JP2005231986A - Quartz glass crucible for pulling up silicon single crystal and method for manufacturing the same - Google Patents

Quartz glass crucible for pulling up silicon single crystal and method for manufacturing the same Download PDF

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JP2005231986A
JP2005231986A JP2004192684A JP2004192684A JP2005231986A JP 2005231986 A JP2005231986 A JP 2005231986A JP 2004192684 A JP2004192684 A JP 2004192684A JP 2004192684 A JP2004192684 A JP 2004192684A JP 2005231986 A JP2005231986 A JP 2005231986A
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quartz glass
single crystal
silicon single
crucible
silica powder
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JP4803784B2 (en
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Yasuo Ohama
康生 大浜
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Shin Etsu Quartz Products Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
    • C03B2201/23—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with hydroxyl groups
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/32—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with aluminium

Abstract

<P>PROBLEM TO BE SOLVED: To provide a quartz glass crucible with which the generation of brown rings is almost suppressed even in the long term operation at a high temperature, the occurrence of vibration in the surface of a silicon melt is prevented, and a silicon single crystal can be pulled up in a high yield; and to provide a method for manufacturing the same. <P>SOLUTION: In the quartz glass crucible for pulling up the silicon single crystal, having an opaque outer layer formed by melting a natural silica powder and a transparent inner layer comprising synthetic quartz glass, the transparent inner layer comprising the synthetic quartz glass has an average aluminum concentration of 1-20 ppm and an average OH-group concentration of 150-300 ppm in a region from the inner surface to the depth of 0.8 mm. The method for manufacturing the quartz glass crucible for pulling up the silicon single crystal comprises supplying synthetic silica powder having an average aluminum concentration of 1-20 ppm into a high temperature atmosphere after or during forming the opaque outer layer, and forming the transparent inner layer comprising the synthetic quartz glass by melting/vitrifying the synthetic silica powder, and at the same time, steam is introduced for at least a certain period when the transparent inner layer is formed. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、シリコン単結晶引上げに用いる石英ガラスルツボ及びその製造方法、さらに詳しくは、単結晶化の歩留まりが高くシリコン単結晶を引き上げることができるシリコン単結晶引上げ用石英ガラスルツボ及びその製造方法に関する。   The present invention relates to a silica glass crucible used for pulling a silicon single crystal and a method for manufacturing the same, and more particularly, to a quartz glass crucible for pulling a silicon single crystal that has a high yield of single crystallization and can pull a silicon single crystal, and a method for manufacturing the same. .

従来、シリコン単結晶の製造には、いわゆるチョクラルスキー法（ＣＺ法）と呼ばれる方法が広く採用されている。このＣＺ法は、石英ガラスで製造したルツボ内でシリコン多結晶を溶融し、このシリコン融液にシリコン単結晶の種結晶を浸漬し、ルツボを回転させながら種結晶を徐々に引上げ、シリコン単結晶を種結晶を核として成長させる方法である。   Conventionally, a so-called Czochralski method (CZ method) has been widely used for the production of silicon single crystals. In this CZ method, a silicon polycrystal is melted in a crucible made of quartz glass, a silicon single crystal seed crystal is immersed in the silicon melt, and the seed crystal is gradually pulled up while rotating the crucible. Is grown using seed crystals as nuclei.

上記ＣＺ法で使用する石英ガラスルツボはシリコンウェーハが大型化するにしたがって１４００℃以上のシリコン融液に長時間接触するようになってきたが、その内表面がシリコン融液と反応し、内表面の浅い層に結晶化が起こり、褐色のリング状のクリストバライト（以下ブラウンリングという）が現れることが起こる。前記ブラウンリング内はクリストバライト層がないか又はあっても大変薄い層であるが、操業時間の経過とともにブラウンリングはその面積を拡大し、互いに融合しながら成長を続け、遂にはその中心部が浸食され、不規則なガラス溶出面となる。このガラス溶出面が出現すると、シリコン単結晶に転位が起こり易くなり、単結晶引上げの歩留まりに支障をきたすことになる。特に、２００ｍｍ以上の大口径のウェーハを製造するシリコン単結晶を成長させるにはＣＺ法の操業を１００時間を超えて行う必要があり、前記ガラス溶出面の出現が顕著となる。   The quartz glass crucible used in the CZ method has come into contact with a silicon melt at 1400 ° C. or higher for a long time as the silicon wafer becomes larger. Crystallization occurs in the shallow layer, and a brown ring-shaped cristobalite (hereinafter referred to as brown ring) appears. The brown ring has a cristobalite layer with or without a cristobalite layer, but as the operating time elapses, the brown ring expands its area and continues to grow while fusing with each other. And an irregular glass elution surface. When this glass elution surface appears, dislocations are likely to occur in the silicon single crystal, which hinders the yield of single crystal pulling. In particular, in order to grow a silicon single crystal for producing a wafer having a large diameter of 200 mm or more, it is necessary to carry out the operation of the CZ method for more than 100 hours, and the appearance of the glass elution surface becomes remarkable.

上記ブラウンリングは、ガラス表面の微細な傷や原料粉の溶け残りである結晶質残留部分、ガラス構造の欠陥などを核として発生すると考えられており、その数を減らすには、ガラスの表面状態を良好に保ったり、結晶質残留成分をなくすために溶融時間を高温、長時間化したり、或いは特許文献１に示すように内表面を形成する原料粉として非晶質である合成粉を使用すればよい。しかしながら、ルツボが更に大型になりシリコン単結晶の引上げ時間が長くなることで更なる改善が求められている。また、その一方で上記方法でブラウンリングの発生数を減らすと、単結晶の引上げ時にシリコン融液の表面が振動し易くなり、作業性を悪化させる欠点があった。   The above brown ring is thought to be caused by fine scratches on the glass surface, crystalline residue that is unmelted raw material powder, defects in the glass structure, etc. In order to maintain good quality, to eliminate residual crystalline components, the melting time is increased to a long time, or as shown in Patent Document 1, an amorphous synthetic powder is used as a raw material powder for forming the inner surface. That's fine. However, further improvement is required because the crucible becomes larger and the pulling time of the silicon single crystal becomes longer. On the other hand, if the number of occurrences of brown rings is reduced by the above method, the surface of the silicon melt tends to vibrate when the single crystal is pulled up, and there is a drawback that workability is deteriorated.

上記欠点を解消するため、本発明者は先に天然石英ガラスからなる不透明な外層、その内側に少なくとも石英ガラスからなる透明層を有する石英ガラスルツボにおいて、シリコン単結晶引上げの使用後に、シリコン融液の初期湯面位置から特定の範囲までと残湯位置上特定の範囲までに観測されるブラウンリングの個数の比が特定の割合になるシリコン単結晶引上げ用石英ガラスルツボを提案した（特許文献２）。前記シリコン単結晶引上げ用石英ガラスルツボは、例えば天然シリカ粉を回転する型に導入し、ルツボ形状に成形したのち、アーク電極によりルツボ状成形体の内部キャビティーを高温ガス雰囲気にして少なくとも部分的に溶融ガラス化して不透明なルツボ基体を形成し、次いで高純度の天然シリカ粉または天然合成混合シリカを供給し、溶融ガラス化して天然石英ガラスまたは天然合成混合石英ガラスからなる透明層を初期湯面位置から特定の範囲に、さらに合成石英ガラスからなる透明層を残湯位置上の特定の範囲に形成するなどその製造方法に少し煩雑なところがあり、より簡便な方法で優れた単結晶化率を達成できるシリコン単結晶引上げ用石英ガラスルツボの出現が熱望されていた。
特許第２８１１２９０号及び特許第２９３３４０４号 特願２００３−１４１７０２ In order to eliminate the above-mentioned drawbacks, the present inventor previously made a silicon melt after using a silicon single crystal pulling in a quartz glass crucible having an opaque outer layer made of natural quartz glass and a transparent layer made of at least quartz glass inside. Proposed a quartz glass crucible for pulling a silicon single crystal in which the ratio of the number of brown rings observed from the initial molten metal surface position to a specific range and a specific range on the remaining molten metal position is a specific ratio (Patent Document 2) ). The silica glass crucible for pulling up the silicon single crystal is, for example, introduced by introducing natural silica powder into a rotating mold and formed into a crucible shape, and then at least partially making the internal cavity of the crucible-shaped body with a high temperature gas atmosphere by an arc electrode. An opaque crucible substrate is formed by melting into vitrified glass, and then a high-purity natural silica powder or natural synthetic mixed silica is supplied to form a transparent layer made of natural quartz glass or natural synthetic mixed quartz glass. There is a little complicated place in the manufacturing method, such as forming a transparent layer made of synthetic quartz glass in a specific range on the remaining hot water position from a position to a specific range, and an excellent single crystallization rate can be achieved with a simpler method. The advent of a quartz glass crucible for pulling a silicon single crystal that can be achieved has been eagerly desired.
Patent No. 2811290 and Patent No. 2933404 Japanese Patent Application No. 2003-141702

こうした現状に鑑み、本発明者は鋭意研究を続けた結果、天然シリカ粉を溶融して形成した不透明な外層と、合成石英ガラスからなる透明な内層を有する石英ガラスルツボにおいて、前記合成石英ガラスからなる透明な内層が内表面から０．８ｍｍまでの深さにおいて平均アルミニウム濃度が１〜２０ｐｐｍ、平均ＯＨ基濃度が１５０〜３００ｐｐｍとなるように調整することで、ブラウンリングの発生が抑えられ、その結果、長時間操業してもガラス溶出面の出現が少なくシリコン単結晶の歩留りが良くなること、更に、ブラウンリングが少なくてもシリコン融液表面の振動が抑えられることを見出して、本発明を完成したものである。すなわち、   In view of such a current situation, the present inventor has conducted intensive research, and as a result, in a quartz glass crucible having an opaque outer layer formed by melting natural silica powder and a transparent inner layer made of synthetic quartz glass, By adjusting the transparent inner layer to have an average aluminum concentration of 1 to 20 ppm and an average OH group concentration of 150 to 300 ppm at a depth of 0.8 mm from the inner surface, the occurrence of brown rings can be suppressed, As a result, even when operated for a long time, the appearance of the glass elution surface is small, the yield of the silicon single crystal is improved, and furthermore, the vibration of the surface of the silicon melt can be suppressed even if the brown ring is small. It has been completed. That is,

本発明は、ブラウンリングの発生が少なく、しかもシリコン融液表面の振動がなく、シリコン単結晶を高歩留まりで引上げることができるシリコン単結晶引上げ用石英ガラスルツボを提供することを目的とする。   An object of the present invention is to provide a quartz glass crucible for pulling up a silicon single crystal that can generate a silicon single crystal with a high yield, with little occurrence of Brownian rings and no vibration of the surface of the silicon melt.

また、本発明は、上記シリコン単結晶引上げ用石英ガラスルツボの製造方法を提供することを目的とする。   Another object of the present invention is to provide a method for producing the silica glass crucible for pulling up the silicon single crystal.

上記目的を達成する本発明は、天然シリカ粉を溶融して形成した不透明な外層と、合成石英ガラスからなる透明な内層を有する石英ガラスルツボにおいて、前記合成石英ガラスからなる透明な内層が内表面から０．８ｍｍまでの深さにおいて１〜２０ｐｐｍの平均アルミニウム濃度と１５０〜３００ｐｐｍの平均ＯＨ基濃度を有することを特徴とするシリコン単結晶引上げ用石英ガラスルツボ及びその製造方法に係る。   To achieve the above object, the present invention provides a quartz glass crucible having an opaque outer layer formed by melting natural silica powder and a transparent inner layer made of synthetic quartz glass, wherein the transparent inner layer made of synthetic quartz glass has an inner surface. The present invention relates to a quartz glass crucible for pulling up a silicon single crystal, characterized by having an average aluminum concentration of 1 to 20 ppm and an average OH group concentration of 150 to 300 ppm at a depth of 1 to 0.8 mm.

本発明のシリコン単結晶引上げ用石英ガラスルツボは、上述のとおり合成石英ガラスからなる透明な内層を有し、その厚さは０．８ｍｍ以上で石英ガラスルツボの肉厚の３５％以下が好ましい。そして、前記合成石英ガラスからなる透明な内層の内表面から０．８ｍｍまでの深さにおいて平均アルミニウム濃度が１〜２０ｐｐｍ、好ましくは３〜８ｐｐｍで、かつ平均ＯＨ基濃度が１５０〜３００ｐｐｍに調整されているルツボである。前記合成石英ガラスからなる透明な内層の厚さが０．８ｍｍ未満では、シリコン単結晶引上げ中に石英ガラスがシリコン融液に溶け出し、不透明な石英ガラス層が現れ単結晶化率を著しく低下させてしまう。また、合成石英ガラスからなる透明な内層の厚さをルツボの肉厚の３５％を超える厚さに形成することは、ルツボ製造の生産性・経済性の観点から好ましくない。合成石英ガラスからなる透明な内層が前記範囲の平均アルミニウム濃度及び平均ＯＨ基濃度を有することでルツボの使用後に発生するブラウンリングの個数が０．１〜０．８個／ｃｍ２の範囲となり、シリコン単結晶の歩留りをよくする。その上、合成石英ガラスからなる透明な内層とシリコン融液の濡れ特性が増し、シリコン融液表面の振動が抑えられ、高歩留まりでシリコン単結晶を引上げることができる。ブラウンリングの個数を０．１個／ｃｍ２未満とすることは困難であり、またブラウンリングの個数が０．８個／ｃｍ２を超えるとシリコン単結晶に転位が多く起こり単結晶化率が低下する。 The silica glass crucible for pulling a silicon single crystal of the present invention has a transparent inner layer made of synthetic quartz glass as described above, and the thickness is preferably 0.8 mm or more and 35% or less of the thickness of the quartz glass crucible. The average aluminum concentration is adjusted to 1 to 20 ppm, preferably 3 to 8 ppm, and the average OH group concentration is adjusted to 150 to 300 ppm at a depth of 0.8 mm from the inner surface of the transparent inner layer made of the synthetic quartz glass. It is a crucible. If the thickness of the transparent inner layer made of the synthetic quartz glass is less than 0.8 mm, the quartz glass dissolves into the silicon melt during the pulling of the silicon single crystal, and an opaque quartz glass layer appears to significantly reduce the single crystallization rate. End up. Moreover, it is not preferable from the viewpoint of productivity and economic efficiency of crucible production that the thickness of the transparent inner layer made of synthetic quartz glass is more than 35% of the thickness of the crucible. The transparent inner layer made of synthetic quartz glass has an average aluminum concentration and an average OH group concentration in the above ranges, so that the number of brown rings generated after use of the crucible is in the range of 0.1 to 0.8 / cm 2 , Improve the yield of silicon single crystal. Moreover, the wettability of the transparent inner layer made of synthetic quartz glass and the silicon melt is increased, the vibration of the silicon melt surface is suppressed, and the silicon single crystal can be pulled up with a high yield. It is difficult to make the number of brown rings less than 0.1 pieces / cm 2 , and when the number of brown rings exceeds 0.8 pieces / cm 2 , many dislocations occur in the silicon single crystal and the single crystallization rate is low. descend.

本発明で使用する合成シリカ粉としては、Ｎａ、Ｋ、Ｌｉ、Ｔｉ、Ｆｅ、Ｃｕなどの不純物濃度が０．１ｐｐｍ以下であるのがよい。不純物濃度が前記範囲にあることでシリコン単結晶への不純物の悪影響はほとんどない。また、前記範囲の平均アルミニウム濃度を有する合成シリカ粉は、シリカ粉にアルミニウム粉を混合する方法、ケイ素化合物とアルミニウム化合物との均一溶液を加水分解、乾燥、焼成する方法又はシリカ粉をアルミニウム化合物の溶液に浸漬したのち、乾燥し、シリカ粉にアルミニウム化合物の被膜を形成する方法などで製造されるが、特にケイ素化合物とアルミニウム化合物との均一溶液を加水分解、乾燥、焼成する方法は、アルミニウムが均一に含有されて好ましい。   The synthetic silica powder used in the present invention preferably has an impurity concentration of Na, K, Li, Ti, Fe, Cu or the like of 0.1 ppm or less. When the impurity concentration is in the above range, there is almost no adverse effect of impurities on the silicon single crystal. The synthetic silica powder having an average aluminum concentration in the above range is a method of mixing aluminum powder with silica powder, a method of hydrolyzing, drying and firing a uniform solution of a silicon compound and an aluminum compound, or silica powder of an aluminum compound. After being immersed in the solution, it is dried and manufactured by a method of forming a film of an aluminum compound on silica powder. In particular, the method of hydrolyzing, drying and firing a uniform solution of a silicon compound and an aluminum compound is the It is preferably contained uniformly.

上記ブラウンリングの個数は、ルツボの使用後の内表面に現れる数をカウントするものであるが、ルツボのシリコン融液との接触時間が長く、ブラウンリングが成長し易い残湯付近においてはブラウンリングが融合する場合があるので、ルツボの同一高さの水平方向において観測される単独のブラウンリングの平均径から１個当たりの面積を計算し、融合部分の面積を前記１個当たりの面積で割った値を求め、その値と前記単独のブラウンリングの個数の総数とをルツボの内表面積で割った値を単位面積（ｃｍ２）当りの個数とする。 The number of brown rings is the number that appears on the inner surface of the crucible after use. However, the length of contact with the silicon melt of the crucible is long and the brown ring is near the remaining hot water where the brown ring is likely to grow. Therefore, the area per piece is calculated from the average diameter of a single brown ring observed in the horizontal direction at the same height of the crucible, and the area of the fused portion is divided by the area per piece. A value obtained by dividing the value and the total number of single brown rings by the inner surface area of the crucible is defined as the number per unit area (cm 2 ).

また、上記平均アルミニウム濃度は、石英ガラスルツボの透明な内層から試験片を切出しＩＣＰ発光分光分析法で測定した値であり、また、平均ＯＨ基濃度は、ルツボの内表面の深さ方向１．０ｍｍまでをＤ．Ｍ． ＤＯＤＤ ａｎｄ Ｄ．Ｂ．ＦＲＡＳＥＲ，Ｏｐｔｉｃａｌ ｄｅｔｅｒｍｉｎａｔｉｏｎ ｏｆ ＯＨ ｉｎ ｆｕｓｅｄ ｓｉｌｉｃａ， Ｊｏｕｒｎａｌ ｏｆ Ａｐｐｌｉｅｄ Ｐｈｙｓｉｃｓ， Ｖｏｌ． ３７（１９６６）ｐ．３９１１に記載の測定法で測定した値である。   The average aluminum concentration is a value obtained by cutting a test piece from a transparent inner layer of a quartz glass crucible and measuring it by ICP emission spectroscopic analysis, and the average OH group concentration is 1. in the depth direction of the inner surface of the crucible. D. up to 0 mm. M.M. DODD and D.D. B. FRASER, Optical determination of OH in fused silica, Journal of Applied Physics, Vol. 37 (1966) p. It is a value measured by the measurement method described in 3911.

さらに、本発明の石英ガラスルツボは、アルミニウムを含有する合成石英ガラスからなる透明層と天然石英ガラスからなる不透明な外層との間に天然石英ガラスからなる透明層を設けることができる。この天然石英ガラスからなる透明層を設けることで内層と外層との剥離が少なくなる上に、ルツボの変形も少なくなる。前記天然石英ガラスからなる透明層の厚さは０．４〜５．０ｍｍ、好ましくは０．７〜４．０ｍｍの範囲がよい。   Furthermore, the quartz glass crucible of the present invention can provide a transparent layer made of natural quartz glass between a transparent layer made of synthetic quartz glass containing aluminum and an opaque outer layer made of natural quartz glass. By providing this transparent layer made of natural quartz glass, peeling between the inner layer and the outer layer is reduced, and deformation of the crucible is reduced. The transparent layer made of natural quartz glass has a thickness of 0.4 to 5.0 mm, preferably 0.7 to 4.0 mm.

本発明のシリコン単結晶引上げ用石英ガラスルツボは、高温での長時間操業においてもルツボの内表面に発生するブラウンリングの個数が少なく、かつシリコン融液表面の振動もなくシリコン単結晶を高歩留まりで引き上げることができる。しかも、前記シリコン単結晶引上げ用石英ガラスルツボは、平均アルミニウム濃度が１〜２０ｐｐｍの合成シリカ粉を用いて形成した合成石英ガラスからなる透明な内層の形成中に水蒸気を導入し、合成石英ガラスからなる透明な内層が内表面から０．８ｍｍまでの深さにおいて平均アルミニウム濃度が１〜２０ｐｐｍ、
平均ＯＨ基濃度が１５０〜３００ｐｐｍとなるように調整するという簡便な方法で製造できる。 The silica glass crucible for pulling a silicon single crystal of the present invention has a high yield of silicon single crystal with a small number of brown rings generated on the inner surface of the crucible even during long-time operation at high temperatures and without vibration of the silicon melt surface. Can be pulled up. In addition, the silica glass crucible for pulling up the silicon single crystal introduces water vapor during the formation of a transparent inner layer made of synthetic silica glass formed using synthetic silica powder having an average aluminum concentration of 1 to 20 ppm, The transparent inner layer has an average aluminum concentration of 1 to 20 ppm at a depth of 0.8 mm from the inner surface,
It can manufacture by the simple method of adjusting so that an average OH group density | concentration may be 150-300 ppm.

次に、本発明の製造方法の実施の態様を図面に基づいて説明するが、本発明はこれに限定されるものではない。   Next, an embodiment of the production method of the present invention will be described with reference to the drawings, but the present invention is not limited to this.

図１に本発明の石英ガラスルツボの製造装置を示す。図１において、１は回転する型、２は不透明な外層、３はシリカ粉供給手段、４は水蒸気導入ノズル、５は板状の蓋体、６はアーク電極、７は高温ガス雰囲気、８はアルミニウムを含有する合成石英ガラスからなる透明な内層である。前記装置を用いて、まず天然シリカ粉を回転する型１に導入し、ルツボ形状に成形したのち、その中にアーク電極６を挿入し、ルツボ状形成体の開口部を板状の蓋体５で覆い、アーク電極６により該ルツボ状形成体の内部キャビティーを高温ガス雰囲気７にし、少なくとも部分的に溶融ガラス化して不透明な外層２を形成し、次いで外層の形成後もしくは形成中にシリカ粉供給手段３から平均アルミニウム濃度が１〜２０ｐｐｍ、好ましくは３〜８ｐｐｍの合成シリカ粉を導入し、溶融ガラス化して合成石英ガラスからなる透明な内層８を厚さが０．８ｍｍ以上で石英ガラスルツボの肉厚の３５％以下に形成する。前記透明な内層の形成の一定期間、水蒸気を水蒸気導入ノズル４から導入し透明な内層が内表面から０．８ｍｍまでの深さにおいて平均アルミニウム濃度が１〜２０ｐｐｍ、平均ＯＨ基濃度が１５０〜３００ｐｐｍとなるように調整する。水蒸気の導入期間は、内層形成工程の少なくとも２５％以上、好ましくは４０％以上の段階で行う。必要な水蒸気導入量は、ルツボの大きさにより異なるが、ルツボ外径が４０〜６３．４ｃｍの場合は、合成シリカ粉１００重量部に対し０．５〜４０重量部、好ましくは１〜３０重量部、ルツボ外径が６３．５〜７３．９ｃｍの場合は、１〜６０重量部、好ましくは１．５〜５０重量部、ルツボ外径が７４〜１２５ｃｍの場合には、１．２５〜１００重量部、好ましくは２〜８０重量部とするのがよい。   FIG. 1 shows an apparatus for producing a silica glass crucible of the present invention. In FIG. 1, 1 is a rotating mold, 2 is an opaque outer layer, 3 is a silica powder supply means, 4 is a water vapor introduction nozzle, 5 is a plate-shaped lid, 6 is an arc electrode, 7 is a hot gas atmosphere, and 8 is It is a transparent inner layer made of synthetic quartz glass containing aluminum. Using the apparatus, first, natural silica powder is introduced into a rotating mold 1 and formed into a crucible shape, and then an arc electrode 6 is inserted therein, and the opening of the crucible-shaped formed body is formed into a plate-shaped lid 5. The inner cavity of the crucible-shaped formed body is made into a high-temperature gas atmosphere 7 by the arc electrode 6, and at least partially melted and vitrified to form the opaque outer layer 2, and then the silica powder after or during the formation of the outer layer Synthetic silica powder having an average aluminum concentration of 1 to 20 ppm, preferably 3 to 8 ppm, is introduced from the supply means 3 and is converted into a molten glass to form a transparent inner layer 8 made of synthetic quartz glass having a thickness of 0.8 mm or more and a quartz glass crucible. It is formed to be 35% or less of the wall thickness. During a certain period of formation of the transparent inner layer, water vapor is introduced from the water vapor introduction nozzle 4 and the transparent inner layer has an average aluminum concentration of 1 to 20 ppm and an average OH group concentration of 150 to 300 ppm at a depth of 0.8 mm from the inner surface. Adjust so that The introduction period of the water vapor is performed at a stage of at least 25%, preferably 40% or more of the inner layer forming step. The necessary water vapor introduction amount varies depending on the size of the crucible, but when the outer diameter of the crucible is 40 to 63.4 cm, 0.5 to 40 parts by weight, preferably 1 to 30 parts by weight with respect to 100 parts by weight of the synthetic silica powder. 1 to 60 parts by weight, preferably 1.5 to 50 parts by weight when the outer diameter of the crucible is 63.5 to 73.9 cm, and 1.25 to 100 when the outer diameter of the crucible is 74 to 125 cm. The weight is preferably 2 to 80 parts by weight.

上記製造方法において、合成石英ガラスからなる透明な内層と天然石英ガラスからなる不透明な外層との間に天然石英ガラスからなる透明層を設ける場合には、不透明な外層を形成したのち、天然シリカ粉をシリカ粉供給手段３から供給し溶融ガラス化し天然石英ガラスからなる透明層を形成し、ついでシリカ粉供給手段３から上記アルミニウムを含有する合成シリカ粉を導入して製造するのがよい。   In the above production method, when a transparent layer made of natural quartz glass is provided between a transparent inner layer made of synthetic quartz glass and an opaque outer layer made of natural quartz glass, the natural silica powder is formed after forming the opaque outer layer. The silica powder supply means 3 is supplied to melt glass to form a transparent layer made of natural quartz glass, and the silica powder supply means 3 is then introduced with the synthetic silica powder containing aluminum.

図１に示す装置を用い、回転する型１内に純化処理した高純度の天然シリカ粉を投入し、遠心力によりルツボ状成形体に形成し、その内にアーク電極６を挿入し、開口部を板状の蓋体５で覆い、アーク電極６により内部キャビティー内を高温ガス雰囲気７とし、溶融ガラス化し、冷却して厚さ８〜１０ｍｍの不透明な外層２を作成した。次いで型１を回転させながら平均アルミニウム濃度５ｐｐｍ、平均ＯＨ基濃度が５０ｐｐｍの合成シリカ粉をシリカ粉供給手段３から１００ｇ／ｍｉｎで供給し、溶融して厚さ１〜３ｍｍ合成石英ガラスからなる透明な内層を形成し２４インチの石英ガラスルツボを１０個製造した。前記合成シリカ粉の供給開始とともに水蒸気を２０ｍｌ／分で３０分間、計６００ｍｌを導入した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は２２０ｐｐｍ、平均アルミニウム濃度は５ｐｐｍであった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。引上げ後のルツボ内表面のブラウンリングの個数は０．３〜０．５個／ｃｍ２にあった。また、シリコン融液表面の振動がなく、平均単結晶化率は９８％と高かった。
（比較例１） Using the apparatus shown in FIG. 1, purified high-purity natural silica powder is put into a rotating mold 1, formed into a crucible shaped body by centrifugal force, an arc electrode 6 is inserted into the crucible-shaped body, and an opening Was covered with a plate-like lid 5, and the inside cavity was made into a high-temperature gas atmosphere 7 by an arc electrode 6, melted into glass, and cooled to prepare an opaque outer layer 2 having a thickness of 8 to 10 mm. Next, while rotating the mold 1, synthetic silica powder having an average aluminum concentration of 5 ppm and an average OH group concentration of 50 ppm is supplied from the silica powder supply means 3 at 100 g / min, and is melted to be transparent made of synthetic quartz glass having a thickness of 1 to 3 mm An inner layer was formed, and ten 24-inch quartz glass crucibles were manufactured. A total of 600 ml of water vapor was introduced at 20 ml / min for 30 minutes with the start of the supply of the synthetic silica powder. The obtained quartz glass crucible had an average OH group concentration of 220 ppm and an average aluminum concentration of 5 ppm up to 0.8 mm in the inner surface depth direction. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible after the pulling was 0.3 to 0.5 / cm 2 . Moreover, there was no vibration of the silicon melt surface, and the average single crystallization rate was as high as 98%.
(Comparative Example 1)

実施例１において、平均アルミニウム濃度が０．１ｐｐｍ以下、平均ＯＨ基濃度が５０ｐｐｍの合成シリカ粉を用い、水蒸気導入を行うことなく、実施例１と同様にして２４インチの石英ガラスルツボを１０個製造した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は８０ｐｐｍ、平均アルミニウム濃度は０．１ｐｐｍ以下であった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。ルツボ内表面のブラウンリングの個数は０．９〜１．１個／ｃｍ２であり、平均単結晶化率は８８％であった。シリコン単結晶の引上げの初期に若干シリコン融液表面の振動がみられた。
（比較例２） In Example 1, synthetic silica powder having an average aluminum concentration of 0.1 ppm or less and an average OH group concentration of 50 ppm was used, and 10 pieces of 24-inch quartz glass crucibles were introduced in the same manner as in Example 1 without introducing water vapor. Manufactured. The obtained quartz glass crucible had an average OH group concentration of 80 ppm up to 0.8 mm in the inner surface depth direction, and an average aluminum concentration of 0.1 ppm or less. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible was 0.9 to 1.1 pieces / cm 2 , and the average single crystallization rate was 88%. A slight vibration of the surface of the silicon melt was observed at the initial stage of pulling the silicon single crystal.
(Comparative Example 2)

実施例１において、平均アルミニウム濃度が５ｐｐｍ、平均ＯＨ基濃度が５０ｐｐｍの合成シリカ粉を用い、かつ水蒸気の導入を行うことなく、実施例１と同様にして２４インチの石英ガラスルツボを１０個製造した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は８０ｐｐｍ、平均アルミニウム濃度が５ｐｐｍであった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。ルツボ内表面のブラウンリングの個数は１．０〜１．２個／ｃｍ２であり、平均単結晶化率は８９％であった。比較例１に比べれば少ないが、シリコン融液表面の振動が若干みられた。
（比較例３） In Example 1, 10 synthetic silica glass crucibles having the average aluminum concentration of 5 ppm and the average OH group concentration of 50 ppm were produced in the same manner as in Example 1 without introducing water vapor. did. The obtained quartz glass crucible had an average OH group concentration of up to 0.8 mm in the inner surface depth direction of 80 ppm and an average aluminum concentration of 5 ppm. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible was 1.0 to 1.2 pieces / cm 2 , and the average single crystallization rate was 89%. Although there were few compared with the comparative example 1, some vibrations of the silicon melt surface were seen.
(Comparative Example 3)

実施例１において、平均アルミニウム濃度が０．１ｐｐｍ以下、平均ＯＨ基濃度が５０ｐｐｍの合成シリカ粉を用いた以外、実施例１と同様に水蒸気を導入して２４インチの石英ガラスルツボを１０個製造した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は２２０ｐｐｍ、平均アルミニウム濃度は０．１ｐｐｍ以下であった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。ルツボ内表面のブラウンリングの個数は０．９〜１．１個／ｃｍ２であり、平均単結晶化率は９０％であった。比較例１、比較例２に比べれば少ないがごくわずかシリコン融液表面の振動がみられた。
（比較例４） In Example 1, 10 24-inch quartz glass crucibles were produced by introducing water vapor in the same manner as in Example 1 except that synthetic silica powder having an average aluminum concentration of 0.1 ppm or less and an average OH group concentration of 50 ppm was used. did. The obtained quartz glass crucible had an average OH group concentration of up to 0.8 mm in the inner surface depth direction of 220 ppm and an average aluminum concentration of 0.1 ppm or less. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible was 0.9 to 1.1 pieces / cm 2 , and the average single crystallization rate was 90%. Compared to Comparative Example 1 and Comparative Example 2, the vibration of the surface of the silicon melt was very small.
(Comparative Example 4)

図１に示す装置を用い、回転する型１内に純化処理した天然シリカ粉を投入し、遠心力によりルツボ状成形体に形成し、その内にアーク電極６を挿入し、開口部を板状の蓋体５で覆い、アーク電極６により内部キャビティー内を高温ガス雰囲気７とし、溶融ガラス化し、冷却して厚さ８〜１０ｍｍの不透明な外層２を作成した。次いで型１を回転させながら平均アルミニウム濃度が５ｐｐｍの天然シリカ粉をシリカ粉供給手段３から１００ｇ／ｍｉｎで供給し、溶融して厚さ１〜３ｍｍ天然石英ガラス透明内層を形成して２４インチの石英ガラスルツボを１０個製造した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は５０ｐｐｍ、平均アルミニウム濃度は５ｐｐｍであった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。ルツボ内表面のブラウンリングの個数は２．８〜４．７個／ｃｍ２であり、平均単結晶化率は６８％であった。
（比較例５） Using the apparatus shown in FIG. 1, purified natural silica powder is put into a rotating mold 1 and formed into a crucible shaped body by centrifugal force, and an arc electrode 6 is inserted therein, and the opening is plate-shaped. The inner cavity was made into a high-temperature gas atmosphere 7 by the arc electrode 6, melted into glass, and cooled to form an opaque outer layer 2 having a thickness of 8 to 10 mm. Next, while rotating the mold 1, natural silica powder having an average aluminum concentration of 5 ppm is supplied from the silica powder supply means 3 at 100 g / min and melted to form a natural quartz glass transparent inner layer having a thickness of 1 to 3 mm. Ten quartz glass crucibles were produced. The obtained quartz glass crucible had an average OH group concentration of up to 0.8 mm in the inner surface depth direction of 50 ppm and an average aluminum concentration of 5 ppm. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible was 2.8 to 4.7 / cm 2 , and the average single crystallization rate was 68%.
(Comparative Example 5)

比較例４において、天然石英ガラスからなる透明内層を形成中、天然シリカ粉の供給開始と同時に水蒸気を２０ｍｌ／分で３０分間、計６００ｍｌを導入した。得られた石英ガラスルツボの内表面深さ方向０．８ｍｍまでの平均ＯＨ基濃度は２００ｐｐｍ、平均アルミニウム濃度は５ｐｐｍであった。前記石英ガラスルツボを用いてＣＺ法でシリコン単結晶の引上げを行った。ルツボ内表面のブラウンリングの個数は３．０〜４．３／ｃｍ２であり、平均単結晶化率は７４％であった。 In Comparative Example 4, while forming a transparent inner layer made of natural quartz glass, water vapor was introduced at a rate of 20 ml / min for 30 minutes simultaneously with the start of the supply of natural silica powder, for a total of 600 ml. The obtained quartz glass crucible had an average OH group concentration of 200 ppm and an average aluminum concentration of 5 ppm up to 0.8 mm in the inner surface depth direction. The silicon single crystal was pulled by the CZ method using the quartz glass crucible. The number of brown rings on the inner surface of the crucible was 3.0 to 4.3 / cm 2 , and the average single crystallization rate was 74%.

本発明のシリコン単結晶引上げ用石英ガラスルツボは、大型のシリコン単結晶を高歩留まりで引き上げることができ、シリコン単結晶の引上げの技術分野で有用である。   The silica glass crucible for pulling a silicon single crystal of the present invention can pull a large silicon single crystal with a high yield, and is useful in the technical field of pulling a silicon single crystal.

本発明の石英ガラスルツボを製造するための製造装置の概略図を示す。The schematic of the manufacturing apparatus for manufacturing the quartz glass crucible of this invention is shown.

符号の説明Explanation of symbols

１：回転する型
２：不透明な外層
３：シリカ粉供給手段
４：水蒸気導入ノズル
５：板状の蓋体
６：アーク電極
７：高温雰囲気
８：合成石英ガラスからなる透明な内層 1: rotating mold 2: opaque outer layer 3: silica powder supply means 4: water vapor introduction nozzle 5: plate-like lid 6: arc electrode 7: high temperature atmosphere 8: transparent inner layer made of synthetic quartz glass

Claims (6)

天然シリカ粉を溶融して形成した不透明な外層と、合成石英ガラスからなる透明な内層を有する石英ガラスルツボにおいて、前記合成石英ガラスからなる透明な内層が内表面から０．８ｍｍまでの深さにおいて１〜２０ｐｐｍの平均アルミニウム濃度と１５０〜３００ｐｐｍの平均ＯＨ基濃度を有することを特徴とするシリコン単結晶引上げ用石英ガラスルツボ。 In a quartz glass crucible having an opaque outer layer formed by melting natural silica powder and a transparent inner layer made of synthetic quartz glass, the transparent inner layer made of synthetic quartz glass has a depth of 0.8 mm from the inner surface. A quartz glass crucible for pulling a silicon single crystal having an average aluminum concentration of 1 to 20 ppm and an average OH group concentration of 150 to 300 ppm. 平均アルミニウム濃度が３〜８ｐｐｍであることを特徴とする請求項１記載のシリコン単結晶引上げ用石英ガラスルツボ。 The quartz glass crucible for pulling up a silicon single crystal according to claim 1, wherein the average aluminum concentration is 3 to 8 ppm. シリコン単結晶引上げ後の合成石英ガラスからなる透明な内層を有するルツボの内表面に現われるブラウンリングの個数が０．１〜０．８個／ｃｍ２であることを特徴とする請求項１又は２記載のシリコン単結晶引上げ用石英ガラスルツボ。 3. The number of brown rings appearing on the inner surface of a crucible having a transparent inner layer made of synthetic quartz glass after pulling a silicon single crystal is 0.1 to 0.8 / cm 2. A quartz glass crucible for pulling up a silicon single crystal as described. 天然シリカ粉を溶融して形成した不透明な外層と合成石英ガラスからなる透明な内層との間に天然シリカ粉からなる透明層を有することを特徴とする請求項１ないし３のいずれか１記載のシリコン単結晶引上げ用石英ガラスルツボ。 4. A transparent layer made of natural silica powder is provided between an opaque outer layer formed by melting natural silica powder and a transparent inner layer made of synthetic quartz glass. A quartz glass crucible for pulling silicon single crystals. 天然シリカ粉を回転する型内に供給して形成した石英ガラスルツボ基体の内部キャビティを高温雰囲気にし部分的に溶融して不透明な外層を形成した後もしくは形成中に、１〜２０ｐｐｍの平均アルミニウム濃度を有する合成シリカ粉を前記高温雰囲気内に供給し溶融ガラス化して合成石英ガラスからなる透明な内層を形成するとともにその形成中の少なくとも一定の期間、水蒸気を導入することを特徴とする請求項１ないし３のいずれか１記載のシリコン単結晶引上げ用石英ガラスルツボの製造方法。 An average aluminum concentration of 1 to 20 ppm after or during the formation of an opaque outer layer by partially melting the internal cavity of a quartz glass crucible substrate formed by supplying natural silica powder into a rotating mold. 2. A synthetic silica powder having the following composition is supplied into the high-temperature atmosphere to form a molten inner glass to form a transparent inner layer made of synthetic quartz glass, and water vapor is introduced for at least a certain period during the formation. 4. A method for producing a quartz glass crucible for pulling a silicon single crystal according to any one of items 1 to 3. 回転する型内に形成した石英ガラスルツボ基体の内部キャビティを高温雰囲気にし部分的に溶融して不透明な外層を形成した後もしくは形成中に、天然シリカ粉を導入し、溶融ガラス化し天然シリカ粉からなる透明層を形成し、更に１〜２０ｐｐｍの平均アルミニウム濃度を有する合成シリカ粉を前記高温雰囲気内に供給し溶融ガラス化して合成石英ガラスからなる透明な内層を形成するとともにその形成中の少なくとも一定の期間、水蒸気を導入することを特徴とする請求項４記載のシリコン単結晶引上げ用石英ガラスルツボの製造方法。 After or during the formation of the opaque outer layer by partially melting the internal cavity of the quartz glass crucible substrate formed in the rotating mold into a high-temperature atmosphere, natural silica powder is introduced to melt and vitrify from the natural silica powder. And forming a transparent inner layer made of synthetic quartz glass by supplying synthetic silica powder having an average aluminum concentration of 1 to 20 ppm into the high-temperature atmosphere to form a transparent inner layer and at least constant during the formation 5. The method for producing a quartz glass crucible for pulling up a silicon single crystal according to claim 4, wherein water vapor is introduced during the period.
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CN113897669A (en) * 2016-09-13 2022-01-07 胜高股份有限公司 Quartz glass crucible and method for producing same
CN113897669B (en) * 2016-09-13 2023-11-07 胜高股份有限公司 Quartz glass crucible and method for producing same
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CN110863241A (en) * 2019-10-12 2020-03-06 内蒙古中环光伏材料有限公司 Manufacturing process of quartz crucible for prolonging minority carrier lifetime of silicon single crystal
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