JP5517868B2 - Silica glass crucible - Google Patents
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- JP5517868B2 JP5517868B2 JP2010219803A JP2010219803A JP5517868B2 JP 5517868 B2 JP5517868 B2 JP 5517868B2 JP 2010219803 A JP2010219803 A JP 2010219803A JP 2010219803 A JP2010219803 A JP 2010219803A JP 5517868 B2 JP5517868 B2 JP 5517868B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 115
- 238000002425 crystallisation Methods 0.000 claims description 72
- 230000008025 crystallization Effects 0.000 claims description 72
- 230000008859 change Effects 0.000 claims description 10
- 238000009751 slip forming Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 description 29
- 229910052710 silicon Inorganic materials 0.000 description 23
- 239000010703 silicon Substances 0.000 description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 229910052799 carbon Inorganic materials 0.000 description 18
- 239000000843 powder Substances 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 241000255925 Diptera Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- -1 silicon alkoxide Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
本発明は、チョクラルスキー法（以下、「ＣＺ法」という）によって単結晶を引上げるためのシリカガラスルツボに関する。 The present invention relates to a silica glass crucible for pulling up a single crystal by the Czochralski method (hereinafter referred to as “CZ method”).
シリコン単結晶の育成に関し、ＣＺ法が広く用いられている。この方法は、シリカガラスルツボ内に収容されたシリコンの溶融液の表面に種結晶を接触させ、ルツボを回転させるとともに、この種結晶を反対方向に回転させながら上方へ引上げることによって、種結晶の下端に単結晶を形成していくものである。 The CZ method is widely used for the growth of silicon single crystals. In this method, the seed crystal is brought into contact with the surface of the silicon melt contained in the silica glass crucible, the crucible is rotated, and the seed crystal is pulled upward while rotating the seed crystal in the opposite direction. A single crystal is formed at the lower end of the substrate.
ところで、シリカガラスルツボは年々大型化しているが、シリカガラスルツボの大型化は、多結晶シリコンの装填量を増大させることができ、スループットが向上するというメリットがある。
しかしながら、その反面、溶融の長時間化、加熱用カーボンヒータの大出力化といった厳しい環境下で使用しなければならず、シリカガラスルツボへの悪影響も大きい。
By the way, although the silica glass crucible is increasing in size year by year, the increase in the size of the silica glass crucible has an advantage that the amount of polycrystalline silicon loaded can be increased and the throughput is improved.
However, on the other hand, it must be used in harsh environments such as a longer melting time and a larger output of the heating carbon heater, and the silica glass crucible is greatly adversely affected.
例えば、従来のシリカガラスルツボは、高温域での粘性値が低く、１４００℃以上の熱環境下では長時間その形状を維持し難かった。そのため、シリカガラスルツボの変形による溶融シリコンの融液面の変動、及び単結晶化率低下など、単結晶引上げ工程で問題が生じていた。
この問題を解決するため、特許文献１には、図５に示すように、ルツボ上端から直胴部、及び底部と底部コーナーとの間の曲率変化点を基準とする所定範囲までが結晶化促進剤添加シリカガラスからなる外層５１、天然原料シリカガラスからなる不透明中間層５２、天然原料シリカガラスまたは合成原料シリカガラスからなる透明内層５３からなる３層構造の石英ガラスルツボ５０について開示されている。
For example, a conventional silica glass crucible has a low viscosity value in a high temperature range, and it has been difficult to maintain its shape for a long time in a thermal environment of 1400 ° C. or higher. Therefore, problems have occurred in the single crystal pulling process, such as fluctuations in the melt surface of the molten silicon due to deformation of the silica glass crucible and reduction in the single crystallization rate.
In order to solve this problem, in Patent Document 1, as shown in FIG. 5, crystallization is promoted from the upper end of the crucible to the straight body portion and a predetermined range based on the curvature change point between the bottom portion and the bottom corner. A quartz glass crucible 50 having a three-layer structure comprising an outer layer 51 made of an agent-added silica glass, an opaque intermediate layer 52 made of a natural raw silica glass, and a transparent inner layer 53 made of a natural raw silica glass or a synthetic raw silica glass is disclosed.
このルツボ５０によれば、シリコン単結晶引上げ工程の加熱昇温過程において、外層５１は１２００℃以上で一定加熱すると、クリストバライトへと結晶化する。
クリストバライトの成長過程においては、粘性が向上し、また、結晶化することで高い耐久性を得ることができるため、前記のようにルツボの変形や破損といった課題を解決することができる。
In the growth process of cristobalite, the viscosity is improved, and high durability can be obtained by crystallization, so that the problems such as deformation and breakage of the crucible as described above can be solved.
しかしながら、前記特許文献１に開示の石英ガラスルツボ５０にあっては、単結晶引上装置においてヒータによる加熱が開始されると、外層５１のＡｌ添加量が均一であっても、ルツボの部位、すなわち、ルツボ上端、直胴部、底部により曝される温度や時間が異なるため、その結晶化が均一に進行せずに、十分に結晶化が進行している部位と、結晶化が不十分な部位が生じる場合があった。
このため、ルツボ５０においては、結晶化が不十分な部位では十分な耐変形性が得られないままシリコン単結晶の引上げが進行し、ルツボ５０が変形してしまう虞があった。
即ち、部位により結晶化が不均一になると、ルツボ５０の耐変形性が悪くなり、その結果、シリコン単結晶の引上げ途中においてルツボ５０が変形し、シリコン単結晶の引上げに悪影響を及ぼすという課題があった。
However, in the quartz glass crucible 50 disclosed in Patent Document 1, when heating by the heater is started in the single crystal pulling apparatus, even if the Al addition amount of the outer layer 51 is uniform, the crucible region, That is, since the temperature and time of exposure differ depending on the upper end of the crucible, the straight barrel part, and the bottom part, the crystallization does not proceed uniformly, and the crystallization is sufficiently progressed and the crystallization is insufficient. Sites may have occurred.
For this reason, in the crucible 50, there is a possibility that the crucible 50 may be deformed due to progress of pulling up of the silicon single crystal without obtaining sufficient deformation resistance at a site where crystallization is insufficient.
That is, if the crystallization is uneven depending on the part, the deformation resistance of the crucible 50 is deteriorated. As a result, the crucible 50 is deformed during the pulling of the silicon single crystal, and the pulling of the silicon single crystal is adversely affected. there were.
本発明は、前記したような事情の下になされたものであり、シリカガラスルツボにおいて、均一な結晶化をさせることで、ルツボの耐久性を向上させ、充分な単結晶化率を得ることのできるシリカガラスルツボを提供することを目的とする。 The present invention has been made under the circumstances as described above, and in a silica glass crucible, by making uniform crystallization, the durability of the crucible can be improved and a sufficient single crystallization rate can be obtained. An object of the present invention is to provide a silica glass crucible.
前記した課題を解決するために、本発明に係るシリカガラスルツボは、第一の曲率を有する底部と、前記底部の周りに形成され、第二の曲率を有する底部コーナーと、前記底部コーナーから上方に延びる直胴部を有するシリカガラスルツボにおいて、ルツボ上端から前記直胴部、及び前記底部と前記底部コーナーとの間の曲率変化点を基準とし前記第一の曲率の曲率中心と前記曲率変化点とを結ぶ直線上を０°として、該直線を前記曲率中心周りに±５°回転させた範囲までが、結晶化促進剤添加シリカガラスからなる外層と天然原料シリカガラスからなる不透明中間層と天然原料シリカガラスまたは合成原料シリカガラスからなる透明内層とで形成された３層構造からなり、前記底部が、前記不透明中間層から連続して形成された天然原料シリカガラスからなる不透明外層と天然原料シリカガラスまたは合成原料シリカガラスからなる透明内層とで形成された２層構造からなり、前記外層は境界部からルツボ上端側の結晶化促進剤添加濃度が、前記境界部から底部側の結晶化促進剤添加濃度よりも高いことに特徴を有する。 In order to solve the above-described problems, a silica glass crucible according to the present invention includes a bottom portion having a first curvature, a bottom corner formed around the bottom portion and having a second curvature, and upward from the bottom corner. In the silica glass crucible having a straight body extending to the center, the curvature center of the first curvature and the curvature change point on the basis of the curvature change point between the straight body from the upper end of the crucible and the bottom and the bottom corner. The range where the straight line connecting the two is 0 ° and the straight line is rotated ± 5 ° around the center of curvature is an outer layer made of crystallization accelerator-added silica glass, an opaque intermediate layer made of natural raw silica glass, and natural It consists of a three-layer structure formed with a transparent inner layer made of raw silica glass or synthetic raw silica glass, and the bottom is a natural raw material system formed continuously from the opaque intermediate layer. It consists of a two-layer structure formed of an opaque outer layer made of mosquito glass and a transparent inner layer made of natural raw silica glass or synthetic raw silica glass, and the outer layer has a concentration of crystallization accelerator added from the boundary to the upper end of the crucible. It is characterized by being higher than the concentration of the crystallization accelerator added from the bottom to the bottom.
尚、前記外層の結晶化促進剤添加濃度の異なる境界部は、前記直胴部の中点から±５０ｍｍであることが好ましい。
また、前記境界部よりルツボ上端側の結晶化促進剤添加濃度が１００ｐｐｍ以上１５０ｐｐｍ以下であり、前記境界部より底部側の結晶化促進剤添加濃度が３５ｐｐｍ以上１００ｐｐｍ以下の範囲で設定されていることが好ましい。
In addition, it is preferable that the boundary part where the crystallization promoter addition density | concentration of the said outer layer differs is +/- 50mm from the midpoint of the said straight body part.
Further, the crystallization accelerator addition concentration at the upper end side of the crucible from the boundary portion is 100 ppm or more and 150 ppm or less, and the crystallization accelerator addition concentration at the bottom portion side from the boundary portion is set in a range of 35 ppm or more and 100 ppm or less. Is preferred.
また、前記外層の厚さ寸法は、０．５〜５．０ｍｍの範囲で設定されていることが好ましい。 Moreover, it is preferable that the thickness dimension of the said outer layer is set in the range of 0.5-5.0 mm.
このように構成することにより、シリコン単結晶引上げの開始初期段階から引上げ開始までの間に、外層の結晶化（クリストバライト化）が均一に進行し、ルツボの耐熱変形性が向上する。
したがって、ルツボの耐熱変形性が確保され、シリコン単結晶の単結晶化率を向上することができる。
尚、前記結晶化促進剤としては、Ａｌ、Ｂａ、Ｃａ、Ｋが挙げられ、これらのいずれか、もしくは、このうちの複数の組合せから選択することができるが、Ａｌのみとすることが最も好ましい。
With such a configuration, the crystallization (cristobaliteization) of the outer layer proceeds uniformly from the initial stage of the pulling of the silicon single crystal to the start of pulling, and the heat distortion resistance of the crucible is improved.
Accordingly, the heat distortion resistance of the crucible is ensured, and the single crystallization rate of the silicon single crystal can be improved.
Examples of the crystallization accelerator include Al, Ba, Ca, and K, which can be selected from any of these or a combination of these, but most preferably only Al. .
本発明によれば、シリカガラスルツボにおいて、均一に結晶化することで、耐熱変形性を十分に確保すし、充分な単結晶化率を得ることのできるシリカガラスルツボを得ることができる。 According to the present invention, in a silica glass crucible, it is possible to obtain a silica glass crucible that can sufficiently ensure heat-resistant deformation and obtain a sufficient single crystallization rate by crystallization uniformly.
以下、本発明に係るシリカガラスルツボの実施の形態について図面に基づき説明する。図１は本発明に係るシリカガラスルツボ１の断面図である。図２は、図１のシリカガラスルツボの一部拡大断面図である。
このシリカガラスルツボ１は、例えば単結晶引上装置（図示せず）において用いられ、装置内でカーボンサセプタ（図示せず）によって抱持された状態で使用される。
即ち、単結晶引上装置では、シリカガラスルツボ１内に原料シリコンが溶融され、溶融液からシリコン単結晶が引上げられる。
Hereinafter, embodiments of a silica glass crucible according to the present invention will be described with reference to the drawings. FIG. 1 is a cross-sectional view of a silica glass crucible 1 according to the present invention. FIG. 2 is a partially enlarged cross-sectional view of the silica glass crucible of FIG.
This silica glass crucible 1 is used, for example, in a single crystal pulling apparatus (not shown), and is used while being held by a carbon susceptor (not shown) in the apparatus.
That is, in the single crystal pulling apparatus, the raw material silicon is melted in the silica glass crucible 1 and the silicon single crystal is pulled from the melt.
シリカガラスルツボ１は、例えば直径８１０ｍｍに形成され、図１に示すように、ルツボ上端６から直胴部７、及び底部９と底部コーナー８との間の曲率変化点を基準とする所定範囲までが、結晶化促進剤添加シリカガラスからなる外層２と、外層２に隣接する天然原料シリカガラス層からなる不透明中間層３と、この中間層３に隣接し、シリコン単結晶引上げ時に溶融シリコンと接する合成原料シリカガラス（または天然原料シリカガラス）からなる透明内層４とで形成された３層構造とした。
尚、ここで不透明とは、シリカガラス中に多数の気孔が内在し、見かけ上、白濁した状態を意味する。また、天然原料シリカガラスとは、水晶等の天然質原料を溶融して製造されるシリカガラスを意味し、合成原料シリカガラスとは、例えばシリコンアルコキシドの加水分解により合成された合成原料を溶融して製造されるシリカガラスを意味する。
The silica glass crucible 1 is formed to have a diameter of 810 mm, for example, and as shown in FIG. 1, up to a predetermined range based on the curvature change point between the crucible upper end 6 to the straight body portion 7 and the bottom portion 9 and the bottom corner 8. Is an outer layer 2 made of crystallization accelerator-added silica glass, an opaque intermediate layer 3 made of a natural raw silica glass layer adjacent to the outer layer 2, and is adjacent to the intermediate layer 3 and comes into contact with molten silicon when the silicon single crystal is pulled up. It was set as the three-layer structure formed with the transparent inner layer 4 which consists of synthetic raw material silica glass (or natural raw material silica glass).
The term “opaque” as used herein means a state in which a large number of pores are inherent in silica glass and apparently cloudy. The natural raw silica glass means silica glass produced by melting a natural raw material such as quartz, and the synthetic raw silica glass means a synthetic raw material synthesized by hydrolysis of silicon alkoxide, for example. Means silica glass produced by
前記外層２は、図示するようにルツボ外側全体に形成されるものではなく、ルツボ底部９は、不透明中間層３から連続して形成された天然原料シリカガラスからなる不透明外層５と、これに隣接する合成原料シリカガラス（または天然原料シリカガラス）からなる透明内層４とで形成された２層構造となされている。
また、前記外層２は、境界部Kよりルツボ上端側の結晶化促進剤添加濃度が、境界部Kより底部側の結晶化促進剤添加濃度よりも高く形成されている。
The outer layer 2 is not formed on the entire outer side of the crucible as shown in the figure, and the crucible bottom 9 is adjacent to the opaque outer layer 5 made of natural raw silica glass continuously formed from the opaque intermediate layer 3. And a transparent inner layer 4 made of synthetic raw silica glass (or natural raw silica glass).
Further, the outer layer 2 is formed such that the crystallization accelerator addition concentration on the crucible upper end side from the boundary portion K is higher than the crystallization accelerator addition concentration on the bottom side from the boundary portion K.
より詳細に説明すると、図２の断面図に示すように、ルツボ内において底部９は半径Ｒの曲率（第１の曲率）を有しており、底部コーナー８では半径ｒの曲率（第２の曲率）を有している。また、ルツボ直胴部７は鉛直方向に直線状に形成されている。
ここで、外層２はルツボ上端６から下方に向けて形成されると共に、外層２の下端は、底部９（曲率半径Ｒ）と底部コーナー８（曲率半径ｒ）との間の曲率変化点Ｐを基準とする所定範囲内まで形成されている。より具体的には、外層２の下端は、半径Ｒの曲率中心Ｃと、曲率変化点Ｐとを結ぶ直線Ｌ上を０°として、この直線Ｌを、曲率中心Ｃ周りに±５°回転させた範囲内まで形成されている。
More specifically, as shown in the cross-sectional view of FIG. 2, the bottom 9 has a radius R curvature (first curvature) in the crucible, and the bottom corner 8 has a radius r curvature (second curvature). Curvature). Moreover, the crucible straight body 7 is formed in a straight line in the vertical direction.
Here, the outer layer 2 is formed downward from the crucible upper end 6, and the lower end of the outer layer 2 has a curvature change point P between the bottom 9 (curvature radius R) and the bottom corner 8 (curvature radius r). It is formed up to a predetermined range as a reference. More specifically, the lower end of the outer layer 2 is rotated by ± 5 ° around the curvature center C, with 0 ° on the straight line L connecting the curvature center C of the radius R and the curvature change point P. It is formed to within the range.
これは、下方向（底部方向）を正方向とした場合、＋５°より大きい範囲まで外層２の下端を形成すると、結晶化（クリストバライト化）が急速に進行して所望の密着性が得られ難く、カーボンサセプタによるルツボの支持が不安定となり、シリコン単結晶化率が低下する傾向にあるためである。
一方、−５°より小さい範囲に外層２の下端を形成すると、ルツボ全体で外層２が占める割合が小さく、耐熱変形性が低くなる傾向があるためである。
This is because, when the lower direction (bottom direction) is a positive direction, if the lower end of the outer layer 2 is formed to a range larger than + 5 °, crystallization (cristobalite formation) proceeds rapidly, making it difficult to obtain desired adhesion. This is because the support of the crucible by the carbon susceptor becomes unstable and the silicon single crystallization rate tends to decrease.
On the other hand, if the lower end of the outer layer 2 is formed in a range smaller than −5 °, the proportion of the outer layer 2 in the entire crucible is small and the heat distortion resistance tends to be low.
尚、前記外層２は、前記直胴部７の中点から±５０ｍｍ以内（ルツボ上端側への距離をプラス、ルツボ底部側への距離をマイナスとする）にある境界部Kを境に、前記境界部Kよりルツボ上端６側の結晶化促進剤添加濃度は１００〜１５０ｐｐｍ（好ましくは１００〜１３０ｐｐｍ）に、前記境界部Kより底部９側の結晶化促進剤添加濃度が３５〜１００ｐｐｍ（好ましくは５０〜８０ｐｐｍ）に形成されている。
これは、外層２の境界部Kからルツボ上端６の領域は、外層２の境界部Kから底部コーナー８の領域に比べ曝される温度が低く、結晶化が進行しにくい環境にあるため、均一に結晶化を進行しやすくするために結晶化促進剤濃度を調整するものである。
The outer layer 2 has a boundary portion K within ± 50 mm from the midpoint of the straight body portion 7 (plus the distance to the crucible upper end side and minus the distance to the crucible bottom side), The crystallization accelerator addition concentration on the crucible upper end 6 side from the boundary K is 100 to 150 ppm (preferably 100 to 130 ppm), and the crystallization accelerator addition concentration on the bottom 9 side from the boundary K is 35 to 100 ppm (preferably 50 to 80 ppm).
This is because the region from the boundary K of the outer layer 2 to the upper end 6 of the crucible is exposed to a lower temperature than the region from the boundary K to the bottom corner 8 of the outer layer 2 and is in an environment where crystallization is difficult to proceed. In order to facilitate the progress of crystallization, the concentration of the crystallization accelerator is adjusted.
外層２の境界部Kの位置が、直胴部７の中点からルツボ上端６側に５０ｍｍより大きく、すなわち+５０ｍｍより大きいと、十分な耐久性が得られず、単結晶化率が低くなる傾向があり、直胴部７の中点からルツボ底部９側に５０ｍｍより大きく、すなわち−５０ｍｍより大きいと、十分な耐久性は得られたものの、ルツボとカーボンサセプタとの密着が良くなく、単結晶化率が低くなる虞があるためである。
外層２の境界部Kからルツボ上端６の領域では、結晶化促進剤濃度が１５０ｐｐｍより高いと結晶化が急速に進行し易く、ルツボとカーボンサセプタとの密着が安定する前に結晶化が完了する虞がある。１００ｐｐｍより低いと結晶化速度が遅くなり、所望の耐熱変形性が得られ難い。
一方、外層２の境界部Kから底部コーナー８の領域では、結晶化促進剤濃度が１００ｐｐｍより高いと結晶化が急速に進行し易く、ルツボとカーボンサセプタとの密着が安定する前に結晶化が完了する虞がある。３５ｐｐｍより低いと結晶化速度が遅くなり、所望の耐熱変形性が得られ難い。
If the position of the boundary portion K of the outer layer 2 is larger than 50 mm from the midpoint of the straight barrel portion 7 to the crucible upper end 6 side, that is, larger than +50 mm, sufficient durability cannot be obtained and the single crystallization rate is lowered. There is a tendency, and if it is larger than 50 mm from the midpoint of the straight barrel part 7 to the crucible bottom 9 side, that is, larger than −50 mm, sufficient durability is obtained, but the adhesion between the crucible and the carbon susceptor is not good. This is because the crystallization rate may be lowered.
In the region from the boundary K of the outer layer 2 to the upper end 6 of the crucible, when the concentration of the crystallization accelerator is higher than 150 ppm, crystallization is likely to proceed rapidly, and crystallization is completed before the adhesion between the crucible and the carbon susceptor is stabilized. There is a fear. When it is lower than 100 ppm, the crystallization speed is slow, and it is difficult to obtain desired heat distortion resistance.
On the other hand, in the region from the boundary K of the outer layer 2 to the bottom corner 8, if the concentration of the crystallization accelerator is higher than 100 ppm, the crystallization is likely to proceed rapidly, and the crystallization occurs before the adhesion between the crucible and the carbon susceptor is stabilized. There is a risk of completion. If it is lower than 35 ppm, the crystallization speed is slow, and it is difficult to obtain the desired heat distortion resistance.
また、図３に示すように、外層２は、ルツボ直胴部７における厚さ寸法ｅｔ１とルツボ底部コーナー８における厚さ寸法ｅｔ２とが共に０．５〜５ｍｍ（好ましくは１〜３ｍｍ）に形成される。これは、厚さが５ｍｍより大きいと、ルツボ壁部層間の熱膨張の差に起因する大きなストレスの発生により、クラック発生の虞があるためであり、０．５ｍｍより小さいと、耐熱変形性が低くなる傾向があるためである。 Further, as shown in FIG. 3, the outer layer 2 is formed such that the thickness dimension et1 at the crucible straight body portion 7 and the thickness dimension et2 at the crucible bottom corner 8 are both 0.5 to 5 mm (preferably 1 to 3 mm). Is done. This is because if the thickness is larger than 5 mm, cracks may occur due to the generation of large stress due to the difference in thermal expansion between the crucible wall layers. This is because it tends to be lower.
また、天然原料シリカガラスからなる不透明中間層３は、ルツボ直胴部７における厚さ寸法ｍｔ１が３ｍｍ以上となされ、ルツボ底部コーナー８における厚さ寸法ｍｔ２は６ｍｍ以上に形成される。
また、不透明中間層３から連続して形成されたルツボ底部９の不透明外層５における厚さ寸法ｍｔ３は６ｍｍ以上に形成される。
これは、３層部分での不透明中間層３の厚さが３ｍｍより小さいと、シリカガラス粉溶融中のアーク炎の不規則な流れによる不透明中間層３の結晶化促進剤化合物の飛散防止効果が減殺され易く、外層２の結晶化促進剤化合物が不透明中間層３を通過して透明内層４に混入し、透明内層４の結晶化促進剤濃度が大きくなる虞があるためである。
また、ルツボ底部コーナー８における不透明中間層３の厚さ寸法ｍｔ２及びルツボ底部９における不透明外層５の厚さ寸法ｍｔ３が６ｍｍより小さいと、充分な耐熱変形性が得られ難いためである。
The opaque intermediate layer 3 made of natural raw silica glass is formed such that the thickness dimension mt1 at the crucible straight body portion 7 is 3 mm or more, and the thickness dimension mt2 at the crucible bottom corner 8 is 6 mm or more.
Moreover, the thickness dimension mt3 of the opaque outer layer 5 of the crucible bottom 9 formed continuously from the opaque intermediate layer 3 is formed to be 6 mm or more.
This is because when the thickness of the opaque intermediate layer 3 in the three-layer portion is smaller than 3 mm, the crystallization accelerator compound of the opaque intermediate layer 3 is prevented from being scattered by the irregular flow of the arc flame during the melting of the silica glass powder. This is because the crystallization accelerator compound in the outer layer 2 passes through the opaque intermediate layer 3 and is mixed into the transparent inner layer 4, and the concentration of the crystallization accelerator in the transparent inner layer 4 may increase.
Further, if the thickness dimension mt2 of the opaque intermediate layer 3 at the crucible bottom corner 8 and the thickness dimension mt3 of the opaque outer layer 5 at the crucible bottom section 9 are smaller than 6 mm, sufficient heat distortion resistance is difficult to obtain.
また、透明内層４は、Ｎａ、Ｋ、Ａｌの金属不純物含有量が各々１ｐｐｍ以下の合成原料シリカガラス（または天然原料シリカガラス）を溶融して形成された実質的に気泡の存在しない透明層である。
透明内層４において、ルツボ直胴部７における厚さ寸法ｉｔ１と、ルツボ底部コーナー８における厚さ寸法ｉｔ２と、ルツボ底部９における厚さ寸法ｉｔ３とは共に、３ｍｍ以上の厚さに形成されている。
これは、透明内層４の厚さが３ｍｍより小さいとシリコン溶融と接する透明内層４の内表面の結晶化促進剤濃度を十分に低く、例えば１ｐｐｍ以下にすることができ難いためである。
The transparent inner layer 4 is a transparent layer substantially free of bubbles formed by melting synthetic raw silica glass (or natural raw silica glass) having a metal impurity content of 1 ppm or less for each of Na, K, and Al. is there.
In the transparent inner layer 4, the thickness dimension it1 in the crucible straight body part 7, the thickness dimension it2 in the crucible bottom corner 8, and the thickness dimension it3 in the crucible bottom part 9 are formed to a thickness of 3 mm or more. .
This is because if the thickness of the transparent inner layer 4 is smaller than 3 mm, the concentration of the crystallization accelerator on the inner surface of the transparent inner layer 4 in contact with the silicon melt cannot be made sufficiently low, for example, 1 ppm or less.
このような構造を有するシリカガラスルツボ１によれば、シリコン単結晶引上げの開始初期段階において、結晶化促進剤添加シリカガラスからなる外層２が存在しない所定範囲の底部９（不透明外層５）が軟化し、ルツボ１を支持するカーボンサセプタと密着する。
その後、引上げの開始からから完了までの間に亘り、高温加熱により所定範囲の底部コーナー８及び直胴部７等の外層２の結晶化（クリストバライト化）が均一に進行し、ルツボ１全体と、これを支持するカーボンサセプタとの密着安定性が向上する。また、結晶化により耐熱変形性が向上する。
したがって、ルツボ１の耐熱変形性を確保しつつ、カーボンサセプタによる支持の密着安定性が得られ、シリコン単結晶の単結晶化率を向上することができる。
According to the silica glass crucible 1 having such a structure, in the initial stage of starting the pulling of the silicon single crystal, the bottom 9 (the opaque outer layer 5) in a predetermined range in which the outer layer 2 made of silica glass containing crystallization accelerator does not exist is softened. Then, it is in close contact with the carbon susceptor that supports the crucible 1.
Thereafter, during the period from the start to the completion of the pulling, the crystallization (cristobalite) of the outer layer 2 such as the bottom corner 8 and the straight body 7 within a predetermined range is uniformly progressed by high temperature heating, and the entire crucible 1; Adhesion stability with the carbon susceptor supporting this is improved. Further, the heat distortion resistance is improved by crystallization.
Accordingly, the adhesion stability of the support by the carbon susceptor can be obtained while ensuring the heat distortion resistance of the crucible 1, and the single crystallization rate of the silicon single crystal can be improved.
次に、前記構造を有するシリカガラスルツボ１の製造方法について説明する。
図４に示すようなシリカガラスルツボ製造装置１０を用いてシリカガラスルツボ１を製造する。シリカガラスルツボ製造装置１０のルツボ成形用型１１は、例えば複数の貫通孔が穿設された金型、もしくは高純化処理した多孔質カーボン型などのガス透過性部材で構成された内側部材１２と、その外周に通気部１３を設けて、前記内側部材１２を保持する保持体１４とから構成されている。
Next, a method for producing the silica glass crucible 1 having the above structure will be described.
A silica glass crucible 1 is manufactured using a silica glass crucible manufacturing apparatus 10 as shown in FIG. The crucible molding die 11 of the silica glass crucible manufacturing apparatus 10 includes an inner member 12 made of a gas permeable member such as a die having a plurality of through holes or a highly purified porous carbon die. In addition, a ventilation portion 13 is provided on the outer periphery thereof, and a holding body 14 that holds the inner member 12 is configured.
また、保持体１４の下部には、図示しない回転手段と連結されている回転軸１５が固着されていて、ルツボ成形用型１１を回転可能に支持している。通気部１３は、保持体１４の下部に設けられた開口部１６を介して、回転軸１５の中央に設けられた排気路１７と連結されており、この排気路１７は、減圧機構１８と連結されている。
内側部材１２に対向する上部にはアーク放電用のアーク電極１９と、結晶化促進剤添加シリカガラス供給ノズル２０と、天然原料シリカガラス供給ノズル２１と、合成原料シリカガラス供給ノズル２２が設けられている。
A rotating shaft 15 connected to a rotating means (not shown) is fixed to the lower portion of the holding body 14, and supports the crucible forming die 11 rotatably. The ventilation portion 13 is connected to an exhaust passage 17 provided in the center of the rotary shaft 15 through an opening 16 provided in the lower portion of the holding body 14, and the exhaust passage 17 is connected to a decompression mechanism 18. Has been.
An arc electrode 19 for arc discharge, a crystallization accelerator-added silica glass supply nozzle 20, a natural raw silica glass supply nozzle 21, and a synthetic raw silica glass supply nozzle 22 are provided on the upper part facing the inner member 12. Yes.
外層２に用いられる結晶化促進剤添加シリカガラス粉は、次のようにして得られる。例えば結晶化促進剤がＡｌの場合、Ａｌ硝酸塩（Ａｌ（ＮＯ3）3）をシリカガラス粉のＡｌ濃度が１００〜１５０ｐｐｍもしくは３５〜１００ｐｐｍとなるような量だけ水に溶かして作られたＡｌ（ＮＯ3）3水溶液を、天然原料シリカガラス粉に添加、攪拌する。Ａｌ（ＮＯ3）3水溶液に浸されたシリカガラス粉は、脱水、酸分除去を目的として８００〜１１００℃で加熱処理される。 The crystallization accelerator-added silica glass powder used for the outer layer 2 is obtained as follows. For example, in the case where the crystallization accelerator is Al, Al (Al (NO 3 ) 3 ) prepared by dissolving Al nitrate (Al (NO 3 ) 3 ) in water in such an amount that the silica glass powder has an Al concentration of 100 to 150 ppm or 35 to 100 ppm. Add the NO 3 ) 3 aqueous solution to the natural raw silica glass powder and stir. The silica glass powder immersed in the Al (NO 3 ) 3 aqueous solution is heat-treated at 800 to 1100 ° C. for the purpose of dehydration and acid removal.
こうして得られたＡｌ添加シリカガラス粉を上述したシリカガラスルツボ製造装置１０を用いてシリカガラスルツボ１の製造を行う場合、図示しない回転駆動源を稼働させて回転軸１８を矢印の方向に回転させ、これによりルツボ成形用型１１を高速で回転させる。
次いで、ルツボ成形用型１１内の底部から直胴部７の中点付近に結晶化促進剤添加シリカガラス供給ノズル２０から上述のようにして得られた３５〜１００ｐｐｍＡｌ添加シリカガラス粉を供給し、直胴部７の中点付近からルツボ上端６までに結晶化促進剤添加シリカガラス供給ノズル２０から上述のようにして得られた１００〜１５０ｐｐｍＡｌ添加シリカガラス粉を供給する。供給されたＡｌ添加シリカガラス粉は、遠心力によって内側部材１２の内面側に押圧され外層２として形成される。
ここで、外層２は、図２を用いて説明したように下端の位置が決められ、底部が除去される。
When manufacturing the silica glass crucible 1 using the silica glass crucible manufacturing apparatus 10 described above for the Al-added silica glass powder thus obtained, a rotary drive source (not shown) is operated to rotate the rotary shaft 18 in the direction of the arrow. Thus, the crucible molding die 11 is rotated at a high speed.
Next, 35 to 100 ppm Al-added silica glass powder obtained as described above from the crystallization accelerator-added silica glass supply nozzle 20 is supplied from the bottom of the crucible molding die 11 to the middle point of the straight barrel portion 7. 100 to 150 ppm Al-added silica glass powder obtained as described above is supplied from the crystallization accelerator-added silica glass supply nozzle 20 to the vicinity of the midpoint of the straight body portion 7 to the upper end 6 of the crucible. The supplied Al-added silica glass powder is pressed to the inner surface side of the inner member 12 by a centrifugal force to be formed as the outer layer 2.
Here, the outer layer 2 is positioned at the lower end as described with reference to FIG. 2, and the bottom is removed.
次いで、Ａｌ添加シリカガラス層からなる外層２の内面側における厚さが３ｍｍ以上、底部コーナー及び底部における厚さが６ｍｍ以上の不透明中間層３及び不透明外層５が形成されるように、天然原料シリカガラス粉を天然原料シリカガラス供給ノズル２１から供給する。供給された天然原料シリカガラス粉は、遠心力によって外層２の内面側及び内側部材１２の底部に押圧されて、不透明中間層３及び不透明外層５の成形体として成形される。 Next, the natural raw material silica is formed so that the opaque intermediate layer 3 and the opaque outer layer 5 having a thickness of 3 mm or more on the inner surface side of the outer layer 2 made of an Al-added silica glass layer and a thickness of 6 mm or more at the bottom corner and the bottom are formed. Glass powder is supplied from the natural raw silica glass supply nozzle 21. The supplied natural raw silica glass powder is pressed against the inner surface side of the outer layer 2 and the bottom of the inner member 12 by centrifugal force, and is molded as a molded body of the opaque intermediate layer 3 and the opaque outer layer 5.
次に、不透明中間層３及び不透明外層５の内面側に３ｍｍ以上の厚さを有する透明層が形成されるように、Ｎａ、Ｋ、Ａｌの金属不純物含有量が各々１ｐｐｍ以下の合成原料シリカガラス粉（または天然原料シリカガラス粉）を合成原料シリカガラス供給ノズル２２から供給する。
供給された合成原料シリカガラス粉は、遠心力によって不透明中間層３及び不透明外層５の内面側に押圧されて、透明内層４の成形体として成形される。
Next, synthetic raw silica glass having a metal impurity content of Na, K, Al of 1 ppm or less so that a transparent layer having a thickness of 3 mm or more is formed on the inner surface side of the opaque intermediate layer 3 and the opaque outer layer 5. Powder (or natural raw silica glass powder) is supplied from the synthetic raw silica glass supply nozzle 22.
The supplied synthetic raw silica glass powder is pressed against the inner surfaces of the opaque intermediate layer 3 and the opaque outer layer 5 by centrifugal force, and is formed as a molded body of the transparent inner layer 4.
このようにして直胴部７の中点付近を境にＡｌ濃度の減少勾配がある外層２、不透明中間層３、不透明外層５および透明内層４のルツボ成形体が得られる。
さらに、減圧機構１８の作動により内側部材１２内を減圧し、アーク電極１９に通電してルツボ成形体の内側から加熱し、ルツボ成形体の透明内層４、不透明中間層３、不透明外層５および外層２を溶融して、シリカガラスルツボ１を製造する。
In this way, a crucible molded body of the outer layer 2, the opaque intermediate layer 3, the opaque outer layer 5 and the transparent inner layer 4 having an Al concentration decreasing gradient from the middle point of the straight barrel portion 7 as a boundary is obtained.
Further, the inside of the inner member 12 is depressurized by the operation of the decompression mechanism 18, the arc electrode 19 is energized and heated from the inside of the crucible molded body, and the transparent inner layer 4, the opaque intermediate layer 3, the opaque outer layer 5 and the outer layer of the crucible molded body. 2 is melted to produce a silica glass crucible 1.
以上のように本実施の形態によれば、結晶化促進剤添加シリカガラス層からなる外層２が、ルツボ上端から下方に向けて形成されると共に、該外層２の下端は、底部の曲率変化点を基準とする所定範囲まで形成される。さらに、外層２の厚さ寸法は０．５〜５ｍｍとされ、直胴部７の中点から±５０ｍｍ以内にある境界部Kを境に、前記境界部Kよりルツボ上端６側の結晶化促進剤添加濃度は１００〜１５０ｐｐｍ、前記境界部Kより底部９側の結晶化促進剤添加濃度が３５〜１００ｐｐｍとなされる。 As described above, according to the present embodiment, the outer layer 2 made of the crystallization accelerator-added silica glass layer is formed downward from the upper end of the crucible, and the lower end of the outer layer 2 has a curvature change point at the bottom. Is formed up to a predetermined range with reference to. Further, the outer layer 2 has a thickness of 0.5 to 5 mm, and promotes crystallization on the crucible upper end 6 side from the boundary K, with the boundary K within ± 50 mm from the midpoint of the straight body 7. The additive addition concentration is 100 to 150 ppm, and the crystallization accelerator addition concentration on the bottom 9 side from the boundary K is 35 to 100 ppm.
これにより、シリコン単結晶引上げの開始初期段階において、結晶化促進剤添加シリカガラスからなる外層２が存在しない所定範囲の底部（不透明外層５）が軟化し、ルツボを支持するカーボンサセプタと密着する。
その後、引上げの開始からから完了までの間に亘り、高温加熱により所定範囲の底部コーナー及び直胴部等の外層２の結晶化（クリストバライト化）が均一に進行し、ルツボ全体と、これを支持するカーボンサセプタとの密着安定性が向上する。また、結晶化により耐熱変形性が向上する。
したがって、ルツボの耐熱変形性を確保しつつ、カーボンサセプタによる支持の密着安定性が得られ、シリコン単結晶の単結晶化率を向上することができる。
Thereby, in the initial stage of starting the pulling of the silicon single crystal, the bottom portion (the opaque outer layer 5) in a predetermined range where the outer layer 2 made of the crystallization accelerator-added silica glass does not exist is softened and is in close contact with the carbon susceptor supporting the crucible.
After that, from the start to the completion of pulling, the crystallization (cristobalite) of the outer layer 2 such as the bottom corner and the straight body in a predetermined range is uniformly progressed by high temperature heating, supporting the whole crucible and this. The adhesion stability with the carbon susceptor is improved. Further, the heat distortion resistance is improved by crystallization.
Accordingly, the adhesion stability of the support by the carbon susceptor can be obtained while ensuring the heat distortion resistance of the crucible, and the single crystallization rate of the silicon single crystal can be improved.
続いて、本発明に係るシリカガラスルツボについて、実施例に基づきさらに説明する。本実施例では、前記実施の形態に示した構成を含むシリカガラスルツボの製造を行い、熱処理を行うことにより、その効果を検証した。
この実験では、図６に示すように、製造したシリカガラスルツボ１００をカーボンサセプタ１０１内に配置し、単結晶引上げ実験を行った。
尚、このシリカガラスルツボ１００の外径は６１０ｍｍ、高さは４００ｍｍ、全体の平均厚さ寸法は１２ｍｍとした。また、シリカガラスルツボ１００を支持するカーボンサセプタ１０１の内周径は６１５ｍｍとした。
Next, the silica glass crucible according to the present invention will be further described based on examples. In this example, a silica glass crucible including the structure described in the above embodiment was manufactured, and the effect was verified by performing heat treatment.
In this experiment, as shown in FIG. 6, the manufactured silica glass crucible 100 was placed in a carbon susceptor 101, and a single crystal pulling experiment was performed.
The silica glass crucible 100 had an outer diameter of 610 mm, a height of 400 mm, and an overall average thickness of 12 mm. The inner diameter of the carbon susceptor 101 that supports the silica glass crucible 100 was 615 mm.
単結晶引上げ工程では、カーボンサセプタ１０１内にシリカガラスルツボ１００を、その上端がカーボンサセプタ１０１の上端よりも高さ寸法Ｈ１＝４０ｍｍだけ突出するように収容し、このルツボ１００内にポリシリコンを約１５０ｋｇチャージ後、８インチシリコン単結晶の引上げ試験を行った。製造されたシリコン単結晶については、通常の評価法により単結晶化率の測定を行った。尚、符号Ｈ１で示す単結晶引上げ前におけるルツボ上端の突出高さ寸法は、単結晶引上げ後においては符号Ｈ２で示すものとする。 In the single crystal pulling step, the silica glass crucible 100 is accommodated in the carbon susceptor 101 so that the upper end protrudes by a height dimension H1 = 40 mm from the upper end of the carbon susceptor 101, and polysilicon is approximately contained in the crucible 100. After charging 150 kg, a pulling test of an 8-inch silicon single crystal was performed. About the manufactured silicon single crystal, the single crystallization rate was measured by the normal evaluation method. In addition, the protrusion height dimension of the crucible upper end before the single crystal pulling shown by the code | symbol H1 shall show with the code | symbol H2 after the single crystal pulling.
製造したシリカガラスルツボ１００の実施例及び比較例ごとの条件及び実験結果を表１に示す。
尚、表１において、耐熱変形性は、沈み込み変形割合を式１により求め（図６参照）、その割合が６０％を○、６０〜８０％を△、８０％超を×とした。また、単結晶化率は、９６％超を○、９０〜９６％を△、９０％未満を×とした。
Table 1 shows conditions and experimental results for each of the manufactured silica glass crucible 100 and comparative examples.
In Table 1, the heat distortion resistance was determined by calculating the subsidence deformation ratio using Equation 1 (see FIG. 6), and the ratio was 60% for ◯, 60-80% for Δ, and over 80% for x. Further, the single crystallization rate was over 96% as ◯, 90 to 96% as Δ, and less than 90% as x.
この実験の結果、表１に示すように、実施例４〜７については、耐熱変形性の点で一部
最良とはいえないものの、単結晶化率において、比較例１、２よりも向上が認められた。
また、実施例１〜３については、耐熱変形性及び単結晶化率の点で共に比較例１、２よ
りも格段に向上が認められた。
したがって、３層構造とする境界位置は、図２に示したように曲率変化点から±５°の
範囲であるのが好ましく、結晶化促進剤添加外層の結晶化促進剤濃度は３５〜１００ｐｐ
ｍの範囲で設定されるのが好ましいと確認された。
As a result of this experiment, as shown in Table 1, although Examples 4 to 7 are not the best in terms of heat distortion resistance, the single crystallization ratio is improved over Comparative Examples 1 and 2. Admitted.
Moreover, about Examples 1-3, the marked improvement was recognized rather than the comparative examples 1 and 2 in the point of heat-resistant deformation property and a single crystallization rate.
Therefore, the boundary position of the three-layer structure is preferably within a range of ± 5 ° from the curvature change point as shown in FIG. 2, and the concentration of the crystallization accelerator in the outer layer to which the crystallization accelerator is added is 35 to 100 pp.
It was confirmed that setting in the range of m was preferable.
以上の実施例の実験結果から、本発明に係るシリカガラスルツボによれば、ルツボの耐熱変形性を確保しつつ、カーボンサセプタによる支持の密着安定性が得られ、シリコン単結晶の単結晶化率を向上することができることを確認した。 From the experimental results of the above examples, according to the silica glass crucible according to the present invention, the adhesion stability of the support by the carbon susceptor can be obtained while ensuring the heat distortion resistance of the crucible, and the single crystallization rate of the silicon single crystal Confirmed that can be improved.
１ シリカガラスルツボ
２ 外層
３ 不透明中間層
４ 透明内層
５ 不透明外層
６ ルツボ上端
７ 直胴部
８ 底部コーナー
９ 底部
１０ シリカガラスルツボ製造装置
Ｋ 境界部
DESCRIPTION OF SYMBOLS 1 Silica glass crucible 2 Outer layer 3 Opaque intermediate layer 4 Transparent inner layer 5 Opaque outer layer 6 Upper end of crucible 7 Straight trunk part 8 Bottom corner 9 Bottom part 10 Silica glass crucible manufacturing device K boundary part
Claims (3)
ルツボ上端から前記直胴部、及び前記底部と前記底部コーナーとの間の曲率変化点を基準とし前記第一の曲率の曲率中心と前記曲率変化点とを結ぶ直線上を０°として、該直線を前記曲率中心周りに±５°回転させた範囲までが、結晶化促進剤添加シリカガラスからなる外層と天然原料シリカガラスからなる不透明中間層と天然原料シリカガラスまたは合成原料シリカガラスからなる透明内層とで形成された３層構造からなり、
前記底部が、前記不透明中間層から連続して形成された天然原料シリカガラスからなる不透明外層と天然原料シリカガラスまたは合成原料シリカガラスからなる透明内層とで形成された２層構造からなり、
前記外層は境界部からルツボ上端側の結晶化促進剤添加濃度が、前記境界部から底部側の結晶化促進剤添加濃度よりも高いことを特徴とするシリカガラスルツボ。 In a silica glass crucible having a bottom portion having a first curvature, a bottom corner formed around the bottom portion and having a second curvature, and a straight body portion extending upward from the bottom corner,
A straight line connecting the curvature center of the first curvature and the curvature change point with respect to the straight barrel portion from the upper end of the crucible and the curvature change point between the bottom portion and the bottom corner is defined as 0 °. Up to a range of ± 5 ° rotated around the center of curvature, an outer layer made of crystallization accelerator-added silica glass, an opaque intermediate layer made of natural raw silica glass, and a transparent inner layer made of natural raw silica glass or synthetic raw silica glass And a three-layer structure formed by
The bottom portion has a two-layer structure formed of an opaque outer layer made of a natural raw silica glass continuously formed from the opaque intermediate layer and a transparent inner layer made of a natural raw silica glass or a synthetic raw silica glass,
The silica glass crucible characterized in that the outer layer has a crystallization accelerator addition concentration from the boundary portion to the upper end side of the crucible and higher than the crystallization accelerator addition concentration from the boundary portion to the bottom portion side.
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