JP4338990B2 - Silica glass crucible and silicon single crystal pulling method using the same - Google Patents
Silica glass crucible and silicon single crystal pulling method using the same Download PDFInfo
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【０００１】
【発明の属する技術分野】
本発明はシリコン単結晶の引き上げに用いる石英ガラスルツボであって、ルツボにチャージした溶融シリコンの湯面振動を抑制したルツボに関する。また、本発明はそのような石英ガラスルツボを用いたシリコン単結晶の引き上げ方法に関する。
【０００２】
【従来の技術】
シリコン単結晶の引き上げに用いる石英ガラスルツボは、従来、ルツボの機械的強度を高めるために外側部分に天然石英ガラスを用い、内側部分には不純物の混入を避けるために合成石英ガラスを用いたルツボが知られている（特開平３−４０９８９号）。しかし、従来の上記石英ルツボはシリコン単結晶引き上げ時に溶融シリコンの湯面振動が大きく、単結晶化率を高めるのが難しい。また、ルツボにチャージした溶融シリコンの液面レベルよりやや上側からルツボ底部に至る内壁部分を合成石英によって形成する一方、該合成石英層の上側からルツボ上端部に至る部分を天然石英によって形成したことを特徴とするシリコン単結晶引上げ用石英ルツボが知られている（特許第２９７３０５７）。この石英ルツボは高温加熱下の使用環境においてもルツボ上端が内傾せず、またルツボ上部の天然石英によって形成された部分はシリコン融液に接触しないので、シリコン融液に不純物が混入せず、高純度の単結晶シリコンを引き上げることができ、しかもルツボの変形による損失がないので、単結晶シリコンの製造コストを低減できる利点を有している。しかし、この石英ルツボでは溶融シリコンの湯面は合成石英ガラス部分に接触しているので、湯面振動については従来と変わらない。
【０００３】
一方、シリコン単結晶の一般的な引き上げ法（ＣＺ法）では、ルツボ高さの４０〜９０％の高さまでチャージした溶融シリコンの湯面に種結晶を付け、この種結晶を中心にして周囲に結晶化を拡げ（肩作り）た後に、胴体引き上げを行って棒状の単結晶を引き上げ、底部を整えてこの単結晶を取り出す。この引き上げの際に、溶融シリコンの湯面が周期的に振動する現象が見られる。湯面振動が発生すると種結晶を湯面に接合できなかったり、引き上げ中にシリコンが多結晶化するなどの問題を生じる。この原因として、引き上げ温度の上昇や雰囲気圧の低下などによって溶融シリコンと石英ガラスの反応が活発化し、ＳｉＯガスが発生することによって振動すると考えられている。
【０００４】
シリコン単結晶の引き上げ工程において、種付けと肩作りの引き上げ開始工程は溶融シリコンの湯面振動の影響を最も受けやすく、胴体引き上げ以降の工程は湯面振動の影響が比較的少ない。従って、引き上げ工程において溶融シリコンの湯面振動を生じないことが求められる。本発明は引き上げ開始湯面付近のルツボ内層を天然石英ガラスによって形成することによって溶融シリコンの湯面振動を効果的に抑制した石英ガラスルツボを提供する。また、本発明は、湯面振動を抑制することが可能なシリコン単結晶の引き上げ方法を提供する。
【０００５】
【課題を解決する手段】
本発明によれば以下の構成からなる石英ガラスルツボが提供される。
（１）シリコン単結晶の引き上げに用いる石英ガラスルツボであって、該ルツボ内の溶融シリコンの引き上げ開始湯面に対して、上記湯面から湯面下所定深さまでのルツボ内層が天然石英ガラスによって形成されており、この天然石英ガラス部分より下側のルツボ内層が合成石英ガラスによって形成されていることを特徴とする石英ガラスルツボ。
（２）上記湯面下の天然石英ガラスによって形成されたルツボ内層部分の表面積Ｓ２が、上記湯面下のルツボ内層全表面積Ｓ１に対して、１５〜４５％の面積比（S2/S1）を有する上記(1)の石英ガラスルツボ。
（３）上記湯面下の天然石英ガラスによって形成されたルツボ内層部分が該湯面下１０cm以上２０cm以下である上記(1)または(2)の石英ガラスルツボ。
（４）開口端から上記湯面下までのルツボ内層が天然石英ガラスによって形成されると共に該天然石英ガラス部分より下側のルツボ内層が合成石英ガラスによって形成されており、外層が天然石英ガラスによって形成されている上記(1)、(2)または(3)の石英ガラスルツボ。
（５）上記湯面から湯面下所定深さまでの天然石英ガラスによって形成されたルツボ内層部分の気泡含有率が０.００５〜０.１％であり、この天然石英ガラス部分よりも下側の合成石英ガラスによって形成されたルツボ内層部分の気泡含有率が天然石英ガラス部分と同等か若しくは小さい上記(1)〜(4)の何れかの石英ガラスルツボ。
【０００６】
【課題を解決する手段】
本発明によれば以下の構成からなる石英ガラスルツボが提供される。
（１）シリコン単結晶の引き上げに用いる石英ガラスルツボであって、ルツボ高さの４０〜９０％の高さにチャージした該ルツボ内の溶融シリコンの引き上げ開始湯面に対して、上記湯面となるルツボ開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内層が天然石英ガラスによって形成されており、この天然石英ガラス部分より下側のルツボ内層が合成石英ガラスによって形成されており、上記天然石英ガラスによって形成されたルツボ内層部分の表面積Ｓ２が、上記所定位置よりも下方のルツボ内層全表面積Ｓ１に対して、１５〜４５％の面積比（Ｓ２／Ｓ１）を有し、上記天然石英ガラスによって形成されたルツボ内層部分の気泡含有率が０．００５〜０．１％であり、この天然石英ガラス部分よりも下側の合成石英ガラスによって形成されたルツボ内層部分の気泡含有率が天然石英ガラス部分よりも小さく、上記帯状部分の下端がルツボ直胴部の下端よりも上方に位置することを特徴とする石英ガラスルツボ。
（２）口径２２インチ（５６ｃｍ）以上および深さ３５ｃｍ以上であり、上記湯面下の天然石英ガラスによって形成されたルツボ内層部分が該湯面下１０ｃｍ以上２０ｃｍ以下である上記（１）の石英ガラスルツボ。
（３）開口端から上記所定位置までのルツボ内層が天然石英ガラスによって形成されており、外層が天然石英ガラスによって形成されている上記（１）または（２）の石英ガラスルツボ。
また、本発明によれば以下に示すシリコン単結晶の引き上げ方法が提供される。
（４）石英ガラスルツボを用いたシリコン単結晶の引き上げ方法であって、上記石英ガラスルツボは、開口端よりも下方の所定位置から所定深さまでの帯状部分に相当するルツボ内層が天然石英ガラスによって形成されており、この天然石英ガラス部分より下側のルツボ内層が合成石英ガラスによって形成されており、上記天然石英ガラスによって形成されたルツボ内層の帯状部分の上端部を溶融シリコンの引き上げ開始湯面として上記シリコン単結晶の引き上げを行うことを特徴とするシリコン単結晶の引き上げ方法。
（５）上記所定位置よりも下方の天然石英ガラスによって形成されたルツボ内層部分の表面積Ｓ２が、上記所定位置よりも下方のルツボ内層全表面積Ｓ１に対して、１５〜４５％の面積比（Ｓ２／Ｓ１）を有する上記（４）のシリコン単結晶の引き上げ方法。
【０００７】
天然石英ガラスは合成石英ガラスよりも溶融シリコンの湯面振動に対する抑制効果が大きい。従って、溶融シリコンの湯面が接触するルツボ内周面に沿った帯状の部分を天然石英ガラスによって形成することにより、引き上げ開始時の溶融シリコンの湯面振動を効果的に抑制することができる。ただし、ルツボ内層において天然石英ガラス部分が多いと単結晶化率が低下するので、湯面下の天然石英ガラス部分の範囲は上記帯状部分の範囲に制限される。
【０００８】
上記ルツボ内層における天然石英ガラス部分と合成石英ガラス部分の割合は、溶融シリコンの引き上げ開始湯面Ｌから該湯面のやや下側まで延びた天然石英ガラス部分Ｈの表面積Ｓ２が、上記湯面下のルツボ内層全表面積Ｓ１に対して、１５〜４５％、好ましくは２０〜３０％の面積比（S2/S1）を有するものが良い。上記天然石英ガラス部分Ｈの面積Ｓ２がこれより小さいと、湯面下において相対的に合成石英ガラス部分が多くなるので溶融シリコンの湯面振動を抑制する効果が低下する。一方、上記天然石英ガラス部分Ｈの面積Ｓ２がこれより大きいと単結晶化率が低下するので好ましくない。
【０００９】
具体的な態様として、口径２２インチ以上および深さ３５cm以上（口径Wと深さDの比W/D=1〜2）の一般的な形状の石英ガラスルツボにおいては、溶融シリコンの引き上げ開始湯面Ｌに対し、この湯面Ｌから概ね湯面下１０cm以上〜２０cm以下までの範囲に相当する帯状のルツボ内層部分を天然石英ガラスによって形成すれば良い。
【００１０】
図１に示す本発明の石英ガラスルツボの一例は、溶融シリコン１４をチャージしたときの引き上げ開始湯面Ｌに対して、ルツボ１０の内層が開口端から上記湯面Ｌのやや下側までの部分Ｈが天然石英ガラス１１によって形成されているである。該天然石英ガラス部分１１より下側の部分Ｇが合成石英ガラス１２によって形成されており、外層が天然石英ガラス１３によって形成されている。なお、本発明の石英ガラスルツボは、溶融シリコンの引き上げ開始湯面Ｌに対して、該湯面付近の帯状部分のルツボ内層が天然石英ガラスによって形成されていれば良いので、図１に示すように、ルツボ開口端から湯面下に延びる範囲が天然石英ガラスによって形成されている構造に限らず、ルツボ開口端から上記湯面Ｌまでの範囲が合成石英ガラスによって形成され、湯面Ｌから所定深さまでの帯状部分Ｈが天然石英カラスによって形成されている構造でも良い。本発明は何れの構造も含む。
【００１１】
上記湯面下部分Ｈよりも下側の部分は溶融シリコンの液圧によってＳｉＯガスの発生が抑制されるので湯面振動に対する影響は少ない。従って、引き上げ開始時の湯面振動を抑制するには、上記湯面下部分Ｈを天然石英ガラスによって形成すれば良い。これより下側の部分Ｇは単結晶化率が低下しないように合成石英ガラスによって形成するのが好ましい。
【００１２】
本発明の上記石英ガラスルツボにおいて、ルツボ内層の天然石英ガラス部分および合成石英ガラス部分の層厚は１mm以上が好ましい。１mmまでの層厚部分はルツボに溶融シリコンをチャージしたときに概ね溶損する部分であり、従ってこの溶損される層厚以上であることが求められる。また、ルツボの機械的強度を高めるにはルツボ外層を天然石英ガラスによって形成すると良い。なお、天然石英ガラス部分および合成石英ガラス部分は、例えば、回転モールド法に基づき、所定部分におのおの天然石英粉または合成石英粉を用い、これを加熱溶融することによって形成することができる。
【００１３】
なお、シリコン単結晶引き上げに用いる石英ガラスルツボにおいて、溶融シリコンの湯面振動は一般にこの湯面に接触するルツボ内表面の気泡含有率によっても影響を受けることが見い出され、ルツボ内周面の上記湯面に接触する帯状部分の気泡含有率をこれより下側の部分よりもやや高く調整することによって、湯面振動を抑制する試みがなされている。この場合、天然石英ガラスは合成石英ガラスよりも湯面振動の抑制効果が高いので、上記帯状部分を天然石英ガラスによって形成する本発明の石英ガラスルツボは、ルツボ内層の全面を合成石英ガラスによって形成するルツボよりも上記帯状部分の気泡含有率の値を広く設定することができる。具体的には、ルツボ内表面の上記帯状部分を天然石英ガラスによって形成する本発明のルツボでは、この帯状部分およびその下側部分の気泡含有率は概ね０.１％以下、好ましくは０.０５％以下であれば良い。より好ましくは、上記帯状部分の気泡含有率が０.００５〜０.１％であって、この帯状部分より下側の合成石英ガラスの気泡含有率が上記帯状部分の気泡含有率と同等か小さいものが良い。
【００１４】
【発明の実施形態】
以下、本発明を実施例によって具体的に示す。
〔実施例１〕
溶融シリコンの引き上げ開始湯面に対して、この湯面下の天然石英ガラスによって形成されたルツボ内層部分Ｈの表面積Ｓ２が、上記湯面下のルツボ内層全表面積Ｓ１に対しておのおの１０〜５０％の面積比（S2/S1）を有する石英ガラスルツボについて、シリコン単結晶引き上げ試験を行った。この結果を表１に示した。面積比１０％のルツボは湯面振動が見られた。面積比２０％以上のルツボには湯面振動が見られなかったが、面積比５０％のルツボは単結晶化率が大幅に低下した。従って、上記天然石英ガラス部分の面積比は概ね１５〜４５％程度が適当であり、２０〜３０％が好ましい。
【００１５】
【表１】
〔実施例２〕
溶融シリコンの引き上げ開始湯面に対して、この湯面下の天然石英ガラスによって形成されたルツボ内層部分の湯面下の長さを表１のように調製した石英ガラスルツボ（口径２８インチ）について、シリコン単結晶引き上げ試験を行った。この結果を表２に示した。湯面下の天然石英ガラス部分の長さが５cmのルツボは湯面振動が見られた。この長さが１０cm以上のルツボは湯面振動が見られないが、湯面下の天然石英ガラス部分が３０cmのルツボは単結晶化率が大幅に低下した。従って、湯面下の天然石英ガラス部分の長さは１０cm〜２０cmが好ましい。
【００１７】
【表２】
【図面の簡単な説明】
【図１】 本発明に係る石英ガラスルツボの模式断面図
【符号の説明】
１０−石英ガラスルツボ、１１−天然石英ガラス、１２−合成石英ガラス、１３−天然石英ガラス、１４−溶融シリコン、Ｌ−湯面、Ｈ−湯面下の天然石英ガラス部分、Ｇ−Ｈ部分より下側の合成石英ガラス部分。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a silica glass crucible used for pulling up a silicon single crystal, and relates to a crucible that suppresses molten metal surface vibration of molten silicon charged in the crucible. The present invention also relates to a method for pulling a silicon single crystal using such a quartz glass crucible.
[0002]
[Prior art]
Silica glass crucibles used for pulling up silicon single crystals have conventionally used crucibles made of natural quartz glass on the outer part to increase the mechanical strength of the crucible and synthetic quartz glass to avoid contamination by impurities on the inner part. Is known (Japanese Patent Laid-Open No. 3-40989). However, the conventional quartz crucible has a large molten silicon surface vibration when the silicon single crystal is pulled, and it is difficult to increase the single crystallization rate. In addition, the inner wall portion from slightly above the liquid level of the molten silicon charged to the crucible to the bottom of the crucible is made of synthetic quartz, while the portion from the upper side of the synthetic quartz layer to the top of the crucible is made of natural quartz. A quartz crucible for pulling a silicon single crystal characterized by the above is known (Japanese Patent No. 2973057). This quartz crucible does not tilt inward at the top of the crucible even in a high temperature heating environment, and the portion formed by natural quartz at the top of the crucible does not come into contact with the silicon melt. Since high-purity single crystal silicon can be pulled and there is no loss due to crucible deformation, there is an advantage that the manufacturing cost of single crystal silicon can be reduced. However, in this quartz crucible, since the molten silicon melt surface is in contact with the synthetic quartz glass portion, the melt surface vibration is not different from the conventional one.
[0003]
On the other hand, in a general pulling method (CZ method) of a silicon single crystal, a seed crystal is attached to the molten silicon surface charged to a height of 40 to 90% of the height of the crucible, and the seed crystal is centered around the seed crystal. After expanding the crystallization (making a shoulder), the body is pulled up to pull up the rod-shaped single crystal, and the bottom is trimmed to take out this single crystal. During this pulling, a phenomenon that the molten silicon melt surface periodically vibrates is observed. When molten metal surface vibration occurs, problems such as failure to join the seed crystal to the molten metal surface and polycrystallization of silicon during pulling occur. As a cause of this, it is considered that the reaction between molten silicon and quartz glass is activated by raising the pulling temperature or lowering the atmospheric pressure, and vibrates when SiO gas is generated.
[0004]
In the silicon single crystal pulling process, the seeding and shouldering pulling start process is most easily affected by the molten silicon surface vibration, and the processes after the body pulling are relatively less affected by the surface vibration. Therefore, it is required that molten metal surface vibration does not occur in the pulling process. The present invention provides a quartz glass crucible in which molten metal surface vibration of molten silicon is effectively suppressed by forming the inner layer of the crucible in the vicinity of the starting surface of the pulling up with natural quartz glass. The present invention also provides a method for pulling up a silicon single crystal that can suppress molten metal surface vibration.
[0005]
[Means for solving the problems]
According to the present invention, a quartz glass crucible having the following configuration is provided.
(1) A quartz glass crucible used for pulling up a silicon single crystal, wherein a crucible inner layer from the molten metal surface to a predetermined depth below the molten metal surface is made of natural quartz glass with respect to a molten silicon start surface of molten silicon in the crucible. A quartz glass crucible which is formed and the inner layer of the crucible below the natural quartz glass portion is made of synthetic quartz glass.
(2) The surface area S2 of the crucible inner layer portion formed of natural quartz glass below the molten metal surface has an area ratio (S2 / S1) of 15 to 45% with respect to the total surface area S1 of the crucible inner layer below the molten metal surface. The quartz glass crucible of (1) above.
(3) The quartz glass crucible according to the above (1) or (2), wherein the crucible inner layer portion formed by natural quartz glass below the molten metal surface is 10 cm or more and 20 cm or less below the molten metal surface.
(4) The crucible inner layer from the open end to the lower surface of the molten metal is formed of natural quartz glass, the crucible inner layer below the natural quartz glass portion is formed of synthetic quartz glass, and the outer layer is formed of natural quartz glass. The quartz glass crucible as described in (1), (2) or (3) above.
(5) The bubble content of the inner layer portion of the crucible formed of natural quartz glass from the molten metal surface to a predetermined depth below the molten metal surface is 0.005 to 0.1%, which is lower than the natural quartz glass portion. The quartz glass crucible according to any one of the above (1) to (4), wherein the bubble content of the inner layer portion of the crucible formed of synthetic quartz glass is equal to or smaller than that of the natural quartz glass portion.
[0006]
[Means for solving the problems]
According to the present invention, a quartz glass crucible having the following configuration is provided.
(1) A quartz glass crucible used for pulling up a silicon single crystal, wherein the molten metal is charged to a height of 40 to 90% of the height of the crucible. A crucible inner layer corresponding to a band-like portion from a predetermined position below a crucible opening end to a predetermined depth is formed of natural quartz glass, and a crucible inner layer below the natural quartz glass portion is formed of synthetic quartz glass. And the surface area S2 of the crucible inner layer portion formed of the natural quartz glass has an area ratio (S2 / S1) of 15 to 45% with respect to the total surface area S1 of the crucible inner layer below the predetermined position. The bubble content of the inner layer portion of the crucible formed by the natural quartz glass is 0.005 to 0.1%, and the lower portion of the natural quartz glass portion Bubble content of the crucible inner layer portion formed of quartz glass is less than a natural quartz glass part, a quartz glass crucible lower end of the band portion, characterized in that located above the lower end of the crucible straight body portion.
(2) The quartz according to (1), which has a diameter of 22 inches (56 cm) or more and a depth of 35 cm or more, and a crucible inner layer portion formed by natural quartz glass below the molten metal surface is 10 cm or more and 20 cm or less below the molten metal surface. Glass crucible.
(3) The quartz glass crucible according to (1) or (2), wherein an inner layer of the crucible from the opening end to the predetermined position is made of natural quartz glass, and an outer layer is made of natural quartz glass.
Further, according to the present invention, the following method for pulling a silicon single crystal is provided.
(4) A method for pulling a silicon single crystal using a quartz glass crucible, wherein the quartz glass crucible is made of natural quartz glass with a crucible inner layer corresponding to a belt-like portion extending from a predetermined position below the opening end to a predetermined depth. The crucible inner layer below the natural quartz glass portion is formed of synthetic quartz glass, and the upper end of the belt-shaped portion of the crucible inner layer formed of the natural quartz glass is used to start pulling up molten silicon. A method for pulling a silicon single crystal, wherein the silicon single crystal is pulled.
(5) The area ratio S2 of the crucible inner layer portion formed by natural quartz glass below the predetermined position is 15 to 45% of the total surface area S1 of the crucible inner layer below the predetermined position (S2 (4) The method for pulling up a silicon single crystal according to (4) above
[0007]
Natural quartz glass has a greater effect of suppressing molten silicon surface vibration than synthetic quartz glass. Therefore, by forming a band-shaped portion along the inner peripheral surface of the crucible with which the molten silicon surface comes into contact with natural quartz glass, it is possible to effectively suppress the molten silicon surface vibration at the start of pulling. However, if there are many natural quartz glass portions in the inner layer of the crucible, the single crystallization rate decreases, so the range of the natural quartz glass portion below the molten metal surface is limited to the range of the band-shaped portion.
[0008]
The ratio of the natural quartz glass portion and the synthetic quartz glass portion in the crucible inner layer is such that the surface area S2 of the natural quartz glass portion H extending from the molten silicon start surface L to a slightly lower side of the molten metal surface is below the molten metal surface. The crucible inner layer has a total area S1 of 15 to 45%, preferably 20 to 30% (S2 / S1). When the area S2 of the natural quartz glass portion H is smaller than this, since the synthetic quartz glass portion relatively increases below the molten metal surface, the effect of suppressing molten metal surface vibration of the molten silicon is lowered. On the other hand, if the area S2 of the natural quartz glass portion H is larger than this, the single crystallization rate is lowered, which is not preferable.
[0009]
As a specific embodiment, in a quartz glass crucible having a general shape having a diameter of 22 inches or more and a depth of 35 cm or more (ratio W / D = 1 to 2 of the diameter W and depth D), For the surface L, a belt-like crucible inner layer portion corresponding to a range from the molten metal surface L to approximately 10 cm to 20 cm below the molten metal surface may be formed of natural quartz glass.
[0010]
An example of the silica glass crucible of the present invention shown in FIG. 1 is a portion where the inner layer of the
[0011]
Since the generation of SiO gas is suppressed by the liquid pressure of the molten silicon in the portion below the molten metal surface portion H, the influence on the molten metal surface vibration is small. Therefore, in order to suppress the molten metal surface vibration at the start of the pulling, the molten metal surface lower portion H may be formed of natural quartz glass. The lower portion G is preferably formed of synthetic quartz glass so that the single crystallization rate does not decrease.
[0012]
In the quartz glass crucible of the present invention, the layer thickness of the natural quartz glass portion and the synthetic quartz glass portion of the crucible inner layer is preferably 1 mm or more. The layer thickness portion up to 1 mm is a portion that is generally melted when the molten silicon is charged to the crucible, and is therefore required to be greater than or equal to the melted layer thickness. In order to increase the mechanical strength of the crucible, the outer layer of the crucible is preferably formed of natural quartz glass. The natural quartz glass portion and the synthetic quartz glass portion can be formed, for example, by using each natural quartz powder or synthetic quartz powder in a predetermined portion and heating and melting it based on a rotational mold method.
[0013]
In addition, in the quartz glass crucible used for pulling up the silicon single crystal, it has been found that the molten silicon surface vibration is generally affected by the bubble content of the inner surface of the crucible in contact with the molten metal surface. Attempts have been made to suppress molten metal surface vibration by adjusting the bubble content of the belt-shaped portion in contact with the molten metal surface to be slightly higher than the lower portion. In this case, natural quartz glass has a higher suppression effect on the molten metal surface surface than synthetic quartz glass. Therefore, the quartz glass crucible of the present invention in which the band-shaped portion is formed of natural quartz glass forms the entire inner surface of the crucible with synthetic quartz glass. The value of the bubble content of the band-like portion can be set wider than that of the crucible. Specifically, in the crucible of the present invention in which the above-described band-shaped portion on the inner surface of the crucible is formed of natural quartz glass, the bubble content in the band-shaped portion and the lower portion thereof is approximately 0.1% or less, preferably 0.05. % Or less. More preferably, the bubble content of the band-shaped portion is 0.005 to 0.1%, and the bubble content of the synthetic quartz glass below the band-shaped portion is equal to or smaller than the bubble content of the band-shaped portion. Things are good.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be specifically described by way of examples.
[Example 1]
The surface area S2 of the crucible inner layer portion H formed of natural quartz glass below the molten silicon surface is 10 to 50% of the total surface area S1 of the crucible inner layer below the molten metal surface with respect to the molten silicon starting surface of the molten silicon. A silica glass crucible having an area ratio of (S2 / S1) was subjected to a silicon single crystal pulling test. The results are shown in Table 1. The crucible with an area ratio of 10% showed hot water surface vibration. The crucible with an area ratio of 20% or more showed no molten metal surface vibration, but the crucible with an area ratio of 50% had a significantly reduced single crystallization rate. Therefore, the area ratio of the natural quartz glass portion is suitably about 15 to 45%, preferably 20 to 30%.
[0015]
[Table 1]
[Example 2]
About the quartz glass crucible (caliber 28 inches) prepared as shown in Table 1 below the length of the inner layer of the crucible inner layer formed by the natural quartz glass below the molten silicon surface. A silicon single crystal pulling test was conducted. The results are shown in Table 2. The crucible with the length of the natural quartz glass under the surface of the molten metal showed a vibration of the molten metal surface. The crucible with a length of 10 cm or more shows no molten metal vibration, but the crucible with the natural quartz glass portion under the molten metal of 30 cm has a significantly reduced single crystallization rate. Therefore, the length of the natural quartz glass portion under the hot water surface is preferably 10 cm to 20 cm.
[0017]
[Table 2]
[Brief description of the drawings]
FIG. 1 is a schematic cross-sectional view of a quartz glass crucible according to the present invention.
10-quartz glass crucible, 11-natural quartz glass, 12-synthetic quartz glass, 13-natural quartz glass, 14-molten silicon, L-hot water surface, H-natural quartz glass part below the hot water surface, GH part Lower synthetic quartz glass part.
Claims (5)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014167788A1 (en) | 2013-04-08 | 2014-10-16 | 信越石英株式会社 | Silica vessel for pulling up single crystal silicon and process for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100847500B1 (en) * | 2006-03-30 | 2008-07-22 | 코바렌트 마테리얼 가부시키가이샤 | Silica glass crucible |
| JP4798714B2 (en) * | 2007-03-28 | 2011-10-19 | コバレントマテリアル株式会社 | Silica glass crucible for pulling silicon single crystals |
| EP2385157B1 (en) * | 2009-12-11 | 2015-02-11 | Japan Super Quartz Corporation | Silica glass crucible |
| CN102583976B (en) * | 2012-02-07 | 2014-03-12 | 湖北菲利华石英玻璃股份有限公司 | Method for repairing quartz glass crucible defects through arc process |
| DE102012109181B4 (en) | 2012-09-27 | 2018-06-28 | Heraeus Quarzglas Gmbh & Co. Kg | Drawing a semiconductor single crystal according to the Czochralski method and suitable quartz glass crucible |
| CN108977879B (en) * | 2018-09-13 | 2021-02-26 | 浙江美晶新材料有限公司 | High-purity quartz crucible for single crystal and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014167788A1 (en) | 2013-04-08 | 2014-10-16 | 信越石英株式会社 | Silica vessel for pulling up single crystal silicon and process for producing same |
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