JP2671062B2 - Method for manufacturing quartz glass crucible - Google Patents
Method for manufacturing quartz glass crucibleInfo
- Publication number
- JP2671062B2 JP2671062B2 JP3098331A JP9833191A JP2671062B2 JP 2671062 B2 JP2671062 B2 JP 2671062B2 JP 3098331 A JP3098331 A JP 3098331A JP 9833191 A JP9833191 A JP 9833191A JP 2671062 B2 JP2671062 B2 JP 2671062B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- hydrogen
- glass crucible
- single crystal
- silicon single
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、アーク回転溶融法によ
るシリコン単結晶引上げ用の石英ガラスルツボの製造方
法に関し、特に、シリコン単結晶の減圧引上げ及びマル
チプーリングに適した耐熱性の高いアーク回転溶融法に
よるシリコン単結晶引上げ用の石英ガラスルツボの製造
方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silica glass crucible for pulling a silicon single crystal by an arc rotary melting method, and more particularly, a high heat resistant arc rotation suitable for vacuum pulling and multi-pooling of a silicon single crystal. The present invention relates to a method for producing a quartz glass crucible for pulling a silicon single crystal by a melting method.
【０００２】[0002]
【従来の技術】シリコン単結晶引上げ用石英ガラスルツ
ボは、一般には、水晶、硅砂等の天然に産する石英材料
を原料として製造されている。また、シリコン単結晶の
高純度化に伴い、石英ガラスルツボは高純度のものが要
求されており、この要求に対処するために、ゾルゲル法
による高純度な合成石英ガラス粉や合成クリストバライ
ト粉が、シリコン単結晶引上げ用石英ガラスルツボの原
料として使用されている。2. Description of the Related Art In general, quartz glass crucibles for pulling a silicon single crystal are manufactured using a naturally occurring quartz material such as quartz or silica sand as a raw material. Further, as the purity of the silicon single crystal is increased, the quartz glass crucible is required to have a high purity, and in order to cope with this requirement, high-purity synthetic quartz glass powder or synthetic cristobalite powder by the sol-gel method, It is used as a raw material for quartz glass crucibles for pulling silicon single crystals.
【０００３】[0003]
【発明が解決しようとする課題】このような高純度石英
ガラスルツボの製造原料として開発されている、ゾルゲ
ル法による石英ガラス粉は、アーク回転溶融法によって
石英ガラスルツボを製造すると、成形性の良好な石英ガ
ラスルツボを得ることができる。しかし、このようにし
て製造された石英ガラスルツボは、減圧下におけるシリ
コン単結晶引上げ時に、ルツボ壁面の膨張や変形が生じ
るので問題とされている。 また天然産の石英粉から製
造される従来の石英ガラスルツボにおいても、長時間の
使用、特に減圧下のシリコン単結晶引上げを行う場合に
は、しばしばルツボ壁面の膨張により変形を生じるので
問題とされている。The silica glass powder produced by the sol-gel method, which has been developed as a raw material for producing such a high-purity silica glass crucible, has good formability when the silica glass crucible is produced by the arc rotary melting method. It is possible to obtain a simple quartz glass crucible. However, the quartz glass crucible manufactured in this manner is problematic because the crucible wall surface expands and deforms when the silicon single crystal is pulled up under reduced pressure. In addition, even in a conventional quartz glass crucible manufactured from naturally occurring quartz powder, when used for a long time, especially when pulling a silicon single crystal under reduced pressure, deformation often occurs due to expansion of the crucible wall surface, which is a problem. ing.
【０００４】このような減圧下のシリコン単結晶引上げ
において、使用される石英ガラスルツボの壁面の膨張に
よる変形は、シリコン単結晶の大径化に伴う石英ガラス
ルツボの大型化を図る上で大きな問題となってきてい
る。このような石英ガラスルツボが、減圧下のシリコン
単結晶の引上げにおいて使用できるようにするために、
外周に減圧を適用してアーク回転溶融法により石英ガラ
スルツボを製造する方法が提案されている。しかし、こ
の減圧アーク回転溶融法により石英ガラスルツボを製造
する場合は、従来の製造方法により製造された石英ガラ
スルツボに比べて、コストが高くなり、しかも、ルツボ
の気泡数が少なくなるために、均熱特性が悪くなり問題
である。本発明は、以上のようなシリコン単結晶引上げ
用の石英ガラスルツボについての問題点を解決すること
を目的としている。In such pulling of the silicon single crystal under reduced pressure, the deformation of the wall surface of the silica glass crucible used due to expansion is a major problem in increasing the size of the silica glass crucible as the diameter of the silicon single crystal increases. Is becoming. In order to enable such a quartz glass crucible to be used in pulling a silicon single crystal under reduced pressure,
A method of manufacturing a quartz glass crucible by an arc rotary melting method by applying reduced pressure to the outer circumference has been proposed. However, when manufacturing a quartz glass crucible by this reduced pressure arc rotation melting method, compared to a quartz glass crucible manufactured by a conventional manufacturing method, the cost is high, and moreover, since the number of bubbles in the crucible is reduced, This is a problem because the soaking properties deteriorate. SUMMARY OF THE INVENTION An object of the present invention is to solve the above-described problems of the quartz glass crucible for pulling a silicon single crystal.
【０００５】[0005]
【課題を解決するための手段】本発明は、シリコン単結
晶の長時間引き上げ、マルチプーリング、特に減圧引き
上げに使用できるように、減圧加熱下において、石英ガ
ラスルツボ壁面の膨張及び変形が少なく、即ち、耐久性
が高く、その上均熱特性が良く、さらに長時間使用可能
な石英ガラスルツボを、安価に製造することができる新
規な石英ガラスルツボの製造方法を提供することを目的
としている。この目的を達成するために、本発明者ら
は、アーク回転溶融法で作られた石英ガラスルツボを、
水素雰囲気下で加熱保持した石英ガラスルツボについて
検討したところ、例えば、真空中、１４８０℃で４時間
加熱した減圧下のシリコン単結晶引上げのシミュレーシ
ョンテストにおいて、著しく低い膨張率を示すことを見
い出した。According to the present invention, the expansion and deformation of the quartz glass crucible wall surface under reduced pressure heating is small, so that the silicon single crystal can be used for long-time pulling, multi-pooling, and particularly, depressurized pulling. It is an object of the present invention to provide a novel method of manufacturing a quartz glass crucible which has high durability, has good heat uniformity characteristics, and can be used for a long time at low cost. To this end, the present inventors have developed a quartz glass crucible made by the arc rotary melting method,
When a quartz glass crucible heated and held in a hydrogen atmosphere was examined, it was found that, for example, in a simulation test of pulling a silicon single crystal under reduced pressure heated at 1480 ° C. for 4 hours in a vacuum, a significantly low expansion coefficient was exhibited.
【０００６】そこで、本発明者らは、石英ガラスルツボ
の原料に、天然石英粉、合成クリストバライト粉又は合
成非晶質シリカ粉を使用して、アーク回転溶融法により
石英ガラスルツボを成形した後、この成形した石英ガラ
スルツボを水素雰囲気中に加熱保持して、熱処理し、こ
の熱処理された石英ガラスルツボを、シリコン単結晶引
き上げ、特に減圧下でのシリコン単結晶引上げに使用し
たところ、ルツボ壁面の膨張も少なく従って変形を起こ
すことなく、シリコン単結晶を製造することを確認し、
本発明に至った。Therefore, the inventors of the present invention used natural quartz powder, synthetic cristobalite powder or synthetic amorphous silica powder as a raw material for the quartz glass crucible, and after molding the quartz glass crucible by the arc rotary melting method, This molded quartz glass crucible was heated and held in a hydrogen atmosphere and heat-treated, and the heat-treated quartz glass crucible was used for pulling a silicon single crystal, particularly for pulling a silicon single crystal under reduced pressure. It is confirmed that a silicon single crystal is produced without causing expansion and therefore deformation.
The present invention has been reached.
【０００７】即ち、本発明は、アーク回転溶融法で製造
されたシリコン石英ガラスルツボを水素又は水素含有雰
囲気中で、加熱保持することを特徴とする減圧雰囲気下
でのシリコン単結晶引上げ用石英ガラスルツボの製造方
法にある。That is, the present invention is characterized in that a silicon quartz glass crucible manufactured by an arc rotary melting method is heated and held in an atmosphere containing hydrogen or hydrogen, and the quartz glass for pulling a silicon single crystal in a reduced pressure atmosphere is characterized. There is a method of manufacturing the crucible.
【０００８】本発明においては、アーク回転溶融法で成
形された石英ガラスルツボを、水素又は水素含有雰囲気
内で加熱処理することにより、従来の石英ガラスルツボ
に比して低膨張の石英ガラスルツボとするものである。
本発明における単結晶引上げ用の石英ガラスルツボは、
アーク回転溶融法により製造された石英ガラスルツボ
を、炉に入れ、炉内を水素雰囲気又は主としてアルゴン
（Ａｒ）若しは窒素（Ｎ２）含有の水素雰囲気に保っ
て、加熱して製造される。In the present invention, a quartz glass crucible molded by the arc rotary melting method is heat-treated in a hydrogen or hydrogen-containing atmosphere to obtain a quartz glass crucible having a lower expansion than that of a conventional quartz glass crucible. To do.
The quartz glass crucible for pulling a single crystal in the present invention,
A quartz glass crucible manufactured by the arc rotary melting method is placed in a furnace, and the furnace is maintained in a hydrogen atmosphere or a hydrogen atmosphere containing mainly argon (Ar) or nitrogen (N 2 ) and heated to manufacture the quartz glass crucible. .
【０００９】本発明において、石英ルツボは、４００℃
乃至１２００℃の範囲内の加熱保持温度で加熱して製造
されるのが好ましい。この石英ガラスルツボの加熱保持
温度を４００℃以下とすると、ルツボ内への水素の拡散
又は反応が遅くなるので好ましくない。また、加熱保持
温度を１２００℃以上とすると、ルツボの変形が生じる
ので好ましくない。本発明において、石英ガラスルツボ
を加熱保持温度で加熱するのは、水素の拡散又は反応を
高めるためであるが、水素の拡散又は反応は、高温にな
るに従い高くなるので、より好ましい加熱保持温度は１
０００〜１１５０℃である。In the present invention, the quartz crucible has a temperature of 400 ° C.
It is preferably manufactured by heating at a heating and holding temperature in the range of 1 to 1200 ° C. If the heating and holding temperature of the quartz glass crucible is 400 ° C. or lower, the diffusion or reaction of hydrogen in the crucible becomes slow, which is not preferable. If the heating and holding temperature is 1200 ° C. or higher, the crucible may be deformed, which is not preferable. In the present invention, heating the quartz glass crucible at the heating and holding temperature is for enhancing the diffusion or reaction of hydrogen. However, since the diffusion or reaction of hydrogen becomes higher as the temperature becomes higher, the more preferable heating and holding temperature is 1
000 to 1150 ° C.
【００１０】石英ガラスルツボに対する水素の拡散又は
反応は、加熱保持時間に影響されるために、本発明にお
いては、石英ガラスルツボの加熱保持時間は、０．５〜
１０時間が適当とされる。０．５時間未満の短時間では
ルツボ壁内部への水素の拡散又は反応が不十分であり、
また、該加熱保持時間が１０時間を越える長時間になる
とコスト的に好ましくない。しかし、水素の拡散又は反
応は、水素又は水素含有雰囲気の圧力に影響されるの
で、大気圧の水素又は水素含有雰囲気においては、石英
ガラスルツボの加熱保持時間は４〜６時間とするのが更
に好ましい。Since the diffusion or reaction of hydrogen with respect to the quartz glass crucible is affected by the heating and holding time, in the present invention, the heating and holding time of the quartz glass crucible is 0.5 to.
10 hours is appropriate. In a short time of less than 0.5 hours, diffusion or reaction of hydrogen inside the crucible wall is insufficient,
Further, if the heating and holding time is longer than 10 hours, it is not preferable in terms of cost. However, since the diffusion or reaction of hydrogen is affected by the pressure of hydrogen or a hydrogen-containing atmosphere, the heat retention time of the quartz glass crucible is more preferably 4 to 6 hours in hydrogen or a hydrogen-containing atmosphere at atmospheric pressure. preferable.
【００１１】石英ガラスルツボの加熱保持時の水素又は
水素含有雰囲気の圧力は、高い程、石英ガラスルツボ内
の水素の拡散又は反応を早めるので好ましい。水素又は
水素含有雰囲気の圧力を高くすれば加熱保持温度を低く
でき、また加熱保持時間を短時間に設定できるが、水素
又は水素含有雰囲気の圧力を高くすると、炉の仕様に影
響するので、本発明において、石英ガラスルツボの水素
又は水素含有雰囲気の加熱保持圧力は大気圧以上とされ
る。It is preferable that the pressure of hydrogen or a hydrogen-containing atmosphere at the time of heating and holding the quartz glass crucible is higher because the diffusion or reaction of hydrogen in the quartz glass crucible is accelerated. The heating and holding temperature can be lowered by increasing the pressure of hydrogen or hydrogen-containing atmosphere, and the heating and holding time can be set to a short time.However, increasing the pressure of hydrogen or hydrogen-containing atmosphere affects the specifications of the furnace. In the invention, the heating and holding pressure of the hydrogen or the hydrogen-containing atmosphere in the quartz glass crucible is set to the atmospheric pressure or higher.
【００１２】本発明において、水素含有雰囲気は水素を
含有する雰囲気であり、水素含有雰囲気内の水素分圧は
大きいのが好ましい。したがって水素含有雰囲気は、主
として水素ガスで組成することが好ましい。しかし、水
素含有雰囲気は、組成する主たる成分として、水素に対
し不活性で拡散し難いアルゴン及び窒素を使用すること
ができる。この場合、水素含有雰囲気の水素濃度は、５
％以上であるのが好ましい。In the present invention, the hydrogen-containing atmosphere is an atmosphere containing hydrogen, and the hydrogen partial pressure in the hydrogen-containing atmosphere is preferably large. Therefore, the hydrogen-containing atmosphere is preferably composed mainly of hydrogen gas. However, the hydrogen-containing atmosphere can use argon and nitrogen, which are inert to hydrogen and hardly diffuse, as the main components to be composed. In this case, the hydrogen concentration in the hydrogen-containing atmosphere is 5
% Or more is preferable.
【００１３】[0013]
【作用】本発明は、アーク回転溶融法で製造された石英
ガラスルツボを水素又は水素含有雰囲気中で加熱保持す
るので、石英ガラスルツボ内に水素ガスが拡散又は反応
して低膨張となるので、該ルツボガラス内に泡を多数含
んでいても、例えば、シリコン単結晶の減圧引き上げ時
の石英ガラスルツボの壁面膨張を抑えることができる。
しかも、本発明によると、石英ガラスルツボ中に泡を多
く含ませることができるので、均熱性の良い石英ガラス
ルツボを製造することができる。したがって、本発明の
石英ガラスルツボを使用することにより常圧及び減圧下
で安定したシリコン単結晶の引き上げを行うことができ
る。本発明においては、大気下でのアーク回転溶融法に
よって製造された気泡を大量に含んだ石英ガラスルツボ
を、水素雰囲気もしくは水素含有雰囲気下で加熱保持し
て、低膨張の石英ガラスルツボとするので、石英ガラス
ルツボ内に生成する気泡を、調整することなく、例え
ば、シリコン単結晶の減圧引上げ用の石英ガラスルツボ
を製造することができる。In the present invention, since the quartz glass crucible manufactured by the arc rotary melting method is heated and held in hydrogen or a hydrogen-containing atmosphere, hydrogen gas diffuses or reacts in the quartz glass crucible, resulting in low expansion. Even if the crucible glass contains a large number of bubbles, for example, it is possible to suppress the wall surface expansion of the quartz glass crucible when the silicon single crystal is pulled down under reduced pressure.
Moreover, according to the present invention, since a large amount of bubbles can be included in the quartz glass crucible, it is possible to manufacture a quartz glass crucible having a good soaking property. Therefore, the use of the quartz glass crucible of the present invention enables stable pulling of a silicon single crystal under normal pressure and reduced pressure. In the present invention, a quartz glass crucible containing a large amount of bubbles produced by an arc rotary melting method under the atmosphere is heated and held in a hydrogen atmosphere or a hydrogen-containing atmosphere to obtain a low-expansion quartz glass crucible. It is possible to manufacture, for example, a quartz glass crucible for pulling up a silicon single crystal under reduced pressure without adjusting bubbles generated in the quartz glass crucible.
【００１４】[0014]
【実施例】以下、例をあげて本発明の実施の態様を説明
するが、本発明は以下の説明及び例示によって、何等の
制限を受けるものではない。The embodiments of the present invention will be described below by way of examples, but the present invention is not limited by the following description and examples.
【例１】アーク回転溶融法により、天然石英粉８０ｋｇ
から１８インチ（４５７．２ｍｍ）径石英ガラスルツボ
を４個製造した。そのうち２個を、水素１００％雰囲気
下で大気圧で１１００℃で５時間加熱保持した。この水
素熱処理された石英ガラスルツボ１個と水素熱処理され
ていない石英ガラスルツボ１個から、各々、石英ガラス
ルツボの側壁から１５×１５ｍｍの試験片を切り取り、
真空下１４８０℃で４時間加熱し、試料の前後の密度差
から密度変化率を、次式： 密度変化率（％）＝（実験前の密度−実験後の密度）×
１００／実験前の密度 により求めた。その結果を次に示す。 水素熱処理無し １３．７（％） （比較例） 水素熱処理有り ６．６（％） （本例） 残る熱処理された石英ガラスルツボ１個と熱処理されて
いない石英ガラスルツボを減圧下のシリコン単結晶引上
げテストに用いた。その結果を次に示す。 水素熱処理無し 側壁の膨張大 長時間 （比較例） 水素熱処理有り 側壁の膨張小 （本例）[Example 1] 80 kg of natural quartz powder by arc rotary melting method
From the four quartz glass crucibles having a diameter of 18 inches (457.2 mm) were manufactured. Two of them were heated and held at 1100 ° C. for 5 hours at atmospheric pressure in a 100% hydrogen atmosphere. 15 × 15 mm test pieces were cut from the side wall of the quartz glass crucible from each of the hydrogen-heat-treated quartz glass crucible and the non-hydrogen-treated quartz glass crucible,
The sample was heated under vacuum at 1480 ° C. for 4 hours, and the density change rate was calculated from the density difference before and after the sample as follows: Density change rate (%) = (density before experiment−density after experiment) ×
It was determined by 100 / density before experiment. The results are shown below. Without hydrogen heat treatment 13.7 (%) (Comparative example) With hydrogen heat treatment 6.6 (%) (this example) A silicon single crystal under reduced pressure was used for the remaining one heat-treated quartz glass crucible and one unheated quartz glass crucible. It was used for the pull-up test. The results are shown below. No hydrogen heat treatment Large expansion of side wall Long time (comparative example) With hydrogen heat treatment Small expansion of side wall (this example)
【００１５】[0015]
【例２】アーク回転溶融法により、高純度合成クリスト
バライト粉４０ｋｇから１８インチ（４５７．２ｍｍ）
径石英ガラスルツボ２個製造し、１個を水素１００％雰
囲気下で大気圧で１０００℃で５時間加熱保持した。水
素熱処理した石英ガラスルツボと水素熱処理されていな
い石英ガラスルツボより側胴部から各々１５×１５ｍｍ
の試験片を切り取り、例１と同様に、真空下１４８０℃
で４時間加熱し、試料の前後の密度差から密度変化を求
めた。その結果を次に示す。 水素熱処理無し １４．１（％） （比較例） 水素熱処理有り ５．６（％） （本例）[Example 2] High-purity synthetic cristobalite powder 40 kg to 18 inches (457.2 mm) by arc rotary melting method
Two quartz glass crucibles each having a diameter were produced, and one crucible was heated and held at 1000 ° C. for 5 hours under an atmosphere of 100% hydrogen at atmospheric pressure. 15 x 15 mm from the side body of the quartz glass crucible that was heat treated with hydrogen and the quartz glass crucible that was not heat treated with hydrogen.
The test piece was cut out and, in the same manner as in Example 1, under vacuum 1480 ° C.
After heating for 4 hours, the change in density was determined from the difference in density before and after the sample. The results are shown below. Without hydrogen heat treatment 14.1 (%) (Comparative example) With hydrogen heat treatment 5.6 (%) (This example)
【００１６】[0016]
【例３】アーク回転溶融法により、高純度低ＯＨ非晶質
シリカ粉４０ｋｇから１８インチ（４５７．２ｍｍ）径
石英ガラスルツボ２個を製造し、ルツボ１個を水素１０
０％雰囲気下で大気圧で１０００℃で５時間加熱保持
し、水素熱処理を行った。例１と同様に、真空下１４８
０℃で４時間加熱し、試料の前後の密度差から密度変化
を求めた。その結果を次に示す。 水素熱処理無し １７．８（％） （比較例） （減圧下でのシリコン単結晶引上げテストは、ルツボの
変形の恐れがあるためにできない。） 水素熱処理有り ７．０（％） （本例） （天然粉を原料とする石英ガラスルツボ以下となり、減
圧下でのシリコン単結晶の引上げも容易となり、ルツボ
の変形のトラブルもなく行えた。）[Example 3] Two 18-inch (457.2 mm) diameter silica glass crucibles were produced from 40 kg of high-purity low-OH amorphous silica powder by the arc rotary melting method, and one crucible was replaced with hydrogen 10.
A hydrogen heat treatment was performed by heating and holding at 1000 ° C. for 5 hours at atmospheric pressure in a 0% atmosphere. As in Example 1, under vacuum 148
The sample was heated at 0 ° C. for 4 hours, and the change in density was obtained from the difference in density before and after the sample. The results are shown below. Without hydrogen heat treatment 17.8 (%) (Comparative example) (Silicone single crystal pull-up test under reduced pressure cannot be performed due to the risk of crucible deformation.) Hydrogen heat treatment included 7.0 (%) (this example) (Since it is less than or equal to the quartz glass crucible made from natural powder, it is easy to pull up the silicon single crystal under reduced pressure, and the crucible deformation can be prevented.)
【００１７】これらの例においては、水素雰囲気は、水
素ガスを補充しながら行われているが、水素ガスの補充
を行わなくとも同様の結果を得ることができた。また、
これらの例については、水素気流中で行っても同様の結
果を得ることができた。In these examples, the hydrogen atmosphere was supplemented with hydrogen gas, but similar results could be obtained without supplementing hydrogen gas. Also,
Similar results could be obtained for these examples even in the hydrogen stream.
【００１８】[0018]
【発明の効果】本発明は、アーク回転溶融法で製造され
た石英ガラスルツボを水素又は水素含有雰囲気中で加熱
保持するので、従来法のように、シリコン単結晶の減圧
引上げ時の石英ガラスルツボの壁面の膨張を抑えるため
に、減圧アーク回転溶融法によるルツボ壁中の気泡数を
減少させる必要がないので、減圧下のシリコン単結晶引
上げ用の石英ガラスルツボを簡単な工程で製造すること
ができる。本発明による石英ガラスルツボは、多くの泡
を含んでいるので、従来の減圧下のシリコン単結晶引上
げ用の石英ガラスルツボに比して、安価であり、均熱性
にも優れている。従って、本発明によると、従来の石英
ガラスルツボの製法に比して、歩留まり良くシリコン単
結晶を製造することができる。According to the present invention, the quartz glass crucible manufactured by the arc rotary melting method is heated and held in the atmosphere containing hydrogen or hydrogen. Therefore, as in the conventional method, the quartz glass crucible is used when the silicon single crystal is pulled under reduced pressure. Since it is not necessary to reduce the number of bubbles in the crucible wall by the low pressure arc rotary melting method in order to suppress the expansion of the wall surface, it is possible to manufacture a quartz glass crucible for pulling a silicon single crystal under reduced pressure in a simple process. it can. Since the quartz glass crucible according to the present invention contains many bubbles, it is inexpensive and has excellent heat uniformity as compared with the conventional quartz glass crucible for pulling a silicon single crystal under reduced pressure. Therefore, according to the present invention, a silicon single crystal can be manufactured with a high yield, as compared with the conventional method for manufacturing a silica glass crucible.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平１−201664（ＪＰ，Ａ) 特開 昭63−215600（ＪＰ，Ａ) 特公 昭40−10228（ＪＰ，Ｂ１) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-1-201664 (JP, A) JP-A-63-215600 (JP, A) JP-B-40-10228 (JP, B1)
Claims (6)
スルツボを、水素又は水素含有雰囲気中で、加熱保持す
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
ルツボの製造方法。1. A method for producing a quartz glass crucible for pulling a silicon single crystal, which comprises heating and holding a quartz glass crucible produced by an arc rotary melting method in hydrogen or a hydrogen-containing atmosphere.
るものであることを特徴とする請求項１に記載のシリコ
ン単結晶引上げ用石英ガラスルツボの製造方法。2. The method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 1, wherein the hydrogen-containing atmosphere contains 5% or more of hydrogen.
含有するものであることを特徴とする請求項１又は２に
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。3. The method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 1 or 2, wherein the hydrogen-containing atmosphere contains argon or nitrogen.
スルツボを加熱保持する加熱保持温度が、４００℃乃至
１２００℃の範囲であることを特徴とする請求項１乃至
３の何れか一項に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。4. The heating and holding temperature for heating and holding the quartz glass crucible manufactured by the arc rotary melting method is in the range of 400 ° C. to 1200 ° C., in any one of claims 1 to 3. A method for producing a quartz glass crucible for pulling up a silicon single crystal as described above.
スルツボを加熱保持する加熱保持時間が、０．５時間乃
至１０時間であることを特徴とする請求項１乃至４の何
れか一項に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。5. The heating and holding time for heating and holding the quartz glass crucible manufactured by the arc rotary melting method is 0.5 hours to 10 hours, according to any one of claims 1 to 4. A method for producing a quartz glass crucible for pulling up a silicon single crystal as described above.
スルツボを加熱保持時の水素又は水素含有雰囲気の圧力
が、大気圧以上であることを特徴とする請求項１乃至５
の何れか一項に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。6. The pressure of hydrogen or a hydrogen-containing atmosphere at the time of heating and holding the quartz glass crucible manufactured by the arc rotary melting method is equal to or higher than atmospheric pressure.
9. A method for manufacturing a quartz glass crucible for pulling a silicon single crystal according to any one of 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3098331A JP2671062B2 (en) | 1991-01-31 | 1991-01-31 | Method for manufacturing quartz glass crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3098331A JP2671062B2 (en) | 1991-01-31 | 1991-01-31 | Method for manufacturing quartz glass crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05208838A JPH05208838A (en) | 1993-08-20 |
| JP2671062B2 true JP2671062B2 (en) | 1997-10-29 |
Family
ID=14216924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3098331A Expired - Lifetime JP2671062B2 (en) | 1991-01-31 | 1991-01-31 | Method for manufacturing quartz glass crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2671062B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11310423A (en) * | 1998-02-27 | 1999-11-09 | Toshiba Ceramics Co Ltd | Synthetic quartz glass and its production |
| JP2002211997A (en) * | 2001-01-10 | 2002-07-31 | Kusuwa Kuorutsu:Kk | Crucible for pulling semiconductor silicon |
| WO2022186067A1 (en) | 2021-03-05 | 2022-09-09 | 信越石英株式会社 | Method for evaluating quartz glass crucible and method for producing said quartz glass crucible, and quartz glass crucible |
-
1991
- 1991-01-31 JP JP3098331A patent/JP2671062B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05208838A (en) | 1993-08-20 |
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