JP2002326889A - Crucible of quartz glass for pulling silicon single crystal - Google Patents
Crucible of quartz glass for pulling silicon single crystalInfo
- Publication number
- JP2002326889A JP2002326889A JP2001131716A JP2001131716A JP2002326889A JP 2002326889 A JP2002326889 A JP 2002326889A JP 2001131716 A JP2001131716 A JP 2001131716A JP 2001131716 A JP2001131716 A JP 2001131716A JP 2002326889 A JP2002326889 A JP 2002326889A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- glass crucible
- single crystal
- crucible
- pulling
- 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
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、シリコン単結晶引
上げ用石英ガラスルツボに係わり、特に石英ガラスルツ
ボの壁体の厚さをルツボの全域に亘って均一にするとと
もに、その部位により透明層の厚さを変えるシリコン単
結晶引上げ用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 a silicon single crystal, and more particularly, to making the wall thickness of the quartz glass crucible uniform over the entire area of the crucible and, at that portion, forming a transparent layer. The present invention relates to a quartz glass crucible for pulling a silicon single crystal having a variable thickness.
【０００２】[0002]
【従来の技術】半導体デバイスの基板に用いられるシリ
コン単結晶は、一般にチョクラルスキー法（ＣＺ法）で
製造されており、このＣＺ法は石英ガラスルツボ内に多
結晶シリコン原料を装填し、装填されたシリコン原料を
周囲から加熱して溶融し、上方から吊り下げられた種結
晶をシリコン融液に接触して引き上げられるものであ
る。2. Description of the Related Art A silicon single crystal used for a substrate of a semiconductor device is generally manufactured by a Czochralski method (CZ method). In the CZ method, a polycrystalline silicon raw material is loaded into a quartz glass crucible and loaded. The melted silicon raw material is heated and melted from the surroundings, and the seed crystal suspended from above is brought into contact with the silicon melt and pulled up.
【０００３】従来ＣＺ法用石英ガラスルツボとして、図
５に示すように、石英ガラスルツボ４１の内側の透明層
４２の厚さが、ルツボの全域に亘って均一であり、この
透明層４２の外周側にさまざまな厚さで形成された不透
明層４３とからなっている。As a conventional quartz glass crucible for the CZ method, as shown in FIG. 5, the thickness of a transparent layer 42 inside a quartz glass crucible 41 is uniform over the entire area of the crucible. The opaque layer 43 has various thicknesses on its side.
【０００４】不透明層４３には、直径１０〜２５０μｍ
の気泡が６００００〜９００００個／ｃｍ３程度存在す
るので、見掛上不透明となっており、この不透明層４３
はルツボ外周に配置されたヒータからの熱を石英ガラス
ルツボ４１中のシリコン融液に均一に伝達する役目をは
たす。石英ガラスルツボ４１の外周側に気泡が存在して
も引上げには影響を与えず、むしろ加熱時の保温効果を
得るには熱放射の少ない不透明層４３が適しており、ま
た不透明層４３は透明層４２よりも熱を拡散して伝える
ために均一な温度分布が得られる利点がある。The opaque layer 43 has a diameter of 10 to 250 μm.
Are present at about 60,000 to 90,000 cells / cm 3 , and are apparently opaque.
Serves to uniformly transfer heat from a heater disposed on the outer periphery of the crucible to the silicon melt in the quartz glass crucible 41. The presence of air bubbles on the outer peripheral side of the quartz glass crucible 41 does not affect the pulling up. Rather, an opaque layer 43 with less heat radiation is suitable for obtaining a heat retaining effect during heating, and the opaque layer 43 is transparent. There is an advantage that a uniform temperature distribution can be obtained because the heat is diffused and transmitted as compared with the layer 42.
【０００５】従来の多くの石英ガラスルツボ４１は、直
線部で形成される周壁部４１ｓあるいは曲線部で形成さ
れる湾曲部４１ｃの厚さが底部４１ｂなどに比べて厚く
なっている。[0005] In many conventional quartz glass crucibles 41, the peripheral wall portion 41s formed by a straight portion or the curved portion 41c formed by a curved portion is thicker than the bottom portion 41b and the like.
【０００６】従来の石英ガラスルツボ４１の周壁部４１
ｓは、その周壁部透明層４２ｓが周壁部不透明層４３ｓ
に比べて薄くなっており、近年のシリコン単結晶の大口
径化に伴う多結晶シリコンの大量装填、引上げの長時間
化により、石英ガラスルツボ４１の自重によって周壁部
４１ｓに変形が発生し、その結果、シリコン溶融の対流
に変化を与えて、単結晶引上げに悪影響を与え、また、
湾曲部４１ｃの湾曲部不透明層４３ｃの気泡の膨張によ
る肉厚の変化も大きくなることにより、ルツボ内面形状
への影響も大きくなり、単結晶引上げに悪影響を与えて
いる。The peripheral wall portion 41 of the conventional quartz glass crucible 41
s is that the peripheral wall portion transparent layer 42s is the peripheral wall portion opaque layer 43s.
Due to the large load of polycrystalline silicon accompanying the recent increase in diameter of silicon single crystal and prolonged pulling, deformation of the peripheral wall portion 41 s occurs due to its own weight of the quartz glass crucible 41. As a result, it changes the convection of silicon melting, adversely affects single crystal pulling,
As the thickness of the curved portion opaque layer 43c of the curved portion 41c changes greatly due to the expansion of bubbles, the influence on the inner surface shape of the crucible also increases, which adversely affects the pulling of the single crystal.
【０００７】[0007]
【発明が解決しようとする課題】そこで、シリコン単結
晶引上げ時、ルツボの変形が少なく、シリコンの対流に
対して悪影響を与えることがなく、高単結晶化率（ＤＦ
率）を達成できる石英ガラスルツボが要望されていた。Therefore, when pulling a silicon single crystal, the crucible is less deformed, does not adversely affect the convection of silicon, and has a high single crystallization ratio (DF).
Rate), a quartz glass crucible capable of achieving the above ratio has been demanded.
【０００８】本発明は上述した事情を考慮してなされた
もので、シリコン単結晶引上げ時、ルツボの変形が少な
く、シリコン融液の対流に対して悪影響を与えることが
なく、高ＤＦ率を達成できる石英ガラスルツボを提供す
ることを目的とする。The present invention has been made in view of the above-mentioned circumstances, and has a small deformation of a crucible when pulling a silicon single crystal, and has a high DF ratio without adversely affecting the convection of a silicon melt. It is an object of the present invention to provide a quartz glass crucible that can be used.
【０００９】[0009]
【課題を解決するための手段】上記目的を達成するため
になされた本願請求項１の発明は、内側に実質的に気泡
を含有しない透明層とこの透明層の外側に気泡を含有す
る不透明層とを有する２層構造の石英ガラスルツボにお
いて、前記石英ガラスルツボの厚さは全域に亘って均一
であり、かつ、直線部で形成される周壁部における透明
層が、前記周壁部に連なり曲線部で形成される湾曲部の
透明層よりも厚く形成され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であることを要旨とし
ている。Means for Solving the Problems To achieve the above object, the invention of claim 1 of the present invention is directed to a transparent layer containing substantially no bubbles inside and an opaque layer containing bubbles outside the transparent layer. In the quartz glass crucible having a two-layer structure, the thickness of the quartz glass crucible is uniform over the entire area, and the transparent layer in the peripheral wall portion formed by the straight portion is connected to the peripheral wall portion and the curved portion is formed. The invention is characterized in that it is a quartz glass crucible for pulling a silicon single crystal, which is formed to be thicker than the transparent layer of the curved portion formed by the above.
【００１０】本願請求項２の発明では、上記湾曲部に連
なり曲線部もしくは直線部で形成される底部における透
明層が、前記湾曲部の透明層の厚さと同等であることを
特徴とする請求項１に記載の単結晶引上げ用石英ガラス
ルツボであることを要旨としている。[0010] In the second aspect of the present invention, the transparent layer at the bottom formed by the curved portion or the straight portion connected to the curved portion is equal in thickness to the transparent layer of the curved portion. The gist is a quartz glass crucible for pulling a single crystal according to 1.
【００１１】本願請求項３の発明では、上記石英ガラス
ルツボの厚さは、１１ｍｍ以下であることを特徴とする
請求項１または２に記載の単結晶引上げ用石英ガラスル
ツボであることを要旨としている。In the invention of claim 3 of the present application, the quartz glass crucible according to claim 1 or 2 is characterized in that the thickness of the quartz glass crucible is 11 mm or less. I have.
【００１２】本願請求項４の発明では、上記周壁部の透
明層の厚さは、周壁部の全体の厚さに対して４０〜７５
％であることを特徴とする請求項１ないし３のいずれか
１項に記載のシリコン単結晶引上げ用石英ガラスルツボ
であることを要旨としている。According to the invention of claim 4 of the present application, the thickness of the transparent layer of the peripheral wall is 40 to 75 with respect to the total thickness of the peripheral wall.
%. The gist of the invention is a quartz glass crucible for pulling a silicon single crystal according to any one of claims 1 to 3.
【００１３】本願請求項５の発明では、上記周壁部の不
透明層の気泡分布は、湾曲部の不透明層の気泡分布より
も大きいことを特徴とする請求項１ないし４のいずれか
１項に記載のシリコン単結晶引上げ用石英ガラスルツボ
であることを要旨としている。[0013] In the fifth aspect of the present invention, the bubble distribution of the opaque layer of the peripheral wall portion is larger than the bubble distribution of the opaque layer of the curved portion. It is a gist of a quartz glass crucible for pulling a silicon single crystal.
【００１４】本願請求項６の発明では、上記周壁部の不
透明層の気泡分布は、直径１０〜２５０μｍの気泡が８
００００〜１２００００個／ｃｍ３であることを特徴と
する請求項１ないし５のいずれか１項に記載のシリコン
単結晶引上げ用石英ガラスルツボであることを要旨とし
ている。According to the invention of claim 6 of the present application, the bubble distribution of the opaque layer on the peripheral wall portion is such that bubbles having a diameter of 10 to 250 μm are 8 bubbles.
The gist of the present invention is a quartz glass crucible for pulling a silicon single crystal according to any one of claims 1 to 5, wherein the number is 0000 to 120,000 / cm 3 .
【００１５】[0015]
【発明の実施の形態】以下、本発明に係わる石英ガラス
ルツボの実施の形態について添付図面を参照して説明す
る。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of a quartz glass crucible according to the present invention will be described below with reference to the accompanying drawings.
【００１６】図１は本発明に係わる石英ガラスルツボの
縦断面図であり、石英ガラスルツボ１は、石英ガラス製
でルツボ形状をなし、上部から直線部で形成される周壁
部１ｓと、この周壁部１ｓに連なり曲線部で形成される
湾曲部１ｃと、この湾曲部に連なる底部１ｂとで形成さ
れている。FIG. 1 is a longitudinal sectional view of a quartz glass crucible according to the present invention. The quartz glass crucible 1 is made of quartz glass, has a crucible shape, and has a peripheral wall portion 1s formed by a straight portion from the top and a peripheral wall portion 1s. It is formed by a curved portion 1c which is continuous with the portion 1s and is formed by a curved portion, and a bottom portion 1b which is continuous with the curved portion.
【００１７】さらに、石英ガラスルツボ１は、石英ガラ
スルツボ１の内側に形成され実質的に気泡を含有しない
透明層２と、この透明層２の外側に気泡を含有する不透
明層３を有する２層構造をなしている。Further, the quartz glass crucible 1 has a transparent layer 2 formed inside the quartz glass crucible 1 and containing substantially no air bubbles, and an opaque layer 3 containing air bubbles outside the transparent layer 2. It has a structure.
【００１８】石英ガラスルツボ１の厚さは、全域に亘っ
て均一であり、かつ、直線部で形成される周壁部１ｓに
おける周壁部透明層２ｓが、周壁部１ｓに連なり曲線部
で形成される湾曲部１ｃの湾曲部透明層２ｃよりも厚く
形成されることによって、シリコン単結晶引き上げ時に
おける石英ガラスルツボ１の特に周壁部１ｓの変形が少
なくなり、シリコン融液の対流に対して悪影響を与える
ことがなく、高ＤＦ率を達成できる。The thickness of the quartz glass crucible 1 is uniform over the entire area, and the peripheral wall portion transparent layer 2s in the peripheral wall portion 1s formed by a linear portion is connected to the peripheral wall portion 1s and formed by a curved portion. By forming the curved portion 1c to be thicker than the curved portion transparent layer 2c, deformation of the quartz glass crucible 1, particularly the peripheral wall portion 1s, during pulling of the silicon single crystal is reduced, which adversely affects the convection of the silicon melt. And a high DF ratio can be achieved.
【００１９】さらに、底部１ｂの底部透明層２ｂが、湾
曲部透明層２ｃの厚さと同等であることによって、シリ
コン単結晶引き上げ開始から早い段階で石英ガラスルツ
ボ１の特に底部１ｂにおけるカーボンルツボとの安定し
た密着性が得られ、これによって、シリコン融液により
安定した対流を与えることができる。Furthermore, since the bottom transparent layer 2b of the bottom 1b is equivalent to the thickness of the curved transparent layer 2c, the quartz glass crucible 1 and the carbon crucible at the bottom 1b of the quartz glass crucible 1 are early in the stage from the start of pulling the silicon single crystal. Stable adhesion is obtained, and thereby, a more stable convection can be given to the silicon melt.
【００２０】この場合、湾曲部透明層２ｃおよび底部透
明層２ｂの厚さは、周壁部透明層２ｓの厚さの４／５以
下に形成されていることが、上記効果をより確実にする
ために好ましい。In this case, the thickness of the curved portion transparent layer 2c and the bottom transparent layer 2b is formed to be 4/5 or less of the thickness of the peripheral wall portion transparent layer 2s. Preferred.
【００２１】石英ガラスルツボ１の厚さは、その全域に
亘って均一、例えば、１１ｍｍ以下であり、その厚さの
精度は±１ｍｍであるのが好ましく、±０．５ｍｍがよ
り好ましい。１１ｍｍを超えると石英ガラスルツボ１
（周壁部１ｓ）の自重によって単結晶引上げ時、変形す
る虞がある。The thickness of the quartz glass crucible 1 is uniform over the entire area, for example, 11 mm or less, and the accuracy of the thickness is preferably ± 1 mm, more preferably ± 0.5 mm. If it exceeds 11mm, quartz glass crucible 1
When the single crystal is pulled by the own weight of the (peripheral wall portion 1s), the single crystal may be deformed.
【００２２】石英ガラスルツボ１の周壁部１ｓは、その
周壁部透明層２ｓの厚さが、当該部分の全体の厚さに対
して４０〜７５％であるのが好ましく、より好ましく
は、５０〜７０％である。In the peripheral wall portion 1s of the quartz glass crucible 1, the thickness of the peripheral wall portion transparent layer 2s is preferably 40 to 75%, more preferably 50 to 75% of the total thickness of the portion. 70%.
【００２３】この周壁部透明層２ｓの厚さが４０％より
小さいと、従来の石英ガラスルツボのように、石英ガラ
スルツボの自重によって周壁部に変形が発生してしま
い、７０％を超えると、熱放射の少ない不透明層が薄く
なってしまい、加熱時の保温効果が低下してルツボ内温
度が低下し、また、透明層は不透明層よりも熱を拡散し
て熱を伝え難いるために均一な温度分布が得られなくな
る。If the thickness of the peripheral wall portion transparent layer 2s is less than 40%, the peripheral wall portion is deformed by the weight of the quartz glass crucible as in the conventional quartz glass crucible. The opaque layer, which emits less heat, becomes thinner, lowering the heat retention effect during heating, lowering the temperature inside the crucible.The transparent layer is more uniform than the opaque layer because it is more difficult to conduct heat by diffusing heat. Temperature distribution cannot be obtained.
【００２４】さらに、周壁部不透明層３ｓには、直径１
０〜２５０μｍの気泡が８００００〜１２０００個／ｃ
ｍ３含有されている。この周壁部不透明層３ｓの気泡の
含有数は、石英ガラスルツボ１の熱変形を防止するため
に、周壁部透明層２ｓは、後述の湾曲部１ｃの湾曲部透
明層２ｃに比べて厚くし、逆に周壁部不透明層３ｓは湾
曲部不透明層３ｃに比べて薄くするが、不透明層による
保温効果を低下させないために、湾曲部不透明層３ｃに
比べて含有気泡量を多くすることが好ましい。The opaque layer 3s has a diameter of 1 mm.
80,000 to 12,000 bubbles / c of 0 to 250 μm
m 3 . The number of bubbles contained in the peripheral wall portion opaque layer 3s is set such that the peripheral wall portion transparent layer 2s is thicker than a curved portion transparent layer 2c of a curved portion 1c described later in order to prevent thermal deformation of the quartz glass crucible 1. Conversely, the peripheral wall portion opaque layer 3s is made thinner than the curved portion opaque layer 3c, but it is preferable to increase the amount of contained bubbles as compared with the curved portion opaque layer 3c so as not to lower the heat retaining effect of the opaque layer.
【００２５】気泡が８００００個／ｃｍ３より少ない
と、加熱時の保温効果が低下してルツボ内温度が低下し
てしまい、１２０００個／ｃｍ３を超えると、ヒータか
ら石英ガラスルツボへの熱透過量が減じられて、ルツボ
内温度の低下をきたして、単結晶引上げに支障をきた
し、また、気泡の膨れにより、肉厚の変化も大きくな
り、ルツボ内面形状への影響も大きくなって、単結晶引
上げに悪影響を与え易い。If the number of air bubbles is less than 80,000 / cm 3 , the heat retention effect during heating is reduced and the temperature in the crucible is reduced. If the number of air bubbles exceeds 12,000 / cm 3 , heat transmission from the heater to the quartz glass crucible is performed. As the amount is reduced, the temperature inside the crucible is lowered, which hinders the pulling of the single crystal.Also, due to the expansion of the bubbles, the change in wall thickness increases, and the influence on the crucible inner surface shape also increases. It tends to have an adverse effect on crystal pulling.
【００２６】湾曲部１ｃの厚さも、例えば、１１ｍｍ以
下であり、湾曲部１ｃの湾曲部透明層２ｃの厚さは３〜
５ｍｍであり、湾曲部不透明層３ｃには直径１０〜２５
０μｍの気泡が６００００〜９００００個／ｃｍ３含有
されている。The thickness of the curved portion 1c is, for example, 11 mm or less, and the thickness of the curved portion transparent layer 2c of the curved portion 1c is 3 to 3 mm.
5 mm, and the diameter of the curved portion opaque layer 3c is 10 to 25.
It contains 60,000 to 90000 bubbles / cm 3 of 0 μm.
【００２７】なお、底部１ｂも湾曲部１ｃと同様に、厚
さが１１ｍｍ以下であり、底部透明層２ｂの厚さは、湾
曲部不透明層３ｃと同等の３〜５ｍｍであり、底部不透
明層３ｂには直径１０〜２５０μｍの気泡が６００００
〜９００００個／ｃｍ３含有されている。The bottom 1b has a thickness of 11 mm or less, similarly to the curved portion 1c, and the thickness of the bottom transparent layer 2b is 3 to 5 mm, which is equivalent to the thickness of the curved portion opaque layer 3c. Contains 60,000 bubbles with a diameter of 10 to 250 μm.
９０90,000 particles / cm 3 .
【００２８】次に本発明に係わるシリコン単結晶引上げ
用石英ガラスルツボを用いたシリコン単結晶の引き上げ
方法について説明する。Next, a method for pulling a silicon single crystal using a quartz glass crucible for pulling a silicon single crystal according to the present invention will be described.
【００２９】図２に示すように、シリコン単結晶引上げ
装置１１には、図１に示すような本発明に係わる石英ガ
ラスルツボ１がカーボンルツボ４中に据付けられてお
り、シリコン単結晶１２を引き上げるには、ナゲット状
ポリシリコンを石英ガラスルツボ１に入れ、ヒータ１３
を付勢して、石英ガラスルツボ１を加熱し、さらに、石
英ガラスルツボ１を透過した熱によりポリシリコンを加
熱し、モータを付勢して、このモータに結合された回転
軸１４を回転させて石英ガラスルツボ１を回転させる。As shown in FIG. 2, in a silicon single crystal pulling apparatus 11, a quartz glass crucible 1 according to the present invention as shown in FIG. 1 is installed in a carbon crucible 4, and the silicon single crystal 12 is pulled up. , The nugget-shaped polysilicon is put into the quartz glass crucible 1 and the heater 13
To heat the quartz glass crucible 1, further heat the polysilicon by the heat transmitted through the quartz glass crucible 1, and urge the motor to rotate the rotating shaft 14 coupled to the motor. Then, the quartz glass crucible 1 is rotated.
【００３０】一定時間が経過しポリシリコンが溶融して
シリコン融液１５になった後、シード軸１６を下ろし、
種結晶１７をシリコン融液１５の液面に接触させ、シリ
コン単結晶１２を引き上げる。After a certain time has passed and the polysilicon has melted into a silicon melt 15, the seed shaft 16 is lowered,
The seed crystal 17 is brought into contact with the liquid surface of the silicon melt 15 to pull up the silicon single crystal 12.
【００３１】このシリコン単結晶引上げ工程において、
石英ガラスルツボ１は融点が１４１０℃のシリコンを溶
融するために、高温に加熱されるが、図１に示すよう
に、石英ガラスルツボ１の全体の厚さが、従来のものよ
りも薄く、均一であり、さらに、周壁部不透明層３ｓに
比べて粘性が大きく熱変形の小さい周壁部透明層２ｓが
厚いので、石英ガラスルツボ１の自重による変形を防止
できる。また、石英ガラスルツボ１の内側は、気泡を実
質的に内在しない透明層２によって形成されており、高
温下で気泡の膨脹によってルツボ内周面が剥離したり、
また気泡の混入によって単結晶化が乱される虞はない。In this silicon single crystal pulling step,
The quartz glass crucible 1 is heated to a high temperature in order to melt silicon having a melting point of 1410 ° C. As shown in FIG. 1, the entire thickness of the quartz glass crucible 1 is thinner and more uniform than the conventional one. Further, since the peripheral wall portion transparent layer 2s having a large viscosity and a small thermal deformation is thicker than the peripheral wall portion opaque layer 3s, the quartz glass crucible 1 can be prevented from being deformed by its own weight. Further, the inside of the quartz glass crucible 1 is formed by a transparent layer 2 having substantially no air bubbles therein, and the inner peripheral surface of the crucible is peeled off due to expansion of the air bubbles at a high temperature.
Further, there is no possibility that the single crystallization is disturbed by the inclusion of bubbles.
【００３２】なお、上記の気泡を実質的に内在しない透
明層とは、シリコン単結晶引き上げ前において、光学顕
微鏡レベルで気泡が確認されず、また、引き上げ後にお
いても、同レベルで気泡が数個程度しか確認できない透
明層を意味する。It should be noted that the above-mentioned transparent layer having substantially no air bubbles means that no air bubbles are observed at the level of an optical microscope before the silicon single crystal is pulled, and that several bubbles are still at the same level after the silicon single crystal is pulled. It means a transparent layer whose degree can be confirmed only.
【００３３】さらに、周壁部透明層２ｓを厚くすること
で周壁部不透明層３ｓの厚さは薄くなるが、周壁部不透
明層３ｓは湾曲部不透明層３ｃに比べて気泡含有量を多
くすること、周壁部不透明層３ｓにより保温効果を低下
させることもなく、ルツボ内温度を均一に保つことがで
き、単結晶引上げに悪影響を与えることがない。従っ
て、高ＤＦ率でシリコン単結晶を引き上げることができ
る。Further, by increasing the thickness of the peripheral wall portion transparent layer 2s, the thickness of the peripheral wall portion opaque layer 3s can be reduced. The temperature inside the crucible can be kept uniform without lowering the heat retaining effect by the peripheral wall portion opaque layer 3s, and the pulling of the single crystal is not adversely affected. Therefore, a silicon single crystal can be pulled at a high DF rate.
【００３４】さらに、本発明に係わ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について説明する。Further, a method of manufacturing a quartz glass crucible for pulling a silicon single crystal according to the present invention will be described.
【００３５】本発明に係わるシリコン単結晶引上げ用石
英ガラスルツボ１の製造は、図３に示すような石英ガラ
スルツボ製造装置２１を用いて行う。例えば、回転軸２
２を矢印の方向に回転させることによってルツボ成形用
型２３を所定の速度で回転させる。このルツボ成形用型
２３内に、原料供給ノズル２４で、上部から高純度のシ
リカ粉末を供給する。供給されたシリカ粉末は、遠心力
によってルツボ成形用型２３の内面部材２５側に押圧さ
れルツボ形状の成形体１ｐとして形成される。The quartz glass crucible 1 for pulling a silicon single crystal according to the present invention is manufactured using a quartz glass crucible manufacturing apparatus 21 as shown in FIG. For example, rotating shaft 2
By rotating 2 in the direction of the arrow, the crucible mold 23 is rotated at a predetermined speed. High-purity silica powder is supplied from above into the crucible-forming mold 23 by the raw material supply nozzle 24. The supplied silica powder is pressed against the inner surface member 25 side of the crucible-forming mold 23 by centrifugal force to form a crucible-shaped formed body 1p.
【００３６】その後、減圧機構２６の作動により内側部
材２５内を減圧し、さらに、不活性ガス供給管２７から
ヘリウムガスを一定量の割合で成形体１ｐの中空部に供
給する。ヘリウムガスの供給後、アーク電極２８に通
電、継続し、成形体１ｐの内側から加熱し、成形体１ｐ
の内表面に溶融層を形成する。所定時間経過後、石英ガ
ラスルツボの外側に気泡を多数含む不透明層を適切に形
成するために、減圧機構２６を調整してルツボ成形用型
２３内の減圧度合を調整させる。Thereafter, the inside of the inner member 25 is depressurized by the operation of the decompression mechanism 26, and helium gas is further supplied from the inert gas supply pipe 27 to the hollow portion of the molded body 1p at a constant rate. After the supply of the helium gas, the electric current is continuously applied to the arc electrode 28, and the arc electrode 28 is heated from the inside of the molded body 1p to form
To form a molten layer on the inner surface. After a lapse of a predetermined time, in order to appropriately form an opaque layer containing a large number of bubbles outside the quartz glass crucible, the pressure reducing mechanism 26 is adjusted to adjust the degree of reduced pressure in the crucible mold 23.
【００３７】減圧溶融を行うことにより、透明層中に残
存する気泡量を低減することができ、また、減圧度合の
調整によって、不透明層中の気泡量および気泡径を制御
することができる。The amount of bubbles remaining in the transparent layer can be reduced by melting under reduced pressure, and the amount and diameter of bubbles in the opaque layer can be controlled by adjusting the degree of reduced pressure.
【００３８】上記のようにして製造された溶融ルツボ１
ｑは、ほぼ所定の肉厚に成形されるが、より精度の高い
肉厚にするため、溶融ルツボ１ｑを研削する。The molten crucible 1 manufactured as described above
Although q is formed to a substantially predetermined thickness, the molten crucible 1q is ground in order to make the thickness more accurate.
【００３９】この研削は、図４に示すような一般的に用
いられるハンディタイプのベルトサンダー３１を用い
て、ダイヤモンド粒径が８０メッシュ（＃）以上の砥石
を用いた粗研削、ダイヤモンド粒径が３０００メッシュ
以上の砥石を用いた再研削の２段階で行われる。この研
削工程により、溶融ルツボ１ｑの厚さをその全域に亘っ
て均一にし、かつ、周壁部透明層を湾曲部透明層よりも
厚く整形することができる。なお、再研削工程後の内表
面の算術平均粗さ（Ｒａ）（ＪＩＳ Ｂ０６０１−１９
９４）は３μｍ以下に平坦化することが好ましい。In this grinding, using a generally used handy type belt sander 31 as shown in FIG. 4, rough grinding using a grindstone having a diamond particle size of 80 mesh (#) or more, It is performed in two stages of re-grinding using a grinding wheel of 3000 mesh or more. By this grinding step, the thickness of the molten crucible 1q can be made uniform over its entire area, and the peripheral wall portion transparent layer can be shaped thicker than the curved portion transparent layer. The arithmetic average roughness (Ra) of the inner surface after the re-grinding step (JIS B0601-19)
94) is preferably flattened to 3 μm or less.
【００４０】さらに、必要に応じて加熱処理を行うこと
により、内表面に目視できるような凹凸を残すことがな
くＲａを１μｍ以下にすることができ、また、引き上げ
られるシリコン単結晶に悪影響を与えることもなく、さ
らに、マイクロクラックダメージを残さないようにする
ことができる。Further, by performing a heat treatment as needed, Ra can be reduced to 1 μm or less without leaving any visible irregularities on the inner surface, and adversely affect the pulled silicon single crystal. Further, no micro crack damage can be left.
【００４１】[0041]
【実施例】図１に示すような本発明に係わるシリコン単
結晶引上げ用石英ガラスルツボを、表１に示すような厚
さの透明層および不透明層を形成し、これを用い、ＣＺ
法によりシリコン単結晶を引き上げ、ＤＦ（単結晶化）
率と使用後の石英ガラスルツボの状態を調べた。なお、
従来例は図５に示すような石英ガラスルツボを用いた。DESCRIPTION OF THE PREFERRED EMBODIMENTS A quartz glass crucible for pulling a silicon single crystal according to the present invention as shown in FIG.
DF (single crystallization)
The rate and the state of the quartz glass crucible after use were examined. In addition,
The conventional example used a quartz glass crucible as shown in FIG.
【００４２】[0042]
【表１】 [Table 1]
【００４３】結果：表２に示す。Results: shown in Table 2.
【００４４】[0044]
【表２】 [Table 2]
【００４５】実施例は使用後のルツボ内面形状に目立っ
たうねりは発生しておらず、耐熱変形性に優れているこ
とがわかり、また、ＤＦ率１００％となることがわかっ
た。In the examples, no noticeable undulation occurred in the inner surface shape of the crucible after use, and it was found that the crucible was excellent in heat deformation resistance and the DF ratio was 100%.
【００４６】[0046]
【発明の効果】本発明に係わるシリコン単結晶引上げ用
石英ガラスルツボによれば、シリコン単結晶引上げ時、
ルツボの変形が少なく、シリコンの対流に対して悪影響
を与えることがなく、高ＤＦ率を達成できる石英ガラス
ルツボを提供することができる。According to the quartz glass crucible for pulling a silicon single crystal according to the present invention, when pulling a silicon single crystal,
A quartz glass crucible capable of achieving a high DF ratio without causing deformation of the crucible and exerting an adverse effect on convection of silicon can be provided.
【００４７】すなわち、石英ガラスルツボの厚さは全域
に亘って均一であり、かつ、直線部で形成される周壁部
における透明層が、上記周壁部に連なり曲線部で形成さ
れる湾曲部の透明層よりも厚く形成されるシリコン単結
晶引上げ用石英ガラスルツボであるので、石英ガラスル
ツボの自重による変形を防止でき、単結晶引上げに悪影
響を与えることがなく高ＤＦ率でシリコン単結晶を引き
上げることができる。That is, the thickness of the quartz glass crucible is uniform over the entire area, and the transparent layer in the peripheral wall formed by the linear portion is connected to the transparent wall of the curved portion formed by the curved portion. Since it is a quartz glass crucible for pulling a silicon single crystal that is formed thicker than a layer, deformation of the quartz glass crucible due to its own weight can be prevented, and the silicon single crystal can be pulled at a high DF rate without adversely affecting the pulling of the single crystal. Can be.
【００４８】また、湾曲部に連なり曲線部もしくは直線
部で形成される底部における透明層が、上記湾曲部の透
明層の厚さと同等であるので、シリコン単結晶引き上げ
開始から早い段階で石英ガラスルツボの特に底部におけ
るカーボンルツボとの安定した密着性が得られ、これに
よって、シリコン融液により安定した対流を与えること
ができる。Further, since the transparent layer at the bottom formed by the curved portion or the straight portion connected to the curved portion is equivalent to the thickness of the transparent layer of the curved portion, a quartz glass crucible is provided at an early stage from the start of pulling the silicon single crystal. In particular, a stable adhesion with the carbon crucible at the bottom is obtained, and thereby a more stable convection can be given to the silicon melt.
【００４９】また、石英ガラスルツボの厚さは、１１ｍ
ｍ以下であるので、石英ガラスルツボの自重による変形
を防止でき、単結晶引上げに悪影響を与えることがなく
高ＤＦ率でシリコン単結晶を引き上げることができる。The thickness of the quartz glass crucible is 11 m.
m or less, deformation of the quartz glass crucible due to its own weight can be prevented, and the silicon single crystal can be pulled at a high DF rate without affecting the single crystal pulling.
【００５０】また、周壁部の透明層の厚さは、周壁部の
全体の厚さに対して４０〜７５％であるので、従来の石
英ガラスルツボのように、石英ガラスルツボの自重によ
って周壁部に変形が発生してしまうことがなく、また、
熱放射の少ない不透明層を過度に薄くしてしまうことが
なく、加熱時の保温効果が維持でき、ルツボ内を均一な
温度分布に保つことができる。Since the thickness of the transparent layer of the peripheral wall is 40 to 75% of the total thickness of the peripheral wall, the thickness of the peripheral wall is changed by the weight of the quartz glass crucible as in the conventional quartz glass crucible. Is not deformed, and
The opaque layer with little heat radiation is not excessively thinned, the heat retention effect at the time of heating can be maintained, and the crucible can be kept at a uniform temperature distribution.
【００５１】また、周壁部の不透明層の気泡分布は、湾
曲部の不透明層の気泡分布よりも大きいので、周壁部の
不透明層を湾曲部の不透明層に比べて薄くしても、不透
明層による保温効果の低下を防ぎ、ルツボ内温度を均一
に保つことができる。Since the bubble distribution of the opaque layer of the peripheral wall is larger than the bubble distribution of the opaque layer of the curved portion, even if the opaque layer of the peripheral wall is thinner than the opaque layer of the curved portion, the opaque layer does not. It is possible to prevent a decrease in the heat retaining effect and keep the temperature inside the crucible uniform.
【００５２】また、周壁部の不透明層の気泡分布は、直
径１０〜２５０μｍの気泡が８００００〜１２００００
個／ｃｍ３であるので、周壁部の透明層を湾曲部の透明
層に比べて厚くし、逆に周壁部の不透明層を湾曲部の不
透明層に比べて薄くしても、不透明層による保温効果の
低下を防ぎ、ルツボ内温度を均一に保つことができる。The bubble distribution of the opaque layer on the peripheral wall is such that bubbles having a diameter of 10 to 250 μm are 80,000 to 120,000.
Pcs / cm 3 , the opaque layer keeps the heat even when the transparent layer on the peripheral wall is made thicker than the transparent layer on the curved part and conversely, the opaque layer on the peripheral wall is thinner than the opaque layer on the curved part. The effect can be prevented from lowering, and the temperature in the crucible can be kept uniform.
【図１】本発明に係わるシリコン単結晶引上げ用石英ガ
ラスルツボの縦断面図。FIG. 1 is a longitudinal sectional view of a quartz glass crucible for pulling a silicon single crystal according to the present invention.
【図２】本発明に係わるシリコン単結晶引上げ用石英ガ
ラスルツボを用いたシリコン単結晶引上げ装置の概念
図。FIG. 2 is a conceptual diagram of a silicon single crystal pulling apparatus using a quartz glass crucible for pulling a silicon single crystal according to the present invention.
【図３】本発明に係わるシリコン単結晶引上げ用石英ガ
ラスルツボの製造装置を示す概念図。FIG. 3 is a conceptual diagram showing an apparatus for manufacturing a quartz glass crucible for pulling a silicon single crystal according to the present invention.
【図４】本発明に係わるシリコン単結晶引上げ用石英ガ
ラスルツボの製造装置に用いられるベルトサンダーの概
念図。FIG. 4 is a conceptual diagram of a belt sander used in the apparatus for manufacturing a quartz glass crucible for pulling a silicon single crystal according to the present invention.
【図５】従来のシリコン単結晶引上げ用石英ガラスルツ
ボの縦断面。FIG. 5 is a longitudinal section of a conventional quartz glass crucible for pulling a silicon single crystal.
１ 石英ガラスルツボ １ｂ 底部 １ｃ 湾曲部 １ｓ 周壁部 ２ 透明層 ２ｂ 底部透明層 ２ｃ 湾曲部透明層 ２ｓ 周壁部透明層 ３ 不透明層 ３ｂ 底部不透明層 ３ｃ 湾曲部不透明層 ３ｓ 周壁部不透明層 DESCRIPTION OF SYMBOLS 1 Quartz glass crucible 1b Bottom part 1c Curved part 1s Peripheral wall part 2 Transparent layer 2b Bottom transparent layer 2c Curved part transparent layer 2s Perimeter wall transparent layer 3 Opaque layer 3b Bottom opaque layer 3c Curved part opaque layer 3s Peripheral wall opaque layer
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G014 AH00 4G077 AA02 BA04 CF10 EG02 HA12 NC02 NC03 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G014 AH00 4G077 AA02 BA04 CF10 EG02 HA12 NC02 NC03
Claims (6)
とこの透明層の外側に気泡を含有する不透明層とを有す
る２層構造の石英ガラスルツボにおいて、前記石英ガラ
スルツボの厚さは全域に亘って均一であり、かつ、直線
部で形成される周壁部における透明層が、前記周壁部に
連なり曲線部で形成される湾曲部の透明層よりも厚く形
成され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。1. A quartz glass crucible having a two-layer structure having a transparent layer containing substantially no air bubbles inside and an opaque layer containing air bubbles outside the transparent layer, wherein the thickness of the quartz glass crucible is the whole. And the transparent layer in the peripheral wall portion formed by the straight portion is formed thicker than the transparent layer in the curved portion formed by the curved portion and connected to the peripheral wall portion. Quartz glass crucible for single crystal pulling.
部で形成される底部における透明層が、前記湾曲部の透
明層の厚さと同等であることを特徴とする請求項１に記
載の単結晶引上げ用石英ガラスルツボ。2. The single crystal according to claim 1, wherein the transparent layer at the bottom formed by the curved portion or the straight portion connected to the curved portion has the same thickness as the transparent layer of the curved portion. Quartz glass crucible for lifting.
ｍ以下であることを特徴とする請求項１または２に記載
の単結晶引上げ用石英ガラスルツボ。3. The quartz glass crucible has a thickness of 11 m.
The quartz glass crucible for pulling a single crystal according to claim 1 or 2, wherein m is not more than m.
全体の厚さに対して４０〜７５％であることを特徴とす
る請求項１ないし３のいずれか１項に記載のシリコン単
結晶引上げ用石英ガラスルツボ。4. The method according to claim 1, wherein the thickness of the transparent layer of the peripheral wall is 40 to 75% of the total thickness of the peripheral wall. Quartz glass crucible for pulling silicon single crystal.
曲部の不透明層の気泡分布よりも大きいことを特徴とす
る請求項１ないし４のいずれか１項に記載のシリコン単
結晶引上げ用石英ガラスルツボ。5. The silicon single crystal pulling-up device according to claim 1, wherein the bubble distribution of the opaque layer of the peripheral wall portion is larger than the bubble distribution of the opaque layer of the curved portion. Quartz glass crucible.
径１０〜２５０μｍの気泡が８００００〜１２００００
個／ｃｍ３であることを特徴とする請求項１ないし５の
いずれか１項に記載のシリコン単結晶引上げ用石英ガラ
スルツボ。6. The bubble distribution of the opaque layer on the peripheral wall portion is such that bubbles having a diameter of 10 to 250 μm are 80,000 to 120,000.
The quartz glass crucible for pulling a silicon single crystal according to any one of claims 1 to 5, characterized in that the number of pieces is / cm 3 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001131716A JP2002326889A (en) | 2001-04-27 | 2001-04-27 | Crucible of quartz glass for pulling silicon single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001131716A JP2002326889A (en) | 2001-04-27 | 2001-04-27 | Crucible of quartz glass for pulling silicon single crystal |
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| Publication Number | Publication Date |
|---|---|
| JP2002326889A true JP2002326889A (en) | 2002-11-12 |
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ID=18979854
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| Application Number | Title | Priority Date | Filing Date |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007000864A1 (en) * | 2005-06-29 | 2007-01-04 | Shin-Etsu Handotai Co., Ltd. | Quartz glass crucible for pulling up of silicon single crystal and process for producing the quartz glass crucible |
| US20090293806A1 (en) * | 2008-05-28 | 2009-12-03 | Japan Super Quartz Corporation | Silica glass crucible and method for manufacturing the same |
| US20100162943A1 (en) * | 2008-06-30 | 2010-07-01 | Japan Super Quartz Corporation | Silica glass crucible and method of pulling silicon single cyrsal with silica glass crucible |
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