JP2000072594A - Large aperture quartz glass crucible for pulling single silicon crystal and its production - Google Patents
Large aperture quartz glass crucible for pulling single silicon crystal and its productionInfo
- Publication number
- JP2000072594A JP2000072594A JP10243021A JP24302198A JP2000072594A JP 2000072594 A JP2000072594 A JP 2000072594A JP 10243021 A JP10243021 A JP 10243021A JP 24302198 A JP24302198 A JP 24302198A JP 2000072594 A JP2000072594 A JP 2000072594A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- glass crucible
- crucible
- pulling
- single crystal
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
Abstract
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【発明の属する技術分野】本発明は、シリコン単結晶の
引き上げに使用される大口径の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 large-diameter quartz glass crucible used for pulling a silicon single crystal and a method for producing the same.
【０００２】[0002]
【関連技術】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。2. Description of the Related Art Conventionally, a so-called Czochralski method has been widely adopted for producing a single crystal substance such as a single crystal semiconductor material. In this method, polycrystalline silicon is melted in a vessel, and the end of the seed crystal is immersed in the melting bath and pulled up while rotating. 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.
【０００３】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
面に周期的な振動波面が発生し、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 a silicon single crystal is pulled up, a periodic vibration wavefront is generated on the surface of the silicon melt, and the silicon seed crystal cannot be bonded to the silicon melt or the silicon single crystal crystal Disordered problems are a common occurrence.
【０００４】この原因のひとつとして、引き上げ時に供
給する加熱エネルギーが大きかったり、引き上げチャン
バー内の減圧度が大きかったりする場合、石英ガラス表
面とシリコンメルト液上面の接触部分の反応が活性化
し、ＳｉＯガスの発生が増大し、シリコンメルト液は石
英ガラス表面からはじかれ易くなり、湯面振動が強く発
生して、シリコンメルト液中央の状態が不安定になるこ
とが考えられている。One of the causes is that when the heating energy supplied at the time of pulling is large or the degree of pressure reduction in the pulling chamber is large, the reaction at the contact portion between the quartz glass surface and the upper surface of the silicon melt liquid is activated and SiO gas is activated. It is considered that the generation of the silicon melt increases, the silicon melt is easily repelled from the surface of the quartz glass, and the vibration of the molten metal surface is strongly generated, and the state of the center of the silicon melt becomes unstable.
【０００５】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、上記
加熱エネルギーと減圧度が増大する傾向にあり、湯面振
動の問題は、重要になってきた。In particular, in recent years, as the silicon single crystal becomes 8 ″ or more and the quartz glass crucible becomes larger in diameter, the above-mentioned heating energy and the degree of decompression tend to increase. Have been.
【０００６】上記のような現象を解決する１手段とし
て、石英ガラスるつぼ内表面のシリコンメルトに対する
濡れ性を向上させる方法が考えられる。濡れ性は、石英
ガラスるつぼ内表面の表面張力（表面自由エネルギー）
で定義できるが、表面張力に影響する特性としていくつ
かの因子がある。As a means for solving the above-mentioned phenomenon, a method of improving the wettability of the inner surface of the quartz glass crucible with respect to the silicon melt can be considered. Wettability is the surface tension (surface free energy) of the inner surface of the quartz glass crucible
There are several factors that affect the surface tension.
【０００７】濡れ性を決定する石英ガラスるつぼの因子
としては、内表面のＯＨ濃度と金属不純物濃度と表面粗
さがあげられる。内表面に存在するＯＨ基はガラス表面
に露出していて容易にＨ+を切り離して−の極性をも
ち、Ｓｉ+と可逆的に結合する。この反応が総じて多い
ほど、石英ガラスるつぼの内表面とシリコンメルトは良
く接着する。Factors of the quartz glass crucible that determine the wettability include the OH concentration on the inner surface, the metal impurity concentration, and the surface roughness. The OH group present on the inner surface is exposed on the glass surface, easily cuts off H + , has a negative polarity, and is reversibly bonded to Si + . The greater the number of reactions, the better the inner surface of the quartz glass crucible adheres to the silicon melt.
【０００８】次に、ＯＨ基と同様な効果を及ぼす因子と
して、石英ガラスるつぼの内表面の金属不純物がある。
金属不純物は、石英ガラスるつぼの内表面から＋イオン
の形で飛び出し、石英ガラスるつぼ内表面は−の極性を
もち、ＯＨ基と同様な機構によって、シリコンメルトと
石英ガラスるつぼの内表面は、良く接着するようにな
る。Next, as a factor having the same effect as the OH group, there is a metal impurity on the inner surface of the quartz glass crucible.
Metal impurities fly out from the inner surface of the quartz glass crucible in the form of + ions, and the inner surface of the quartz glass crucible has a negative polarity. By the same mechanism as that of the OH group, the inner surfaces of the silicon melt and the quartz glass crucible are improved. It comes to adhere.
【０００９】また、石英ガラスるつぼの内表面の表面粗
さが大きいと、内表面積が大きくなり、露出するＯＨ基
や金属不純物の飛び出しが増え、上記機構によって、シ
リコンメルトと石英ガラスるつぼ内表面は強い接着力を
もつようになる。Also, if the surface roughness of the inner surface of the quartz glass crucible is large, the inner surface area is increased, and the projection of exposed OH groups and metal impurities is increased, and the silicon melt and the inner surface of the quartz glass crucible are increased by the above mechanism. It comes to have strong adhesive strength.
【００１０】[0010]
【発明が解決しようとする課題】本発明は、上記した事
情に鑑みなされたもので、濡れ性を石英ガラスるつぼ内
表面に作り出すことによって、この石英ガラスるつぼを
用いてシリコン単結晶を引き上げる際にシリコンメルト
の湯面振動を抑制することができるようにしたシリコン
単結晶引き上げ用大口径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ものである。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned circumstances, and is intended to provide a wettability on the inner surface of a quartz glass crucible so that a silicon single crystal can be pulled up using the quartz glass crucible. An object of the present invention is to provide a large-diameter quartz glass crucible for pulling a silicon single crystal and a method of manufacturing the same, which can suppress the surface vibration of a silicon melt.
【００１１】[0011]
【課題を解決するための手段】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大口径石英ガラ
スるつぼの第１の態様は、半透明石英ガラス層のるつぼ
基体と、該るつぼ基体の内壁面に形成された透明石英ガ
ラス層からなるシリコン単結晶引き上げ用石英ガラスる
つぼであり、該石英ガラスるつぼの内表面の表面張力
が、５０ｍＮ／ｍ以下であることを特徴とする。この表
面張力が５０ｍＮ／ｍを越えると、シリコンメルトの湯
面振動が常に発生するという不利がある。In order to solve the above-mentioned problems, a first embodiment of a large-diameter quartz glass crucible for pulling a silicon single crystal according to the present invention is a crucible substrate having a translucent quartz glass layer and a crucible substrate. A quartz glass crucible for pulling a silicon single crystal, comprising a transparent quartz glass layer formed on the inner wall surface of the quartz glass crucible, wherein the surface tension of the inner surface of the quartz glass crucible is 50 mN / m or less. When the surface tension exceeds 50 mN / m, there is a disadvantage that the surface vibration of the silicon melt always occurs.
【００１２】上記石英ガラスるつぼの内表面の深さ方向
１．０ｍｍまでの平均ＯＨ濃度を調整することによって
上記表面張力の値を所定範囲に設定するのが好適であ
る。この平均ＯＨ濃度は１００ｐｐｍ以上であればよい
が、好ましくは、２００〜５００ｐｐｍである。Preferably, the value of the surface tension is set within a predetermined range by adjusting the average OH concentration of the inner surface of the quartz glass crucible up to 1.0 mm in the depth direction. The average OH concentration may be 100 ppm or more, but is preferably 200 to 500 ppm.
【００１３】上記石英ガラスるつぼの内表面の表面粗さ
を調整することによって前記表面張力の値を所定範囲に
設定するのが好適である。この表面粗さは、４μの距離
中で１０ｎｍ以上の高低差であればよいが、好ましく
は、２０〜５０，０００ｎｍの高低差である。It is preferable that the value of the surface tension is set within a predetermined range by adjusting the surface roughness of the inner surface of the quartz glass crucible. The surface roughness may have a height difference of 10 nm or more in a distance of 4 μm, and preferably has a height difference of 20 to 50,000 nm.
【００１４】上記石英ガラスるつぼの内表面の深さ方向
１ｍｍ以内の金属不純物濃度を調整することによって前
記表面張力の値を所定範囲に設定するのが好適である。
この金属不純物濃度は１ｐｐｍ以上であればよいが、好
ましくは、１０〜２００ｐｐｍである。It is preferable to set the value of the surface tension in a predetermined range by adjusting the concentration of metal impurities within 1 mm in the depth direction of the inner surface of the quartz glass crucible.
This metal impurity concentration may be 1 ppm or more, but is preferably 10 to 200 ppm.
【００１５】上記石英ガラスるつぼの内表面の深さ方向
１ｍｍ以内に使用する石英ガラス原料の含有ＯＨ濃度を
調整することによって前記表面張力の値を所定範囲に設
定するのが好適である。このＯＨ濃度は、２０ｐｐｍ以
上であればよいが、好ましくは、１００〜５００ｐｐｍ
である。It is preferable that the value of the surface tension is set in a predetermined range by adjusting the OH concentration of the quartz glass raw material used within 1 mm in the depth direction of the inner surface of the quartz glass crucible. The OH concentration may be 20 ppm or more, but is preferably 100 to 500 ppm.
It is.
【００１６】上記石英ガラスるつぼの内表面の１ｍｍ以
内の深さ範囲に使用する石英ガラス原料の比表面積を調
整することによって前記表面張力の値を所定範囲に設定
するのが好適である。この比表面積は、好ましくは、
１．０〜１００ｍ2 ／１００ｇである。It is preferable that the value of the surface tension is set in a predetermined range by adjusting the specific surface area of the quartz glass raw material used in a depth range of 1 mm or less of the inner surface of the quartz glass crucible. This specific surface area is preferably
1.0~100m is a 2 / 100g.
【００１７】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の第１の態様は、回転する上部開
口型を使用して石英ガラスるつぼの内表面の深さ方向
１．０ｍｍまでの平均ＯＨ濃度を調整することによって
表面張力を調節したシリコン単結晶引き上げ用石英ガラ
スるつぼを製造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、該るつぼ基体内の溶融加熱エリアの絶対湿度
を調整することによって製造される石英ガラスるつぼの
内表面の深さ方向１．０ｍｍまでの平均ＯＨ濃度を調整
し、該石英ガラスるつぼの表面張力の値を所定範囲に設
定することを特徴とする。The first aspect of the method for producing a quartz glass crucible for pulling a silicon single crystal according to the present invention is that an average OH of the inner surface of the quartz glass crucible up to 1.0 mm in the depth direction is set using a rotating upper opening die. A method for producing a quartz glass crucible for pulling a silicon single crystal in which the surface tension is adjusted by adjusting the concentration, comprising the steps of: (a) supplying silicon dioxide powder into the mold, and preforming along the inner surface of the mold; (B) a step of heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after the formation of the crucible substrate, a high-temperature gas atmosphere in the crucible substrate Forming a transparent quartz glass layer by supplying silicon dioxide powder inside and scattering and fusing toward the inner wall surface, and adjusting the absolute humidity of the melting and heating area in the crucible base. Thus, the average OH concentration of the inner surface of the quartz glass crucible manufactured up to 1.0 mm in the depth direction is adjusted, and the value of the surface tension of the quartz glass crucible is set within a predetermined range.
【００１８】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の第２の態様は、回転する上部開
口型を使用して石英ガラスるつぼの内表面の表面粗さを
調整して表面張力を調節したシリコン単結晶引き上げ用
石英ガラスるつぼを製造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、製造された石英ガラスるつぼの上端から該石
英ガラスるつぼにポリシリコンを充填し溶融した際のシ
リコンメルトの湯面の下方に位置する位置までの内表面
部を、加工研削手段で研削することによって該石英ガラ
スるつぼの内表面の表面粗さを調整し、該石英ガラスる
つぼの表面張力の値を所定範囲に設定することを特徴と
する。加工研削手段としては、ダイヤ砥石による研削な
どをあげることができる。In a second aspect of the method for producing a quartz glass crucible for pulling a silicon single crystal according to the present invention, the surface tension of the inner surface of the quartz glass crucible is adjusted by using a rotating upper opening die to reduce the surface tension. A method of manufacturing a controlled quartz glass crucible for pulling a silicon single crystal, comprising: (a) supplying silicon dioxide powder into the mold to form a pre-molded body along the inner surface of the mold; Heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after forming the crucible substrate, supplying silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate; A step of forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface, and filling the quartz glass crucible with polysilicon from the upper end of the manufactured quartz glass crucible and melting the silicon. The surface roughness of the inner surface of the quartz glass crucible is adjusted by grinding the inner surface portion to a position located below the melt surface of the melt by processing grinding means, and the value of the surface tension of the quartz glass crucible is adjusted. It is characterized in that it is set within a predetermined range. Examples of the processing and grinding means include grinding with a diamond whetstone.
【００１９】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の第３の態様は、回転する上部開
口型を使用して石英ガラスるつぼの内表面の表面粗さを
調整して表面張力を調節したシリコン単結晶引き上げ用
石英ガラスるつぼを製造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、製造された石英ガラスるつぼの上端から該石
英ガラスるつぼにポリシリコンを充填し溶融した際のシ
リコンメルトの湯面の下方に位置する位置までの内表面
部を、溶解液手段で溶解することによって該石英ガラス
るつぼの内表面の表面粗さを調整し、該石英ガラスるつ
ぼの表面張力の値を所定範囲に設定することを特徴とす
る。融解液手段としては、２０％ＨＦ溶液などをあげる
ことができる。In a third aspect of the method for producing a quartz glass crucible for pulling a silicon single crystal according to the present invention, the surface tension of the inner surface of the quartz glass crucible is adjusted by using a rotating upper opening die to reduce the surface tension. A method of manufacturing a controlled quartz glass crucible for pulling a silicon single crystal, comprising: (a) supplying silicon dioxide powder into the mold to form a pre-molded body along the inner surface of the mold; Heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after forming the crucible substrate, supplying silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate; A step of forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface, and filling the quartz glass crucible with polysilicon from the upper end of the manufactured quartz glass crucible and melting the silicon. The surface roughness of the inner surface of the quartz glass crucible is adjusted by dissolving the inner surface portion up to a position located below the melt surface of the melt by a dissolving means, and the value of the surface tension of the quartz glass crucible is adjusted. It is characterized in that it is set within a predetermined range. Examples of the melt solution include a 20% HF solution.
【００２０】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の第４の態様は、回転する上部開
口型を使用して石英ガラスるつぼの内表面の表面粗さを
調整して表面張力を調節したシリコン単結晶引き上げ用
石英ガラスるつぼを製造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、製造された石英ガラスるつぼの上端から該石
英ガラスるつぼにポリシリコンを充填し溶融した際のシ
リコンメルトの湯面の下方に位置する位置までの内表面
部を、加熱手段で昇華させることによって該石英ガラス
るつぼの内表面の表面粗さを調整し、該石英ガラスるつ
ぼの表面張力の値を所定範囲に設定することを特徴とす
る。加熱手段としては、酸水素バーナー等をあげること
ができる。この昇華によってＳｉＯ2 をとばしてアルミ
ナ部分を残留させて石英ガラスるつぼの内表面の表面粗
さを調整することができる。In a fourth aspect of the method for producing a quartz glass crucible for pulling a silicon single crystal according to the present invention, the surface tension of the inner surface of the quartz glass crucible is adjusted by using a rotating upper opening die to reduce the surface tension. A method of manufacturing a controlled quartz glass crucible for pulling a silicon single crystal, comprising: (a) supplying silicon dioxide powder into the mold to form a pre-molded body along the inner surface of the mold; Heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after forming the crucible substrate, supplying silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate; A step of forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface, and filling the quartz glass crucible with polysilicon from the upper end of the manufactured quartz glass crucible and melting the silicon. The surface roughness of the inner surface of the quartz glass crucible is adjusted by sublimating the inner surface portion up to a position located below the melt surface of the melt by a heating means, and the value of the surface tension of the quartz glass crucible is set to a predetermined value. It is characterized in that it is set in a range. Examples of the heating means include an oxyhydrogen burner. By this sublimation, SiO 2 is skipped, and the alumina portion is left, so that the surface roughness of the inner surface of the quartz glass crucible can be adjusted.
【００２１】上記した石英ガラスるつぼの上端から該石
英ガラスるつぼにポリシリコンを充填し溶融した際のシ
リコンメルトの湯面の下方に位置する位置までの内表面
部は、シリコンメルトの量に応じて変動するが、例えば
石英ガラスるつぼの上端からその全高さの７０％までに
すれば充分であり、好適には５０％までである。石英ガ
ラスるつぼの内表面部の表面粗さがあまり広範囲である
と、シリコン単結晶の引上げ作業に伴う面劣化が進み易
くなる不利がある。The inner surface portion from the upper end of the quartz glass crucible to a position below the surface of the silicon melt when the quartz glass crucible is filled with polysilicon and melted depends on the amount of the silicon melt. Although it fluctuates, it is sufficient to set, for example, 70% of the total height from the upper end of the quartz glass crucible, and preferably 50%. If the surface roughness of the inner surface of the quartz glass crucible is too wide, there is a disadvantage that the surface degradation accompanying the work of pulling the silicon single crystal is apt to progress.
【００２２】[0022]
【発明の実施の形態】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。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, 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 illustrative and should not be construed as limiting. Absent.
【００２３】図１は本発明方法の実施に使用される装置
と該装置を使用する石英ガラスるつぼ製造方法を示す断
面説明図である。図２は本発明の方法により得られたシ
リコン単結晶引上げ用石英ガラスるつぼの一部断面図で
ある。FIG. 1 is an explanatory sectional view showing an apparatus used for carrying out the method of the present invention and a method for manufacturing a quartz glass crucible using the apparatus. FIG. 2 is a partial cross-sectional view of a quartz glass crucible for pulling a silicon single crystal obtained by the method of the present invention.
【００２４】図１において、回転型１は回転軸２を備え
る。型１にはキャビティ１ａが形成され、この型キャビ
ティ１ａ内に二酸化珪素粉末、例えば天然石英粉末から
形成される半透明石英ガラス、すなわち外層を構成する
石英ガラスるつぼの基体３が配置されている。In FIG. 1, a rotary mold 1 has a rotating shaft 2. A cavity 1a is formed in the mold 1, and a semi-transparent quartz glass formed of silicon dioxide powder, for example, natural quartz powder, that is, a base 3 of a quartz glass crucible constituting an outer layer is arranged in the mold cavity 1a.
【００２５】該基体３は、二酸化珪素粉末を回転する型
１の中に投入し、該型１の内壁に沿って形成して所要の
るつぼ形状の前成型体とし、この前成型体を内面から加
熱して二酸化珪素粉末を溶融させたのち、冷却すること
により製造される。The substrate 3 is prepared by charging silicon dioxide powder into a rotating mold 1 and forming it along the inner wall of the mold 1 to obtain a required crucible-shaped preformed body. It is manufactured by heating to melt the silicon dioxide powder and then cooling.
【００２６】内面からの加熱のために、図１に示すよう
に電源１０に接続されたカーボン電極５１、５２を備え
るアーク放電装置５を使用することができる。アーク放
電装置５の代わりにプラズマ放電装置をしてもよい。こ
の基体３の製造については、特公平４−２２８６１号公
報に詳細な記載がある。For heating from the inner surface, an arc discharge device 5 having carbon electrodes 51 and 52 connected to a power source 10 as shown in FIG. 1 can be used. A plasma discharge device may be used instead of the arc discharge device 5. The production of the base 3 is described in detail in Japanese Patent Publication No. 4-22861.
【００２７】図１に示す装置は、内層４を形成するため
に、型１の上方に合成石英粉末６を収容する石英粉末供
給槽を備える。この供給槽９には計量フィーダ９２が設
けられた吐出パイプ９３に接続されている。供給槽９内
には攪拌羽根９１が配置される。型の上部は、スリット
開口７５を残して蓋７１により覆われる。The apparatus shown in FIG. 1 is provided with a quartz powder supply tank containing synthetic quartz powder 6 above the mold 1 for forming the inner layer 4. The supply tank 9 is connected to a discharge pipe 93 provided with a measuring feeder 92. A stirring blade 91 is disposed in the supply tank 9. The upper part of the mold is covered by a lid 71 leaving a slit opening 75.
【００２８】基体３が形成された後、又は基体３の形成
の途中において、アーク放電装置５のカーボン電極５
１、５２からの放電による加熱を継続しながら、合成石
英粉末６供給のための計量フィーダ９２を調整した開度
に開いて、吐出パイプ９３から合成石英粉末を基体３の
内部に供給する。アーク放電装置５の作動により、基体
３内には高温ガス雰囲気８が形成されている。したがっ
て、合成石英粉末は、この高温ガス雰囲気８中に供給さ
れることとなる。After or during the formation of the base 3, the carbon electrode 5 of the arc discharge device 5
The metering feeder 92 for supplying the synthetic quartz powder 6 is opened to an adjusted opening while the heating by the discharge from the discharges 1 and 52 is continued, and the synthetic quartz powder is supplied from the discharge pipe 93 into the base 3. By the operation of the arc discharge device 5, a high-temperature gas atmosphere 8 is formed in the substrate 3. Therefore, the synthetic quartz powder is supplied into the high-temperature gas atmosphere 8.
【００２９】なお、高温ガス雰囲気とは、カーボン電極
５１、５２を用いたアーク放電によりその周囲に形成さ
れた雰囲気を指し、石英ガラスを溶かすに十分な温度、
つまり２千数百度の高温になっている。The high-temperature gas atmosphere refers to an atmosphere formed by arc discharge using the carbon electrodes 51 and 52, and has a temperature sufficient to melt quartz glass.
That is, the temperature is as high as 2,000 and several hundred degrees.
【００３０】高温ガス雰囲気８中に供給された合成石英
粉末は、高温ガス雰囲気８内の熱により少なくとも一部
が溶融され、同時に基体３の内壁面に向けて飛散させら
れて、該基体３の内壁面に付着し、基体３と一体融合的
に基体３の内面に実質的に無気泡の石英ガラス層すなわ
ち内層４を形成する。この内層４の形成方法について
は、上述した特公平４−２２８６１号公報に詳細な記載
がある。The synthetic quartz powder supplied into the high-temperature gas atmosphere 8 is at least partially melted by the heat in the high-temperature gas atmosphere 8, and is simultaneously scattered toward the inner wall surface of the base 3, and A substantially bubble-free quartz glass layer, that is, an inner layer 4 is formed on the inner surface of the base 3 so as to adhere to the inner wall surface and integrally with the base 3. The method for forming the inner layer 4 is described in detail in the above-mentioned Japanese Patent Publication No. 4-22861.
【００３１】図２に、この方法により得られる石英ガラ
スるつぼの断面を示す。本発明による石英ガラスるつぼ
は、二酸化珪素粉末、例えば天然石英粉末を内面から加
熱溶融して形成された外層すなわち基体３と、合成石英
粉末を高温ガス雰囲気中に放出して、溶融飛散させ、基
体３の内壁面に付着させて形成した内層４とを有してい
るものである。FIG. 2 shows a cross section of a quartz glass crucible obtained by this method. The quartz glass crucible according to the present invention comprises an outer layer or base 3 formed by heating and melting silicon dioxide powder, for example, natural quartz powder from the inner surface, and a synthetic quartz powder which is released into a high-temperature gas atmosphere and melted and scattered. 3 and an inner layer 4 formed by adhering to the inner wall surface.
【００３２】[0032]
【実施例】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。EXAMPLES Hereinafter, the present invention will be described more specifically with reference to Examples, but the present invention is not limited to these Examples, and various modifications may be made without departing from the technical concept of the present invention. Is of course possible.
【００３３】（実施例１）絶対湿度が２５ｇ／ｍ3 以上
の溶融エリアにおいて、比表面積が１０ｍ2 ／１００ｇ
であり、粒径が５０ミクロンから５００ミクロンの天然
石英ガラス粉を、１００ｒｐｍで回転する内径７３０ｍ
ｍの成形型中に３０ｍｍの均一な厚さで堆積させ、アー
ク放電により内部から加熱溶融させると同時に、上方向
からＯＨ濃度が１００ｐｐｍの合成石英ガラス粉を、１
００ｇ／ｍｉｎの割合で供給し、泡のない透明ガラス層
を全内面領域にわたり、１〜３ｍｍの厚さで形成する。
溶融が終了し、冷却した石英ガラスるつぼを、成形型か
ら取り出し、その内面の状況を表１及び表２に示した測
定項目について測定し、その結果をあわせて表１及び表
２に示した。[0033] (Example 1) absolute humidity 25 g / m 3 or more melting area, a specific surface area of 10 m 2/100 g
, A natural quartz glass powder having a particle diameter of 50 to 500 microns is rotated at 100 rpm to an inner diameter of 730 m.
m in a mold having a uniform thickness of 30 mm and heated and melted from the inside by arc discharge. At the same time, synthetic quartz glass powder having an OH concentration of 100 ppm
The transparent glass layer is supplied at a rate of 00 g / min and has a thickness of 1 to 3 mm over the entire inner surface area.
After the melting was completed, the cooled quartz glass crucible was taken out of the mold, and the condition of the inner surface was measured for the measurement items shown in Tables 1 and 2, and the results are shown in Tables 1 and 2.
【００３４】[0034]
【表１】 [Table 1]
【００３５】[0035]
【表２】 [Table 2]
【００３６】表２において、ＡＡＳは原子吸光分析法(A
tomic Absorption Spectrometry)、ＩＣＰ−ＡＥＳは誘
導結合高周波プラズマ発光分光分析法(Inductively Cou
pledPlasma Atomic Emission Spectroscopy)及びＩＣＰ
−ＭＳは誘導結合高周波プラズマ質量分光光度計(Induc
tively Coupled Plasma Mass Spectrometer)をそれぞれ
指称する。In Table 2, AAS was determined by atomic absorption spectrometry (A
tomic Absorption Spectrometry), ICP-AES is an inductively coupled high frequency plasma emission spectroscopy (Inductively Cou
pledPlasma Atomic Emission Spectroscopy) and ICP
-MS is an inductively coupled high frequency plasma mass spectrophotometer (Induc
tively Coupled Plasma Mass Spectrometer).
【００３７】この石英ガラスるつぼにポリシリコンを充
填し溶融し、シリコン単結晶の引き上げを行った。シリ
コンメルトへの種付け、シリコン単結晶の引き上げ中に
シリコンメルトの振動は確認されず（表３）、安定して
引き上げが終了した。The quartz glass crucible was filled with polysilicon and melted, and a silicon single crystal was pulled. During the seeding of the silicon melt and the pulling of the silicon single crystal, no vibration of the silicon melt was confirmed (Table 3), and the pulling was completed stably.
【００３８】（実施例２）るつぼ内面透明層を形成する
とき使用する合成石英ガラス原料の含有ＯＨ濃度が５ｐ
ｐｍであるものを使用して実施例１と同様の手順で石英
ガラスるつぼを作成した。次に、この石英ガラスるつぼ
の高さの上端から７０％までの部分の内面を、２０％Ｈ
Ｆ溶液で６０分間洗浄した。この石英ガラスるつぼの性
状は表３に示した通りであった。さらに、この石英ガラ
スるつぼによって実施例１と同様にシリコン単結晶の引
き上げを行なったが、湯面振動がなかった（表３）。(Example 2) The synthetic quartz glass raw material used for forming the inner crucible inner transparent layer had an OH concentration of 5 p.
A quartz glass crucible was prepared in the same procedure as in Example 1 using a material having a pm capacity. Next, the inner surface of the portion up to 70% from the upper end of the height of the quartz glass crucible was polished by 20% H.
Washed with F solution for 60 minutes. The properties of the quartz glass crucible were as shown in Table 3. Further, a silicon single crystal was pulled up by using this quartz glass crucible in the same manner as in Example 1, but no surface vibration was observed (Table 3).
【００３９】（実施例３）るつぼ内面透明層を形成する
とき使用する合成石英ガラス原料の含有ＯＨ濃度が５ｐ
ｐｍで、かつ金属不純物濃度の総量が２０ｐｐｍである
ものを使用して実施例１と同様に石英ガラスるつぼを作
成した。次に、この石英ガラスるつぼの高さの上端から
７０％までの部分の内面をダイヤ砥石による研削によっ
て粗く削った。この石英ガラスるつぼの性状は表３に示
した通りであった。この石英ガラスるつぼによって実施
例１と同様にシリコン単結晶の引き上げを行なったが、
湯面振動はなかった（表３）。Example 3 The synthetic quartz glass raw material used when forming the inner crucible inner transparent layer had an OH concentration of 5 p.
A quartz glass crucible was prepared in the same manner as in Example 1 using a material having a pm and a total metal impurity concentration of 20 ppm. Next, the inner surface of the portion up to 70% from the upper end of the height of the quartz glass crucible was roughly ground by grinding with a diamond grindstone. The properties of the quartz glass crucible were as shown in Table 3. The silicon single crystal was pulled up using this quartz glass crucible in the same manner as in Example 1,
There was no level vibration (Table 3).
【００４０】（実施例４）るつぼ内面透明層を形成する
とき使用する天然石英ガラス原料の含有ＯＨ濃度が５ｐ
ｐｍであるものを使用して実施例１と同様に石英ガラス
るつぼを作成した。次に、この石英ガラスるつぼの高さ
の上端から７０％までの部分の内面を酸水素バーナーで
昇華した。この石英ガラスるつぼの性状は表３に示した
通りであった。この石英ガラスるつぼを用いて、実施例
１と同様にシリコン単結晶の引き上げを行った。シリコ
ンメルトへの種付け、単結晶の引き上げ中にシリコンメ
ルトの振動は確認されず、安定して引き上げが終了した
（表３）。Example 4 The natural quartz glass raw material used when forming the crucible inner transparent layer had an OH concentration of 5 p.
A quartz glass crucible was prepared in the same manner as in Example 1 using a material having the same pm. Next, the inner surface of the portion up to 70% from the upper end of the height of the quartz glass crucible was sublimated with an oxyhydrogen burner. The properties of the quartz glass crucible were as shown in Table 3. Using this quartz glass crucible, a silicon single crystal was pulled in the same manner as in Example 1. Vibration of the silicon melt was not confirmed during the seeding of the silicon melt and the pulling of the single crystal, and the pulling was stably completed (Table 3).
【００４１】（実施例５）るつぼ内面透明層を形成する
とき使用する石英原料粉として、含有ＯＨ濃度が５ｐｐ
ｍでかつ金属不純物濃度の総量が２０ｐｐｍである天然
石英ガラス粉を使用した以外は、実施例１と同様に石英
ガラスるつぼを作成した。この石英ガラスるつぼの性状
は表３に示した通りであった。この石英ガラスるつぼを
用いて、実施例１と同様にシリコン単結晶の引き上げを
行った。シリコンメルトへの種付け、単結晶の引き上げ
中にシリコンメルトの振動は確認されず、安定して引き
上げが終了した（表３）。(Example 5) As a quartz raw material powder used for forming a crucible inner transparent layer, the OH concentration was 5 pp.
m and a quartz glass crucible was prepared in the same manner as in Example 1 except that a natural quartz glass powder having a total metal impurity concentration of 20 ppm was used. The properties of the quartz glass crucible were as shown in Table 3. Using this quartz glass crucible, a silicon single crystal was pulled in the same manner as in Example 1. Vibration of the silicon melt was not confirmed during the seeding of the silicon melt and the pulling of the single crystal, and the pulling was stably completed (Table 3).
【００４２】（実施例６）実施例１と同様の手順で石英
ガラスるつぼを作成して、この石英ガラスるつぼの内面
全域を２０％ＨＦ溶液で６０分間洗浄した。この石英ガ
ラスるつぼの性状は表３に示した通りであった。さら
に、この石英ガラスるつぼによって実施例１と同様にシ
リコン単結晶の引上げを行ったが、湯面振動はなかった
（表３）。Example 6 A quartz glass crucible was prepared in the same procedure as in Example 1, and the entire inner surface of the quartz glass crucible was washed with a 20% HF solution for 60 minutes. The properties of the quartz glass crucible were as shown in Table 3. Further, a silicon single crystal was pulled up using this quartz glass crucible in the same manner as in Example 1, but no surface vibration was observed (Table 3).
【００４３】（比較例１）るつぼ内面透明層を形成する
とき使用する合成石英ガラス原料の含有ＯＨ濃度が５ｐ
ｐｍであるものを使用して実施例１と同様に石英ガラス
るつぼを作成した。この石英ガラスるつぼの性状は表３
に示した通りであった。この石英ガラスるつぼを用い
て、実施例１と同様にシリコン単結晶の引き上げを行っ
た。シリコンメルトへの種付け、単結晶の引き上げ中に
シリコンメルトの振動が強く確認され、引き上げを途中
で中止した（表３）。(Comparative Example 1) The synthetic quartz glass raw material used when forming the crucible inner transparent layer had an OH concentration of 5 p.
A quartz glass crucible was prepared in the same manner as in Example 1 using a material having the same pm. Table 3 shows the properties of this quartz glass crucible.
As shown in FIG. Using this quartz glass crucible, a silicon single crystal was pulled in the same manner as in Example 1. Vibration of the silicon melt was strongly confirmed during seeding of the silicon melt and pulling of the single crystal, and the pulling was stopped halfway (Table 3).
【００４４】[0044]
【表３】 [Table 3]
【００４５】[0045]
【発明の効果】以上述べたごとく、本発明によれば、濡
れ性を石英ガラスるつぼの内表面に作り出すことによっ
て、この石英ガラスるつぼを用いてシリコン単結晶を引
き上げる際にシリコンメルト液面の湯面振動を抑制する
ことができるという効果が達成されるものである。As described above, according to the present invention, wettability is created on the inner surface of a quartz glass crucible so that when a silicon single crystal is pulled up using the quartz glass crucible, hot water on the silicon melt liquid level is formed. The effect that surface vibration can be suppressed is achieved.
【図１】 本発明方法の実施に使用される装置と該装置
を使用する石英ガラスるつぼ製造方法を示す概略断面説
明図である。FIG. 1 is a schematic sectional explanatory view showing an apparatus used for carrying out the method of the present invention and a method for manufacturing a quartz glass crucible using the apparatus.
【図２】 本発明の方法により得られたシリコン単結晶
引上げ用石英ガラスるつぼの一部断面図である。FIG. 2 is a partial sectional view of a quartz glass crucible for pulling a silicon single crystal obtained by the method of the present invention.
１：型、１ａ：キャビティ、２：回転軸、３：基体、
４：内層、５：アーク放電装置、６：合成石英粉末、
８：高温ガス雰囲気、９：供給槽、１０：電源、５１、
５２：カーボン電極、７１：蓋、７５：スリット開口、
９１：攪拌羽根、９２：計量フィーダ、９３：吐出パイ
プ。1: mold, 1a: cavity, 2: rotating shaft, 3: base,
4: inner layer, 5: arc discharge device, 6: synthetic quartz powder,
8: high temperature gas atmosphere, 9: supply tank, 10: power supply, 51,
52: carbon electrode, 71: lid, 75: slit opening,
91: stirring blade, 92: metering feeder, 93: discharge pipe.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 岩谷 富士雄 福島県郡山市田村町金屋字川久保88番地 信越石英株式会社石英技術研究所内 Ｆターム(参考） 4G050 FD01 FD05 4G077 AA02 BA04 CF00 EG02 ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Fujio Iwatani 88, Kawakubo, Kanaya, Tamura-cho, Koriyama-shi, Fukushima Prefecture F-term in the Quartz Research Laboratory, Shin-Etsu Quartz Co., Ltd. (Reference) 4G050 FD01 FD05 4G077 AA02 BA04 CF00 EG02
Claims (10)
るつぼ基体の内壁面に形成された透明石英ガラス層から
なるシリコン単結晶引き上げ用石英ガラスるつぼであ
り、該石英ガラスるつぼの内表面の表面張力が、５０ｍ
Ｎ／ｍ以下であることを特徴とするシリコン単結晶引き
上げ用大口径石英ガラスるつぼ。1. A quartz glass crucible for pulling a silicon single crystal, comprising a crucible substrate of a translucent quartz glass layer and a transparent quartz glass layer formed on the inner wall surface of the crucible substrate. Surface tension is 50m
A large-diameter quartz glass crucible for pulling a silicon single crystal, which is not more than N / m.
向１．０ｍｍまでの平均ＯＨ濃度を調整することによっ
て、前記表面張力の値を所定範囲に設定してなることを
特徴とする請求項１記載のシリコン単結晶引き上げ用大
口径石英ガラスるつぼ。2. The value of the surface tension is set in a predetermined range by adjusting an average OH concentration up to 1.0 mm in a depth direction of an inner surface of the quartz glass crucible. 2. A large-diameter quartz glass crucible for pulling a silicon single crystal according to 1.
さを調整することによって前記表面張力の値を所定範囲
に設定してなることを特徴とする請求項１又は２記載の
シリコン単結晶引き上げ用大口径石英ガラスるつぼ。3. The silicon single crystal pulling method according to claim 1, wherein the value of the surface tension is set within a predetermined range by adjusting the surface roughness of the inner surface of the quartz glass crucible. Large diameter quartz glass crucible.
向１ｍｍ以内の金属不純物濃度を調整することによって
前記表面張力の値を所定範囲に設定してなることを特徴
とする請求項１〜３のいずれか１項記載のシリコン単結
晶引き上げ用大口径石英ガラスるつぼ。4. The value of the surface tension is set in a predetermined range by adjusting a metal impurity concentration within 1 mm in a depth direction of an inner surface of the quartz glass crucible. A large-diameter quartz glass crucible for pulling a silicon single crystal according to any one of the above.
向１ｍｍ以内に使用する石英ガラス原料の含有ＯＨ濃度
を調整することによって前記表面張力の値を所定範囲に
設定してなることを特徴とする請求項１〜４のいずれか
１項記載のシリコン単結晶引き上げ用大口径石英ガスる
つぼ。5. The value of the surface tension is set to a predetermined range by adjusting the OH concentration of a quartz glass raw material used within 1 mm in the depth direction of the inner surface of the quartz glass crucible. The large-diameter quartz gas crucible for pulling a silicon single crystal according to claim 1.
以内の深さ範囲に使用する石英ガラス原料の比表面積を
調整することによって前記表面張力の値を所定範囲に設
定してなることを特徴とする請求項１〜５のいずれか１
項記載のシリコン単結晶引き上げ用大口径石英ガラスる
つぼ。6. 1 mm of the inner surface of the quartz glass crucible
The value of the surface tension is set in a predetermined range by adjusting a specific surface area of a quartz glass raw material used in a depth range of not more than 1.
A large-diameter quartz glass crucible for pulling a silicon single crystal according to the above item.
記載のシリコン単結晶引き上げ用石英ガラスるつぼを製
造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、該るつぼ基体内の溶融加熱エリアの絶対湿度
を調整することによって製造される石英ガラスるつぼの
内表面の深さ方向１．０ｍｍまでの平均ＯＨ濃度を調整
し、該石英ガラスるつぼの表面張力の値を所定範囲に設
定することを特徴とする石英ガラスるつぼの製造方法。7. The method according to claim 2, wherein a rotating upper opening type is used.
A method for producing a quartz glass crucible for pulling a silicon single crystal according to the above, comprising: (a) supplying silicon dioxide powder into the mold to form a pre-molded body along the inner surface of the mold; Heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after forming the crucible substrate, supplying silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate; Forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface, wherein the depth direction 1 of the inner surface of the quartz glass crucible manufactured by adjusting the absolute humidity of the melting and heating area in the crucible base is adjusted. A method of manufacturing a quartz glass crucible, comprising adjusting an average OH concentration up to 0.0 mm and setting a surface tension value of the quartz glass crucible within a predetermined range.
記載のシリコン単結晶引き上げ用石英ガラスるつぼを製
造する方法であって、 （ａ）二酸化珪素粉末を前記型内に供給して、該型内面
に沿って前成型体を形成する工程 （ｂ）前記前成型体を加熱溶融して、半透明石英ガラス
製るつぼ基体を形成する工程 （ｃ）このるつぼ基体の形成中もしくは形成後に、該る
つぼ基体内の高温ガス雰囲気中に二酸化珪素粉末を供給
し、内壁面に向って飛散融合させて透明石英ガラス層を
形成する工程 からなり、製造された石英ガラスるつぼの上端から該石
英ガラスるつぼにポリシリコンを充填し溶融した際のシ
リコンメルトの湯面の下方に位置する位置までの内表面
部を、加工研削手段で研削することによって該石英ガラ
スるつぼの内表面の表面粗さを調整し、該石英ガラスる
つぼの表面張力の値を所定範囲に設定することを特徴と
する石英ガラスるつぼの製造方法。8. The method according to claim 3, wherein a rotating upper opening type is used.
A method for producing a quartz glass crucible for pulling a silicon single crystal according to the above, comprising: (a) supplying silicon dioxide powder into the mold to form a pre-molded body along the inner surface of the mold; Heating and melting the pre-molded body to form a translucent quartz glass crucible substrate (c) during or after forming the crucible substrate, supplying silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate; A step of forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface, from the upper end of the manufactured quartz glass crucible, to filling the quartz glass crucible with polysilicon and lowering the surface of the silicon melt when melted. The surface roughness of the inner surface of the quartz glass crucible is adjusted by grinding the inner surface portion up to the position of the quartz glass crucible by processing grinding means, and the value of the surface tension of the quartz glass crucible is adjusted to a predetermined range. A method for manufacturing a quartz glass crucible, characterized in that the crucible is set in an enclosure.
３記載のシリコン単結晶引き上げ用石英ガラスるつぼを
製造する方法であって、（ａ）二酸化珪素粉末を前記型
内に供給して、該型内面に沿って前成型体を形成する工
程（ｂ）前記前成型体を加熱溶融して、半透明石英ガラ
ス製るつぼ基体を形成する工程（ｃ）このるつぼ基体の
形成中もしくは形成後に、該るつぼ基体内の高温ガス雰
囲気中に二酸化珪素粉末を供給し、内壁面に向って飛散
融合させて透明石英ガラス層を形成する工程からなり、
製造された石英ガラスるつぼの上端から該石英ガラスる
つぼにポリシリコンを充填し溶融した際のシリコンメル
トの湯面の下方に位置する位置までの内表面部を、溶解
液手段で溶解することによって該石英ガラスるつぼの内
表面の表面粗さを調整し、該石英ガラスるつぼの表面張
力の値を所定範囲に設定することを特徴とする石英ガラ
スるつぼの製造方法。9. The method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 3, using a rotating upper opening mold, comprising: (a) supplying silicon dioxide powder into the mold; Step (b) of forming a pre-molded body along the inner surface of the mold, and heating and melting the pre-molded body to form a translucent quartz glass crucible base (c) during or after forming the crucible base, Supplying a silicon dioxide powder into a high-temperature gas atmosphere in the crucible substrate, forming a transparent quartz glass layer by scattering and fusing toward the inner wall surface,
The inner surface portion from the upper end of the manufactured quartz glass crucible to a position below the surface of the silicon melt when the quartz glass crucible is filled with polysilicon and melted is melted by a dissolving solution means. A method for manufacturing a quartz glass crucible, comprising adjusting the surface roughness of the inner surface of a quartz glass crucible and setting the value of the surface tension of the quartz glass crucible to a predetermined range.
項３記載のシリコン単結晶引き上げ用石英ガラスるつぼ
を製造する方法であって、（ａ）二酸化珪素粉末を前記
型内に供給して、該型内面に沿って前成型体を形成する
工程（ｂ）前記前成型体を加熱溶融して、半透明石英ガ
ラス製るつぼ基体を形成する工程（ｃ）このるつぼ基体
の形成中もしくは形成後に、該るつぼ基体内の高温ガス
雰囲気中に二酸化珪素粉末を供給し、内壁面に向って飛
散融合させて透明石英ガラス層を形成する工程からな
り、製造された石英ガラスるつぼの上端から該石英ガラ
スるつぼにポリシリコンを充填し溶融した際のシリコン
メルトの湯面の下方に位置する位置までの内表面部を、
加熱手段で昇華させることによって該石英ガラスるつぼ
の内表面の表面粗さを調整し、該石英ガラスるつぼの表
面張力の値を所定範囲に設定することを特徴とする石英
ガラスるつぼの製造方法。10. The method for producing a quartz glass crucible for pulling a silicon single crystal using a rotating upper opening mold according to claim 3, wherein (a) supplying silicon dioxide powder into the mold; Step (b) of forming a pre-molded body along the inner surface of the mold, and heating and melting the pre-molded body to form a translucent quartz glass crucible base (c) during or after forming the crucible base, Supplying a silicon dioxide powder into a high-temperature gas atmosphere in the crucible base, and scattering and fusing the powder toward the inner wall surface to form a transparent quartz glass layer. The quartz glass crucible is formed from the upper end of the manufactured quartz glass crucible. The inner surface part up to the position located below the surface of the silicon melt when it is filled with polysilicon and melted,
A method for producing a quartz glass crucible, wherein the surface roughness of the inner surface of the quartz glass crucible is adjusted by sublimation by a heating means, and the value of the surface tension of the quartz glass crucible is set within a predetermined range.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24302198A JP4138959B2 (en) | 1998-08-28 | 1998-08-28 | Large diameter quartz glass crucible for pulling silicon single crystal and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24302198A JP4138959B2 (en) | 1998-08-28 | 1998-08-28 | Large diameter quartz glass crucible for pulling silicon single crystal and method for producing the same |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2007041697A Division JP4651119B2 (en) | 2007-02-22 | 2007-02-22 | Large diameter quartz glass crucible for pulling silicon single crystal |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2000072594A true JP2000072594A (en) | 2000-03-07 |
| JP2000072594A5 JP2000072594A5 (en) | 2007-04-12 |
| JP4138959B2 JP4138959B2 (en) | 2008-08-27 |
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ID=17097701
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24302198A Expired - Lifetime JP4138959B2 (en) | 1998-08-28 | 1998-08-28 | Large diameter quartz glass crucible for pulling silicon single crystal and method for producing the same |
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| Country | Link |
|---|---|
| JP (1) | JP4138959B2 (en) |
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|---|---|---|---|---|
| JP2001348240A (en) * | 2000-05-31 | 2001-12-18 | Shinetsu Quartz Prod Co Ltd | Method for manufacturing quartz glass crucible |
| CN1316074C (en) * | 2002-10-22 | 2007-05-16 | 日本超精石英株式会社 | Evaluation technology of reactivity of quartz glass and fused silicon and vibration of fused silicon surface |
| WO2009017071A1 (en) * | 2007-07-27 | 2009-02-05 | Japan Super Quartz Corporation | Method for manufacturing quartz glass crucible |
| JP2010168240A (en) * | 2009-01-21 | 2010-08-05 | Sumco Corp | Quartz glass crucible for pulling silicon single crystal and method for manufacturing the same |
| EP2075354A3 (en) * | 2007-12-28 | 2010-08-11 | Japan Super Quartz Corporation | Vitreous silica crucible for pulling single-crystal silicon |
| WO2011016177A1 (en) * | 2009-08-05 | 2011-02-10 | 信越石英株式会社 | Silica vessel and process for producing same |
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| JP2001348240A (en) * | 2000-05-31 | 2001-12-18 | Shinetsu Quartz Prod Co Ltd | Method for manufacturing quartz glass crucible |
| JP4592037B2 (en) * | 2000-05-31 | 2010-12-01 | 信越石英株式会社 | Method for producing quartz glass crucible |
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| WO2009017071A1 (en) * | 2007-07-27 | 2009-02-05 | Japan Super Quartz Corporation | Method for manufacturing quartz glass crucible |
| EP2174917A1 (en) * | 2007-07-27 | 2010-04-14 | Japan Super Quartz Corporation | Method for manufacturing quartz glass crucible |
| KR101331180B1 (en) * | 2007-07-27 | 2013-11-20 | 쟈판 스파 쿼츠 가부시키가이샤 | Method and apparatus for manufacturing vitreous silica crucible |
| JP5245129B2 (en) * | 2007-07-27 | 2013-07-24 | 株式会社Ｓｕｍｃｏ | Method for producing quartz glass crucible |
| US8047020B2 (en) | 2007-07-27 | 2011-11-01 | Japan Super Quartz Corporation | Method of producing vitreous silica crucible |
| EP2075354A3 (en) * | 2007-12-28 | 2010-08-11 | Japan Super Quartz Corporation | Vitreous silica crucible for pulling single-crystal silicon |
| JP2010168240A (en) * | 2009-01-21 | 2010-08-05 | Sumco Corp | Quartz glass crucible for pulling silicon single crystal and method for manufacturing the same |
| CN102471125A (en) * | 2009-08-05 | 2012-05-23 | 信越石英株式会社 | Silica vessel and process for producing same |
| JP2011032147A (en) * | 2009-08-05 | 2011-02-17 | Shinetsu Quartz Prod Co Ltd | Silica container and method of manufacturing the same |
| WO2011016177A1 (en) * | 2009-08-05 | 2011-02-10 | 信越石英株式会社 | Silica vessel and process for producing same |
| CN102471125B (en) * | 2009-08-05 | 2014-05-07 | 信越石英株式会社 | Silica vessel and process for producing same |
| US8815403B2 (en) | 2009-08-05 | 2014-08-26 | Shin-Etsu Quartz Products Co., Ltd. | Silica container and method for producing the same |
| US9145325B2 (en) | 2009-08-05 | 2015-09-29 | Shin-Etsu Quartz Products Co., Ltd. | Silica container and method for producing the same |
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