JP5901072B2 - Method for producing quartz glass crucible for pulling silicon single crystal - Google Patents
Method for producing quartz glass crucible for pulling silicon single crystal Download PDFInfo
- Publication number
- JP5901072B2 JP5901072B2 JP2012520388A JP2012520388A JP5901072B2 JP 5901072 B2 JP5901072 B2 JP 5901072B2 JP 2012520388 A JP2012520388 A JP 2012520388A JP 2012520388 A JP2012520388 A JP 2012520388A JP 5901072 B2 JP5901072 B2 JP 5901072B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- region
- rough surface
- single crystal
- belt
- 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.)
- Active
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 93
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 78
- 229910052710 silicon Inorganic materials 0.000 title claims description 78
- 239000010703 silicon Substances 0.000 title claims description 78
- 239000013078 crystal Substances 0.000 title claims description 65
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000007788 liquid Substances 0.000 claims description 47
- 239000000843 powder Substances 0.000 claims description 23
- 239000010453 quartz Substances 0.000 claims description 21
- 238000005422 blasting Methods 0.000 claims description 15
- 238000007788 roughening Methods 0.000 description 38
- 230000000873 masking effect Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 229920005591 polysilicon Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
Description
本発明は、シリコン単結晶の引き上げに使用される石英ガラスるつぼ及びその製造方法に関する。 The present invention relates to a quartz glass crucible used for pulling a silicon single crystal and a method for manufacturing the same.
従来、単結晶半導体材料のような単結晶物質の製造には、いわゆるチョクラルスキー法と呼ばれる方法が広く採用されている。この方法は多結晶シリコンを容器内で溶融させ、この溶融浴内に種結晶の端部を浸けて回転させながら引き上げるもので、種結晶上に同一の結晶方位を持つ単結晶が成長する。この単結晶引き上げ容器には石英ガラスるつぼが一般的に使用されている。 Conventionally, a so-called Czochralski method has been widely used for manufacturing a single crystal material such as a single crystal semiconductor material. In this method, polycrystalline silicon is melted in a container, and the end portion of the seed crystal is immersed in the molten bath and pulled up while rotating, so that a single crystal having the same crystal orientation grows on the seed crystal. A quartz glass crucible is generally used for the single crystal pulling container.
ポリシリコンを石英ガラスるつぼ中で溶かし、シリコン単結晶を引き上げる際、シリコンメルト表面に振動波面が発生し、シリコン種結晶がシリコンメルトに接合できなかったり、シリコン単結晶の結晶性が乱れる問題は、通常よく発生する現象である。 When polysilicon is melted in a quartz glass crucible and the silicon single crystal is pulled up, a vibration wave front is generated on the surface of the silicon melt, the silicon seed crystal cannot be bonded to the silicon melt, or the crystallinity of the silicon single crystal is disturbed. This is a common phenomenon.
この原因の一つとして、石英ガラスるつぼの内表面が合成石英ガラス層とされていることが挙げられる。石英ガラスるつぼの内表面が合成石英ガラス層とされている場合、合成石英ガラス層は実質無気泡であるため、シリコン単結晶を引き上げる際に液面振動が起こりやすくなる。 One reason for this is that the inner surface of the quartz glass crucible is a synthetic quartz glass layer. In the case where the inner surface of the quartz glass crucible is a synthetic quartz glass layer, the synthetic quartz glass layer is substantially bubble-free, so that liquid surface vibration is likely to occur when pulling up the silicon single crystal.
特に、近年、シリコン単結晶が8”以上になり、石英ガラスるつぼも大口径になるに従って、液面振動の問題は、益々重要になってきた。 In particular, the problem of liquid surface vibration has become more and more important in recent years as silicon single crystals have become larger than 8 "and quartz glass crucibles have become larger diameters.
上記のような液面振動の問題を解決するべく、例えば、特許文献1〜4には、るつぼ内表面を粗面化することで液面振動を抑制する技術が開示されている。 In order to solve the problem of liquid level vibration as described above, for example, Patent Documents 1 to 4 disclose techniques for suppressing liquid level vibration by roughening the inner surface of the crucible.
しかしながら、本発明者らが鋭意研究を重ねた結果、粗面化させた場合であっても、液面振動の抑制効果に差が生じる場合があることを見出し、本発明を完成させた。 However, as a result of repeated studies by the present inventors, it has been found that even when the surface is roughened, a difference may occur in the effect of suppressing liquid surface vibration, and the present invention has been completed.
本発明は、上記した事情に鑑みなされたもので、シリコン単結晶の引き上げ時の液面振動の発生を効率的に抑制することができるようにしたシリコン単結晶引き上げ用石英ガラスるつぼ及びその製造方法を提供することを目的とする。 The present invention has been made in view of the above circumstances, and a quartz glass crucible for pulling a silicon single crystal capable of efficiently suppressing the occurrence of liquid level vibration during pulling of the silicon single crystal, and a method for manufacturing the same. The purpose is to provide.
上記課題を解決するために、本発明のシリコン単結晶引き上げ用石英ガラスるつぼは、種結晶をシリコン融液に接触させて引上げることでシリコン単結晶を育成するシリコン単結晶引き上げ用石英ガラスるつぼであり、
半透明石英ガラス層のるつぼ基体と、前記るつぼ基体の内壁面に形成された透明合成石英ガラス層とを含み、上端部が開口されてなる直胴部と該直胴部に円弧状に形成された底部とを有し、
前記透明合成石英ガラス層の直胴部表面の一部に帯状粗面領域を設け、前記帯状粗面領域よりも下方の前記透明合成石英ガラス層表面の下部領域は滑面とし、
前記帯状粗面領域は前記シリコン融液の初期状態における液面を中心に少なくとも±１０ｍｍでありかつ前記液面から下方への最大幅が５０ｍｍであり、
前記帯状粗面領域が石英粉を用いた乾式又は湿式のブラスト処理により形成されてなり、
前記帯状粗面領域の算術平均粗さ(Ra)が2〜9μmであり、
前記下部領域の算術平均粗さ(Ra)が0.09μm以下であり、
前記シリコン融液の初期状態における液面が前記帯状粗面領域に接するように前記帯状粗面領域が設けられてなることを特徴とする。
In order to solve the above problems, a quartz glass crucible for pulling a silicon single crystal according to the present invention is a quartz glass crucible for pulling a silicon single crystal that grows a silicon single crystal by pulling a seed crystal in contact with a silicon melt. Yes,
A translucent quartz glass layer crucible base, and a transparent synthetic quartz glass layer formed on the inner wall of the crucible base, the upper end of which is formed into a straight body portion and the straight body portion formed in an arc shape And a bottom
A belt-like rough surface region is provided in a part of the surface of the straight body portion of the transparent synthetic quartz glass layer, and a lower region of the surface of the transparent synthetic quartz glass layer below the belt-like rough surface region is a smooth surface,
The belt-like rough surface area is at least ± 10 mm centered on the liquid surface in the initial state of the silicon melt, and the maximum width downward from the liquid surface is 50 mm,
The belt-like rough surface region is formed by dry or wet blasting using quartz powder,
Arithmetic mean roughness (Ra) of the band-like rough surface area is 2-9μm,
The arithmetic average roughness (Ra) of the lower region is 0.09 μm or less,
The band-shaped rough surface region is provided so that the liquid surface in the initial state of the silicon melt is in contact with the band-shaped rough surface region.
本明細書において、算術平均粗さ(Ra)とは、JISB0601に記載の算術平均粗さを指す。 In this specification, the arithmetic average roughness (Ra) refers to the arithmetic average roughness described in JISB0601.
前記帯状粗面領域とは、前記透明合成石英ガラス層表面の一部に帯状するように形成された帯状の粗面領域を指す。 The band-shaped rough surface region refers to a band-shaped rough surface region formed so as to be banded on a part of the surface of the transparent synthetic quartz glass layer.
前記シリコン融液の初期状態における液面とは、シリコン単結晶を引き上げる前のシリコン融液が前記石英ガラスるつぼ内に入っている状態での液面のことを指す。 The liquid level in the initial state of the silicon melt refers to the liquid level in a state where the silicon melt before pulling up the silicon single crystal is in the quartz glass crucible.
なお、本発明におけるシリコン単結晶の引き上げ時の液面振動とは、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間に見られる液面振動を指す。 In the present invention, the liquid level vibration at the time of pulling up the silicon single crystal means that the seed crystal is bonded to the silicon melt, passed through seed drawing (necking), and the shoulder portion of the silicon single crystal starts to be formed. This refers to the liquid level vibration.
前記帯状粗面領域の前記石英ガラスるつぼの端部からの位置は、前記石英ガラスるつぼの径や製造条件などによって適宜設定すればよいものであるが、前記シリコン融液の初期状態における液面位置が前記帯状粗面領域の範囲内となるように前記帯状粗面領域を設ける必要がある。前記帯状粗面領域としては、前記シリコン融液の初期状態における液面を中心に少なくとも±10mmであり、液面から下方への最大幅が50mm以内となるようにするのが好ましい。 The position of the band-shaped rough surface region from the end of the quartz glass crucible may be set as appropriate depending on the diameter of the quartz glass crucible, manufacturing conditions, etc., but the liquid surface position in the initial state of the silicon melt It is necessary to provide the band-shaped roughened surface area so that is within the range of the band-shaped roughened surface area. The band-like rough surface region is preferably at least ± 10 mm centering on the liquid surface in the initial state of the silicon melt, and the maximum width downward from the liquid surface is preferably within 50 mm.
また、前記帯状粗面領域が石英粉を用いたブラスト処理により形成されてなるのが好適である。前記石英粉としては、合成石英粉又は高純度天然石英粉が用いられる。 Further, it is preferable that the belt-like rough surface region is formed by blasting using quartz powder. As the quartz powder, synthetic quartz powder or high-purity natural quartz powder is used.
さらに、前記滑面とした下部領域の算術平均粗さ(Ra)がRa:0.09μm以下であるのが好ましく、Ra:0.03μm以下であるのがより好ましい。 Further, the arithmetic average roughness (Ra) of the lower region as the smooth surface is preferably Ra: 0.09 μm or less, and more preferably Ra: 0.03 μm or less.
前記ブラスト処理が乾式又は湿式であるのが好適である。 The blasting process is preferably dry or wet.
前記ブラスト処理は、石英粉を圧縮空気や遠心力で吹き付けることにより、前記石英ガラスるつぼ内表面を粗面化するものである。前記ブラスト処理としては、石英粉を吹き付ける乾式ブラストでもよいし、水などの流体とともに石英粉を吹き付ける湿式ブラストでもよい。石英粉としては、粒径106μm〜355μmの範囲の石英粉の重量積算が80%以上であるのが好適である。粒径の測定及び選別にあたっては例えば篩いを用いればよい。 The blasting treatment is to roughen the inner surface of the quartz glass crucible by blowing quartz powder with compressed air or centrifugal force. The blasting process may be dry blasting that blows quartz powder, or wet blasting that blows quartz powder together with a fluid such as water. As the quartz powder, it is preferable that the weight integration of the quartz powder having a particle size of 106 μm to 355 μm is 80% or more. For the measurement and selection of the particle diameter, for example, a sieve may be used.
本発明のシリコン単結晶引き上げ用石英ガラスるつぼの製造方法は、種結晶をシリコン融液に接触させて引上げることでシリコン単結晶を育成するシリコン単結晶引き上げ用石英ガラスるつぼの製造方法であり、
半透明石英ガラス層のるつぼ基体と、前記るつぼ基体の内壁面に形成された透明合成石英ガラス層とを含み、上端部が開口されてなる直胴部と該直胴部に円弧状に形成された底部とを有する石英ガラスるつぼを作製し、
前記透明合成石英ガラス層表面の直胴部表面の一部に帯状粗面領域を設け、前記帯状粗面領域よりも下方の前記透明合成石英ガラス層表面の下部領域を滑面とし、
前記帯状粗面領域は前記シリコン融液の初期状態における液面を中心に少なくとも±１０ｍｍでありかつ前記液面から下方への最大幅が５０ｍｍであり、
前記帯状粗面領域を石英粉を用いた乾式又は湿式のブラスト処理で形成し、
前記帯状粗面領域の算術平均粗さ(Ra)が2〜9μmであり、
前記下部領域の算術平均粗さ(Ra)が0.09μm以下であり、
前記シリコン融液の初期状態における液面が前記帯状粗面領域に接するように前記帯状粗面領域を設けることを特徴とする。
The method for producing a quartz glass crucible for pulling a silicon single crystal of the present invention is a method for producing a quartz glass crucible for pulling a silicon single crystal by growing a silicon single crystal by bringing a seed crystal into contact with a silicon melt and pulling it up.
A translucent quartz glass layer crucible base, and a transparent synthetic quartz glass layer formed on the inner wall of the crucible base, the upper end of which is formed into a straight body portion and the straight body portion formed in an arc shape A quartz glass crucible having a bottom and
A belt-like rough surface region is provided in a part of the surface of the straight body portion of the transparent synthetic quartz glass layer surface, and a lower region of the transparent synthetic quartz glass layer surface below the belt-like rough surface region is a smooth surface,
The belt-like rough surface area is at least ± 10 mm centered on the liquid surface in the initial state of the silicon melt, and the maximum width downward from the liquid surface is 50 mm,
The belt-like rough surface region is formed by dry or wet blasting using quartz powder,
Arithmetic mean roughness (Ra) of the band-like rough surface area is 2-9μm,
The arithmetic average roughness (Ra) of the lower region is 0.09 μm or less,
The belt-like rough surface region is provided so that the liquid surface in the initial state of the silicon melt is in contact with the belt-like rough surface region.
また、前記帯状粗面領域を石英粉を用いたブラスト処理で形成するのが好ましい。 Moreover, it is preferable to form the said strip | belt-shaped rough surface area | region by the blast process using quartz powder.
前記滑面領域の算術平均粗さ(Ra)がRa:0.09μm以下であるのが好ましく、Ra:0.03μm以下であるのがより好ましい。 The arithmetic average roughness (Ra) of the smooth surface region is preferably Ra: 0.09 μm or less, and more preferably Ra: 0.03 μm or less.
さらに、前記ブラスト処理が乾式又は湿式であるのが好適である。 Furthermore, it is preferable that the blast treatment is dry or wet.
なお、本発明の適用にあって、るつぼの口径に特別の限定はなく、様々な口径のるつぼに適用可能である。 In addition, in application of this invention, there is no special limitation in the diameter of a crucible, It can apply to the crucible of various diameters.
本発明によれば、シリコン単結晶の引き上げ時の液面振動の発生を効率的に抑制することができるようにしたシリコン単結晶引き上げ用石英ガラスるつぼ及びその製造方法を提供することができるという著大な効果を有する。 According to the present invention, it is possible to provide a quartz glass crucible for pulling up a silicon single crystal and a method for manufacturing the same, which can efficiently suppress the occurrence of liquid surface vibration during the pulling of the silicon single crystal. Has a great effect.
また、本発明によれば、操業時間の短縮及び歩留まりの向上にもつながるという著大な効果を有する。 Moreover, according to this invention, it has the remarkable effect that it leads also to the shortening of operation time and the improvement of a yield.
以下、本発明の一つの実施の形態を添付図面に基づいて説明するが、これらの説明は例示的に示されるもので限定的に解釈すべきものでないことはいうまでもない。 In the following, one embodiment of the present invention will be described with reference to the accompanying drawings. However, it is needless to say that these descriptions are given by way of example and should not be construed as limiting.
図1において、符号10は本発明に係るシリコン単結晶引上げ用石英ガラスるつぼを示す。シリコン単結晶引上げ用石英ガラスるつぼ10は、種結晶をシリコン融液に接触させて引上げることでシリコン単結晶を育成するシリコン単結晶引き上げ用石英ガラスるつぼであり、半透明石英ガラス層のるつぼ基体12と、前記るつぼ基体12の内壁面に形成された透明合成石英ガラス層14とを含み、上端部22が開口されてなる直胴部24と該直胴部24に円弧状に形成された底部26とを有し、前記透明合成石英ガラス層14の直胴部24の一部に帯状粗面領域18を設け、前記帯状粗面領域18よりも下方の前記透明合成石英ガラス層表面の下部領域28は滑面とされている。なお、符号20は、帯状粗面領域18の凹部である。
In FIG. 1,
前記帯状粗面領域18の算術平均粗さ(Ra)は2〜9μmであり、シリコン融液の初期状態における液面16が前記帯状粗面領域18に接するように前記帯状粗面領域18が設けられている。図1の例では、前記帯状粗面領域18の幅Wのちょうど中間部分にシリコン融液の初期状態における液面16がくるようにされている。また、上端部22から帯状粗面領域18までの距離dについては、るつぼの口径やシリコン融液の量など、種々の製造条件によって変わるものであるため、特別の限定はない。シリコン融液の初期状態における液面16が前記帯状粗面領域18に接するように、距離dを調節して前記帯状粗面領域18を設ければよい。また、前記滑面とした下部領域の算術平均粗さ(Ra)は好ましくはRa:0.09μm以下、より好ましくはRa:0.03μm以下とされている。
The belt-like
また、前記帯状粗面領域18よりも上方の前記透明合成石英ガラス層表面の上部領域30については、粗面としてもよいし、滑面としてもよいが、原料である多結晶シリコンとの接触による石英片の剥離を勘案すると滑面の方がより好ましい。図示例では、上部領域30を下部領域28と同様の滑面とした例を示した。
Further, the
このように、シリコン融液の初期状態における液面16が前記帯状粗面領域18に接するように前記帯状粗面領域18が設けられているため、シリコン単結晶の引き上げ時の液面振動の発生を抑制することができる。
Thus, since the band-like
以下に、本発明の実施例をあげてさらに具体的に説明するが、本発明はこれらの実施例に限定されるものではなく、本発明の技術思想から逸脱しない限り様々の変形が可能であることは勿論である。 Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples, and various modifications can be made without departing from the technical idea of the present invention. Of course.
（実施例1）
粒径50〜500μmの天然石英粉を回転する内径570mmのモールド内に供給し、厚さ25mmの粉体層からなる成型体を成型し、アーク放電により該成型体の内部から加熱熔融すると同時に、その高温雰囲気中にOH濃度が40ppmの合成石英ガラス粉を100g/minの割合で供給し、泡の無い透明ガラス層を全内面領域にわたり、1〜3mmの厚さで形成した。熔融が終了し、冷却した直径555〜560mmの石英ガラスるつぼについて、高さが370mmとなるよう上端部をカットし、石英ガラスるつぼを20個作成した。前記石英ガラスるつぼについて、直胴部内面において、上端部からの距離ｄが60mm、幅Wが40mm（即ち、上端部から60mm〜100mmの範囲）の帯状粗面領域にのみ、サクション式エアーブラスト処理で粗面化を行った石英ガラスるつぼを10個作成した。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。ブラスト材として使用した高純度天然石英粉について粒度分布を測定したところφ106μm〜355μmの占める割合は87重量%であった。各るつぼの帯状粗面領域の面粗さを測定したところRa：3.72〜3.88μmであり、また上部領域、下部領域のRaはそれぞれ0.00〜0.02μm、0.00〜0.02μmであった。この石英ガラスるつぼにポリシリコンを140kg充填した操業条件Aでシリコン単結晶の引き上げを行ったところ、全てのるつぼにおいて従来発生していた、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間に見られるシリコン融液面の振動は見られず、自動で操業可能であり、操業時間の短縮とシリコン単結晶の歩留り向上が確認された。結果を表1に示す。なお、表１及び２において、サンドブラスト処理条件の範囲とは、サンドブラスト処理を行った帯状粗面領域の位置、即ち、上端部からの距離d〜該距離d＋帯状粗面領域の幅Wを示したものである。(Example 1)
A natural quartz powder having a particle size of 50 to 500 μm is fed into a rotating mold having an inner diameter of 570 mm, and a molded body composed of a powder layer having a thickness of 25 mm is molded and simultaneously melted by heating from the inside of the molded body by arc discharge. In this high temperature atmosphere, synthetic quartz glass powder having an OH concentration of 40 ppm was supplied at a rate of 100 g / min, and a transparent glass layer without bubbles was formed to a thickness of 1 to 3 mm over the entire inner surface area. For the fused quartz glass crucible having a diameter of 555 to 560 mm after melting, the upper end was cut to a height of 370 mm, and 20 quartz glass crucibles were prepared. For the silica glass crucible, the suction type air blast treatment is applied only to the belt-like rough surface area having the distance d from the upper end of 60 mm and the width W of 40 mm (that is, in the range of 60 mm to 100 mm from the upper end) on the inner surface of the straight body. Ten quartz glass crucibles roughened by using 10 were prepared. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. When the particle size distribution of the high-purity natural quartz powder used as the blast material was measured, the ratio of φ106 μm to 355 μm was 87% by weight. When the surface roughness of the band-like rough surface region of each crucible was measured, Ra was 3.72 to 3.88 μm, and Ra of the upper region and the lower region was 0.00 to 0.02 μm and 0.00 to 0.02 μm, respectively. When a silicon single crystal was pulled up under the operating condition A in which 140 kg of polysilicon was filled in this quartz glass crucible, the seed crystal that had been generated in all the crucibles was joined to the silicon melt and seed drawing (necking). Through this process, the vibration of the silicon melt surface seen before the formation of the shoulder portion of the silicon single crystal is not observed, and it can be operated automatically, and it has been confirmed that the operation time is shortened and the yield of the silicon single crystal is improved. It was. The results are shown in Table 1. In Tables 1 and 2, the range of the sandblast treatment condition indicates the position of the band-like rough surface area subjected to the sandblast treatment, that is, the distance d from the upper end to the distance d + the width W of the band-like rough surface area. Is.
本明細書において、操業時間とは、シリコン単結晶の引き上げ開始から引き上げ完了までに要する時間を指す。表1において、操業時間率とは、従来の例である比較例1の操業時間を1とした場合の比率であり、例えば実施例1の操業時間率の場合、実施例1の操業時間÷比較例1の操業時間＝実施例1の操業時間率、によって算出される。操業時間率が低いほど、オペレータによる手動調整などが不要で自動操業が可能であるなど、操業時間が短縮されていることを示す。また、歩留まり率とは、従来の例である比較例1のシリコン単結晶の歩留りを1とした場合の比率である。例えば実施例1の歩留り率の場合、実施例1の歩留まり÷比較例1の歩留まり＝実施例1の歩留まり率、によって算出される。歩留まり率が高いほど、歩留まりが向上していることを示す。 In this specification, the operation time refers to the time required from the start of pulling of the silicon single crystal to the completion of pulling. In Table 1, the operation time rate is a ratio when the operation time of Comparative Example 1, which is a conventional example, is 1, for example, in the case of the operation time rate of Example 1, the operation time of Example 1 ÷ comparison Calculated by the operation time of Example 1 = the operation time rate of Example 1. The lower the operation time rate, the shorter the operation time, such as the need for manual adjustment by the operator and automatic operation. The yield rate is a ratio when the yield of the silicon single crystal of Comparative Example 1 as a conventional example is 1. For example, in the case of the yield rate of the first embodiment, the yield is calculated by the yield of the first embodiment / the yield of the first comparative example = the yield rate of the first embodiment. The higher the yield rate, the higher the yield.
（実施例2）
実施例１とブラスト処理条件を変更し、上端部から50mm〜110mmの範囲の帯状粗面領域の粗面化処理を行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表1に示す。表1に示すように液面振動は生じなかった。(Example 2)
The blasting treatment conditions were changed from that in Example 1, and the roughening treatment of the band-like roughened surface region in the range of 50 mm to 110 mm from the upper end portion was performed. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 1. As shown in Table 1, liquid level vibration did not occur.
（実施例3）
サクション式エアーブラストの代わりにウエットブラスト処理にて、上端部から60mm〜110mmの範囲の帯状粗面領域の粗面化処理を行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。また、ブラスト材は実施例1のエアーブラストに使用したものと同じ天然石英粉を使用した。結果を表1に示す。表1に示すように、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間に液面振動は生じなかった。(Example 3)
Instead of the suction-type air blasting, a roughening treatment of a band-like rough surface region in a range of 60 mm to 110 mm from the upper end portion was performed by wet blasting. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. Further, the same natural quartz powder as that used for the air blast of Example 1 was used as the blast material. The results are shown in Table 1. As shown in Table 1, there was no liquid level vibration until the seed crystal was joined to the silicon melt, seed drawing (necking), and the shoulder portion formation of the silicon single crystal started.
（実施例4）
帯状粗面領域（上端部から60mm〜100mmの範囲）よりも上方の上部領域についても粗面化処理を行った。下部領域のみマスキングテープによるマスキングを行い、上部領域はマスキングを行わなかった。結果を表1に示す。表1に示すように液面振動は生じなかった。また、粗面化処理は、石英ガラスるつぼをひっくり返さず行った。マスキングを行った下部領域の算術平均粗さ(Ra)は低い値となり、マスキングを行わなかった上部領域の算術平均粗さ(Ra)は比較的高い値となった。(Example 4)
The surface roughening treatment was also performed on the upper region above the band-shaped rough surface region (range of 60 mm to 100 mm from the upper end). Only the lower region was masked with masking tape, and the upper region was not masked. The results are shown in Table 1. As shown in Table 1, liquid level vibration did not occur. Further, the roughening treatment was performed without turning the quartz glass crucible over. The arithmetic average roughness (Ra) of the lower region where masking was performed was a low value, and the arithmetic average roughness (Ra) of the upper region where masking was not performed was a relatively high value.
（実施例5）
サクション式エアーブラストの代わりにウエットブラスト処理にて実施し、石英ガラスるつぼをひっくり返さず、また、マスキングを行わず、上端部から60mm〜110mmの範囲の帯状粗面領域の粗面化処理を行った。また、ブラスト材は実施例1のエアーブラストに使用したものと同じ天然石英粉を使用した。結果を表1に示す。表1に示すように、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間に液面振動は生じなかった。マスキングをしなかったにもかかわらず、上部領域及び下部領域ともに、算術平均粗さ(Ra)は低い値となった。(Example 5)
Instead of suction type air blasting, wet blasting was used, and the quartz glass crucible was not turned over, masking was not performed, and the roughening treatment of the belt-like rough surface area in the range of 60 mm to 110 mm was performed from the upper end. . Further, the same natural quartz powder as that used for the air blast of Example 1 was used as the blast material. The results are shown in Table 1. As shown in Table 1, there was no liquid level vibration until the seed crystal was joined to the silicon melt, seed drawing (necking), and the shoulder portion formation of the silicon single crystal started. Despite the absence of masking, the arithmetic average roughness (Ra) was low in both the upper and lower regions.
（実施例6）
上端部から60mm〜110mmの範囲の帯状粗面領域の粗面化処理をウエットブラスト処理にて実施し、石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。また、ブラスト材は実施例1のエアーブラストに使用したものと同じ天然石英粉を使用した。ただし、マスキングは行わなかった。結果を表1に示す。表1に示すように液面振動は生じなかった。粗面化処理は、実施例１と同様に、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行ったため、下部領域の算術平均粗さ(Ra)は低い値となり、上部領域の算術平均粗さ(Ra)は、下部領域の算術平均粗さ(Ra)よりも高い値となった。(Example 6)
A surface roughening treatment of a band-like rough surface region in a range of 60 mm to 110 mm from the upper end portion was performed by wet blasting, and the inner wall surface was performed with the quartz glass crucible turned upside down. Further, the same natural quartz powder as that used for the air blast of Example 1 was used as the blast material. However, no masking was performed. The results are shown in Table 1. As shown in Table 1, liquid level vibration did not occur. As in Example 1, the roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down, so the arithmetic average roughness (Ra) of the lower region was low. The arithmetic average roughness (Ra) of the upper region was higher than the arithmetic average roughness (Ra) of the lower region.
（比較例1）
粒径50〜500μmの天然石英粉を回転する内径570mmのモールド内に供給し、厚さ25mmの粉体層からなる成型体を成型し、アーク放電により該成型体の内部から加熱熔融すると同時に、その高温雰囲気中にOH濃度が40ppmの合成石英ガラス粉を100g/minの割合で供給し、泡の無い透明ガラス層を全内面領域にわたり、1〜3mmの厚さで形成した。熔融が終了し、冷却した直径555〜560mmの石英ガラスるつぼについて、高さが370mmとなるよう上端部をカットし、石英ガラスるつぼを20個作成した。そのうちの10個について、操業条件A(ポリシリコンを140kg充填)で、シリコン単結晶の引き上げを行ったところ、何れの場合においても、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間(種付け〜ショルダー部形成)にシリコン融液面に振動が発生した為、自動操業が出来ず、オペレーターによる手動調整が必要であったばかりか、初期のトラブルにより操業時間が長くなり、結果としてシリコン単結晶の歩留りも低めであった。尚、上記るつぼの使用前における内表面の表面粗さを前もって測定したところ、全領域にわたって表1に示す値であり、使用後のるつぼから操業開始時の初期液面位置を測定したところ、平均で上端部から74mm(最大78mm、最小72mm)であり、表1に示すように液面振動が生じた。(Comparative Example 1)
A natural quartz powder having a particle size of 50 to 500 μm is fed into a rotating mold having an inner diameter of 570 mm, and a molded body composed of a powder layer having a thickness of 25 mm is molded and simultaneously melted by heating from the inside of the molded body by arc discharge. In this high temperature atmosphere, synthetic quartz glass powder having an OH concentration of 40 ppm was supplied at a rate of 100 g / min, and a transparent glass layer without bubbles was formed to a thickness of 1 to 3 mm over the entire inner surface area. For the fused quartz glass crucible having a diameter of 555 to 560 mm after melting, the upper end was cut to a height of 370 mm, and 20 quartz glass crucibles were prepared. About 10 of them, the silicon single crystal was pulled up under the operating condition A (filled with 140 kg of polysilicon). In any case, the seed crystal was bonded to the silicon melt, and the seed squeezing (necking) was performed. After that, until the shoulder formation of the silicon single crystal began (seeding-shoulder formation), the silicon melt surface vibrated, so automatic operation was not possible and manual adjustment by the operator was necessary. Due to the initial trouble, the operation time was long, and as a result, the yield of silicon single crystals was also low. In addition, when the surface roughness of the inner surface before use of the crucible was measured in advance, the values shown in Table 1 over the entire region, the initial liquid level position at the start of operation from the crucible after use was measured, the average And 74 mm from the upper end (maximum 78 mm, minimum 72 mm), and liquid level vibration occurred as shown in Table 1.
（比較例2）
帯状粗面領域のＲａを変えた以外は、実施例1と同様に行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表1に示す。表1に示すように液面振動が生じた。(Comparative Example 2)
The same operation as in Example 1 was performed except that Ra of the band-shaped rough surface region was changed. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 1. As shown in Table 1, liquid level vibration occurred.
（比較例3）
帯状粗面領域（上端部から60mm〜100mmの範囲）、該帯状粗面領域よりも上方の上部領域及び該帯状粗面領域よりも下方の下部領域を表1に示すように全て粗面化処理を行った。すなわち、前記透明合成石英ガラス層の内表面全てを粗面化した以外は、実施例1と同様に行った。結果を表1に示す。表1に示すように液面振動は生じなかったが、特にるつぼの直胴部から底部にかけてのＲ部（湾曲部）や底部の面状態が悪化し、歩留まりが大幅に低下してしまった。(Comparative Example 3)
As shown in Table 1, the surface of the belt-like rough surface area (in the range of 60 to 100 mm from the upper end), the upper region above the belt-like rough surface region, and the lower region below the belt-like rough surface region are all roughened. Went. That is, the same procedure as in Example 1 was performed except that the entire inner surface of the transparent synthetic quartz glass layer was roughened. The results are shown in Table 1. As shown in Table 1, liquid surface vibration did not occur, but the surface state of the R part (curved part) and the bottom part from the straight body part to the bottom part of the crucible and the bottom part deteriorated, and the yield was greatly reduced.
（比較例4）
帯状粗面領域のＲａを変え、上端部から50mm〜110mmの範囲の帯状粗面領域の粗面化処理を行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表1に示す。表1に示すように液面振動は生じなかったが、粗面処理した処理面より石英片が剥離する為、結晶が乱れ易くなってしまうという問題が生じ、操業時間が長くなってしまった。(Comparative Example 4)
Ra of the band-shaped rough surface region was changed, and the surface roughening treatment of the band-shaped rough surface region in the range of 50 mm to 110 mm from the upper end portion was performed. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 1. As shown in Table 1, liquid level vibration did not occur, but the quartz piece was peeled off from the roughened treated surface, which caused a problem that the crystal was easily disturbed, and the operation time was prolonged.
（実施例7）
上端部から110mm〜140mmの範囲の帯状粗面領域の粗面化処理を行った。帯状粗面領域のＲａを変更し、液面位置を変更し、シリコン単結晶引き上げ条件操業条件B(ポリシリコンを100kg充填)でシリコン単結晶の引き上げを行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表2に示す。表2に示すように液面振動は生じなかった。(Example 7)
A roughening treatment was performed on a belt-like rough surface region in the range of 110 mm to 140 mm from the upper end. The Ra of the band-like rough surface region was changed, the liquid surface position was changed, and the silicon single crystal was pulled up under the operation condition B of silicon single crystal pulling condition (filled with 100 kg of polysilicon). During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 2. As shown in Table 2, liquid level vibration did not occur.
表2において、操業時間率とは、従来の例である比較例5の操業時間を1とした場合の比率であり、例えば実施例7の操業時間率の場合、実施例7の操業時間÷比較例5の操業時間＝実施例7の操業時間率、によって算出される。操業時間率が低いほど、オペレータによる手動調整などが不要で自動操業が可能であるなど、操業時間が短縮されていることを示す。また、歩留まり率とは、従来の例である比較例5のシリコン単結晶の歩留りを1とした場合の比率である。例えば実施例7の歩留り率の場合、実施例7の歩留まり÷比較例5の歩留まり＝実施例7の歩留まり率、によって算出される。歩留まり率が高いほど、歩留まりが向上していることを示す。 In Table 2, the operation time rate is a ratio when the operation time of Comparative Example 5 which is a conventional example is set to 1, for example, in the case of the operation time rate of Example 7, the operation time of Example 7 ÷ comparison Calculated by the operation time of Example 5 = the operation time rate of Example 7. The lower the operation time rate, the shorter the operation time is. For example, automatic adjustment is possible without requiring manual adjustment by the operator. The yield rate is a ratio when the yield of the silicon single crystal of Comparative Example 5 as a conventional example is 1. For example, in the case of the yield rate of Example 7, the yield of Example 7 / the yield of Comparative Example 5 = the yield rate of Example 7 is calculated. The higher the yield rate, the higher the yield.
（実施例8）
帯状粗面領域の幅Wを実施例7よりも広くし（上端部から110mm〜250mmの範囲）、粗面化処理を行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表2に示す。表2に示すように液面振動は生じなかった。(Example 8)
The width W of the belt-like rough surface region was made wider than that in Example 7 (range from 110 mm to 250 mm from the upper end), and the roughening treatment was performed. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 2. As shown in Table 2, liquid level vibration did not occur.
（実施例9）
表2に示したように、帯状粗面領域のRaの他、該帯状粗面領域よりも上方の上部領域及び該帯状粗面領域よりも下方の下部領域をRaがそれぞれ0.03〜0.09μmである滑面となるように処理した以外は、実施例7と同様に行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表2に示す。表2に示すように液面振動は生じなかった。(Example 9)
As shown in Table 2, Ra is 0.03 to 0.09 μm in the upper region above the belt-like rough surface region and the lower region below the belt-like rough surface region in addition to Ra of the belt-like rough surface region. The same procedure as in Example 7 was performed except that the surface was smoothed. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 2. As shown in Table 2, liquid level vibration did not occur.
（比較例5）
比較例1で作製した石英ガラスるつぼのうち残りの10個を用いて、操業条件B(同100kg充填)にてシリコン単結晶の引き上げを行ったところ、種結晶をシリコン融液に接合させ、種絞り（ネッキング）を経て、シリコン単結晶のショルダー部形成が始まるまでの間 (種付け〜ショルダー部形成)にシリコン融液面に振動が発生した為、自動操業が出来ず、オペレーターによる手動調整が必要であったばかりか、初期のトラブルにより操業時間が長くなり、結果としてシリコン単結晶の歩留りも低めであった。尚、上記るつぼの使用前における内表面の表面粗さを前もって測定したところ、全領域にわたって表2に示す値であり、使用後のるつぼから操業開始時の初期液面位置を測定したところ、平均で上端部から124mm(最大127mm、最小122mm) であり、表2に示すように液面振動が生じた。(Comparative Example 5)
Using the remaining 10 quartz glass crucibles produced in Comparative Example 1, the silicon single crystal was pulled up under the operating condition B (filled with 100 kg), the seed crystal was bonded to the silicon melt, The vibration of the silicon melt surface occurs during the period from the necking (necking) until the shoulder formation of the silicon single crystal begins (seeding to shoulder formation), so automatic operation is not possible and manual adjustment by the operator is required. In addition, the operation time was prolonged due to the initial trouble, and as a result, the yield of the silicon single crystal was also low. In addition, when the surface roughness of the inner surface before use of the crucible was measured in advance, the values shown in Table 2 over the entire region, the initial liquid level position at the start of operation from the crucible after use was measured, the average And 124 mm (maximum 127 mm, minimum 122 mm) from the upper end, and liquid level vibration occurred as shown in Table 2.
（比較例6）
帯状粗面領域のRaを変えた以外は、実施例7と同様に行った。結果を表2に示す。表2に示すように液面振動が生じてしまった。(Comparative Example 6)
The same operation as in Example 7 was performed except that Ra of the band-shaped rough surface region was changed. The results are shown in Table 2. As shown in Table 2, liquid level vibration has occurred.
（比較例7）
上端部から60mm〜100mmの範囲の帯状粗面領域の粗面化処理を行い、実施例1と同様のるつぼを用いてシリコン融液の液面位置が帯状粗面領域から外れた状態で、シリコン単結晶の引き上げを行った。粗面化処理の際、粗面化処理を行わない上部領域及び下部領域については、マスキングテープを用いて予めマスキングをしておいた。粗面化処理は、上端部が下になるように石英ガラスるつぼをひっくり返した状態で内壁面に対して行った。結果を表2に示す。表2に示すように液面振動が生じてしまった。(Comparative Example 7)
The surface of the belt-like rough surface area in the range of 60 mm to 100 mm from the upper end is roughened, and the silicon melt is removed from the belt-like rough surface area using the same crucible as in Example 1. The single crystal was pulled up. During the roughening treatment, the upper region and the lower region that are not subjected to the roughening treatment were previously masked using a masking tape. The roughening treatment was performed on the inner wall surface with the quartz glass crucible turned upside down so that the upper end portion was down. The results are shown in Table 2. As shown in Table 2, liquid level vibration has occurred.
10:本発明に係るシリコン単結晶引上げ用石英ガラスるつぼ、12:るつぼ基体、14:透明合成石英ガラス層、16:シリコン融液の初期状態における液面位置、18:帯状粗面領域、20:凹部、22:上端部、24:直胴部、26:底部、28:下部領域、30:上部領域、d:上端部から帯状粗面領域までの距離、W:帯状粗面領域の幅。 10: quartz glass crucible for pulling up a silicon single crystal according to the present invention, 12: crucible base, 14: transparent synthetic quartz glass layer, 16: liquid surface position in the initial state of silicon melt, 18: band-like rough surface region, 20: Concave part, 22: upper end part, 24: straight body part, 26: bottom part, 28: lower area, 30: upper area, d: distance from upper end part to belt-like rough surface area, W: width of belt-like rough surface area.
Claims (1)
半透明石英ガラス層のるつぼ基体と、前記るつぼ基体の内壁面に形成された透明合成石英ガラス層とを含み、上端部が開口されてなる直胴部と該直胴部に円弧状に形成された底部とを有する石英ガラスるつぼを作製し、
前記透明合成石英ガラス層表面の直胴部表面の一部に帯状粗面領域を設け、前記帯状粗面領域よりも下方の前記透明合成石英ガラス層表面の下部領域を滑面とし、
前記帯状粗面領域は前記シリコン融液の初期状態における液面を中心に少なくとも±１０ｍｍでありかつ前記液面から下方への最大幅が５０ｍｍであり、
前記帯状粗面領域を石英粉を用いた乾式又は湿式のブラスト処理で形成し、
前記帯状粗面領域の算術平均粗さ(Ra)が2〜9μmであり、
前記下部領域の算術平均粗さ(Ra)が0.09μm以下であり、
前記シリコン融液の初期状態における液面が前記帯状粗面領域に接するように前記帯状粗面領域を設けることを特徴とするシリコン単結晶引き上げ用石英ガラスるつぼの製造方法。 A method for producing a quartz glass crucible for pulling a silicon single crystal by growing the silicon single crystal by bringing the seed crystal into contact with a silicon melt and pulling it up.
It includes a crucible base of a semi-transparent quartz glass layer and a transparent synthetic quartz glass layer formed on the inner wall surface of the crucible base. A quartz glass crucible having a bottom and
A belt-like rough surface region is provided in a part of the surface of the straight body portion of the transparent synthetic quartz glass layer surface, and a lower region of the transparent synthetic quartz glass layer surface below the belt-like rough surface region is a smooth surface,
The belt-like rough surface area is at least ± 10 mm centered on the liquid surface in the initial state of the silicon melt, and the maximum width downward from the liquid surface is 50 mm,
The belt-like rough surface region is formed by dry or wet blasting using quartz powder,
Arithmetic mean roughness (Ra) of the band-like rough surface area is 2-9μm,
The arithmetic average roughness (Ra) of the lower region is 0.09 μm or less,
A method for producing a quartz glass crucible for pulling a silicon single crystal, characterized in that the belt-like rough surface region is provided so that the liquid surface in the initial state of the silicon melt is in contact with the belt-like rough surface region.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012520388A JP5901072B2 (en) | 2010-06-16 | 2011-06-08 | Method for producing quartz glass crucible for pulling silicon single crystal |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010137623 | 2010-06-16 | ||
| JP2010137623 | 2010-06-16 | ||
| JP2012520388A JP5901072B2 (en) | 2010-06-16 | 2011-06-08 | Method for producing quartz glass crucible for pulling silicon single crystal |
| PCT/JP2011/063121 WO2011158712A1 (en) | 2010-06-16 | 2011-06-08 | Quartz glass crucible for pulling silicon single crystals, and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPWO2011158712A1 JPWO2011158712A1 (en) | 2013-08-19 |
| JP5901072B2 true JP5901072B2 (en) | 2016-04-06 |
Family
ID=45348114
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2012520388A Active JP5901072B2 (en) | 2010-06-16 | 2011-06-08 | Method for producing quartz glass crucible for pulling silicon single crystal |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP5901072B2 (en) |
| TW (1) | TWI554657B (en) |
| WO (1) | WO2011158712A1 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5823857B2 (en) * | 2011-12-29 | 2015-11-25 | 株式会社Sumco | Silica glass crucible with micron-level wavefront on the inner surface |
| 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 |
| US20150114284A1 (en) | 2013-04-08 | 2015-04-30 | Shin-Etsu Quartz Products Co., Ltd. | Silica container for pulling single crystal silicon and method for manufacturing the same |
| JP6546721B2 (en) * | 2014-05-19 | 2019-07-17 | 信越石英株式会社 | Quartz glass crucible for pulling single crystal silicon |
| JP6324837B2 (en) | 2014-07-31 | 2018-05-16 | 信越石英株式会社 | Manufacturing method of quartz glass crucible for pulling single crystal silicon |
| CN106012005A (en) * | 2016-07-13 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Measuring quartz rod |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11292694A (en) * | 1998-04-14 | 1999-10-26 | Nippon Steel Corp | Quartz crucible for pulling up silicon single crystal |
| JP2000327478A (en) * | 1999-04-16 | 2000-11-28 | Shinetsu Quartz Prod Co Ltd | Quartz glass crucible and production of the crucible |
| JP2004107163A (en) * | 2002-09-20 | 2004-04-08 | Toshiba Ceramics Co Ltd | Quartz crucible and its manufacturing method |
-
2011
- 2011-06-08 JP JP2012520388A patent/JP5901072B2/en active Active
- 2011-06-08 WO PCT/JP2011/063121 patent/WO2011158712A1/en active Application Filing
- 2011-06-10 TW TW100120357A patent/TWI554657B/en active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11292694A (en) * | 1998-04-14 | 1999-10-26 | Nippon Steel Corp | Quartz crucible for pulling up silicon single crystal |
| JP2000327478A (en) * | 1999-04-16 | 2000-11-28 | Shinetsu Quartz Prod Co Ltd | Quartz glass crucible and production of the crucible |
| JP2004107163A (en) * | 2002-09-20 | 2004-04-08 | Toshiba Ceramics Co Ltd | Quartz crucible and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2011158712A1 (en) | 2013-08-19 |
| TW201211329A (en) | 2012-03-16 |
| TWI554657B (en) | 2016-10-21 |
| WO2011158712A1 (en) | 2011-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5901072B2 (en) | Method for producing quartz glass crucible for pulling silicon single crystal | |
| JP5069663B2 (en) | Quartz glass crucible with multilayer structure | |
| JP4948504B2 (en) | Silicon single crystal pulling method | |
| JP4799536B2 (en) | High-purity quartz glass crucible for pulling up large-diameter silicon single crystal ingots that can reduce pinhole defects in large-diameter silicon single crystal ingots | |
| JP4918473B2 (en) | High-purity quartz glass crucible for pulling up large-diameter silicon single crystal ingot with high strength | |
| JP2001348240A (en) | Method for manufacturing quartz glass crucible | |
| JP4233059B2 (en) | Silica glass crucible for pulling silicon single crystal and method for producing the same | |
| JP4789437B2 (en) | Silica glass crucible for pulling silicon single crystal and method for producing the same | |
| WO2002068732A1 (en) | Recharge pipe for solid multicrystal material, and single crystal producing method using the same | |
| JP4975012B2 (en) | Silica glass crucible for pulling silicon single crystal and manufacturing method thereof | |
| JP4076416B2 (en) | Quartz crucible and its manufacturing method | |
| JP6324837B2 (en) | Manufacturing method of quartz glass crucible for pulling single crystal silicon | |
| JP6546721B2 (en) | Quartz glass crucible for pulling single crystal silicon | |
| JP2007191393A (en) | Large-caliber quartz glass crucible for pulling silicon single crystal, and its production method | |
| JP4338990B2 (en) | Silica glass crucible and silicon single crystal pulling method using the same | |
| JP5344767B2 (en) | Method for producing quartz glass crucible for pulling silicon single crystal | |
| JP2008162840A (en) | Method for producing quartz glass crucible | |
| JP4641760B2 (en) | Silica glass crucible for pulling silicon single crystals | |
| JP6451333B2 (en) | Method for producing silicon single crystal | |
| JP5226754B2 (en) | Manufacturing method of large diameter quartz glass crucible for pulling silicon single crystal | |
| JP2020196651A (en) | Method for manufacturing silica glass crucible | |
| JPH09241093A (en) | Quartz crucible having double layer structure for fusing of silicon | |
| JP2602442C (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20140328 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20150129 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20150327 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20150619 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20150727 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20151203 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20160118 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20160303 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20160307 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 5901072 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |