of silicon nitride and silicon dioxide must be set to 28:72 to 75:25. Further, when silicon nitride and silicon dioxide are applied to the inner surface of the mold in an amount of 0.13 g / cm 2 or more, even if the weight ratio of silicon nitride is 28%, neither the mold release material and the mold nor the silicon ingot and the mold adhere to each other. Further, when the weight ratio of silicon nitride is 38%, even if the coating amount of silicon nitride and silicon dioxide is 0.03 g / cm 2 , there is no adhesion between the mold release material and the mold or between silicon and the mold.
【００１９】[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、窒化シリコンと二酸化シリコンを２
８：７２〜７５：２５の重量比率で混合したものを用い
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。As described above, according to the silicon casting method of the present invention, silicon nitride and silicon dioxide
Since the mixture in the weight ratio of 8:72 to 75:25 is used, the mold release material can be applied to the inner surface of the mold at one time, and the mold release material adheres to the mold or the mold is made of silicon. It is possible to prevent silicon chipping that occurs due to adhesion to the ingot.
【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。FIG. 1 is a diagram showing an example of a mold used in a method for casting silicon according to the present invention.
１・・・鋳型、２・・・離型材 1 ... Mold, 2 ... Release material
Claims (3)
ン融液を注湯す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ことを特
徴とするシリコンの鋳造法。1. A method of casting silicon in which a mold release material is applied to the inner surface of a mold and a silicon melt is poured into the mold, wherein silicon nitride and silicon dioxide are used as the mold release material from 28:72.
A method for casting silicon, characterized in that a mixture of 75:25 by weight is used.
０．１３ｇ／ｃｍ2 以上塗布することを特徴とする請求
項１に記載のシリコンの鋳造法。2. The method for casting silicon according to claim 1, wherein the silicon nitride and silicon dioxide are applied in an amount of 0.13 g / cm 2 or more.
シリコンを３８：６２〜７５：２５の重量比率で混合し
たものを用いると共に、０．０３ｇ／ｃｍ2以上塗布す
ることを特徴とする請求項１に記載のシリコンの鋳造
法。3. A mold release material comprising a mixture of silicon nitride and silicon dioxide in a weight ratio of 38:62 to 75:25 and coated with 0.03 g / cm 2 or more. The method for casting silicon described in.
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 true JPH09175809A (en) | 1997-07-08 |
| JP3450109B2 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 |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3450109B2 (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003095632A (en) * | 2001-09-26 | 2003-04-03 | Yutaka Kamaike | Apparatus and method for producing silicon |
| JP2006334671A (en) * | 2006-09-25 | 2006-12-14 | Kyocera Corp | Method for manufacturing silicon casting mold |
| WO2007010622A1 (en) * | 2005-07-22 | 2007-01-25 | Kyocera Corporation | Polycrystal silicon substrate, fabrication method thereof, photoelectric conversion element, and photoelectric conversion module |
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- 1995-12-27 JP JP34012595A patent/JP3450109B2/en not_active Expired - Fee Related
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| JP2003095632A (en) * | 2001-09-26 | 2003-04-03 | Yutaka Kamaike | Apparatus and method for producing silicon |
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