JP2002154894A - Crucible for pulling semiconductor silicon, almost free from vibration at liquid surface - Google Patents
Crucible for pulling semiconductor silicon, almost free from vibration at liquid surfaceInfo
- Publication number
- JP2002154894A JP2002154894A JP2000350504A JP2000350504A JP2002154894A JP 2002154894 A JP2002154894 A JP 2002154894A JP 2000350504 A JP2000350504 A JP 2000350504A JP 2000350504 A JP2000350504 A JP 2000350504A JP 2002154894 A JP2002154894 A JP 2002154894A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- vibration
- silicon
- liquid surface
- free
- 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.)
- Pending
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、単結晶シリコン引
上げ用の石英ガラスルツボに関するものである。特に大
口径シリコンインゴットを引き上げる為に最適な石英ガ
ラスルツボに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a quartz glass crucible for pulling single crystal silicon. Particularly, the present invention relates to a quartz glass crucible which is most suitable for pulling a large-diameter silicon ingot.
【0002】[0002]
【従来の技術】シリコン単結晶を製造する方法であるCZ
(チョコラルスキー)法は石英ガラスにポリシリコンを
入れ、溶解したのち種結晶を融液につけ、単結晶を引き
上げるが、近年、コストダウンのためにポリシリコンの
チャージ量を増やして一回に引き上げる重量を多くして
いる。この方法に耐える石英ガラスルツボとして失透し
にくい、内面に合成石英ガラスの層を持つルツボが使わ
れている。2. Description of the Related Art CZ which is a method of manufacturing a silicon single crystal
In the (Czochralski) method, polysilicon is put into quartz glass, melted with a seed crystal after melting, and a single crystal is pulled up. In recent years, however, the amount of polysilicon charged has been increased and pulled up at a time to reduce costs. Have many. As a quartz glass crucible resistant to this method, a crucible having a layer of synthetic quartz glass on its inner surface, which is hardly devitrified, is used.
【0003】[0003]
【発明が解決しようとする課題】しかし、この合成石英
ルツボを用いると、シリコンの液面が振動する現象が起
き、ひどいときには種結晶が液面につかないという不具
合が発生する。この液面振動により総合歩留まりは著し
く低下するため、この解決が急務となっている。However, when this synthetic quartz crucible is used, a phenomenon occurs in which the liquid surface of silicon vibrates, and in a severe case, there occurs a problem that the seed crystal does not adhere to the liquid surface. This solution level is urgently needed because the liquid level vibration significantly lowers the overall yield.
【0004】[0004]
【課題を解決するための手段】本発明者等は、この液面
振動の原因が石英ルツボとシリコンとの反応で発生する
SiOガスによるものであることをつきとめ、評価方法を
確立し、液面振動が実用上問題なくなるまで小さくなる
ルツボを発明した。The inventors of the present invention have found that the cause of the liquid level vibration is a reaction between a quartz crucible and silicon.
We have determined that this is due to SiO gas, established an evaluation method, and invented a crucible that reduces liquid level vibration until practically no problem occurs.
【0005】[0005]
【発明の実施の形態】本発明によれば、切断されたルツ
ボの試料の上にシリコンを0.125gから0.130gを乗せ、Ar
ガス中、1500℃、常圧で30分保持し、発生したSiO2べー
パーを除去したのちの減量が0.013g以下であれば液面振
動が少ないことを特徴とする石英ガラスルツボが提供さ
れる。本発明者らは信州大学の干川教授と共同でドロッ
プ法による酸素溶解量の測定を行っていた。(第58回応
物学会 2aT/I-8)この方法によれば、簡単に石英ガラ
スの溶解量を求めることが可能である。本発明者らはそ
れとは別に、合成ルツボの液面振動による問題に苦慮し
ていた。この原因を解析していくうちに、石英ルツボと
シリコン融液との界面から発生するガスに注目した。本
発明者らはこの二つを結び付け、液面振動の評価および
それにより液面振動の少ないルツボを発明したものであ
る。シリコンインゴットを引き上げるには石英ルツボに
ポリシリコンを投入し、1500℃から1600℃まで温度を上
げて溶解する。溶解時間を短くするために最近はますま
す高温化の傾向にある。このとき石英ガラスとシリコン
は次のような反応をしている。 SiO2 + Si→2SiO(gas)
SiOはガスであるため、シリコンの上部より蒸発し
てゆくのであるが、このときのガス量が液面振動に影響
しているのである。このガス量の石英ルツボによる差は
ドロップ法によって、簡単に知ることが可能である。ま
ず切断されたルツボの試料の上にシリコンを0.125gから
0.130gを乗せ、Arガス中、1500℃、常圧で30分保持し、
発生したSiO2べーパーを除去したのちの減量を測定す
る。この値は実際のシリコン引き上げ時の石英ルツボよ
りかなり大きな値となる。これは、接触面積が蒸発面積
に比較して小さいからである。しかしながらこの値を実
際に液面振動のあったルツボとなかったルツボで求めた
ところ、0.013g以下の減量の場合、液面振動が発生しな
いことがわかった。According to the present invention, 0.125 g to 0.130 g of silicon is placed on a cut crucible sample, and Ar
Provided is a quartz glass crucible characterized by having low liquid level vibration when kept in a gas at 1500 ° C. and normal pressure for 30 minutes, and the weight loss after removing generated SiO 2 vapor is 0.013 g or less. The present inventors have measured the amount of dissolved oxygen by the drop method in cooperation with Prof. Hirakawa of Shinshu University. According to this method, the amount of quartz glass dissolved can be easily obtained. The present inventors separately struggled with the problem due to liquid level vibration of the synthetic crucible. While analyzing the cause, we focused on the gas generated from the interface between the quartz crucible and the silicon melt. The present inventors have linked the two, and have invented a crucible with less liquid surface vibration evaluation and liquid surface vibration. To raise the silicon ingot, add polysilicon to the quartz crucible and raise the temperature from 1500 ° C to 1600 ° C to dissolve it. Recently, there is a tendency to increase the temperature in order to shorten the dissolution time. At this time, quartz glass and silicon are reacting as follows. SiO2 + Si → 2SiO (gas)
Since SiO is a gas, it evaporates from the upper part of silicon, and the amount of gas at this time affects the liquid surface vibration. The difference in the gas amount due to the quartz crucible can be easily known by the drop method. First, put 0.125 g of silicon on the cut crucible sample
0.130g, put in Ar gas, 1500 ℃, hold at normal pressure for 30 minutes,
The weight loss after removing the generated SiO2 vapor is measured. This value is much larger than the actual quartz crucible at the time of pulling up silicon. This is because the contact area is smaller than the evaporation area. However, when this value was obtained for a crucible having a liquid level vibration and a crucible not having the liquid level vibration, it was found that when the weight was reduced to 0.013 g or less, the liquid level vibration did not occur.
【0006】[0006]
【実施例】以下本発明の実施例と比較例を示す。 実施例1 22"合成石英ルツボを常法にてOH含有量の異なるルツボ8
個を作製した。これを6mm×6mmに切断し、HF洗浄したあ
と乾燥して重量を測定した。この試料を石英板の上に置
き、0.13gのポリシリコンをのせた。この炉の中をアル
ゴンで置換し、1500℃まで2時間で昇温し、30分保持し
たのち電源を切り、自然冷却した。試料をとりだし、超
音波洗浄器で付着したSiO2を除去し、乾燥後、重量を測
定した。その結果を表1に示す。またこのルツボにポリ
シリコンを120kg投入し、20torrに保持した後溶解し、
液面振動の有無を調べた。この結果も表1に示す。表 1 EXAMPLES Examples of the present invention and comparative examples are shown below. Example 1 A 22 "synthetic quartz crucible was crucible 8 having a different OH content by a conventional method.
Individual pieces were produced. This was cut into 6 mm x 6 mm, washed with HF, dried and weighed. This sample was placed on a quartz plate, and 0.13 g of polysilicon was placed thereon. The inside of this furnace was replaced with argon, the temperature was raised to 1500 ° C. in 2 hours, and after maintaining for 30 minutes, the power was turned off and the product was naturally cooled. The sample was taken out, the attached SiO2 was removed with an ultrasonic cleaner, dried, and weighed. The results are shown in Table 1. Also put 120kg of polysilicon into this crucible, dissolve after holding at 20torr,
The presence or absence of liquid level vibration was examined. The results are also shown in Table 1. table 1
【0007】[0007]
【発明の効果】本発明は液面振動が少なく、実用上使用
でき得る石英ルツボを提供できるものである。According to the present invention, there is provided a quartz crucible which can be practically used with little liquid surface vibration.
Claims (1)
を0.125gから0.130gを乗せ、Arガス中、1500℃、常圧で
30分保持し、発生したSiO2べーパーを除去したのちの減
量が0.013g以下であることを特徴とした液面振動が少な
い半導体シリコン引上げ用ルツボ1. Place 0.125 g to 0.130 g of silicon on a cut crucible sample, and in Ar gas at 1500 ° C. and normal pressure.
A crucible for pulling up semiconductor silicon with low liquid surface vibration, characterized in that the weight loss after removing the generated SiO2 vapor for 30 minutes is 0.013g or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000350504A JP2002154894A (en) | 2000-11-17 | 2000-11-17 | Crucible for pulling semiconductor silicon, almost free from vibration at liquid surface |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000350504A JP2002154894A (en) | 2000-11-17 | 2000-11-17 | Crucible for pulling semiconductor silicon, almost free from vibration at liquid surface |
Publications (1)
Publication Number | Publication Date |
---|---|
JP2002154894A true JP2002154894A (en) | 2002-05-28 |
Family
ID=18823720
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000350504A Pending JP2002154894A (en) | 2000-11-17 | 2000-11-17 | Crucible for pulling semiconductor silicon, almost free from vibration at liquid surface |
Country Status (1)
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JP (1) | JP2002154894A (en) |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1413652A1 (en) * | 2002-10-22 | 2004-04-28 | Japan Super Quartz Corporation | Evaluation process of reactivity of silicia glass with silicon melt and vibration at its surface, and silicia glass crucible not causing the surface vibration |
EP2141266A2 (en) | 2008-06-30 | 2010-01-06 | Japan Super Quartz Corporation | Silica glass crucible and method of pulling silicon single crystal with silica glass crucible |
WO2011019012A1 (en) | 2009-08-12 | 2011-02-17 | ジャパンスーパークォーツ株式会社 | Production device for silica glass crucible and production method for silica glass crucible |
EP2305611A2 (en) | 2009-10-02 | 2011-04-06 | Japan Super Quartz Corporation | Apparatus and method for manufacturing vitreous silica crucible |
EP2460912A2 (en) | 2010-12-01 | 2012-06-06 | Japan Super Quartz Corporation | Vitreous silica crucible |
EP2471754A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471752A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471753A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471755A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471751A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method and apparatus for manufacturing vitreous silica crucible |
-
2000
- 2000-11-17 JP JP2000350504A patent/JP2002154894A/en active Pending
Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1413652A1 (en) * | 2002-10-22 | 2004-04-28 | Japan Super Quartz Corporation | Evaluation process of reactivity of silicia glass with silicon melt and vibration at its surface, and silicia glass crucible not causing the surface vibration |
CN1316074C (en) * | 2002-10-22 | 2007-05-16 | 日本超精石英株式会社 | Evaluation technology of reactivity of quartz glass and fused silicon and vibration of fused silicon surface |
KR101064923B1 (en) * | 2002-10-22 | 2011-09-16 | 재팬수퍼쿼츠 가부시키가이샤 | Evaluation process of reactivity of silica glass with silicon melt and vibration at its surface, and silica glass crucible not causing the surface vibration |
EP2141266A2 (en) | 2008-06-30 | 2010-01-06 | Japan Super Quartz Corporation | Silica glass crucible and method of pulling silicon single crystal with silica glass crucible |
WO2011019012A1 (en) | 2009-08-12 | 2011-02-17 | ジャパンスーパークォーツ株式会社 | Production device for silica glass crucible and production method for silica glass crucible |
US8739573B2 (en) | 2009-08-12 | 2014-06-03 | Japan Super Quartz Corporation | Apparatus and method for manufacturing vitreous silica crucible |
EP2305611A2 (en) | 2009-10-02 | 2011-04-06 | Japan Super Quartz Corporation | Apparatus and method for manufacturing vitreous silica crucible |
US8844321B2 (en) | 2009-10-02 | 2014-09-30 | Japan Super Quartz Corporation | Apparatus and method for manufacturing vitreous silica crucible |
EP2460912A2 (en) | 2010-12-01 | 2012-06-06 | Japan Super Quartz Corporation | Vitreous silica crucible |
US9347148B2 (en) | 2010-12-01 | 2016-05-24 | Sumco Corporation | Vitreous silica crucible with specific ratio of transparent layer and bubble-containing layer thicknesses |
EP2471755A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471751A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method and apparatus for manufacturing vitreous silica crucible |
US8689584B2 (en) | 2010-12-31 | 2014-04-08 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
US8726692B2 (en) | 2010-12-31 | 2014-05-20 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471753A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
US8806892B2 (en) | 2010-12-31 | 2014-08-19 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
EP2471752A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
US9085480B2 (en) | 2010-12-31 | 2015-07-21 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
US9181121B2 (en) | 2010-12-31 | 2015-11-10 | Sumco Corporation | Method for manufacturing vitreous silica crucible |
EP2471754A2 (en) | 2010-12-31 | 2012-07-04 | Japan Super Quartz Corporation | Method of manufacturing vitreous silica crucible |
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