JP4390461B2 - Silica glass crucible and silicon single crystal pulling method using the same - Google Patents

Silica glass crucible and silicon single crystal pulling method using the same Download PDF

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Publication number
JP4390461B2
JP4390461B2 JP2003045074A JP2003045074A JP4390461B2 JP 4390461 B2 JP4390461 B2 JP 4390461B2 JP 2003045074 A JP2003045074 A JP 2003045074A JP 2003045074 A JP2003045074 A JP 2003045074A JP 4390461 B2 JP4390461 B2 JP 4390461B2
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crucible
inner peripheral
peripheral surface
bubble content
belt
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JP2004250304A (en
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弘史 岸
正徳 福井
義行 辻
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Sumco Corp
Japan Super Quartz Corp
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Sumco Corp
Japan Super Quartz Corp
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Description

【0001】
【発明の属する技術分野】
本発明はシリコン単結晶の引き上げに用いる石英ガラスルツボであって、ルツボに充填した溶融シリコンの湯面振動を抑制したルツボに関する。また、本発明はそのような石英ガラスルツボを用いたシリコン単結晶の引き上げ方法に関する。
【0002】
【従来の技術】
シリコン単結晶の引き上げに用いる石英ガラスルツボは、外周側の気泡を含む不透明層と内周側の気泡の少ない透明層からなるものが一般に用いられている。この石英ガラスルツボは内表面層の気泡含有率によって単結晶化率が大きな影響を受けることから、単結晶化率を高めるために出来るだけ気泡含有率の小さいものが求められてきた。例えば、多数の気泡を含む半透明ガラス層と、この内表面に一体融合された実質的に無気泡でかつ表面が平滑な透明ガラス層からなる単結晶引き上げ用石英ルツボが知られている(特開平1−148783号)。また、石英ガラスルツボの内表面の残留気泡を皆無にし、かつ目視や顕微鏡レベルでは確認されないが使用時に内表面近傍に気泡を発生させる要因となる気泡核も実質的に存在せず、内表面が滑らかで、高い単結晶化率が得られる石英ガラスルツボが知られている(特開2001−2430)。さらに、気泡含有率の高い内側表面層を除去し、また底部内側表面層の気泡体積率を0.001%以下にしたシリコン単結晶引上げ用石英ガラスルツボが知られている(特開平11−116388号)。
【0003】
一方、シリコン単結晶の一般的な引き上げ法(CZ法)では、ルツボ高さの40〜90%の高さにチャージした溶融シリコンの湯面に種結晶を付け、この種結晶を中心にして周囲に結晶化を拡げ(肩作り)た後に、胴体引き上げを行って棒状の単結晶を引き上げ、底部を整えてこの単結晶を取り出す。この引き上げの際に、溶融シリコンの湯面が周期的に振動する現象が見られる。湯面振動が発生すると種結晶を湯面に接合できなかったり、引き上げ中にシリコンが多結晶化するなどの問題を生じる。この原因として、引き上げ温度の上昇や雰囲気圧の低下などによって溶融シリコンと石英ガラスの反応が活発化し、SiOガスが発生することによって振動すると考えられている。
【0004】
【発明が解決しようとする課題】
シリコン単結晶の引き上げ工程において、引き上げ開始工程において種付けと肩作りの工程は溶融シリコンの湯面振動の影響を最も受けやすく、胴体引き上げ以降の工程は湯面振動の影響が比較的少ない。従って、引き上げ開始工程において溶融シリコンの湯面振動を生じないことが求められる。一方、従来の石英ルツボは単結晶化率を高めるためにルツボ内表面の気泡含有率を出来るだけ低減したものが求められてきたが、本発明によればシリコン引き上げ開始時の溶融シリコンの湯面振動はこの湯面付近のルツボ内表面層の気泡含有率に影響されることが見出された。すなわち、引き上げ開始時の湯面付近におけるルツボ内表面の気泡含有率が低すぎると湯面振動を発生し易い傾向がある。
【0005】
本発明は、引き上げ開始湯面付近のルツボ内表面層の気泡含有率を一定範囲に調整することによって、この湯面振動を抑制した石英ガラスルツボを提供する。また、本発明は、湯面振動を抑制することが可能なシリコン単結晶の引き上げ方法を提供する。
【0006】
【課題を解決する手段】
本発明によれば以下の構成からなる石英ガラスルツボが提供される。
(1)シリコン単結晶の引き上げに用いる石英ガラスルツボであって、ルツボ高さの40〜90%の高さにチャージした該ルツボ内の溶融シリコンの引き上げ開始湯面に対して、この湯面となるルツボ開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%であり、この帯状部分よりも下側の内周面層、湾曲部、底部の内側透明層の気泡含有率が0.1%以下であって上記帯状部分の気泡含有率よりも小さく、ルツボ内表面のうち上記帯状部分及びそれよりも下側の内周面層、湾曲部、底部の全面積S1に対する上記帯状部分の面積S2の比(S2/S1)が15〜35%であり、上記帯状部分の下端が上記内周面層の下端よりも上方に位置することによって溶融シリコンの湯面振動を抑制したことを特徴とする石英ガラスルツボ。
(2)口径22インチ(56cm)以上および深さ35cm以上であり、溶融シリコンの引き上げ開始湯面となる開口端よりも下側の所定位置から10cmまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%である上記(1)の石英ガラスルツボ。
(3)上記帯状部分の内周面層の気泡含有率が表面下0.3mmまでの層厚における気泡含有率である上記(1)または(2)の石英ガラスルツボ。
また、本発明によれば以下に示すシリコン単結晶の引き上げ方法が提供される。
(4)石英ガラスルツボを用いたシリコン単結晶の引き上げ方法であって、上記石英ガラスルツボは、開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%であり、この帯状部分よりも下側の内周面層、湾曲部、底部の内側透明層の気泡含有率が0.1%以下であって上記帯状部分の気泡含有率よりも小さく、ルツボ内表面の溶融シリコンとの全接触面積S1に対する上記帯状部分の面積S2の比(S2/S1)が15〜35%であり、上記帯状部分の下端が上記内周面層の下端よりも上方に位置し、上記帯状部分に相当する範囲を溶融シリコンの引き上げ開始湯面として上記シリコン単結晶の引き上げを行うことを特徴とするシリコン単結晶の引き上げ方法。
【0007】
【具体的な説明】
シリコン単結晶の引き上げに用いる石英ガラスルツボは、ルツボ内に多結晶シリコンを入れて加熱溶融することによって溶融シリコンを充填した状態にし、これを引き上げに用いる。本発明の石英ガラスルツボは、図1に示すように、ルツボ10に充填した溶融シリコン11の引き上げ開始湯面Lに対し、この湯面Lから所定深さDまでの帯状部分Hに相当するルツボ内周面層の気泡含有率を0.01〜0.2%とし、さらにルツボ内表面の溶融シリコンとの全接触面積S1に対する上記帯状部分の面積S2の比(S2/S1)を15〜35%に調整することによって溶融シリコンの湯面振動を抑制したことを特徴とするものである。
【0008】
図示するように、上記帯状部分Hは引き上げ開始湯面Lから深さDまでの部分であり、概ねルツボ内周面の上側部分を帯状に囲む部分である。この帯状部分Hの気泡含有率を0.01〜0.2%に調整することによって引き上げ開始時の湯面振動を効果的に抑制することができる。この気泡含有率が上記範囲よりも低いと湯面振動を生じ易くなり、また、この部分の気泡含有率が上記範囲を上回ると単結晶化率が低下するので適当ではない。この帯状部分Hの気泡含有率は0.02〜0.1%がさらに好ましい。
【0009】
上記気泡含有率を有する帯状部分Hの範囲は、ルツボ内表面の溶融シリコンとの全接触面積S1(湯面下の全内表面積)に対して帯状部分Hの面積S2の比(S2/S1)が15〜35%であるものが好ましい。帯状部分Hの面積S2がこれより小さいと、ルツボ全内表面に対して帯状部分Hの深さDが相対的に少なく、溶融シリコンの湯面振動を抑制する効果が低下する。一方、帯状部分Hの面積S2がこれより大きいと気泡含有率の高い部分が相対的に多くなるので単結晶化率が低下するので好ましくない。
【0010】
具体的な態様として、口径22インチ以上および深さ35cm以上(口径Wと深さDの比W/D=1〜2)の一般的な形状の石英ガラスルツボにおいては、チャージしたときの溶融シリコンの引き上げ開始湯面Lに対し、この湯面Lから概ね湯面下10cmまでに相当する帯状のルツボ内周面層の気泡含有率を0.01〜0.2%、好ましくは0.02〜0.1%にすると良い。この帯状部分Hの気泡含有率を上記範囲に調整することによって効果的に溶融シリコンの湯面振動を抑制することができる。
【0011】
上記帯状部分Hよりも下側のルツボ内表面は溶融シリコンの液圧によってSiOの沸騰が抑制されるので湯面振動に対する影響は少ない。従って、引き上げ開始時の湯面振動を抑制するには、上記帯状部分Hの気泡含有率を上記範囲に調整すれば良い。一方、ルツボ内表面の気泡含有率は単結晶化率に影響を与え、気泡含有率が高いものはシリコンの多結晶化や再溶融を招き、さらに引き上げ時間を長引かせるなどの問題を生じる。従って、上記帯状部分Hよりも下側の部分、すなわち上記帯状部分Hより下側の内周面層、湾曲部、底部の透明層の気泡含有率はできるだけ気泡含有率の低いものが好ましく、具体的には、これらの気泡含有率は0.1%以下であって上記帯状部分の気泡含有率より小さいものが良い。
【0012】
本発明の上記石英ガラスルツボにおいて、溶融シリコン湯面下の上記帯状部分Hの気泡含有率は概ね内表面下0.3mmまでの層厚における気泡含有率であれば良い。シリコン単結晶の引き上げによって溶融シリコンの湯面は次第に低下するので、上記帯状部分Hが溶融シリコン接触する時間は比較的短く、従って、上記帯状部分Hは概ね上記層厚内の気泡含有率を上記範囲に調整すれば良い。なお、上記帯状部分Hより下側の内周面層、湾曲部、底部については溶融シリコンに接触している時間が帯状部分より長く、約1mm程度溶損するので、これら各部分については内側透明層全体についての気泡含有率を上記範囲に調整すれば良い。
【0013】
【発明の実施形態】
以下、本発明を実施例によって具体的に示す。
【0014】
〔実施例1〕
ルツボ内周面の各部分の気泡含有率を表1のように調整した石英ガラスルツボ(口径28インチ)を用いてシリコン単結晶を引き上げた。この結果を表1に示した。なお、表中の上部内周面とは溶融シリコンの引き上げ開始湯面に対して、この湯面から湯面下10cmまでの帯状部分に相当する範囲である。下部内周面とはこの帯状部分より下側の内周面である。また、帯状部分の面積は湯面下のルツボ全内表面積の20%である。
表1の結果に示すように、上部内周面の気泡含有率が本発明の範囲より小さいルツボは引き上げ開始時の湯面振動を抑制できない。しかも上記内周面と共に湾曲部・底部の気泡含有率も小さいルツボは引き上不能であり(試料No.A1)、また下部内周面や湾曲部・底部の気泡含有率を本発明の範囲に調整しても上部内周面の気泡含有率が本発明の範囲より小さいルツボは湯面振動が発生し、単結晶化率も低い(試料No.A2、A3)。一方、上部内周面の気泡含有率を0.02〜0.2%にし、下部内周面と湾曲部・底部の気泡含有率をこれより小さくしたルツボは溶融シリコンの湯面振動が見られず単結晶化率も高い(試料No.A4、A5)。ただし、上部内周面の気泡含有率を本発明の範囲に調整しても下部内周面や湾曲部・底部の何れかの気泡含有率が0.1%より高いルツボは湯面振動が抑制されるものの単結晶化率が低い(試料No.A6〜A8)。
【0015】
【表1】

Figure 0004390461
【0016】
〔実施例2〕
溶融シリコンの引き上げ開始湯面から所定深さまでの帯状部分に相当するルツボ内周面層の気泡含有率を0.01〜0.2%とし、湯面より下側の全内表面積S1に対する上記帯状部分の面積S2の割合(S2/S1比)を10〜40%にした石英ガラスルツボを調製した。この石英ガラスルツボを用いてシリコン単結晶を引き上げた。この結果を表2に示した。上記面積比(S2/S1比)が10%の試料No1は溶融シリコンの湯面振動が発生した。上記面積比15〜35%の試料No2〜No5は溶融シリコンの湯面振動がなく、かつ単結晶化率が高い。一方、上記面積比40%の試料No6は溶融シリコンの湯面振動はみられないが単結晶化率が低い。従って、上記帯状部分の面積比は15〜35%が適当であり、20〜30%が好ましい。
【0017】
【表2】
Figure 0004390461

【図面の簡単な説明】
【図1】 本発明に係る石英ガラスルツボの模式断面図
【符号の説明】
10−石英ガラスルツボ、11−溶融シリコン、D−湯面下深さ、L−湯面、H−帯状部分[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a quartz glass crucible used for pulling up a silicon single crystal, and relates to a crucible which suppresses molten metal surface vibration of molten silicon filled in the crucible. The present invention also relates to a method for pulling a silicon single crystal using such a quartz glass crucible.
[0002]
[Prior art]
A quartz glass crucible used for pulling up a silicon single crystal is generally composed of an opaque layer containing bubbles on the outer peripheral side and a transparent layer having few bubbles on the inner peripheral side. Since this quartz glass crucible is greatly influenced by the single crystallization rate due to the bubble content of the inner surface layer, it has been demanded that the bubble content be as low as possible in order to increase the single crystallization rate. For example, there is known a quartz crucible for pulling a single crystal comprising a translucent glass layer containing a large number of bubbles and a transparent glass layer which is integrally fused to the inner surface and is substantially bubble-free and has a smooth surface (special feature). (Kaihei 1-148883). In addition, there is no residual bubbles on the inner surface of the quartz glass crucible, and there is virtually no bubble nuclei that cause bubbles in the vicinity of the inner surface during use, although it is not confirmed visually or under the microscope level. A quartz glass crucible is known which is smooth and provides a high single crystallization rate (Japanese Patent Laid-Open No. 2001-2430). Further, there is known a quartz glass crucible for pulling a silicon single crystal in which an inner surface layer having a high bubble content is removed and a bubble volume ratio of a bottom inner surface layer is 0.001% or less (Japanese Patent Laid-Open No. 11-116388). issue).
[0003]
On the other hand, in the general pulling method (CZ method) of a silicon single crystal, a seed crystal is attached to the molten silicon surface charged to a height of 40 to 90% of the crucible height, and this seed crystal is used as a center. After expanding the crystallization (making shoulder), the body is pulled up to pull up the rod-shaped single crystal, and the bottom is trimmed to take out this single crystal. During this pulling, a phenomenon that the molten silicon melt surface periodically vibrates is observed. When molten metal surface vibration occurs, problems such as failure to join the seed crystal to the molten metal surface and polycrystallization of silicon during pulling occur. As a cause of this, it is considered that the reaction between molten silicon and quartz glass is activated by raising the pulling temperature or lowering the atmospheric pressure, and vibrates when SiO gas is generated.
[0004]
[Problems to be solved by the invention]
In the silicon single crystal pulling process, the seeding and shouldering processes in the pulling start process are most easily affected by molten silicon surface vibration, and the processes after the body pulling are relatively less affected by the surface vibration. Accordingly, it is required that no molten silicon surface vibration occurs in the pulling start process. On the other hand, the conventional quartz crucible has been required to reduce the bubble content of the inner surface of the crucible as much as possible in order to increase the single crystallization rate. It was found that the vibration was influenced by the bubble content of the inner surface layer of the crucible near the molten metal surface. That is, if the bubble content on the inner surface of the crucible in the vicinity of the hot water surface at the start of pulling is too low, hot water surface vibration tends to occur.
[0005]
The present invention provides a quartz glass crucible in which the molten metal surface vibration is suppressed by adjusting the bubble content of the inner surface layer of the crucible in the vicinity of the hot water surface where pulling is started. The present invention also provides a method for pulling up a silicon single crystal that can suppress molten metal surface vibration.
[0006]
[Means for solving the problems]
According to the present invention, a quartz glass crucible having the following configuration is provided.
(1) A quartz glass crucible used for pulling up a silicon single crystal, and with respect to the surface of the molten silicon in the crucible charged to 40 to 90% of the height of the crucible, The bubble content of the inner peripheral surface layer of the crucible corresponding to the band-shaped portion from the predetermined position below the crucible opening end to the predetermined depth is 0.01 to 0.2%. The bubble content of the inner surface transparent layer of the peripheral layer, the curved portion, and the bottom is 0.1% or less and smaller than the bubble content of the band-shaped portion, and the band-shaped portion of the inner surface of the crucible and the lower side thereof The ratio (S2 / S1) of the area S2 of the band-shaped portion to the total area S1 of the inner peripheral surface layer, the curved portion, and the bottom portion (S2 / S1) is 15 to 35%, and the lower end of the band-shaped portion is lower than the lower end of the inner peripheral surface layer Also located above the molten silicon hot water Quartz glass crucible is characterized in that to suppress vibrations.
(2) A crucible inner circumferential surface layer having a diameter of 22 inches (56 cm) or more and a depth of 35 cm or more and corresponding to a belt-like portion from a predetermined position below the opening end serving as a molten metal surface for starting molten silicon to 10 cm. The quartz glass crucible of the above (1), wherein the bubble content of is 0.01 to 0.2%.
(3) The quartz glass crucible as described in (1) or (2) above, wherein the bubble content of the inner peripheral surface layer of the belt-shaped portion is the bubble content in the layer thickness up to 0.3 mm below the surface.
Further, according to the present invention, the following method for pulling a silicon single crystal is provided.
(4) A silicon single crystal pulling method using a quartz glass crucible, wherein the quartz glass crucible is a bubble in a crucible inner peripheral surface layer corresponding to a belt-like portion from a predetermined position below the opening end to a predetermined depth. The content rate is 0.01 to 0.2%, and the bubble content in the inner peripheral surface layer, the curved portion, and the inner transparent layer on the bottom side below the band-shaped portion is 0.1% or less, and the band shape The ratio of the area S2 of the band-shaped part to the total contact area S1 with the molten silicon on the inner surface of the crucible (S2 / S1) is 15 to 35% smaller than the bubble content of the part, and the lower end of the band-shaped part is the above-mentioned A method for pulling a silicon single crystal, wherein the silicon single crystal is pulled with a range corresponding to the band-shaped portion positioned above a lower end of an inner peripheral surface layer as a molten silicon pulling start surface.
[0007]
[Specific explanation]
A quartz glass crucible used for pulling up a silicon single crystal is filled with molten silicon by placing polycrystalline silicon in the crucible and heating and melting it, and this is used for pulling up. As shown in FIG. 1, the quartz glass crucible of the present invention is a crucible corresponding to a belt-like portion H from the molten metal surface L to a predetermined depth D with respect to the molten metal surface L of the molten silicon 11 filled in the crucible 10. The bubble content of the inner peripheral surface layer is 0.01 to 0.2%, and the ratio (S2 / S1) of the area S2 of the strip portion to the total contact area S1 with the molten silicon on the inner surface of the crucible is 15 to 35. It is characterized by suppressing the molten-metal surface vibration of the molten silicon by adjusting to%.
[0008]
As shown in the figure, the band-shaped portion H is a portion from the starting surface L of the pulling up to the depth D, and is a portion that substantially surrounds the upper portion of the inner peripheral surface of the crucible in a band shape. By adjusting the bubble content of the belt-like portion H to 0.01 to 0.2%, it is possible to effectively suppress the hot water surface vibration at the start of pulling. If this bubble content is lower than the above range, hot water surface vibration is likely to occur, and if the bubble content in this portion exceeds the above range, the single crystallization rate is lowered. The bubble content of the belt-like portion H is more preferably 0.02 to 0.1%.
[0009]
The range of the band-shaped portion H having the bubble content is the ratio of the area S2 of the band-shaped portion H to the total contact area S1 (total internal surface area under the molten metal surface) with the molten silicon on the inner surface of the crucible (S2 / S1). Is preferably 15 to 35%. If the area S2 of the belt-like portion H is smaller than this, the depth D of the belt-like portion H is relatively small with respect to the entire inner surface of the crucible, and the effect of suppressing the molten silicon surface vibration is reduced. On the other hand, if the area S2 of the belt-like portion H is larger than this, the portion having a high bubble content rate is relatively increased, so that the single crystallization rate is lowered, which is not preferable.
[0010]
As a specific embodiment, in a quartz glass crucible having a general shape having a diameter of 22 inches or more and a depth of 35 cm or more (ratio W / D = 1 to 2 of the diameter W and the depth D), molten silicon when charged is used. The bubble content of the inner peripheral surface layer of the belt-like crucible corresponding to the surface L from the surface L to approximately 10 cm below the surface is 0.01 to 0.2%, preferably 0.02 to It should be 0.1%. By adjusting the bubble content of the belt-like portion H to the above range, it is possible to effectively suppress the molten-metal surface vibration of the molten silicon.
[0011]
Since the inner surface of the crucible below the belt-like portion H is suppressed from boiling of SiO by the liquid pressure of the molten silicon, there is little influence on the molten metal surface vibration. Therefore, in order to suppress the hot water surface vibration at the start of pulling up, the bubble content of the band-like portion H may be adjusted to the above range. On the other hand, the bubble content on the inner surface of the crucible affects the single crystallization rate, and those having a high bubble content cause problems such as polycrystallization of silicon and remelting, and prolonged pulling time. Therefore, it is preferable that the bubble content of the portion below the belt-like portion H, that is, the inner peripheral surface layer, the curved portion, and the bottom transparent layer below the belt-like portion H is as low as possible. Specifically, the bubble content is preferably 0.1% or less and smaller than the bubble content of the band-shaped portion.
[0012]
In the quartz glass crucible of the present invention, the bubble content of the band-like portion H below the molten silicon surface may be the bubble content at a layer thickness of approximately 0.3 mm below the inner surface. Since the molten silicon surface gradually decreases due to the pulling of the silicon single crystal, the time during which the band-shaped portion H is in contact with the molten silicon is relatively short. Therefore, the band-shaped portion H substantially increases the bubble content in the layer thickness as described above. Adjust to the range. In addition, the inner peripheral surface layer, the curved portion, and the bottom portion below the belt-shaped portion H are in contact with the molten silicon for a longer time than the belt-shaped portion and melt about 1 mm. What is necessary is just to adjust the bubble content rate about the whole to the said range.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be specifically described by way of examples.
[0014]
[Example 1]
The silicon single crystal was pulled up using a quartz glass crucible (caliber 28 inches) in which the bubble content in each part of the inner peripheral surface of the crucible was adjusted as shown in Table 1. The results are shown in Table 1. In addition, the upper inner peripheral surface in the table is a range corresponding to a belt-like portion from the molten metal surface to 10 cm below the molten metal surface with respect to the molten silicon starting surface of the molten silicon. The lower inner peripheral surface is an inner peripheral surface below the belt-shaped portion. Further, the area of the belt-like portion is 20% of the total inner surface area of the crucible below the hot water surface.
As shown in the results of Table 1, a crucible having a bubble content on the upper inner peripheral surface that is smaller than the range of the present invention cannot suppress melt surface vibration at the start of pulling up. In addition, the crucible having a small bubble content at the curved portion / bottom along with the inner peripheral surface cannot be pulled up (Sample No. A1), and the bubble content at the lower inner peripheral surface, curved portion / bottom is within the scope of the present invention. Even if the adjustment is made, the crucible whose bubble content on the upper inner peripheral surface is smaller than the range of the present invention causes the molten metal surface vibration and the single crystallization rate is also low (Sample Nos. A2 and A3). On the other hand, the crucible with the bubble content of the upper inner peripheral surface set to 0.02 to 0.2% and the bubble content of the lower inner peripheral surface and the curved portion / bottom portion smaller than this shows the molten silicon surface vibration. The single crystallization rate is also high (Sample Nos. A4 and A5). However, even if the bubble content of the upper inner peripheral surface is adjusted within the range of the present invention, the crucible with a bubble content higher than 0.1% on the lower inner peripheral surface, curved portion, or bottom portion suppresses hot water surface vibration. However, the single crystallization rate is low (Sample Nos. A6 to A8).
[0015]
[Table 1]
Figure 0004390461
[0016]
[Example 2]
The bubble content of the inner peripheral surface layer of the crucible corresponding to the band-shaped portion from the molten metal surface where the molten silicon starts to be pulled up to a predetermined depth is set to 0.01 to 0.2%, and the above-mentioned band shape with respect to the total inner surface area S1 below the molten metal surface. A quartz glass crucible in which the ratio of the area S2 of the portion (S2 / S1 ratio) was 10 to 40% was prepared. The quartz single crystal was pulled up using this quartz glass crucible. The results are shown in Table 2. In sample No. 1 where the area ratio (S2 / S1 ratio) was 10%, molten metal surface vibration occurred. Samples No. 2 to No. 5 having an area ratio of 15 to 35% have no molten silicon surface vibration and have a high single crystallization rate. On the other hand, Sample No. 6 with an area ratio of 40% does not show molten-metal surface vibration of molten silicon, but has a low single crystallization rate. Accordingly, the area ratio of the band-shaped portion is suitably 15 to 35%, and preferably 20 to 30%.
[0017]
[Table 2]
Figure 0004390461

[Brief description of the drawings]
FIG. 1 is a schematic cross-sectional view of a quartz glass crucible according to the present invention.
10-quartz glass crucible, 11-molten silicon, D-depth below the molten metal surface, L- molten metal surface, H-banded portion

Claims (4)

シリコン単結晶の引き上げに用いる石英ガラスルツボであって、ルツボ高さの40〜90%の高さにチャージした該ルツボ内の溶融シリコンの引き上げ開始湯面に対して、この湯面となるルツボ開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%であり、この帯状部分よりも下側の内周面層、湾曲部、底部の内側透明層の気泡含有率が0.005%以下であり、ルツボ内表面のうち上記帯状部分及びそれよりも下側の内周面層、湾曲部、底部の全面積S1に対する上記帯状部分の面積S2の比(S2/S1)が15〜35%であり、上記帯状部分の下端が上記内周面層の下端よりも上方に位置することによって溶融シリコンの湯面振動を抑制したことを特徴とする石英ガラスルツボ。A quartz glass crucible used for pulling up a silicon single crystal, and a crucible opening serving as a hot water surface with respect to a molten silicon start surface of molten silicon in the crucible charged to a height of 40 to 90% of the height of the crucible The bubble content of the inner peripheral surface layer of the crucible corresponding to the band-shaped portion from the predetermined position below the end to the predetermined depth is 0.01 to 0.2%, and the inner peripheral surface layer below the band-shaped portion The bubble content of the inner transparent layer at the bent portion and the bottom portion is 0.005% or less, and the total area S1 of the belt-like portion and the inner peripheral surface layer, the bent portion, and the lower portion of the inner surface of the crucible. The ratio (S2 / S1) of the area S2 of the belt-like portion to 15 to 35%, and the lower end of the belt-like portion is located above the lower end of the inner peripheral surface layer, thereby causing the molten silicon surface vibration to occur. Quartz glass characterized by suppression Crucible. 口径22インチ(56cm)以上および深さ35cm以上であり、溶融シリコンの引き上げ開始湯面となる開口端よりも下側の所定位置から10cmまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%である請求項1の石英ガラスルツボ。Containing bubbles in the inner peripheral surface layer of the crucible corresponding to a belt-like portion having a diameter of 22 inches (56 cm) or more and a depth of 35 cm or more and corresponding to a belt-like portion from a predetermined position below the opening end serving as a molten metal surface for starting molten silicon to 10 cm The quartz glass crucible according to claim 1, which has a rate of 0.01 to 0.2%. 上記帯状部分の内周面層の気泡含有率が表面下0.3mmまでの層厚における気泡含有率である請求項1または2の石英ガラスルツボ。The quartz glass crucible according to claim 1 or 2, wherein the bubble content of the inner peripheral surface layer of the band-shaped portion is the bubble content at a layer thickness of 0.3 mm below the surface. 石英ガラスルツボを用いたシリコン単結晶の引き上げ方法であって、上記石英ガラスルツボは、開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内周面層の気泡含有率が0.01〜0.2%であり、この帯状部分よりも下側の内周面層、湾曲部、底部の内側透明層の気泡含有率が0.005%以下であり、ルツボ内表面の溶融シリコンとの全接触面積S1に対する上記帯状部分の面積S2の比(S2/S1)が15〜35%であり、上記帯状部分の下端が上記内周面層の下端よりも上方に位置し、上記帯状部分に相当する範囲を溶融シリコンの引き上げ開始湯面として上記シリコン単結晶の引き上げを行うことを特徴とするシリコン単結晶の引き上げ方法。A method for pulling a silicon single crystal using a quartz glass crucible, wherein the quartz glass crucible has a bubble content of an inner peripheral surface layer of a crucible corresponding to a belt-like portion from a predetermined position below a opening end to a predetermined depth. 0.01 to 0.2%, and the bubble content of the inner peripheral surface layer, the curved portion, and the inner transparent layer at the bottom of the strip-shaped portion is 0.005% or less, and the inner surface of the crucible is melted. The ratio (S2 / S1) of the area S2 of the band-shaped part to the total contact area S1 with silicon is 15 to 35%, the lower end of the band-shaped part is located above the lower end of the inner peripheral surface layer, and A method for pulling up a silicon single crystal, wherein the silicon single crystal is pulled up using a range corresponding to a belt-like portion as a molten silicon pulling start surface.
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