JPH11199369A - Quartz glass crucible for pulling up silicon single crystal and its production - Google Patents

Quartz glass crucible for pulling up silicon single crystal and its production

Info

Publication number
JPH11199369A
JPH11199369A JP10002548A JP254898A JPH11199369A JP H11199369 A JPH11199369 A JP H11199369A JP 10002548 A JP10002548 A JP 10002548A JP 254898 A JP254898 A JP 254898A JP H11199369 A JPH11199369 A JP H11199369A
Authority
JP
Japan
Prior art keywords
crucible
quartz glass
single crystal
glass crucible
mold
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
Application number
JP10002548A
Other languages
Japanese (ja)
Other versions
JP3625636B2 (en
Inventor
Kozo Kitano
浩三 北野
Hiroyuki Honma
浩幸 本間
Naoyuki Obata
直之 小畑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coorstek KK
Original Assignee
Toshiba Ceramics Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toshiba Ceramics Co Ltd filed Critical Toshiba Ceramics Co Ltd
Priority to JP00254898A priority Critical patent/JP3625636B2/en
Publication of JPH11199369A publication Critical patent/JPH11199369A/en
Application granted granted Critical
Publication of JP3625636B2 publication Critical patent/JP3625636B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/09Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C03B19/095Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Abstract

PROBLEM TO BE SOLVED: To produce a quartz glass crucible capable of improving the yield of a pulled-up silicon single crystal by forming a specific amount of oxygen-lacking defects in a layer at a specified distance from the inner surface of the crucible. SOLUTION: An oxygen-lacking defect part of 20-150 ppm is formed in a layer within 1 mm from an inner surface of a crucible. A carbon mold 12 is charged with a quartz powder 11 so as to form a crucible shape by rotating a crucible-forming mold 10 by a motor 17. The crucible-forming mold 10 charged with the quartz is transferred to a melting room 5. An inert gas (e.g. nitrogen) is flowed from a flowing-in opening 6 to the melting room 5 to replace the atmosphere so that the oxygen concentration of the atmosphere of the melting room 5 may be <=21% (e.g. <=1%). The quartz powder 11 is serially melted by charging an arc electrode 15 with electricity. A vacuum pump 20 is operated just after the start of the arc discharge, and a reduced pressure state is kept for a prescribed time (e.g. 10 min). A reducing gas (e.g. hydrogen) is flowed into the melting room at a 50-300 L/min from the time just before the start of the arc discharge for 5-15 min. Thereafter, the flowing in of the hydrogen is stopped and the arc discharge is maintained for a prescribed time (e.g. 30 min) to provide the objective crucible.

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、シリコン単結晶引
上げ用石英ガラスルツボおよびその製造方法に係わり、
特にシリコン単結晶引上げ収率を向上させたシリコン単
結晶引上げ用石英ガラスルツボおよびその製造方法に関
する。
The present invention relates to a quartz glass crucible for pulling a silicon single crystal and a method for producing the same.
In particular, the present invention relates to a quartz glass crucible for pulling a silicon single crystal having an improved silicon single crystal pulling yield and a method for producing the same.

【0002】[0002]

【従来の技術】半導体デバイスの基板に用いられるシリ
コン単結晶は、一般にチョクラルスキー法(CZ法)で
製造されており、このCZ法は石英ガラスルツボ内に多
結晶シリコン原料を装填し、装填されたシリコン原料を
周囲から加熱して溶融し、上方から吊り下げた種結晶を
シリコン融液に接触してから引き上げるものである。
2. Description of the Related Art A silicon single crystal used for a substrate of a semiconductor device is generally manufactured by a Czochralski method (CZ method). In the CZ method, a polycrystalline silicon raw material is loaded into a quartz glass crucible and loaded. The obtained silicon raw material is heated and melted from the surroundings, and the seed crystal suspended from above is brought into contact with the silicon melt and then pulled up.

【0003】CZ法に使用される石英ガラスルツボは、
シリコン単結晶の高純度化に伴い、石英ガラスルツボに
も高純度のものが要求されている。
[0003] The quartz glass crucible used in the CZ method is:
As the purity of silicon single crystals increases, high-purity quartz glass crucibles are also required.

【0004】このCZ法に使用される石英ガラスルツボ
は、一般に粉砕して精製した石英粉を回転可能な型を回
転させながらこの型内に供給し遠心力により型の周囲に
石英粉をルツボ状に充填させ、同時に内側からアークな
どで溶融して造られている。
A quartz glass crucible used in the CZ method is generally a method in which quartz powder refined by grinding is supplied into the mold while rotating a rotatable mold, and the quartz powder is crucible-shaped around the mold by centrifugal force. And fused at the same time from the inside with an arc or the like.

【0005】しかしながら、この型製法で造られた石英
ガラスルツボは、石英ガラスの中に気泡が多く含まれる
といった問題があった。
[0005] However, the quartz glass crucible manufactured by this mold manufacturing method has a problem that the quartz glass contains many air bubbles.

【0006】一方、このような気泡を含む石英ガラスル
ツボを用いてCZ法により多結晶シリコンから単結晶を
製造する場合、石英ガラスルツボ内に存在する気泡に起
因して結晶化が不安定になり、引上げられたシリコン単
結晶に転移が生じ易くなり、歩留まり低下の原因となっ
ていた。
On the other hand, when a single crystal is produced from polycrystalline silicon by the CZ method using a quartz glass crucible containing such bubbles, crystallization becomes unstable due to bubbles present in the quartz glass crucible. In addition, dislocation is likely to occur in the pulled silicon single crystal, which causes a reduction in yield.

【0007】その主な理由としては、斑点状のクリスト
バライトの融液シリコンへの混入である。
[0007] The main reason for this is that cristobalite in the form of spots is mixed into the molten silicon.

【0008】すなわち、この斑点状のクリストバライト
は石英ガラスルツボに次のような現象により形成される
と考えられる。
That is, it is considered that the cristobalite in the form of spots is formed in a quartz glass crucible by the following phenomenon.

【0009】第一に、シリコン単結晶の引上げ中に、シ
リコン融液によってシリコンルツボの内面が浸食され気
泡が開裂状態となりルツボ内面が荒れ、この荒れにより
生じた微細な突起が石英ガラスの結晶化の核となり斑点
状のクリストバライトが形成される。
First, during the pulling of the silicon single crystal, the inner surface of the silicon crucible is eroded by the silicon melt, and the bubbles are broken, so that the inner surface of the crucible is roughened. And cristobalite in the form of spots are formed.

【0010】次に、単結晶引上げ中に、ルツボの内表面
近傍に存在する析出不純物がルツボ内面におけるクリス
トバライトの形成を促進して上記同様の斑点状のクリス
トバライトを形成する。
Next, during pulling of the single crystal, precipitated impurities existing near the inner surface of the crucible promote formation of cristobalite on the inner surface of the crucible to form spotted cristobalite similar to the above.

【0011】このようにして生成されたクリストバライ
トがルツボから剥離し、溶融多結晶シリコン中に混入
し、引上げられるシリコン単結晶の成長に悪影響を与え
るなどの問題があった。
The cristobalite produced in this manner is separated from the crucible, mixed into the molten polycrystalline silicon, and has a problem of adversely affecting the growth of the pulled silicon single crystal.

【0012】この問題を解決するため、例えば特開平4
−22861号公報に記載されているように回転する型
内にシリカの基体を載置し、この基体内面にシリカ粉末
を供給し実質的に無気泡の透明石英ガラス層を形成して
2層とする石英ガラスルツボの製造方法の開示がある。
In order to solve this problem, see, for example,
A silica base is placed in a rotating mold as described in JP-A-22861, silica powder is supplied to the inner surface of the base to form a substantially bubble-free transparent quartz glass layer, and two layers are formed. There is a disclosure of a method for manufacturing a quartz glass crucible.

【0013】しかし、この方法は工程が複雑でかつ無気
泡の透明石英ガラス層の厚さを適正に制御するのが難し
いなどの問題点がある。
However, this method has problems that the process is complicated and it is difficult to appropriately control the thickness of the bubble-free transparent quartz glass layer.

【0014】また、クリストバライトに起因する不純物
の溶融シリコン中に混入するのを防止するために、失透
促進剤を石英ガラスルツボの内面に付着させ、石英ガラ
スルツボが高温に加熱されたとき失透したシリカの層を
形成し、結晶シリカ粒子が溶融シリコン中に混入するの
を防止する方法が特開平9−110579号公報に開示
されている。
Further, in order to prevent impurities caused by cristobalite from being mixed into the molten silicon, a devitrification promoting agent is adhered to the inner surface of the quartz glass crucible, and when the quartz glass crucible is heated to a high temperature, it is devitrified. Japanese Patent Application Laid-Open No. Hei 9-110579 discloses a method for forming a layer of silica and preventing crystalline silica particles from being mixed into molten silicon.

【0015】しかし、この方法は例えば金属酸化物やそ
の他の酸化物を失透促進剤として用いるので、これら酸
化物が溶融シリコンに融出し、単結晶化およびシリコン
ウェーハ特性に悪影響を与える虞があり、また信頼性に
も疑問がある。
However, since this method uses, for example, metal oxides and other oxides as devitrification accelerators, these oxides may be melted into molten silicon, which may adversely affect single crystallization and silicon wafer characteristics. There is also a question of reliability.

【0016】さらに、石英ガラスルツボの気泡の膨脹を
抑制し、気泡の開裂によるSiO2の破片が溶融シリコ
ン中に混入するのを防止するために、石英ガラスルツボ
の内面を所定の温度で、長時間加熱処理して石英ガラス
ルツボを製造する方法が特開平5−124889号公報
に開示されているが、この方法は比較的高温で、長時間
加熱するものであるので、生産性が悪く製造コストも高
くなるなどの問題点がある。
Further, in order to suppress the expansion of the bubbles in the quartz glass crucible and to prevent the fragments of SiO 2 from being mixed into the molten silicon due to the cleavage of the bubbles, the inner surface of the quartz glass crucible is maintained at a predetermined temperature. Japanese Patent Application Laid-Open No. 5-124889 discloses a method for producing a quartz glass crucible by heating for a long time. However, since this method involves heating at a relatively high temperature for a long time, the productivity is poor and the production cost is low. There is a problem that the cost increases.

【0017】[0017]

【発明が解決しようとする課題】このため、シリコン単
結晶引上げ収率が高く生産性に優れたシリコン単結晶引
上げ用石英ガラスルツボおよびその製造方法が要望され
ていた。
Therefore, there is a need for a quartz glass crucible for pulling a silicon single crystal which has a high silicon single crystal pulling yield and is excellent in productivity and a method for producing the same.

【0018】本発明は上述した事情を考慮してなされた
もので、石英ガラスルツボの内表面に酸素欠乏欠陥を形
成し、シリコン単結晶引上げ収率を向上させたシリコン
単結晶引上げ用石英ガラスルツボおよびその製造方法を
提供することを目的とする。
The present invention has been made in view of the above-mentioned circumstances, and has been made in view of the above circumstances. A quartz glass crucible for pulling a silicon single crystal has an oxygen deficiency defect formed on the inner surface of the quartz glass crucible and has an improved silicon single crystal pulling yield. And a method for producing the same.

【0019】[0019]

【課題を解決するための手段】上記目的を達成するため
になされた本願請求項1の発明は、ルツボ内表面から1
mm以内の層に酸素欠乏欠陥を20〜150ppm有す
ることを特徴とするシリコン単結晶引上げ用石英ガラス
ルツボであることを要旨としている。
Means for Solving the Problems In order to achieve the above-mentioned object, the invention of claim 1 of the present application is directed to a method in which an inner surface of a crucible is positioned at a distance of 1 mm.
The gist of the present invention is a quartz glass crucible for pulling a silicon single crystal, which has an oxygen deficiency defect of 20 to 150 ppm in a layer within mm.

【0020】本願請求項2の発明は、酸素濃度が21%
以下の溶融室に石英粉がルツボ状に充填され減圧可能な
ルツボ成形用型を用意し、このルツボ成形用型を減圧し
ながら所定時間保持し、さらにルツボ成形用型を減圧し
ながらアーク放電を開始するとともにアーク放電の開始
直後より所定量の還元性ガスを溶融室に所定時間流し、
その後ルツボ成形用型の減圧を停止し、この停止状態で
さらに所定時間アーク放電を行うことにより、還元雰囲
気中で溶融され、ルツボ内表面から1mm以内の層に酸
素欠乏欠陥を20〜150ppm有することを特徴とす
るシリコン単結晶引上げ用石英ガラスルツボの製造方法
であることを要旨としている。
According to the second aspect of the present invention, the oxygen concentration is 21%
A quartz crucible is filled in the following melting chamber in the form of a crucible, and a crucible-forming mold is prepared.The crucible-forming mold is held for a predetermined time while the pressure is reduced. Starting and flowing a predetermined amount of reducing gas into the melting chamber for a predetermined time immediately after the start of arc discharge,
After that, the depressurization of the crucible mold is stopped, and an arc discharge is further performed for a predetermined time in this stopped state, whereby the layer is melted in a reducing atmosphere, and the layer within 1 mm from the inner surface of the crucible has oxygen deficiency defects of 20 to 150 ppm. It is intended to provide a method for producing a quartz glass crucible for pulling a silicon single crystal characterized by the following.

【0021】本願請求項3の発明は、ルツボ成形用型を
減圧しながら所定時間保持し、さらにルツボ成形用型を
減圧しながらアーク放電を開始するとともにアーク放電
の開始直後より50〜300リットル/分の水素を溶融
室に5〜15分間流し、その後ルツボ成形用型の減圧を
停止し、この停止状態でさらに所定時間アーク放電を行
うことにより、還元雰囲気中で溶融され、ルツボ内表面
から1mm以内の層に酸素欠乏欠陥を20〜150pp
m有することを特徴とする請求項3に記載のシリコン単
結晶引上げ用石英ガラスルツボの製造方法であることを
要旨としている。
According to a third aspect of the present invention, the crucible mold is held for a predetermined time while depressurizing, the arc discharge is started while the crucible mold is further depressurized, and 50 to 300 liters / min. Per minute of hydrogen in the melting chamber for 5 to 15 minutes, and then the depressurization of the crucible-forming mold is stopped. By continuing arc discharge for a predetermined time in this stopped state, the crucible is melted in a reducing atmosphere and 1 mm from the crucible inner surface. Oxygen deficiency defects in layers within 20 to 150 pp
The gist of the present invention is a method for manufacturing a quartz glass crucible for pulling a silicon single crystal according to claim 3, wherein

【0022】本願請求項4の発明は、ルツボ成形用型の
減圧の停止と共に水素の流入を停止し、この状態でさら
に所定時間アーク放電を行うことにより、還元雰囲気中
で溶融され、ルツボ内表面から1mm以内の層に酸素欠
乏欠陥を20〜150ppm有することを特徴とする請
求項4に記載のシリコン単結晶引上げ用石英ガラスルツ
ボの製造方法であることを要旨としている。
According to a fourth aspect of the present invention, the flow of hydrogen is stopped at the same time as the depressurization of the crucible mold is stopped, and an arc discharge is further performed for a predetermined time in this state, whereby the crucible is melted in a reducing atmosphere and the inner surface of the crucible is melted. A method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 4, characterized in that the layer within 1 mm from the surface has oxygen deficiency defects of 20 to 150 ppm.

【0023】本願請求項5の発明は、還元雰囲気中で加
熱処理され、ルツボ内表面から1mm以内の層に酸素欠
乏欠陥を20〜150ppm有することを特徴とするシ
リコン単結晶引上げ用石英ガラスルツボであることを要
旨としている。
The invention according to claim 5 of the present invention is a quartz glass crucible for pulling a silicon single crystal, which is heat-treated in a reducing atmosphere and has 20 to 150 ppm of oxygen deficiency defects in a layer within 1 mm from the inner surface of the crucible. The gist is that there is.

【0024】本願請求項6の発明は、処理炉内に石英ガ
ラスルツボを用意し、石英ガラスルツボ内部に不活性ガ
スを所定量流して酸素濃度を1%以下にし、処理炉内を
所定の温度まで昇温し、この温度を維持しながら不活性
ガスを還元性ガスと置換して所定時間維持し、この時間
経過後再度処理炉内に不活性ガスを流入し炉内温度を室
温まで降温することにより、還元雰囲気中で加熱処理さ
れ、ルツボ内表面から1mm以内の層に酸素欠乏欠陥を
20〜150ppm有することを特徴とするシリコン単
結晶引上げ用石英ガラスルツボの製造方法であることを
要旨としている。
According to the invention of claim 6 of the present application, a quartz glass crucible is prepared in a processing furnace, a predetermined amount of an inert gas is flowed into the quartz glass crucible to reduce the oxygen concentration to 1% or less, and the inside of the processing furnace is heated to a predetermined temperature. The inert gas is replaced with a reducing gas while maintaining this temperature, and is maintained for a predetermined time. After the elapse of this time, the inert gas flows into the processing furnace again to lower the furnace temperature to room temperature. The gist of the present invention is to provide a method for producing a quartz glass crucible for pulling a silicon single crystal, which is heat-treated in a reducing atmosphere and has oxygen deficiency defects in a layer within 1 mm from the inner surface of the crucible having 20 to 150 ppm. I have.

【0025】本願請求項7の発明は、処理炉内に石英ガ
ラスルツボを用意し、石英ガラスルツボ内部に不活性ガ
スを所定量流して酸素濃度を1%以下にし、処理炉内を
800〜1200℃まで昇温し、この温度を維持しなが
ら不活性ガスを水素と置換して0.5〜10時間維持
し、この時間経過後に再度処理炉内に不活性ガスを流入
させて室温まで降温させることにより、還元雰囲気中で
加熱処理し、ルツボ内表面から1mm以内の層に酸素欠
乏欠陥を20〜150ppm有することを特徴とするシ
リコン単結晶引上げ用石英ガラスルツボの製造方法であ
ることを要旨としている。
According to a seventh aspect of the present invention, a quartz glass crucible is prepared in a processing furnace, and a predetermined amount of an inert gas is flowed into the quartz glass crucible to reduce the oxygen concentration to 1% or less. C., maintaining the temperature, replacing the inert gas with hydrogen and maintaining the temperature for 0.5 to 10 hours. After the elapse of this time, the inert gas is allowed to flow into the processing furnace again to lower the temperature to room temperature. In summary, it is a method of manufacturing a quartz glass crucible for pulling a silicon single crystal, which is heat-treated in a reducing atmosphere and has 20 to 150 ppm of oxygen deficiency defects in a layer within 1 mm from the inner surface of the crucible. I have.

【0026】[0026]

【発明の実施の形態】以下、本発明に係わる石英ガラス
ルツボの実施の形態およびその製造方法について添付図
面に基づき説明する。
DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of a quartz glass crucible according to the present invention and a method for manufacturing the same will be described below with reference to the accompanying drawings.

【0027】図1は本発明に係わる石英ガラスルツボ1
で、石英ガラスルツボ1の内表面2から1mm以内の層
3は酸素欠乏欠陥を20〜150ppm有する酸素欠乏
欠陥層として形成されている。
FIG. 1 shows a quartz glass crucible 1 according to the present invention.
The layer 3 within 1 mm from the inner surface 2 of the quartz glass crucible 1 is formed as an oxygen deficiency defect layer having 20 to 150 ppm of oxygen deficiency defects.

【0028】このような石英ガラスルツボ1を製造する
のに用いる製造装置を図2に従い説明する。
A manufacturing apparatus used for manufacturing such a quartz glass crucible 1 will be described with reference to FIG.

【0029】建屋内に隔壁4で仕切られた、例えば床が
3×3m、高さが5mの溶融室5が形成されこの溶融室
5に雰囲気ガスの流入口6と流出口7が備えられてい
る。溶融室5には、ルツボ製造装置8が設置され、この
ルツボ製造装置8は回転台9に載置されたルツボ成形用
型10を有する。
In the building, there is formed a melting chamber 5 having a floor of 3 × 3 m and a height of 5 m, for example, which is partitioned by a partition wall 4. The melting chamber 5 is provided with an inlet 6 and an outlet 7 for the atmospheric gas. I have. A crucible manufacturing device 8 is provided in the melting chamber 5, and the crucible manufacturing device 8 has a crucible forming die 10 mounted on a turntable 9.

【0030】このルツボ成形用型10は、ガス透過性部
材、例えばカーボンで形成され、ルツボ状に石英粉11
が充填されるカーボン型12と、このカーボン型12の
外周にガス通気路13を設けて配置された耐熱性、例え
ばSUS製で水冷される保持ジャケット14から構成さ
れている。
The crucible molding die 10 is formed of a gas permeable member, for example, carbon, and has a quartz powder 11 in a crucible shape.
And a holding jacket 14 which is heat-resistant, for example, made of SUS and is water-cooled. The holding jacket 14 is provided with a gas ventilation path 13 provided on the outer periphery of the carbon mold 12.

【0031】前記ルツボ成形用型10の上方には、ルツ
ボ状に充填された石英粉11に対向して熱源として、例
えばアーク電極15が設けられている。
Above the crucible-forming mold 10, for example, an arc electrode 15 is provided as a heat source facing the quartz powder 11 filled in a crucible shape.

【0032】前記ガス通気路13は、保持ジャケット1
4の下部に設けられた開口部16を介して、モータ17
によって駆動される回転軸18の中央に設けられたガス
導入路19と連結され、このガス導入路19は真空ポン
プ20に接続されている。
The gas passage 13 is provided with the holding jacket 1.
4 through an opening 16 provided in the lower part of the motor 4.
Is connected to a gas introduction path 19 provided at the center of a rotating shaft 18 driven by the motor, and the gas introduction path 19 is connected to a vacuum pump 20.

【0033】また、前記保持ジャケット14には水冷用
の冷却路21が設けられ、この冷却路21は回転軸18
の中心に設けられた水路22に接続されている。
The holding jacket 14 is provided with a cooling passage 21 for water cooling.
Is connected to a water channel 22 provided at the center of the

【0034】本発明に係わる石英ガラスルツボの製造方
法に用いられる製造装置は以上のような構造になってお
り、次に、本発明に係わる石英ガラスルツボの製造方法
を説明する。
The manufacturing apparatus used in the method for manufacturing a quartz glass crucible according to the present invention has the above-described structure. Next, a method for manufacturing a quartz glass crucible according to the present invention will be described.

【0035】最初に、モータ17を付勢し回転軸18を
介してルツボ成形用型10を回転させて、ルツボ成形用
型10を構成するカーボン型12と保持ジャケット14
を回転させ、カーボン型12に石英粉11をルツボ状に
充填する。
First, the motor 17 is urged to rotate the crucible-molding mold 10 via the rotating shaft 18 so that the carbon mold 12 and the holding jacket 14 constituting the crucible-molding mold 10 are formed.
Is rotated to fill the carbon mold 12 with the quartz powder 11 in a crucible shape.

【0036】次に、溶融室5に石英が充填されたルツボ
成形用型10を移す。そして、流入口6から不活性ガ
ス、例えば窒素を溶融室5に流して置換し、溶融室5の
雰囲気を酸素濃度21%以下、例えば1%以下とする。
Next, the crucible-forming mold 10 filled with quartz is transferred to the melting chamber 5. Then, an inert gas, for example, nitrogen is flown from the inflow port 6 into the melting chamber 5 for replacement, and the atmosphere in the melting chamber 5 is set to an oxygen concentration of 21% or less, for example, 1% or less.

【0037】なお、不活性ガスには窒素を含め、窒素の
ほかアルゴン、ヘリウム等、またはこれらと窒素との混
合ガスでもよい。
The inert gas includes nitrogen, and may be nitrogen, argon, helium, or a mixture of these and nitrogen.

【0038】しかる後、アーク電極15に通電し、ルツ
ボ状に充填された石英粉11をアーク放電による加熱に
よって内側から順次溶融する。アーク開始直後、真空ポ
ンプ20を作動させ、所定時間、例えば10分間減圧状
態に保持する。
Thereafter, the arc electrode 15 is energized, and the crucible-filled quartz powder 11 is sequentially melted from the inside by heating by arc discharge. Immediately after the start of the arc, the vacuum pump 20 is operated and kept in a reduced pressure state for a predetermined time, for example, 10 minutes.

【0039】アーク放電の開始直前から還元性ガス、例
えば水素を50〜300リットル/分、例えば150リ
ットル/分溶融室に流入させ、この状態を5〜15分
間、例えば10分間継続させ、溶融室3を還元雰囲気、
すなわち水素雰囲気に保つ。
Immediately before the start of the arc discharge, a reducing gas, for example, hydrogen is introduced into the melting chamber at 50 to 300 l / min, for example, 150 l / min, and this state is maintained for 5 to 15 minutes, for example, 10 minutes. 3 is a reducing atmosphere,
That is, a hydrogen atmosphere is maintained.

【0040】所定時間経過後、例えば10分経過後減圧
を止め大気圧に戻し、水素の流入も停止させ、この状態
で所定時間、例えば30分間アーク放電を維持し、石英
ガラスルツボ1を製造した。
After a lapse of a predetermined time, for example, 10 minutes, the depressurization is stopped and the pressure is returned to the atmospheric pressure, and the inflow of hydrogen is also stopped. In this state, the arc discharge is maintained for a predetermined time, for example, 30 minutes to produce a quartz glass crucible 1. .

【0041】なお、この製造工程ではルツボ1の層3以
外の層の溶融が行われているので、必ずしも水素を溶融
室5に送り完全な還元雰囲気を維持する必要はなく水素
の供給を止めてもよいが、水素を継続的に流し続けても
よい。
In this manufacturing process, since the layers other than the layer 3 of the crucible 1 are melted, it is not always necessary to send hydrogen to the melting chamber 5 to maintain a complete reducing atmosphere. Alternatively, the hydrogen may be continuously supplied.

【0042】また、還元性ガスは一酸化炭素、あるいは
メタン等の炭化水素ガスでもよい。
The reducing gas may be carbon monoxide or a hydrocarbon gas such as methane.

【0043】上述のように還元性雰囲気中で溶融されて
製造されたルツボ1は肉厚12〜20mmであり、内側
には3〜7mmの透明層部を有し、この透明層部につい
て可視・紫外分光光度計により測定したところ、245
nmに強い吸収が見られ、約120ppmの酸素欠乏欠
陥を有していた。
The crucible 1 produced by melting in a reducing atmosphere as described above has a thickness of 12 to 20 mm, and has a transparent layer portion of 3 to 7 mm inside, and the transparent layer portion is visible and transparent. When measured with an ultraviolet spectrophotometer, 245
Strong absorption was observed at nm, with about 120 ppm oxygen deficiency defects.

【0044】次に他の本発明に係わる石英ガラスルツボ
の製造方法の他の実施の形態について説明する。
Next, another embodiment of the method for manufacturing a quartz glass crucible according to the present invention will be described.

【0045】図3は本発明に係わる石英ガラスルツボの
製造方法の他の実施の形態に用いられる雰囲気処理炉を
示す概略図で、処理炉31は本体32と、この本体32
内に設けられ本体32の底部33に固定された炉台34
と、この炉台34に不活性ガス、例えば窒素、および還
元性ガス、例えば水素を送る仕切弁35、36が設けら
れた送気管37と石英ガラスルツボ38内のガスを排出
する排気管39が設けられている。
FIG. 3 is a schematic view showing an atmosphere processing furnace used in another embodiment of the method for manufacturing a quartz glass crucible according to the present invention. The processing furnace 31 includes a main body 32 and this main body 32.
Furnace base 34 provided inside and fixed to bottom 33 of main body 32
The furnace base 34 is provided with an air supply pipe 37 provided with gate valves 35 and 36 for sending an inert gas, for example, nitrogen, and a reducing gas, for example, hydrogen, and an exhaust pipe 39 for discharging gas in a quartz glass crucible 38. Have been.

【0046】前記炉台34には底面を上にして載置され
る石英ガラスルツボ38の上端部40の外周に位置して
石英リング41が設けられ、この石英リング41と上端
部40間には、気密用のパウダーシール42が敷き詰め
られている。
A quartz ring 41 is provided on the furnace base 34 at an outer periphery of an upper end portion 40 of a quartz glass crucible 38 placed on a bottom surface thereof. An airtight powder seal 42 is spread.

【0047】また、底部33および炉台34に設けら
れ、送気管37と排気管39が貫通する透孔43はパウ
ダーシールと石英ウールよりなるシール部材44で封止
されている。
A through hole 43 provided in the bottom 33 and the furnace base 34 and through which the air supply pipe 37 and the exhaust pipe 39 pass is sealed with a seal member 44 made of a powder seal and quartz wool.

【0048】本発明に係わる石英ガラスルツボの製造方
法の他の実施の形態に用いられる雰囲気処理炉は以上の
ような構造になっているから、石英ガラスルツボを製造
するには、上述石英ガラスルツボの製造方法の一部の製
造工程と同様にする。
The atmosphere treatment furnace used in another embodiment of the method for manufacturing a quartz glass crucible according to the present invention has the above-described structure. And some of the manufacturing steps of the manufacturing method described above.

【0049】すなわち、例えば28インチのルツボ成形
用型に石英粉をルツボ状に充填し、このルツボ成形用型
を回転させ、アーク放電により溶融し、外径28インチ
の石英ガラスルツボを製造する。
That is, for example, a 28-inch crucible-forming mold is filled with quartz powder in a crucible shape, and the crucible-forming mold is rotated and melted by arc discharge to produce a quartz glass crucible having an outer diameter of 28 inches.

【0050】このようにして製造された石英ガラスルツ
ボの上端部を一定幅、例えば100mm切除し、この上
端部の平行度をそろえる。
The upper end of the quartz glass crucible thus manufactured is cut off by a predetermined width, for example, 100 mm, and the upper end is made parallel.

【0051】しかる後、図3に示されるように、送気管
37と排気管39が石英ガラスルツボ38の内部に位置
するように石英ガラスルツボ38の底面を上にして石英
ガラスルツボ38を炉台34に載置し、上端部40の外
側と石英リング41間にパウダーシール42を敷き詰
め、石英ガラスルツボ38の内外の気密を保つ。
Thereafter, as shown in FIG. 3, the quartz glass crucible 38 is placed on the furnace base 34 with the bottom surface of the quartz glass crucible 38 facing upward so that the air supply pipe 37 and the exhaust pipe 39 are located inside the quartz glass crucible 38. , And a powder seal 42 is spread between the outside of the upper end portion 40 and the quartz ring 41 to keep the inside and outside of the quartz glass crucible 38 airtight.

【0052】その後、仕切弁35、送気管37を介して
石英ガラスルツボ38内に所定量、例えば0.5m3
時間の不活性ガス、例えば窒素を流しながら処理炉31
内の温度を800〜1200℃、例えば1100℃まで
上昇させ、仕切弁35を閉じる一方、仕切弁36を開放
し、窒素に代わる還元ガス、例えば水素を送気管37を
介して所定量、例えば0.5立方米/時間供給する。還
元ガスである水素を0.5〜10時間、例えば3時間供
給し続け、この状態を保持する。
Thereafter, a predetermined amount, for example, 0.5 m 3 / cm, is put into the quartz glass crucible 38 through the gate valve 35 and the air supply pipe 37.
Processing furnace 31 while flowing an inert gas such as nitrogen for a long time.
The internal temperature is raised to 800 to 1200 ° C., for example, 1100 ° C., and the gate valve 35 is closed, while the gate valve 36 is opened, and a reducing gas instead of nitrogen, for example, hydrogen is supplied through the air supply pipe 37 to a predetermined amount, for example, 0 °. Supply 5 cubic rice / hour. Hydrogen as a reducing gas is continuously supplied for 0.5 to 10 hours, for example, 3 hours, and this state is maintained.

【0053】しかる後、仕切弁36を閉じ、仕切弁35
を開放して水素を窒素に切替え、窒素を流しながら室温
まで降温する。
Thereafter, the gate valve 36 is closed, and the gate valve 35 is closed.
Is opened to switch hydrogen to nitrogen, and the temperature is lowered to room temperature while flowing nitrogen.

【0054】上述のように還元性雰囲気中で加熱処理さ
れて製造された石英ガラスルツボ1は、肉厚12〜20
mmであり、内側には3〜7mmの透明層部を有し、こ
の透明層部について可視・紫外分光光度計により測定し
たところ、245nmに強い吸収が見られ、100pp
mの酸素欠乏欠陥を有していた。
The quartz glass crucible 1 manufactured by the heat treatment in the reducing atmosphere as described above has a thickness of 12 to 20 mm.
mm, and has a transparent layer portion of 3 to 7 mm inside. When the transparent layer portion is measured by a visible / ultraviolet spectrophotometer, strong absorption at 245 nm is observed and 100 pp.
m oxygen deficiency defects.

【0055】なお、この245nmの吸収波長は、Si
−O−SiからOがとれた状態の酸素欠乏欠陥を示すも
のであり、この濃度はLamber−Beerの法則に
基づき、
The absorption wavelength of 245 nm is
This indicates oxygen deficiency defects in a state where O is removed from -O-Si, and the concentration is based on Lamber-Beer's law.

【数1】A=loge I0/I =kcd の式によって、c(吸収成分濃度)の値として算出する
ことができる。
## EQU1 ## The value of c (absorbed component concentration) can be calculated by the following equation: A = log I0 / I = kcd.

【0056】上記式においては、Aは吸光度、I0 は入
射光の強さ、Iは透過光の強さ、kは吸光係数、dは試
料の厚さを示すものである。
In the above equation, A is the absorbance, I0 is the intensity of the incident light, I is the intensity of the transmitted light, k is the extinction coefficient, and d is the thickness of the sample.

【0057】[0057]

【実施例】 実施例1 上記外径28インチで120ppmの酸素欠乏欠陥を有
する石英ガラスルツボを用い、カスプ(CUSP)型M
CZ単結晶引上装置を用いて例えば直径300mmシリ
コン単結晶の引上げを行った。原料であるポリシリコン
の200kgチャージで約100時間使用しても、転位
の発生が全く見られず、完全なシリコン単結晶が得られ
た。
Example 1 A cusp (CUSP) type M using a quartz glass crucible having an oxygen deficiency defect of 120 ppm with an outer diameter of 28 inches.
Using a CZ single crystal pulling apparatus, for example, a silicon single crystal having a diameter of 300 mm was pulled. Even when the raw material polysilicon was used for about 100 hours at a charge of 200 kg, no dislocation was observed at all, and a complete silicon single crystal was obtained.

【0058】単結晶引上げに使用した後の石英ガラスル
ツボの内表面は、全体に光沢のある状態を維持してお
り、クリストバライトの発生が見られた面積は約20%
であった。
The inner surface of the quartz glass crucible after being used for pulling a single crystal maintains a glossy state as a whole, and the area where cristobalite is observed is about 20%.
Met.

【0059】 実施例2 上述本発明に係わる石英ガラスルツボの製造方法の他の
実施の形態により製造された石英ガラスルツボを用い、
カスプ型MCZ単結晶引上装置を用いて例えば直径30
0mmシリコン単結晶の引上げを行った。ポリシリコン
200kgチャージで約100時間使用しても、転位の
発生が全く見られず、完全なシリコン単結晶が得られ
た。
Example 2 A quartz glass crucible manufactured according to another embodiment of the method for manufacturing a quartz glass crucible according to the present invention was used,
Using a cusp type MCZ single crystal pulling device, for example, with a diameter of 30
A 0 mm silicon single crystal was pulled. Even when used with 200 kg of polysilicon for about 100 hours, generation of dislocations was not observed at all, and a complete silicon single crystal was obtained.

【0060】単結晶引上げに使用した後の石英ガラスル
ツボの内表面は、全体に光沢のある状態を維持してお
り、クリストバライトの発生が見られた面積は20%で
あった。
The inner surface of the quartz glass crucible after being used for pulling a single crystal maintained a glossy state as a whole, and the area where cristobalite was observed was 20%.

【0061】 比較例1 カーボン型とSUS製水冷ジャケットからなる減圧可能
な回転型内に石英粉充填し、大気雰囲気の溶融室ヘ型を
移動し、アーク放電により溶融を開始し、アーク開始直
後から水素を150リットル/分流入した。
Comparative Example 1 Quartz powder was charged into a decompressible rotary mold composed of a carbon mold and a water-cooled SUS jacket, and the mold was moved to a melting chamber in the atmosphere to start melting by arc discharge. Hydrogen was introduced at 150 liter / min.

【0062】10分後に減圧と水素流入を停止し、さら
に20分間アークを維持して溶融し、外径28インチの
石英ルツボを製作した。
After 10 minutes, the pressure was reduced and the flow of hydrogen was stopped, and the arc was maintained for an additional 20 minutes to melt, thereby producing a quartz crucible having an outer diameter of 28 inches.

【0063】このルツボは肉厚12〜20mmであり内
面側には3〜7mmの透明層を有していた。透明層部に
つき可視・紫外分光光度計により測定したところ、24
5nmに弱い吸収が見られ、20ppm酸素欠乏欠陥を
有していた。
This crucible had a thickness of 12 to 20 mm and had a transparent layer of 3 to 7 mm on the inner surface side. The transparent layer was measured with a visible / ultraviolet spectrophotometer.
A weak absorption was observed at 5 nm, and had a 20 ppm oxygen deficiency defect.

【0064】このルツボを用いてカスプ型MCZ引上装
置により単結晶引上げを行った。
Using this crucible, a single crystal was pulled by a cusp type MCZ pulling apparatus.

【0065】ポリシリコン200kgチャージで約10
0時間使用し、直径300mm単結晶の引上げを行っ
た。引上げテイル部で転位が発生し、単結晶化率は80
%であった。引上げに使用した後の石英ガラスルツボの
内表面は全体に粗れが目立ち、クリストバライトの発生
が見られた面積は約70%であった。
Approximately 10 with a 200 kg charge of polysilicon
It was used for 0 hours, and a single crystal having a diameter of 300 mm was pulled. Dislocations occurred in the pull tail, and the single crystallization ratio was 80.
%Met. The inner surface of the quartz glass crucible after use for pulling was noticeably rough overall, and the area where cristobalite was observed was about 70%.

【0066】 比較例2 カーボン型とSUS製水冷ジャケットからなる減圧可能
な回転型内に石英粉充填し、窒素フローにより酸素濃度
1%以下に置換された溶融室ヘ型を移動し、減圧しなが
ら10分間保持した。その後、アーク放電により溶融を
開始し、アーク開始直後から水素を300リットル/分
流入したところ、SiO2 のべーパーが激しく発生し、
電極への付着によりアークの中断が頻発した。10分後
に減圧と水素流入を停止し、さらに20分間アークを維
持して溶融し、外径28インチの石英ルツボを製作し
た。
Comparative Example 2 Quartz powder was charged into a decompressible rotary mold composed of a carbon mold and a SUS water-cooled jacket, and the mold was moved to a melting chamber where the oxygen concentration was reduced to 1% or less by a nitrogen flow, and the pressure was reduced. Hold for 10 minutes. After that, melting was started by arc discharge. When hydrogen was introduced at a flow rate of 300 liters / minute immediately after the start of the arc, vapor of SiO 2 was generated violently,
Arc interruption frequently occurred due to adhesion to the electrode. After 10 minutes, the decompression and the inflow of hydrogen were stopped, and the arc was maintained for an additional 20 minutes for melting to produce a quartz crucible having an outer diameter of 28 inches.

【0067】このルツボの内表面は、電極からのペーパ
ーの落下による不具合が多数見られた。また、透明層部
は200ppmの酸素欠乏欠陥を有していた。
On the inner surface of this crucible, many problems were found due to the paper falling from the electrode. The transparent layer had 200 ppm oxygen deficiency defects.

【0068】[0068]

【発明の効果】以上に述べたように本発明に係わる石英
ガラスルツボは、ルツボの内表面から1mm以内の層に
酸素欠乏欠陥を20〜150ppmを存在させることに
より、単結晶引上げ中にクリストバライトの発生が少な
く、従って単結晶の転位が発生せずシリコン単結晶の収
率を改善することができる。また、このような石英ガラ
スルツボを容易に製造する方法を提供する。
As described above, the quartz glass crucible according to the present invention has an oxygen deficiency defect of 20 to 150 ppm in a layer within 1 mm from the inner surface of the crucible. Since the generation is small, the dislocation of the single crystal does not occur, and the yield of the silicon single crystal can be improved. Also, a method for easily manufacturing such a quartz glass crucible is provided.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明に係わる石英ガラスルツボの断面図。FIG. 1 is a sectional view of a quartz glass crucible according to the present invention.

【図2】本発明に係わる石英ガラスルツボの製造方法に
用いられる製造装置の概念図。
FIG. 2 is a conceptual diagram of a manufacturing apparatus used in a method for manufacturing a quartz glass crucible according to the present invention.

【図3】本発明に係わる石英ガラスルツボの製造方法の
他の実施の形態に用いられる製造装置の概念図。
FIG. 3 is a conceptual diagram of a manufacturing apparatus used in another embodiment of the method for manufacturing a quartz glass crucible according to the present invention.

【符号の説明】[Explanation of symbols]

1 石英ガラスルツボ 2 内表面 3 層 4 隔壁 5 溶融室 6 流入口 7 流出口 8 ルツボ製造装置 9 回転台 10 ルツボ成形用型 11 石英粉 12 カーボン型 13 通気路 14 保持ジャケット 15 アーク電極 16 開口部 17 モータ 18 回転軸 19 ガス導入路 20 真空ポンプ 21 冷却路 22 水路 31 処理炉 32 本体 33 底部 34 炉台 35 仕切弁 36 仕切弁 37 送気管 38 石英ガラスルツボ 39 排気管 40 上端部 41 石英リング 42 パウダーシール 43 透孔 44 シール部材 DESCRIPTION OF SYMBOLS 1 Quartz glass crucible 2 Inner surface 3 layer 4 Partition wall 5 Melting chamber 6 Inflow port 7 Outflow port 8 Crucible manufacturing apparatus 9 Turntable 10 Mold for crucible molding 11 Quartz powder 12 Carbon mold 13 Vent path 14 Holding jacket 15 Arc electrode 16 Opening 17 Motor 18 Rotating shaft 19 Gas introduction path 20 Vacuum pump 21 Cooling path 22 Water path 31 Processing furnace 32 Main body 33 Bottom part 34 Furnace base 35 Gate valve 36 Gate valve 37 Air supply pipe 38 Quartz glass crucible 39 Exhaust pipe 40 Upper end 41 Quartz ring 42 Powder Seal 43 Through hole 44 Seal member

Claims (7)

【特許請求の範囲】[Claims] 【請求項1】 ルツボ内表面から1mm以内の層に酸素
欠乏欠陥を20〜150ppm有することを特徴とする
シリコン単結晶引上げ用石英ガラスルツボ。
1. A quartz glass crucible for pulling a silicon single crystal, characterized in that a layer within 1 mm from the inner surface of the crucible has 20 to 150 ppm of oxygen deficiency defects.
【請求項2】 酸素濃度が21%以下の溶融室に石英粉
がルツボ状に充填され減圧可能なルツボ成形用型を用意
し、このルツボ成形用型を減圧しながら所定時間保持
し、さらにルツボ成形用型を減圧しながらアーク放電を
開始するとともにアーク放電の開始直後より所定量の還
元性ガスを溶融室に所定時間流し、その後ルツボ成形用
型の減圧を停止し、この停止状態でさらに所定時間アー
ク放電を行うことにより、還元雰囲気中で溶融され、ル
ツボ内表面から1mm以内の層に酸素欠乏欠陥を20〜
150ppm有することを特徴とするシリコン単結晶引
上げ用石英ガラスルツボの製造方法。
2. A crucible-forming mold is prepared in a melting chamber having an oxygen concentration of 21% or less, which is filled with quartz powder in a crucible shape, and the crucible-forming mold is held for a predetermined time while depressurizing the crucible-forming mold. Arc discharge is started while the mold is depressurized, and a predetermined amount of reducing gas is flowed into the melting chamber for a predetermined time immediately after the start of the arc discharge, and then the depressurization of the crucible mold is stopped. By performing the arc discharge for a time, it is melted in a reducing atmosphere, and oxygen-deficient defects are formed in a layer within 1 mm from the inner surface of the crucible.
A method for producing a quartz glass crucible for pulling a silicon single crystal, comprising 150 ppm.
【請求項3】 ルツボ成形用型を減圧しながら所定時間
保持し、さらにルツボ成形用型を減圧しながらアーク放
電を開始するとともにアーク放電の開始直後より50〜
300リットル/分の水素を溶融室に5〜15分間流
し、その後ルツボ成形用型の減圧を停止し、この停止状
態でさらに所定時間アーク放電を行うことにより、還元
雰囲気中で溶融され、ルツボ内表面から1mm以内の層
に酸素欠乏欠陥を20〜150ppm有することを特徴
とする請求項3に記載のシリコン単結晶引上げ用石英ガ
ラスルツボの製造方法。
3. Holding the crucible mold for a predetermined time while depressurizing the mold, further starting arc discharge while decompressing the crucible mold, and starting 50 to 50 minutes after the start of the arc discharge.
300 liters / minute of hydrogen was flowed into the melting chamber for 5 to 15 minutes, and then the depressurization of the crucible mold was stopped. By continuing arc discharge for a predetermined time in this stopped state, the crucible was melted in a reducing atmosphere and melted in the crucible. The method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 3, wherein the layer within 1 mm from the surface has oxygen deficiency defects of 20 to 150 ppm.
【請求項4】 ルツボ成形用型の減圧の停止と共に水素
の流入を停止し、この状態でさらに所定時間アーク放電
を行うことにより、還元雰囲気中で溶融され、ルツボ内
表面から1mm以内の層に酸素欠乏欠陥を20〜150
ppm有することを特徴とする請求項4に記載のシリコ
ン単結晶引上げ用石英ガラスルツボの製造方法。
4. The flow of hydrogen is stopped at the same time as the decompression of the crucible mold is stopped, and an arc discharge is further performed for a predetermined time in this state to melt in a reducing atmosphere and form a layer within 1 mm from the inner surface of the crucible. 20-150 oxygen deficiency defects
The method for producing a quartz glass crucible for pulling a silicon single crystal according to claim 4, wherein the crucible has a content of 1 ppm.
【請求項5】 還元雰囲気中で加熱処理され、ルツボ内
表面から1mm以内の層に酸素欠乏欠陥を20〜150
ppm有することを特徴とするシリコン単結晶引上げ用
石英ガラスルツボ。
5. A heat treatment in a reducing atmosphere, wherein the layer within 1 mm from the inner surface of the crucible has an oxygen deficiency defect of 20 to 150 mm.
A quartz glass crucible for pulling a silicon single crystal, characterized by having ppm.
【請求項6】 処理炉内に石英ガラスルツボを用意し、
石英ガラスルツボ内部に不活性ガスを所定量流して酸素
濃度を1%以下にし、処理炉内を所定の温度まで昇温
し、この温度を維持しながら不活性ガスを還元性ガスと
置換して所定時間維持し、この時間経過後再度処理炉内
に不活性ガスを流入し炉内温度を室温まで降温すること
により、還元雰囲気中で加熱処理され、ルツボ内表面か
ら1mm以内の層に酸素欠乏欠陥を20〜150ppm
有することを特徴とするシリコン単結晶引上げ用石英ガ
ラスルツボの製造方法。
6. A quartz glass crucible is prepared in a processing furnace,
A predetermined amount of an inert gas is flowed into the quartz glass crucible to lower the oxygen concentration to 1% or less, and the inside of the processing furnace is heated to a predetermined temperature, and while maintaining this temperature, the inert gas is replaced with a reducing gas. After a predetermined time is maintained, an inert gas is flown into the processing furnace again after the elapse of this time, and the temperature in the furnace is lowered to room temperature, whereby the heat treatment is performed in a reducing atmosphere, and oxygen deficiency occurs in a layer within 1 mm from the inner surface of the crucible. 20-150ppm defect
A method for producing a quartz glass crucible for pulling a silicon single crystal, comprising:
【請求項7】 処理炉内に石英ガラスルツボを用意し、
石英ガラスルツボ内部に不活性ガスを所定量流して酸素
濃度を1%以下にし、処理炉内を800〜1200℃ま
で昇温し、この温度を維持しながら不活性ガスを水素と
置換して0.5〜10時間維持し、この時間経過後に再
度処理炉内に不活性ガスを流入させて室温まで降温させ
ることにより、還元雰囲気中で加熱処理し、ルツボ内表
面から1mm以内の層に酸素欠乏欠陥を20〜150p
pm有することを特徴とするシリコン単結晶引上げ用石
英ガラスルツボの製造方法。
7. A quartz glass crucible is prepared in a processing furnace,
A predetermined amount of an inert gas is flowed into the quartz glass crucible to reduce the oxygen concentration to 1% or less, the temperature in the processing furnace is raised to 800 to 1200 ° C., and the inert gas is replaced with hydrogen while maintaining this temperature to 0%. 0.5 to 10 hours, after this time elapses, an inert gas is again flown into the processing furnace to lower the temperature to room temperature, thereby performing heat treatment in a reducing atmosphere, and oxygen deficiency in a layer within 1 mm from the inner surface of the crucible. 20-150p defect
pm, a method for producing a quartz glass crucible for pulling a silicon single crystal.
JP00254898A 1998-01-08 1998-01-08 Method for producing quartz glass crucible for pulling silicon single crystal Expired - Lifetime JP3625636B2 (en)

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Application Number Priority Date Filing Date Title
JP00254898A JP3625636B2 (en) 1998-01-08 1998-01-08 Method for producing quartz glass crucible for pulling silicon single crystal

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