JP2008260649A - Method of solidification of residual melt in crucible - Google Patents

Method of solidification of residual melt in crucible Download PDF

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JP2008260649A
JP2008260649A JP2007103482A JP2007103482A JP2008260649A JP 2008260649 A JP2008260649 A JP 2008260649A JP 2007103482 A JP2007103482 A JP 2007103482A JP 2007103482 A JP2007103482 A JP 2007103482A JP 2008260649 A JP2008260649 A JP 2008260649A
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heater
crucible
melt
residual melt
residual
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JP4770776B2 (en
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Yuichi Miyahara
祐一 宮原
Tetsuhiro Oda
哲宏 小田
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Shin Etsu Handotai Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method by which cracking of a quartz crucible and leakage of a residual melt are prevented and the residual melt in the crucible is solidified more safely in Czochralski method. <P>SOLUTION: The invention relates to a method to solidify a melt (residual melt) left in a quartz crucible 45 after the melt in the quartz crucible 45 is heated with a heater 47 and a crystal is pulled. The method comprises a step of keeping the height of the central position 48 of the heat generation of the heater 47 within 20 mm from the surface 44 of the melt after the pulling of the crystal is completed by relatively moving up and down the crucible 45 and the heater 47 and a step of cutting off the supply of electricity. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、チョクラルスキー法により石英ルツボ内の融液をヒーターで加熱しつつ結晶を引上げた後の石英ルツボ内に残留した融液（残融液）の固化方法に関するものである。   The present invention relates to a method for solidifying a melt (residual melt) remaining in a quartz crucible after pulling up a crystal while heating the melt in the quartz crucible with a heater by the Czochralski method.

一般に、チョクラルスキー法（Ｃｚｏｃｈｒａｌｓｋｉ Ｍｅｔｈｏｄ、以下ＣＺ法と略称する）によりシリコン単結晶を製造する際には、例えば図３に示すような単結晶製造装置２０を用いて単結晶の製造が行われる。
この単結晶製造装置２０は、例えばシリコンのような原料多結晶を収容するルツボやヒーター及び熱を遮断するための断熱部材等を格納するメインチャンバ１を有している。このメインチャンバ１の上部には育成した単結晶３を収容し、取り出すための引上げチャンバ２が連接されており、この上部に単結晶３をワイヤー１４で引上げる引上げ機構（不図示）が設けられている。 In general, when a silicon single crystal is manufactured by the Czochralski method (hereinafter abbreviated as CZ method), a single crystal is manufactured using, for example, a single crystal manufacturing apparatus 20 as shown in FIG. .
This single crystal manufacturing apparatus 20 has a main chamber 1 for storing a crucible for containing a raw material polycrystal such as silicon, a heater, a heat insulating member for cutting off heat, and the like. A pulling chamber 2 for accommodating and taking out the grown single crystal 3 is connected to the upper portion of the main chamber 1, and a pulling mechanism (not shown) for pulling the single crystal 3 with a wire 14 is provided on the upper portion. ing.

メインチャンバ１内には、溶融された原料融液４を収容する石英ルツボ５とその石英ルツボ５を支持する黒鉛ルツボ６が設けられ、これらのルツボ５、６は駆動機構（不図示）によって回転昇降自在に支持軸１３で支持されている。このルツボ５、６の駆動機構は、単結晶３の引上げに伴う原料融液４の液面低下を補償すべく、ルツボ５、６を液面低下分だけ上昇させるようにしている。   A quartz crucible 5 for containing the melted raw material melt 4 and a graphite crucible 6 for supporting the quartz crucible 5 are provided in the main chamber 1, and these crucibles 5 and 6 are rotated by a drive mechanism (not shown). It is supported by a support shaft 13 so as to be movable up and down. The driving mechanism of the crucibles 5 and 6 raises the crucibles 5 and 6 by the amount corresponding to the liquid level drop in order to compensate for the liquid level drop of the raw material melt 4 accompanying the pulling of the single crystal 3.

そして、ルツボ５、６を囲繞するように、円筒形状のヒーター７が配置されている。このヒーター７の外側には、ヒーター７からの熱がメインチャンバ１に直接輻射されるのを防止するために、断熱材８がその周囲を取り囲むように設けられている。   A cylindrical heater 7 is arranged so as to surround the crucibles 5 and 6. In order to prevent heat from the heater 7 from being directly radiated to the main chamber 1, a heat insulating material 8 is provided outside the heater 7 so as to surround the periphery thereof.

このような単結晶製造装置２０を用いてシリコン単結晶を引上げる。その後、次のシリコン単結晶引上に備え、チャンバー内のクリーニングおよび原材料の再充填が必要になる。これらの作業を行う為、シリコン単結晶の引上が終了した後に切電を行う。この時、ルツボ内に残ったシリコン融液が冷却され凝固するが、シリコン融液の表面と底部では温度差が生じ表面の方が速く凝固する。その為、残シリコン融液の量が多い場合は、シリコン融液表面と底部の凝固速度差が大きくなり、シリコン融液底部が凝固する前に表面の凝固および膨張により石英ルツボが割れてしまう。その結果、シリコン融液底部のまだ未凝固のものが黒鉛ルツボに漏れだしてしまう。この黒鉛ルツボに漏れたシリコン融液が黒鉛と反応することで、黒鉛ルツボが劣化し寿命を縮めてしまう。また、漏れだしたシリコン融液の量が多かった場合は、黒鉛ルツボからもシリコン融液が漏れ出してしまい、他の黒鉛製の炉内部品の寿命を縮めることがある。また、漏れだしたシリコン融液がチャンバーを溶解し、チャンバーに損傷を生じる可能性がある。   A silicon single crystal is pulled up using such a single crystal manufacturing apparatus 20. After that, it is necessary to clean the chamber and refill the raw materials in preparation for the next silicon single crystal pulling. In order to perform these operations, the power is turned off after the pulling of the silicon single crystal is completed. At this time, the silicon melt remaining in the crucible is cooled and solidified, but a temperature difference occurs between the surface and the bottom of the silicon melt, and the surface solidifies faster. Therefore, when the amount of residual silicon melt is large, the difference in solidification rate between the surface of the silicon melt and the bottom becomes large, and the quartz crucible is broken by the solidification and expansion of the surface before the bottom of the silicon melt is solidified. As a result, the non-solidified silicon melt bottom leaks into the graphite crucible. When the silicon melt leaked into the graphite crucible reacts with graphite, the graphite crucible deteriorates and the life is shortened. In addition, when the amount of leaked silicon melt is large, the silicon melt leaks from the graphite crucible, which may shorten the life of other graphite furnace components. In addition, the leaked silicon melt may dissolve the chamber and cause damage to the chamber.

このような問題に対して、特許文献１にはルツボ内の残融液を下部から上部に向けて固化させることが開示されている。これは残融液がルツボ内で固化する際に、表面から固化を始めることにより、一体型ルツボが使用できないという問題を解決するためになされたものである。   For such a problem, Patent Document 1 discloses that the residual melt in the crucible is solidified from the lower part toward the upper part. This is made to solve the problem that the integrated crucible cannot be used by starting solidification from the surface when the residual melt is solidified in the crucible.

特に、特許文献１の請求項５には、固化工程において、ヒーターを動作させて、残融液の表面を加熱することが記載されている。
しかし、この方法では結晶引上げ終了後に切電してしまうと残融液表面が先に固化してしまうので、ルツボ内の残融液を下部から上部に向けて固化させるためには、結晶成長終了後もヒーターを切電せずに残融液表面を加熱する必要があるため、残融液の固化工程の完了に長時間を要していた。 In particular, claim 5 of Patent Document 1 describes that in the solidification step, a heater is operated to heat the surface of the residual melt.
However, in this method, if the power is turned off after the pulling of the crystal, the residual melt surface solidifies first, so in order to solidify the residual melt in the crucible from the bottom to the top, the crystal growth is completed. Since it was necessary to heat the surface of the residual melt without turning off the heater, it took a long time to complete the solidification step of the residual melt.

また、特許文献１の請求項２には、固化工程において、ルツボの底部がヒーターの下限位置よりも下方に位置するように、ルツボを下方移動することが記載されている。   Further, claim 2 of Patent Document 1 describes that in the solidification step, the crucible is moved downward so that the bottom of the crucible is located below the lower limit position of the heater.

しかし、この方法を用いても残融液が完全に固化する前に石英ルツボが割れてしまうことがあった。したがって、残融液が固化する前の石英ルツボ割れを防止することができ、より安全にルツボ内残融液を固化できる方法が求められていた。   However, even if this method is used, the quartz crucible may break before the residual melt is completely solidified. Therefore, there has been a demand for a method that can prevent the cracking of the quartz crucible before the residual melt is solidified and can solidify the residual melt in the crucible more safely.

特開２０００−１６８９３号公報JP 2000-16893 A

本発明は、このような問題点に鑑みてなされたもので、本発明の目的は、チョクラルスキー法により石英ルツボ内の融液をヒーターで加熱しつつ結晶を引上げた後の石英ルツボ内に残留した融液（残融液）の固化方法であって、石英ルツボ割れを防止することができ、残融液の漏れを防ぐことができ、より安全にルツボ内残融液を固化できる方法を提供することである。   The present invention has been made in view of such problems, and an object of the present invention is to place the crystal in the quartz crucible after pulling up the crystal while heating the melt in the quartz crucible with a heater by the Czochralski method. A method for solidifying a residual melt (residual melt), which can prevent cracking of a quartz crucible, prevent leakage of the residual melt, and can solidify the residual melt in the crucible more safely. Is to provide.

本発明は、上記課題を解決するためになされたもので、チョクラルスキー法により石英ルツボ内の融液をヒーターで加熱しつつ結晶を引上げた後の石英ルツボ内に残留した融液（残融液）の固化方法であって、結晶引上げ終了後、前記ルツボと前記ヒーターを相対的に昇降させて、該ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程と、該ヒーターへの供給電力を停止する工程を含むことを特徴とする残融液の固化方法を提供する（請求項１）。   The present invention has been made to solve the above-described problems. The melt (residual melt) remaining in the quartz crucible after the crystal is pulled up while heating the melt in the quartz crucible with a heater by the Czochralski method. Liquid), the step of raising and lowering the crucible and the heater relative to each other after the completion of pulling the crystal so that the height of the heating center position of the heater is within 20 mm from the surface of the residual melt, A method for solidifying a residual melt characterized in that it includes a step of stopping power supply to a heater (claim 1).

このように、結晶引上げ終了後、前記ルツボと前記ヒーターを相対的に昇降させて、該ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程と、該ヒーターへの供給電力を停止する工程を含む残融液の固化方法を行うことで、残融液の表面を高温とし、残融液の表面と底部の温度差を小さくし、残融液表面と底部の凝固速度差を小さくすることができる。これによって、残融液の表面が先に凝固して膨張し石英ルツボが割れ、残融液が漏れることを防止できる。   Thus, after the crystal pulling is completed, the crucible and the heater are moved up and down relatively so that the height of the heat generation center position of the heater is within 20 mm from the residual melt surface, and the power supplied to the heater By performing the residual melt solidification method including the step of stopping the process, the surface of the residual melt is heated to a high temperature, the temperature difference between the surface and the bottom of the residual melt is reduced, and the solidification rate difference between the surface and the bottom of the residual melt is reduced. Can be reduced. As a result, it is possible to prevent the surface of the residual melt from first solidifying and expanding, cracking the quartz crucible, and leaking the residual melt.

この場合、前記石英ルツボを、２つ以上に分割された部分から構成された黒鉛ルツボで保護することができる（請求項２）。   In this case, the quartz crucible can be protected by a graphite crucible composed of two or more parts (claim 2).

このように、前記石英ルツボを、２つ以上に分割された部分から構成された黒鉛ルツボで保護すれば、石英ルツボおよび黒鉛ルツボの割れをより抑制でき、また黒鉛ルツボの一部が破損しても破損した部分を交換すればよいので、一体型の黒鉛ルツボより経済的である。   Thus, if the quartz crucible is protected with a graphite crucible composed of two or more parts, the cracking of the quartz crucible and the graphite crucible can be further suppressed, and a part of the graphite crucible is damaged. This is more economical than an integrated graphite crucible because the damaged part only needs to be replaced.

また、前記ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程において、前記ヒーターの発熱中心位置の高さを残融液表面と一致させることが好ましい（請求項３）。   Further, in the step of setting the height of the heat generation center position of the heater to within 20 mm from the residual melt surface, it is preferable that the height of the heat generation center position of the heater coincides with the residual melt surface.

このように前記ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程において、前記ヒーターの発熱中心位置の高さを残融液表面と一致させれば、残融液の表面と底部の温度差をより小さくし、石英ルツボが割れることをより確実に防止できるため好ましい。   Thus, in the step of setting the height of the heat generation center position of the heater to within 20 mm from the surface of the residual melt, if the height of the heat generation center position of the heater coincides with the surface of the residual melt, the surface of the residual melt This is preferable because the temperature difference between the bottom and the bottom can be made smaller and the quartz crucible can be more reliably prevented from cracking.

また、前記石英ルツボの下方に、結晶引上げ時に該ルツボ下部を保温するための断熱部材が設けられ、該断熱部材が前記ヒーターと同期して昇降することが好ましい（請求項４）。   Further, it is preferable that a heat insulating member is provided below the quartz crucible to keep the lower portion of the crucible warm when the crystal is pulled, and the heat insulating member moves up and down in synchronization with the heater.

このように前記石英ルツボの下方に、結晶引上げ時に該ルツボ下部を保温するための断熱部材が設けられ、該断熱部材が前記ヒーターと同期して昇降すれば、結晶引上げ中はヒーターの発する熱を効率的に利用できるため好ましいが、このような炉内構造を有する装置を用いる場合に、より固化時に石英ルツボの割れが発生しやすいので、本発明が有効である。   As described above, a heat insulating member is provided below the quartz crucible to keep the lower portion of the crucible warm when the crystal is pulled. If the heat insulating member moves up and down in synchronization with the heater, the heat generated by the heater is raised during the pulling of the crystal. Although it is preferable because it can be efficiently used, when using an apparatus having such an in-furnace structure, the quartz crucible is more easily cracked during solidification, and thus the present invention is effective.

前記ヒーターへの供給電力を停止する工程は、残融液の表面が固化する前に行うことができる（請求項５）。
前記ヒーターへの供給電力を停止する工程は、残融液の表面が固化する前に行えばよく、前記ヒーターへの供給電力を最終的に停止する前に、たとえば前記ヒーターへの供給電力を徐々に低下させてもよい。 The step of stopping the power supplied to the heater can be performed before the surface of the residual melt is solidified (Claim 5).
The step of stopping the supply power to the heater may be performed before the surface of the residual melt is solidified. Before the supply power to the heater is finally stopped, for example, the supply power to the heater is gradually reduced. It may be lowered.

以上説明したように、本発明の残融液の固化方法によれば、結晶引上げ終了後、前記ルツボと前記ヒーターを相対的に昇降させて、該ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程を行うことで、残融液の表面を高温とし、残融液の表面と底部の温度差を小さくし、残融液表面と底部の凝固速度差を小さくすることができる。これによって、残融液の表面が先に凝固して膨張し石英ルツボが割れることを防止できる。すなわち残融液の漏れを防ぐことができ、より安全にルツボ内残融液を固化することができる。   As described above, according to the solidification method of the residual melt of the present invention, after the completion of the pulling of the crystal, the crucible and the heater are relatively moved up and down, and the height of the heat generation center position of the heater is set to the residual melt. By performing the process within 20 mm from the surface, the surface of the residual melt can be made high temperature, the temperature difference between the surface of the residual melt and the bottom can be reduced, and the difference in solidification rate between the surface of the residual melt and the bottom can be reduced. it can. As a result, it is possible to prevent the surface of the residual melt from first solidifying and expanding to crack the quartz crucible. That is, leakage of the residual melt can be prevented, and the residual melt in the crucible can be solidified more safely.

以下、本発明についてより詳細に説明するが、本発明はこれらに限定されるものではない。   Hereinafter, although this invention is demonstrated in detail, this invention is not limited to these.

結晶引上げ終了後、石英ルツボ内に残留した融液（残融液）の固化工程において、ルツボの底部がヒーターの下端位置よりも下方に位置するように、ルツボを下方移動したとしても、石英ルツボが割れてしまうことがあった。そこで、本発明者らは、石英ルツボ割れおよび残融液の漏れを防止することができ、より安全にルツボ内残融液を固化できる方法について鋭意検討を行い、本発明を完成した。   Even if the crucible is moved downward so that the bottom of the crucible is positioned below the lower end position of the heater in the solidification process of the melt remaining in the quartz crucible (residual melt) after the completion of the crystal pulling, the quartz crucible Sometimes broke. Accordingly, the present inventors have conducted extensive studies on a method capable of preventing the quartz crucible cracking and leakage of the residual melt and solidifying the residual melt in the crucible more safely, and completed the present invention.

すなわち、本発明は、チョクラルスキー法により石英ルツボ内の融液をヒーターで加熱しつつ結晶を引上げた後の石英ルツボ内に残留した融液（残融液）の固化方法であって、結晶引上げ終了後、前記ルツボと前記ヒーターを相対的に昇降させて、該ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程と、該ヒーターへの供給電力を停止する工程を含むことを特徴とする残融液の固化方法を提供する。   That is, the present invention is a method for solidifying a melt (residual melt) remaining in a quartz crucible after pulling up the crystal while heating the melt in the quartz crucible with a heater by the Czochralski method. After the pulling is finished, the crucible and the heater are moved up and down relatively so that the height of the heat generation center position of the heater is within 20 mm from the surface of the residual melt, and the power supply to the heater is stopped. A method for solidifying a residual melt is provided.

図１を参照して、本発明をより具体的に説明する。
図１(a)は、単結晶製造装置４０を用いて、チョクラルスキー法により石英ルツボ４５内の融液をヒーター４７で加熱しつつ結晶を引上げた後の状態を示す。 The present invention will be described more specifically with reference to FIG.
FIG. 1A shows a state after using the single crystal manufacturing apparatus 40 to pull up the crystal while heating the melt in the quartz crucible 45 with the heater 47 by the Czochralski method.

石英ルツボ４５は黒鉛ルツボ４６で保護されている。この黒鉛ルツボは、一体型のものであってもよいし、２つ以上に分割された部分から構成された黒鉛ルツボとしてもよい。一体型の黒鉛ルツボにくらべて、分割型の黒鉛ルツボの方が、融液が固化して膨張した際に、分割部で開くことができるので石英ルツボおよび黒鉛ルツボの割れの発生を抑えることができるし、また、ルツボ全体を交換せずとも破損したパーツを交換すれば操業を再開できる等の利点があって好ましい。   The quartz crucible 45 is protected by a graphite crucible 46. This graphite crucible may be an integral type or may be a graphite crucible composed of two or more parts. Compared with the integrated graphite crucible, the split graphite crucible can be opened at the split part when the melt is solidified and expanded, thus preventing the cracking of the quartz crucible and the graphite crucible. Moreover, it is preferable because there is an advantage that the operation can be resumed by replacing the damaged part without replacing the entire crucible.

図１では、ヒーター４７は、結晶引上げ時にルツボ下部を保温するための断熱部材４９と一体となっており、断熱部材４９がヒーター４７と同期して昇降するようになっている。   In FIG. 1, the heater 47 is integrated with a heat insulating member 49 for keeping the crucible lower part when the crystal is pulled up, and the heat insulating member 49 moves up and down in synchronization with the heater 47.

本発明では、結晶引上げ終了後、石英ルツボ４５内の残融液を固化するにあたって、ルツボ４５とヒーター４７を相対的に昇降させて、ヒーター４７の発熱中心位置４８の高さを残融液表面４４から２０ｍｍ以内とする工程を行う。
この工程では、ルツボ４５のみ、あるいはヒーター４７のみを昇降させてもよいし、たとえば、図１では、ルツボ４５およびヒーター４７をともに降下して、ヒーター４７の発熱中心位置４８の高さを残融液表面４４から２０ｍｍ以内としている（図１（ｂ））。 In the present invention, when the residual melt in the quartz crucible 45 is solidified after the completion of the crystal pulling, the crucible 45 and the heater 47 are moved up and down relatively so that the height of the heat generation center position 48 of the heater 47 is set to the surface of the residual melt. The process which makes it within 44 to 20 mm is performed.
In this step, only the crucible 45 or only the heater 47 may be raised or lowered. For example, in FIG. 1, both the crucible 45 and the heater 47 are lowered so that the height of the heat generation center position 48 of the heater 47 remains. It is within 20 mm from the liquid surface 44 (FIG. 1B).

このヒーター４７の発熱中心位置４８の高さを残融液表面４４から２０ｍｍ以内とする際に、発熱中心位置４８の高さを残融液表面４４と一致させれば、残融液の表面とルツボ底部の温度差をより小さくし、残融液表面と底部の凝固速度差を小さくすることができ、石英ルツボが割れることをより確実に防止できるため好ましい。   When the height of the heat generation center position 48 of the heater 47 is set to be within 20 mm from the residual melt surface 44, if the height of the heat generation center position 48 matches the residual melt surface 44, the surface of the residual melt This is preferable because the temperature difference at the bottom of the crucible can be further reduced, the difference in the solidification rate between the surface of the residual melt and the bottom can be reduced, and the quartz crucible can be more reliably prevented from cracking.

このとき、従来のようにヒーターに対してルツボ４５のみを降下させるのではなく、ヒーター４７をともに降下することで、図１（ｂ）に示すように、ルツボ４５の底部と断熱部材４９の距離を従来より大きく取ることができる。これによって、残融液の固化時に、従来よりルツボ下部の保温効果を低減できるので、残融液の表面と底部の温度差をより小さくすることができる。したがって、残融液の表面が先に凝固して膨張し石英ルツボが割れることをより確実に防止できる。   At this time, instead of lowering only the crucible 45 with respect to the heater as in the prior art, by lowering the heater 47 together, the distance between the bottom of the crucible 45 and the heat insulating member 49 is shown in FIG. Can be taken larger than before. Thereby, when the residual melt is solidified, the heat retaining effect at the lower part of the crucible can be reduced as compared with the prior art, so that the temperature difference between the surface and bottom of the residual melt can be further reduced. Accordingly, it is possible to more reliably prevent the surface of the residual melt from first solidifying and expanding to crack the quartz crucible.

さらに本発明では、ヒーター４７への供給電力を停止する工程を行う。このヒーター４７への供給電力を停止する工程は、上記ヒーター４７の発熱中心位置４８の高さを残融液表面４４から２０ｍｍ以内とする工程の前または後にまたは同時に行ってもよい。また、結晶引上げ終了後にヒーター４７への供給電力を徐々に低下して、最終的な供給電力の停止は、残融液の表面が固化する前に行ってもよい。
しかし、特許文献１に記載するように必ずしも残融液を下部から上部に固化させずとも本発明の目的は達成できるので、結晶引上げ終了後すぐにヒーターへの供給電力を停止する方が経済的で好ましい。 Furthermore, in the present invention, a process of stopping the power supplied to the heater 47 is performed. The step of stopping the power supplied to the heater 47 may be performed before, after, or simultaneously with the step of setting the height of the heat generation center position 48 of the heater 47 within 20 mm from the residual melt surface 44. Further, the power supplied to the heater 47 may be gradually reduced after the crystal pulling is finished, and the final power supply may be stopped before the surface of the residual melt is solidified.
However, since the object of the present invention can be achieved without necessarily solidifying the residual melt from the lower part to the upper part as described in Patent Document 1, it is more economical to stop the power supply to the heater immediately after the completion of the crystal pulling. Is preferable.

以上の工程を行って、石英ルツボ内の残融液を固化する。
このような残融液の固化方法を用いることで、残融液の表面を高温とし、残融液の表面と底部の温度差を小さくし、残融液表面と底部の凝固速度差を小さくすることができる。これによって、残融液の表面が先に凝固して膨張し石英ルツボが割れることを防止できる。すなわち黒鉛ルツボおよび黒鉛ルツボの下部のＨＺ部品への残融液の漏れが防止できる。その結果、残融液との接触および反応による黒鉛ルツボおよび黒鉛ルツボの下部の炉内部品の劣化が防止できる。また、残融液が漏れないので、チャンバーの破損等も生じない。 By performing the above steps, the residual melt in the quartz crucible is solidified.
By using such a solidification method of the residual melt, the surface of the residual melt is heated, the temperature difference between the surface and the bottom of the residual melt is reduced, and the solidification rate difference between the surface and the bottom of the residual melt is reduced. be able to. As a result, it is possible to prevent the surface of the residual melt from first solidifying and expanding to crack the quartz crucible. That is, leakage of the residual melt to the graphite crucible and the HZ part below the graphite crucible can be prevented. As a result, it is possible to prevent deterioration of the graphite crucible and in-furnace parts below the graphite crucible due to contact and reaction with the residual melt. Further, since the residual melt does not leak, the chamber is not damaged.

以下、本発明を実施例、比較例を挙げて具体的に説明するが、本発明はこれに限定されるものではない。なお、図１は本発明を明瞭に説明するために描かれており、実際の寸法を反映したものではない。
（実施例）
図１に示すような、直径５５０mmの石英ルツボ４５とヒーター４７を独立して昇降可能な昇降装置を具備し、かつヒーター４７と一体に昇降するよう設置された、ルツボ下部を保温する断熱部材４９を有する単結晶製造装置４０を用いて、結晶の引上げを行った。 EXAMPLES Hereinafter, although an Example and a comparative example are given and this invention is demonstrated concretely, this invention is not limited to this. FIG. 1 is drawn for the purpose of clearly explaining the present invention, and does not reflect actual dimensions.
(Example)
As shown in FIG. 1, a heat insulating member 49 that retains the lower part of the crucible and includes an elevating device capable of independently elevating and lowering the quartz crucible 45 having a diameter of 550 mm and the heater 47, and ascending and descending integrally with the heater 47. The crystal was pulled using a single crystal manufacturing apparatus 40 having

具体的には、石英ルツボ４５内の融液を１１０kgのSi融液とし、８５kgの直径１５０mm Si単結晶を引上げた。このとき、結晶引上げ開始から終了迄の間ヒーター４７は移動させず、Si融液（残融液）表面４４の高さがヒーター４７に対して常に一定の位置となるようにルツボ４５を移動させて結晶引上を行った。すなわち、ヒーター４７の発熱中心位置４８の高さは、結晶引上げ開始から終了迄の間、常にSi融液表面４４の６０mm下方に一定であった。   Specifically, the melt in the quartz crucible 45 was used as a 110 kg Si melt, and an 85 kg 150 mm diameter Si single crystal was pulled up. At this time, the heater 47 is not moved from the start to the end of crystal pulling, and the crucible 45 is moved so that the height of the Si melt (residual melt) surface 44 is always at a fixed position with respect to the heater 47. The crystal was pulled up. That is, the height of the heating center position 48 of the heater 47 was always constant 60 mm below the Si melt surface 44 from the start to the end of crystal pulling.

上記結晶の引上げ後、石英ルツボ４５内の残融液は２５kgであり、残融液深さは８１mmであった。すなわち、ヒーター４７の発熱中心位置４８はほぼ石英ルツボ４５底部の高さに位置していた（図１(a)）。   After pulling up the crystal, the residual melt in the quartz crucible 45 was 25 kg, and the residual melt depth was 81 mm. That is, the heat generation center position 48 of the heater 47 was positioned substantially at the height of the bottom of the quartz crucible 45 (FIG. 1 (a)).

次に、残融液の固化を行った。
石英ルツボ４５を１５０mm下げるとともにヒーター４７も１００mm下げた。このとき、ヒーター４７の発熱中心位置４８は残融液表面４４から１０mm下方となった。これとともにヒーター４７への供給電力を停止し、残融液を固化した。 Next, the residual melt was solidified.
The quartz crucible 45 was lowered 150 mm and the heater 47 was lowered 100 mm. At this time, the heating center position 48 of the heater 47 was 10 mm below the residual melt surface 44. At the same time, the power supplied to the heater 47 was stopped, and the residual melt was solidified.

（比較例）
上記実施例と同様の単結晶製造装置６０を用いて、上記実施例と同様に結晶の引上げを行った。
結晶の引上げ後の状態は、上記実施例と同様であった（図２(a)）。
次に、残融液の固化を行った。
石英ルツボ６５のみを１５０mm下げてルツボの底部がヒーター６７の下端位置よりも下方に位置するようにした。このとき、ヒーター６７の発熱中心位置６８は残融液表面６４から９０mm上方となった。そして残融液表面６４が固化してからヒーター６７への供給電力を停止した（図２(b)）。 (Comparative example)
Using the same single crystal manufacturing apparatus 60 as in the above example, the crystal was pulled up as in the above example.
The state after pulling up the crystals was the same as in the above example (FIG. 2 (a)).
Next, the residual melt was solidified.
Only the quartz crucible 65 was lowered by 150 mm so that the bottom of the crucible was positioned below the lower end position of the heater 67. At this time, the heat generation center position 68 of the heater 67 was 90 mm above the residual melt surface 64. Then, after the residual melt surface 64 was solidified, the power supplied to the heater 67 was stopped (FIG. 2 (b)).

上記実施例、比較例はそれぞれ１０バッチ行った。実施例の断熱部材４９は、比較例の断熱部材６９にくらべて石英ルツボ底部との距離が１００mm離れていた。
実施例においては、石英ルツボの割れは一切生じず、残融液の漏れは発生しなかった。一方、比較例では、７０％の確率で石英ルツボが割れて、残融液の漏れが発生した。 The above Examples and Comparative Examples were each performed 10 batches. The heat insulating member 49 of the example was 100 mm away from the bottom of the quartz crucible compared to the heat insulating member 69 of the comparative example.
In the examples, no cracking of the quartz crucible occurred, and no leakage of the residual melt occurred. On the other hand, in the comparative example, the quartz crucible cracked with a probability of 70%, and leakage of the residual melt occurred.

このように、比較例では、ルツボの底部がヒーターの下端位置よりも下方に位置するようにし、残融液表面が固化するまでヒーターを加熱させておいたにもかかわらず、石英ルツボの割れが高い確率で生じた。一方、実施例では結晶の引上げ後すぐにヒーターを切電したが、石英ルツボの割れは一切生じておらず、本発明が経済的で安全性が高い残融液の固化方法であることが確認できた。   As described above, in the comparative example, the quartz crucible was cracked even though the bottom of the crucible was positioned below the lower end position of the heater and the heater was heated until the residual melt surface solidified. It occurred with a high probability. On the other hand, in the examples, the heater was turned off immediately after the crystal was pulled up, but the quartz crucible was not cracked at all, and it was confirmed that the present invention is an economical and safe solidification method of the residual melt. did it.

尚、本発明は、上記実施形態に限定されるものではない。上記実施形態は、例示であり、本発明の特許請求の範囲に記載された技術的思想と実質的に同一な構成を有し、同様な作用効果を奏するものは、いかなるものであっても本発明の技術的範囲に包含される。   The present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

本発明に係る残融液の固化方法の一例を説明する概略図である。It is the schematic explaining an example of the solidification method of the residual melt which concerns on this invention. 従来（比較例）の残融液の固化方法の一例を説明する概略図である。It is the schematic explaining an example of the solidification method of the conventional residual melt (comparative example). 従来の単結晶製造装置の一例を示す概略図である。It is the schematic which shows an example of the conventional single crystal manufacturing apparatus.

符号の説明Explanation of symbols

１…メインチャンバ、 ２…引上げチャンバ、 ３…単結晶、 ４…原料融液、
５、４５、６５…石英ルツボ、 ６、４６…黒鉛ルツボ、
７、４７、６７…ヒーター、 ８…断熱材、 １３…支持軸、
１４…ワイヤー、 ２０、４０、６０…単結晶製造装置、
４４、６４…残融液表面、 ４８、６８…発熱中心位置、 ４９、６９…断熱部材。 1 ... main chamber, 2 ... pulling chamber, 3 ... single crystal, 4 ... raw material melt,
5, 45, 65 ... quartz crucible, 6, 46 ... graphite crucible,
7, 47, 67 ... heater, 8 ... heat insulating material, 13 ... support shaft,
14 ... Wire, 20, 40, 60 ... Single crystal manufacturing equipment,
44, 64 ... residual melt surface, 48, 68 ... heat generation center position, 49, 69 ... heat insulation member.

Claims (5)

チョクラルスキー法により石英ルツボ内の融液をヒーターで加熱しつつ結晶を引上げた後の石英ルツボ内に残留した融液（残融液）の固化方法であって、結晶引上げ終了後、前記ルツボと前記ヒーターを相対的に昇降させて、該ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程と、該ヒーターへの供給電力を停止する工程を含むことを特徴とする残融液の固化方法。   A method of solidifying a melt (residual melt) remaining in a quartz crucible after pulling up a crystal while heating the melt in the quartz crucible with a heater by the Czochralski method. And raising and lowering the heater relative to each other so that the height of the heat generation center position of the heater is within 20 mm from the surface of the residual melt, and stopping the power supplied to the heater. Solidification method of residual melt. 前記石英ルツボを、２つ以上に分割された部分から構成された黒鉛ルツボで保護することを特徴とする請求項１に記載の残融液の固化方法。   2. The method for solidifying a residual melt according to claim 1, wherein the quartz crucible is protected with a graphite crucible composed of two or more parts. 前記ヒーターの発熱中心位置の高さを残融液表面から２０ｍｍ以内とする工程において、前記ヒーターの発熱中心位置の高さを残融液表面と一致させることを特徴とする請求項１または請求項２に記載の残融液の固化方法。   2. The height of the heat generation center position of the heater is made to coincide with the surface of the residual melt in the step of setting the height of the heat generation center position of the heater to within 20 mm from the surface of the residual melt. The solidification method of the residual melt as described in 2. 前記石英ルツボの下方に、結晶引上げ時に該ルツボ下部を保温するための断熱部材が設けられ、該断熱部材が前記ヒーターと同期して昇降することを特徴とする請求項１乃至請求項３のいずれか一項に記載の残融液の固化方法。   4. A heat insulating member for keeping a temperature of a lower portion of the crucible when the crystal is pulled up is provided below the quartz crucible, and the heat insulating member moves up and down in synchronization with the heater. The method for solidifying the residual melt according to claim 1. 前記ヒーターへの供給電力を停止する工程は、残融液の表面が固化する前に行うことを特徴とする請求項１乃至請求項４のいずれか一項に記載の残融液の固化方法。   The method of solidifying the residual melt according to any one of claims 1 to 4, wherein the step of stopping the power supplied to the heater is performed before the surface of the residual melt is solidified.
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