JP3026088B2 - Quartz crucible for pulling silicon single crystal - Google Patents
Quartz crucible for pulling silicon single crystalInfo
- Publication number
- JP3026088B2 JP3026088B2 JP1221571A JP22157189A JP3026088B2 JP 3026088 B2 JP3026088 B2 JP 3026088B2 JP 1221571 A JP1221571 A JP 1221571A JP 22157189 A JP22157189 A JP 22157189A JP 3026088 B2 JP3026088 B2 JP 3026088B2
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- JP
- Japan
- Prior art keywords
- quartz crucible
- bubbles
- bubble content
- crucible
- quartz
- 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.)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は多結晶シリコンを溶融して単結晶シリコンを
製造する際に用いられる石英ルツボに関する。より具体
的には、単結晶シリコン製造の際の単結晶歩留りの良い
石英ルツボに関する。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a quartz crucible used for producing polycrystalline silicon by melting polycrystalline silicon. More specifically, the present invention relates to a quartz crucible having a good single crystal yield when manufacturing single crystal silicon.
半導体用シリコン単結晶の製造においては、多結晶シ
リコンを溶融する石英ルツボの品質が引上げられる単結
晶シリコンの単結晶化歩留りに大きな影響を与える。特
に、石英ルツボ内表面近傍に気泡が含まれる場合、単結
晶引上げ時の加熱により気泡が膨張し、このため石英ル
ツボ内表面から石英片が剥離して溶融シリコン中に混入
し、単結晶化を妨げる原因となる。従って、内表面近傍
に出来るだけ気泡を含まない高品質の石英ルツボが必要
とされる。In the production of silicon single crystals for semiconductors, the quality of a quartz crucible that melts polycrystalline silicon has a great influence on the yield of single crystal silicon to be crystallized. In particular, when bubbles are contained near the inner surface of the quartz crucible, the bubbles expand due to heating during the pulling of the single crystal, and the quartz pieces peel off from the inner surface of the quartz crucible and mix into the molten silicon, thereby causing single crystallization. It can be a hindrance. Therefore, a high-quality quartz crucible containing bubbles as little as possible near the inner surface is required.
従来から気泡を含まない石英ルツボが工夫されてきた
が、現在の製造方法の主流である回転モールド法でルツ
ボを製造する場合、モールド内表面に堆積した石英粉を
加熱溶融してガラス化する方法であるため、粉体の間に
含まれる内部気泡を除去するのが難しく、気泡を吸引除
去する減圧方法に工夫が施されている。また、この製造
時に、溶融した石英が揮発して器壁上部に付着し、これ
が析出してルツボ表面に落下し、この時に気泡を巻き込
み、石英ルツボ内表面に微小な気泡が生ずる場合があ
る。Conventionally, quartz crucibles that do not contain air bubbles have been devised, but in the case of producing crucibles by the rotary molding method, which is the mainstream of the current production method, a method of heating and melting quartz powder deposited on the inner surface of the mold to vitrify it Therefore, it is difficult to remove the internal bubbles contained between the powders, and a decompression method for sucking and removing the bubbles has been devised. Further, at the time of this production, the fused quartz volatilizes and adheres to the upper portion of the vessel wall, which precipitates and falls on the surface of the crucible. At this time, bubbles are involved, and fine bubbles may be generated on the inner surface of the quartz crucible.
このように、従来から内表面近傍に出来るだけ気泡を
含まない石英ルツボが求められているが、石英ルツボの
内部気泡を完全に除去するのは極めて難しい。As described above, a quartz crucible containing as little bubbles as possible near the inner surface has been demanded, but it is extremely difficult to completely remove bubbles inside the quartz crucible.
本発明において、シリコン単結晶引上げの際の単結晶
化率を低下させる原因となる気泡について検討し、単結
晶化率に対する気泡の影響は、従来認識されているよう
な石英ルツボ全体の平均気泡含有率に他に、基準面積当
たりの最大気泡含有率およびその気泡の大きさも重要な
要因となることが見い出された。In the present invention, the bubbles that reduce the single crystallization rate when pulling a silicon single crystal are examined, and the influence of the bubbles on the single crystallization rate is determined by the average bubble content of the whole quartz crucible as conventionally recognized. In addition to the rate, the maximum bubble content per reference area and the size of the bubbles have also been found to be important factors.
本発明は上記知見に基づき、従来の石英ルツボ全体の
平均気泡含有率に代えて、基準面積当たりの最大気泡含
有率およびその気泡の平均径を特定することにより、単
結晶化率に優れた石英ルツボを提供するものである。The present invention is based on the above findings, and instead of the conventional average bubble content of the entire quartz crucible, specifies the maximum bubble content per reference area and the average diameter of the bubbles, thereby providing a quartz having an excellent single crystallization rate. It provides a crucible.
本発明は、以下の構成からなるシリコン単結晶引上げ
用石英ルツボに関する。The present invention relates to a quartz crucible for pulling a silicon single crystal having the following configuration.
（１）シリコン単結晶の引上げに用いられる石英ルツボ
であって、シリコン融液に接する内表面近傍に含有され
る気泡含有率Ｐが４〜6mm角の基準面積当たり0.1％以下
である石英ルツボ。(1) A quartz crucible used for pulling a silicon single crystal, wherein the bubble content P in the vicinity of the inner surface in contact with the silicon melt is 0.1% or less per 4 to 6 mm square reference area.
（２）シリコン単結晶の引上げに用いられる石英ルツボ
であって、シリコン融液に接する内表面近傍に含有され
る気泡含有率Ｐが４〜6mm角の基準面積当たり0.1〜0.5
％であり、気泡の平均径ｒが0.1〜0.3mmである石英ルツ
ボ。(2) A quartz crucible used for pulling a silicon single crystal, wherein the bubble content P contained in the vicinity of the inner surface in contact with the silicon melt is 0.1 to 0.5 per reference area of 4 to 6 mm square.
% And the average diameter r of the bubbles is 0.1 to 0.3 mm.
以下、本発明を実施例と共に詳細に説明する。 Hereinafter, the present invention will be described in detail with examples.
（Ｉ）気泡含有率 本発明において、気泡含有率Ｐとは、石英ルツボの一
定面積（W1）に含まれる気泡の占有面積（W2）割合をい
い、W2/W1×100（％）で表わされる。本発明の石英ルツ
ボは、シリコン融液と接する内表面近傍の気泡含有率を
特定したものである。ここで、ルツボの内表面近傍とは
ルツボ内表面を含み該内表面から一定深さの範囲であ
る。即ち、シリコン単結晶の引き上げの際、石英ルツボ
内表面はシリコン融液に接触して溶損するが、この溶損
する部分を云い、通常はルツボ内表面から0.7mm厚の範
囲である。(I) Bubble Content In the present invention, the bubble content P refers to a ratio of an occupied area (W2) of bubbles contained in a fixed area (W1) of a quartz crucible, and is represented by W2 / W1 × 100 (%). . The quartz crucible of the present invention specifies the bubble content near the inner surface in contact with the silicon melt. Here, the vicinity of the inner surface of the crucible is a range including the inner surface of the crucible and having a certain depth from the inner surface. That is, when the silicon single crystal is pulled up, the inner surface of the quartz crucible is melted by contact with the silicon melt, and this portion is eroded, and usually has a thickness of 0.7 mm from the inner surface of the crucible.
石英ルツボの内表面近傍に含まれる気泡は不均一に分
布している。ルツボ内壁の剥離等はそのうち気泡の最も
密集する部分で生じ易く、石英ルツボ全体の平均気泡含
有率が小さくても、局所的に気泡が偏在している石英ル
ツボが単結晶化率が低い。Bubbles contained near the inner surface of the quartz crucible are unevenly distributed. Separation of the inner wall of the crucible or the like is likely to occur at the most densely populated portion of the bubbles. Even if the average bubble content of the whole quartz crucible is small, the quartz crucible in which bubbles are locally distributed has a low single crystallization rate.
そこで本発明では、石英ルツボの内表面を一定面積ご
とに区画してこれを基準面積とし、この基準面積ごとに
上記気泡含有率Ｐを求め、この基準面積ごとの気泡含有
率Ｐによって石英ルツボを評価する。この基準面積の大
きさは、例えば、約16mm2（4mm角）〜36mm2（6mm角）が
適当であり、本発明では４〜6mm角の面積を基準面積と
する。従って、本発明の気泡含有率Ｐは微小面積を基準
としたものであり、石英ルツボの全体または広範囲な部
分を基準とした平均的な気泡含有率とは異なる。なお、
以下の説明において、便宜上、基準面積ごとの各々の気
泡含有率Ｐを単に気泡含有率Ｐと云う。Therefore, in the present invention, the inner surface of the quartz crucible is divided into fixed areas, and this is used as a reference area. The bubble content P is determined for each reference area, and the quartz crucible is determined by the bubble content P for each reference area. evaluate. An appropriate size of the reference area is, for example, about 16 mm 2 (4 mm square) to 36 mm 2 (6 mm square). In the present invention, the area of 4 to 6 mm square is used as the reference area. Therefore, the bubble content P of the present invention is based on the minute area, and is different from the average bubble content based on the whole or a wide range of the quartz crucible. In addition,
In the following description, each bubble content P for each reference area is simply referred to as a bubble content P for convenience.
因みに、各基準面積ごとに求めた気泡含有率Ｐの最も
高い値を最大気泡含有率Pmとするとき、最大気泡含有率
Pmが一定の限界値以下であれば各基準面積ごとの気泡含
有率は全てこの限界値以下であり、同様に最大気泡含有
率Pmが一定範囲内であれば各基準面積の気泡含有率Ｐが
この範囲を超えることはないので、便宜上、最大気泡含
有率Pmを利用して石英ルツボを評価することができる。
すなわち、本発明の石英ルツボは、上記最大気泡含有率
Pmが一定の限界値（0.1％）以下であるか、またはこの
限界値を超えるものでも、それが一定範囲内（0.1〜0.5
％）であって、かつ気泡の平均径ｒが一定範囲（0.1〜
0.3mm）の石英ルツボであると云うことができる。Incidentally, when the highest value of the bubble content P obtained for each reference area is defined as the maximum bubble content Pm, the maximum bubble content Pm
If Pm is below a certain limit value, the bubble content for each reference area is all below this limit value. Similarly, if the maximum bubble content Pm is within a certain range, the bubble content P for each reference area is Since it does not exceed this range, the quartz crucible can be evaluated using the maximum bubble content Pm for convenience.
That is, the quartz crucible of the present invention has the maximum bubble content
Even if Pm is below a certain limit value (0.1%) or exceeds this limit value, it is within a certain range (0.1 to 0.5%).
%) And the average diameter r of the bubbles is in a certain range (0.1 to 0.1%).
0.3 mm) quartz crucible.
（II）気泡含有率の範囲 （イ）本発明に係る石英ルツボの一つは、内表面近傍に
含有される気泡含有率Ｐが４〜6mm角の基準面積当た
り、0.1％以下、好ましくは0.05％以下のものである。(II) Range of bubble content (a) One of the quartz crucibles according to the present invention is such that the bubble content P contained in the vicinity of the inner surface is 0.1% or less, preferably 0.05%, per 4 to 6 mm square reference area. % Or less.
（ロ）本発明に係る他の石英ルツボは、内表面近傍に含
有される気泡含有率Ｐが４〜6mm角の基準面積当たり0.1
〜0.5％であり、気泡の平均径ｒが0.1〜0.3mmであるも
のである。(B) In another quartz crucible according to the present invention, the bubble content P contained in the vicinity of the inner surface is 0.1% per 4 to 6 mm square reference area.
0.5%, and the average diameter r of the bubbles is 0.1 to 0.3 mm.
気泡含有率Ｐが0.1％を超えると、気泡が微細な場
合、例えば、気泡の平均径ｒが0.1mm以下の場合、気泡
の個数が多くなり剥離箇所が増大する。従って、石英ル
ツボの基準面積当たりの気泡含有率は一般に0.1％以下
が適当である。When the bubble content P exceeds 0.1%, when the bubbles are fine, for example, when the average diameter r of the bubbles is 0.1 mm or less, the number of bubbles increases and the number of peeled portions increases. Accordingly, it is generally appropriate that the bubble content per reference area of the quartz crucible is 0.1% or less.
ただし、気泡の平均径が0.1〜0.3mmの範囲であれば、
気泡含有率Ｐが0.1％を超えても、0.1〜0.5％の範囲で
あれば適度なシリコン単結晶化率を達成できる。一般に
気泡含有率Ｐが0.1％を超えると、通常は気泡の膨張箇
所が増加してシリコン単結晶化率を低下させるが、気泡
含有率Ｐが0.5％以下であって気泡の平均径ｒが0.1〜0.
3mmである場合には、気泡含有率はやや高いものの相対
的に気泡の個数は少なく、従って、ルツボ内壁面の膨張
箇所は少ないので、適度なシリコン単結晶化率を達成で
きる。一方、気泡含有率Ｐが0.5％を超える場合には気
泡の大きさに拘わらず、ルツボ内壁面の剥離が著しく、
単結晶化率が低い、また、気泡含有率Ｐが0.1〜0.3％の
範囲でも気泡の平均径ｒが0.1mmより小さいと、相対的
に気泡の個数が多く、その熱膨張による壁面の剥離箇所
が増大する。また気泡の平均径ｒが0.3mmを上回ると概
ね気泡含有率が0.5％を越えることになる。However, if the average diameter of the bubbles is in the range of 0.1 to 0.3 mm,
Even if the bubble content P exceeds 0.1%, an appropriate silicon single crystallization rate can be achieved within the range of 0.1 to 0.5%. In general, when the bubble content P exceeds 0.1%, the number of expanded portions of the bubbles usually increases to lower the silicon single crystallization rate, but the bubble content P is 0.5% or less and the average diameter r of the bubbles is 0.1%. ~ 0.
In the case of 3 mm, although the bubble content is slightly high, the number of bubbles is relatively small, and therefore the expansion portion of the inner wall surface of the crucible is small, so that an appropriate silicon single crystallization rate can be achieved. On the other hand, when the bubble content P exceeds 0.5%, the inner wall surface of the crucible peels remarkably regardless of the size of the bubbles,
If the single crystallization ratio is low, and the bubble content P is in the range of 0.1 to 0.3% and the average diameter r of the bubbles is smaller than 0.1 mm, the number of bubbles is relatively large, and the portion of the wall surface peeled off due to the thermal expansion. Increase. If the average diameter r of the bubbles exceeds 0.3 mm, the bubble content will generally exceed 0.5%.
上記気泡の測定は、光学的検査手段を用いた非破壊検
査が好ましい。例えば、光学カメラをルツボ内表面に沿
って回転自在に設置し、ルツボ内表面上を走査させるこ
とにより内表面に接する気泡を検出できる。また、光学
カメラの焦点をルツボ壁の深さ方向に移動することによ
り、内表面から一定深さの範囲に含まれる気泡を検出で
きる（特願平01−221567号）。本発明の石英ルツボは、
例えばこのような検査手段を用い、石英ルツボの内表面
を４〜6mm各の基準面積ごとに区画して気泡含有率Ｐお
よび気泡の平均径を測定し、各基準面積についてこの気
泡含有率や気泡の平均径が本発明の基準に適するものを
選び出すことによって得ることができる。The measurement of the air bubbles is preferably a nondestructive inspection using an optical inspection means. For example, an optical camera is installed rotatably along the inner surface of the crucible, and by scanning over the inner surface of the crucible, bubbles in contact with the inner surface can be detected. Further, by moving the focal point of the optical camera in the depth direction of the crucible wall, it is possible to detect bubbles contained in a range of a certain depth from the inner surface (Japanese Patent Application No. 01-221567). The quartz crucible of the present invention
For example, using such an inspection means, the inner surface of the quartz crucible is sectioned for each reference area of 4 to 6 mm, and the bubble content P and the average diameter of the bubbles are measured. Can be obtained by selecting those having an average diameter suitable for the criteria of the present invention.
本発明の石英ルツボは、従来の石英ルツボに比べて、
シリコンの単結晶化歩留り（単結晶化率）が格段によ
い、実用上、石英ルツボのシリコン単結晶化率は70％以
上であることを求められるが、本発明の石英ルツボの単
結晶化率は75％以上であり、従来より高い単結晶化率を
示す。The quartz crucible of the present invention, compared to the conventional quartz crucible,
The silicon single crystallization yield (single crystallization ratio) of silicon is remarkably good. In practice, the silicon single crystallization ratio of a quartz crucible is required to be 70% or more, but the single crystallization ratio of the quartz crucible of the present invention is required. Is 75% or more, which indicates a higher single crystallization ratio than the conventional one.
なお、気泡含有率Ｐが0.1％を上回る石英ルツボは、
その部分を削り取り、削り痕を平滑に仕上げることによ
り気泡含有率Ｐを0.1％以下にすれば良品としてシリコ
ン単結晶の引上げに使用することができる。また、気泡
含有率Ｐが0.1〜0.5％の石英ルツボでも、気泡の平均径
ｒが0.1mm以上のものは良品として使用できるので、石
英ルツボの製品歩留まりが向上する。A quartz crucible having a bubble content P of more than 0.1% is
If the portion is scraped off and the scraping marks are finished smoothly so that the bubble content P is 0.1% or less, it can be used for pulling a silicon single crystal as a good product. Further, even with a quartz crucible having a bubble content P of 0.1 to 0.5%, a quartz crucible having an average bubble diameter r of 0.1 mm or more can be used as a non-defective product, thereby improving the product yield of the quartz crucible.
実施例１−２、比較例１ 石英粉をルツボ状のモールド内表面上に一定厚さに堆
積させ、アーク放電により該石英粉を加熱し、内表面を
溶融し同時に外周面から石英層内部の気泡を吸引除去し
ながら石英層の外側層を半溶融して焼結させ、最大気泡
含有率がおのおの0.02％、0.08％（ie.気泡含有率が各
々0.02％以下、0.08％以下）のシリコン単結晶引上げ用
石英ルツボを製造した。この石英ルツボを用いてシリコ
ン単結晶を引上げた。この単結晶化率を第１表に示した
（実施例1,2）。Example 1-2, Comparative Example 1 Quartz powder was deposited to a constant thickness on the crucible-shaped mold inner surface, the quartz powder was heated by arc discharge, the inner surface was melted, and at the same time the inner surface of the quartz layer was melted from the outer peripheral surface While the air bubbles are removed by suction, the outer layer of the quartz layer is semi-melted and sintered, and the maximum silicon content is 0.02% and 0.08% (ie. The air bubble content is 0.02% or less and 0.08% or less, respectively). A quartz crucible for crystal pulling was manufactured. Using this quartz crucible, a silicon single crystal was pulled. The single crystallization ratio is shown in Table 1 (Examples 1 and 2).
同様の方法により製造した最大気泡含有率が0.15％の
石英ルツボを用いて、そのシリコン単結晶化率を求め
た。この結果を併せて第１表に示した（比較例１）。な
お、実施例1,2および比較例１はいずれも気泡の平均径
ｒは0.1mm以下であり、基準面積は4mm2である。Using a quartz crucible having a maximum bubble content of 0.15% manufactured by the same method, the silicon single crystallization ratio was determined. The results are shown in Table 1 (Comparative Example 1). In Examples 1 and 2 and Comparative Example 1, the average diameter r of the bubbles was 0.1 mm or less, and the reference area was 4 mm 2 .
実施例３〜５、比較例２〜３ 上記実施例1,2と同様の製造方法により第２表に示す
最大気泡含有率と気泡の平均径を有する石英ルツボを製
造した。この石英ルツボを用いてシリコン単結晶を引上
げた。この単結晶化率を同表に示した。なお、各例の基
準面積は何れも4mm2である。 Examples 3 to 5 and Comparative Examples 2 to 3 Quartz crucibles having the maximum cell content and the average cell diameter shown in Table 2 were produced by the same production method as in Examples 1 and 2. Using this quartz crucible, a silicon single crystal was pulled. The single crystallization ratio is shown in the same table. The reference area in each example is 4 mm 2 .
フロントページの続き (56)参考文献 特開 平１−197382（ＪＰ，Ａ) 特開 昭63−222091（ＪＰ，Ａ) 特開 平１−197381（ＪＰ，Ａ) 特開 平１−148783（ＪＰ，Ａ)Continuation of the front page (56) References JP-A-1-197382 (JP, A) JP-A-63-222091 (JP, A) JP-A-1-197381 (JP, A) JP-A-1-148783 (JP) , A)
Claims (2)
ルツボであって、シリコン融液に接する内表面近傍に含
有される気泡含有率Ｐが４〜6mm角の基準面積当たり0.1
％以下である石英ルツボ。1. A quartz crucible used for pulling a silicon single crystal, wherein the bubble content P contained in the vicinity of an inner surface in contact with a silicon melt is 0.1 to 0.1% per reference area of 4 to 6 mm square.
% Or less.
ルツボであって、シリコン融液に接する内表面近傍に含
有される気泡含有率Ｐが４〜6mm角の基準面積当たり0.1
〜0.5％であり、気泡の平均径ｒが0.1〜0.3mmである石
英ルツボ。2. A quartz crucible used for pulling a silicon single crystal, wherein the bubble content P contained in the vicinity of the inner surface in contact with the silicon melt is 0.1 to 0.1% per 4 to 6 mm square reference area.
A quartz crucible having an average diameter r of bubbles of 0.1 to 0.3 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1221571A JP3026088B2 (en) | 1989-08-30 | 1989-08-30 | Quartz crucible for pulling silicon single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1221571A JP3026088B2 (en) | 1989-08-30 | 1989-08-30 | Quartz crucible for pulling silicon single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0388793A JPH0388793A (en) | 1991-04-15 |
| JP3026088B2 true JP3026088B2 (en) | 2000-03-27 |
Family
ID=16768822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1221571A Expired - Lifetime JP3026088B2 (en) | 1989-08-30 | 1989-08-30 | Quartz crucible for pulling silicon single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3026088B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3123155B2 (en) * | 1991-10-30 | 2001-01-09 | 信越半導体株式会社 | Single crystal pulling device |
| JP7024700B2 (en) * | 2018-12-19 | 2022-02-24 | 株式会社Sumco | Quartz glass crucible |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0788269B2 (en) * | 1987-03-10 | 1995-09-27 | 東芝セラミツクス株式会社 | Crucible for pulling silicon single crystal |
| JPH01148783A (en) * | 1987-12-03 | 1989-06-12 | Shin Etsu Handotai Co Ltd | Quartz crucible for pulling up single crystal |
| JPH0692276B2 (en) * | 1988-02-03 | 1994-11-16 | 三菱マテリアル株式会社 | Quartz crucible for pulling silicon single crystal |
| JP2602442B2 (en) * | 1988-02-03 | 1997-04-23 | 三菱マテリアル 株式会社 | Quartz crucible for pulling silicon single crystal |
-
1989
- 1989-08-30 JP JP1221571A patent/JP3026088B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0388793A (en) | 1991-04-15 |
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