JP5121226B2 - Method for producing quartz glass crucible - Google Patents

Method for producing quartz glass crucible Download PDF

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JP5121226B2
JP5121226B2 JP2006353529A JP2006353529A JP5121226B2 JP 5121226 B2 JP5121226 B2 JP 5121226B2 JP 2006353529 A JP2006353529 A JP 2006353529A JP 2006353529 A JP2006353529 A JP 2006353529A JP 5121226 B2 JP5121226 B2 JP 5121226B2
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crucible
quartz powder
rim end
quartz
melted
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JP2008162839A (en
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弘史 岸
稔 神田
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Japan Super Quartz Corp
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    • 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

Description

本発明は、シリコン単結晶の引上げに用いる石英ガラスルツボについて、内部気泡の少ない均一なガラス層を有する石英ガラスルツボの製造方法に関する。   The present invention relates to a method for producing a quartz glass crucible having a uniform glass layer with few internal bubbles, with respect to a quartz glass crucible used for pulling up a silicon single crystal.

単結晶シリコンは主にＣＺ法によって製造されている。この方法は、高温下、石英ルツボ中のシリコン融液に種結晶を浸し、これを徐々に引き上げて単結晶シリコンを製造する方法であり、シリコン融液を溜める高純度の石英ガラスルツボが用いられている。   Single crystal silicon is mainly manufactured by the CZ method. In this method, a seed crystal is immersed in a silicon melt in a quartz crucible at a high temperature, and this is gradually pulled up to produce single crystal silicon. A high-purity quartz glass crucible for storing the silicon melt is used. ing.

単結晶シリコンの引上げに用いる石英ガラスルツボは主にアーク溶融法によって製造されている。この方法は、カーボン製の回転モールドの内表面に石英粉を一定厚さに堆積して石英粉成形体を形成し、モールドの内側上方に設置した電極のアーク放電によって石英粉を加熱溶融してガラス化し、石英ガラスルツボを製造する方法（回転モールド法）である。   Quartz glass crucibles used for pulling single crystal silicon are mainly manufactured by the arc melting method. In this method, quartz powder is deposited on the inner surface of a rotating mold made of carbon to a certain thickness to form a quartz powder compact, and the quartz powder is heated and melted by arc discharge of an electrode placed inside the mold. This is a method (rotating mold method) for producing a vitreous silica glass crucible.

上記製造方法において、ガラス層内部の気泡を除去するため、モールド側から吸引して石英粉成形体を減圧脱気しながら石英粉を溶融する方法が知られている（特許文献１、特許文献２）。この溶融工程において石英粉成形体を減圧脱気（これを真空引きと云う）するには、石英粉成形体の内表面を均一に薄く溶融させて表面に薄いガラス層を形成することによって内面をシールし、石英粉成形体内の真空度を上げる必要がある。   In the above manufacturing method, in order to remove bubbles inside the glass layer, a method is known in which quartz powder is melted while being sucked from the mold side and degassing the quartz powder molded body under reduced pressure (Patent Document 1, Patent Document 2). ). In this melting step, the quartz powder molded body is degassed under reduced pressure (this is called evacuation) by melting the inner surface of the quartz powder molded body uniformly and thinly to form a thin glass layer on the surface. It is necessary to seal and increase the degree of vacuum in the quartz powder molded body.

石英粉成形体を溶融してガラスルツボを製造する上記製造方法において、アーク溶融がモールド中心で始まる既存の製造方法では、ルツボ内面全体が同時に加熱されるので、石英粉を均一に溶融することができるが、石英粉成形体上部のリム端は、成形体の湾曲部や底部よりも保温性が低いためにリム端の溶融速度が遅く、リム端表面に薄いガラス層が十分に形成されないため、石英粉成形体の真空度が上がらず、ガラス層の内部気泡が少ないルツボを得ることができない。一方、リム端の溶融不足を補うために、アーク溶融の発熱量を増やして上記リム端を溶融すると、湾曲部や底部が過剰に加熱されて溶融し、石英粉成形体の形状が崩れやすくなると云う問題がある。
特開平０６−１９１９８６号公報 特開平１０−０２５１８４号公報 In the above manufacturing method for manufacturing a glass crucible by melting a quartz powder compact, in the existing manufacturing method in which arc melting starts at the center of the mold, the entire inner surface of the crucible is heated at the same time, so that the quartz powder can be uniformly melted. However, the rim end at the top of the quartz powder molded body has a lower heat retention than the curved part and bottom of the molded body, so the melting speed of the rim end is slow, and a thin glass layer is not sufficiently formed on the rim end surface. The degree of vacuum of the quartz powder compact does not increase, and a crucible with few internal bubbles in the glass layer cannot be obtained. On the other hand, when the rim end is melted by increasing the amount of heat generated by arc melting in order to compensate for the insufficient melting of the rim end, the curved part and the bottom part are excessively heated and melted, and the shape of the quartz powder compact tends to collapse. There is a problem.
Japanese Patent Laid-Open No. 06-191986 Japanese Patent Laid-Open No. 10-025184

本発明は、従来の製造方法における上記問題を解決したものであり、内部気泡の少ない均一なガラス層を有する石英ガラスルツボの製造方法を提供する。   This invention solves the said problem in the conventional manufacturing method, and provides the manufacturing method of the quartz glass crucible which has a uniform glass layer with few internal bubbles.

本発明の製造方法は、以下の構成によって従来の上記問題を解決した石英ガラスルツボの製造方法である。
（１）モールド内面に充填した石英粉成形体を真空引きしながらアーク溶融するルツボの製造方法において、石英粉成形体のリム端から石英粉の溶融を開始し、その後にアーク電極を下げまたはモールドを上げて、リム端から下側部分を加熱し溶融することを特徴とする石英ガラスルツボの製造方法。
（２）石英粉成形体のリム端から石英粉の溶融を開始し、その後、ルツボ壁部から湾曲部および底部の順に加熱し、ルツボの内面をシールする上記(１)に記載する石英カラスルツボの製造方法。
（３）アーク溶融開始からアーク総時間の１０％以内の時間内にルツボ内表面（リム端から側壁部、湾曲部、および底部）をシールする上記(１)または上記(２)に記載する石英ガラスルツボの製造方法。
（４）ルツボ内表面がシールされるまでに溶融した石英ガラス層厚（シール厚）が３mm以下である請求項１〜請求項３の何れかに記載する石英ガラスルツボの製造方法。 The manufacturing method of the present invention is a method for manufacturing a quartz glass crucible which has solved the above-described problems with the following configuration.
(1) In a crucible manufacturing method for arc melting while evacuating a quartz powder molded body filled in the mold inner surface, melting of the quartz powder is started from the rim end of the quartz powder molded body, and then the arc electrode is lowered or molded And a method for producing a quartz glass crucible, wherein the lower part is heated and melted from the rim end.
(2) The quartz powder crucible described in the above (1), in which the melting of the quartz powder is started from the rim end of the quartz powder molded body, and then the crucible wall portion is heated in the order of the curved portion and the bottom portion to seal the inner surface of the crucible. Production method.
(3) Quartz as described in (1) or (2) above, wherein the inner surface of the crucible (from the rim end to the side wall portion, the curved portion, and the bottom portion) is sealed within 10% of the total arc time from the start of arc melting. A method for producing a glass crucible.
(4) The method for producing a quartz glass crucible according to any one of claims 1 to 3, wherein the thickness of the fused silica glass (seal thickness) until the inner surface of the crucible is sealed is 3 mm or less.

本発明の製造方法は、モールド内面に充填した石英粉成形体を真空引きしながらアーク溶融するルツボの製造方法において、石英粉成形体のリム端から石英粉の溶融を開始するので上記リム端が十分に加熱され、リム端に内面シールが確実に形成される。また、リム端を溶融した後に、アーク電極を下げ、またはモールドを上げて、ルツボ側壁部から湾曲部および底部を加熱し溶融するので、これらの部分が過剰に加熱されず、石英粉成形体の内面全体に薄いガラス層の内面シールが均一に形成される。従って、石英粉成形体の真空度を高めることができ、内部気泡の少ない石英ガラスルツボを製造することができる。   In the manufacturing method of the present invention, in the crucible manufacturing method for arc melting while evacuating the quartz powder molded body filled in the mold inner surface, the melting of the quartz powder is started from the rim end of the quartz powder molded body. Sufficiently heated to ensure an internal seal at the rim end. Further, after melting the rim end, the arc electrode is lowered or the mold is raised, and the curved portion and the bottom portion are heated and melted from the crucible side wall, so that these portions are not excessively heated, and the quartz powder molded body A thin glass layer inner surface seal is uniformly formed on the entire inner surface. Therefore, the degree of vacuum of the quartz powder molded body can be increased, and a quartz glass crucible with few internal bubbles can be manufactured.

本発明の製造方法において、アーク溶融開始からアーク総時間の１０％以内の時間内にルツボ内表面を溶融してシールすることが好ましく、またルツボ内表面を加熱溶融して形成したシール厚みが３mm以下であることが好ましい。これにより、リム端を含めて側壁部および湾曲部、底部に至るルツボ全体を均一に適度に加熱溶融されて、ルツボ内面全体に薄いガラス層のシールが均一に形成することができる。   In the production method of the present invention, the inner surface of the crucible is preferably melted and sealed within 10% of the total arc time from the start of arc melting, and the seal thickness formed by heating and melting the inner surface of the crucible is 3 mm. The following is preferable. As a result, the entire crucible extending from the rim end to the side wall portion, the curved portion, and the bottom portion can be uniformly heated and melted uniformly and a thin glass layer seal can be uniformly formed on the entire inner surface of the crucible.

以下、本発明を実施形態に従って具体的に説明する。
本発明の製造方法は、モールド内面に充填した石英粉成形体を真空引きしながらアーク溶融するルツボの製造方法において、石英粉成形体のリム端から石英粉の溶融を開始し、その後にアーク電極を下げまたはモールドを上げて、リム端から下側部分を加熱し溶融することを特徴とする石英ガラスルツボの製造方法である。 Hereinafter, the present invention will be specifically described according to embodiments.
The manufacturing method of the present invention is a crucible manufacturing method for arc melting while evacuating a quartz powder molded body filled on the mold inner surface, and starts melting quartz powder from the rim end of the quartz powder molded body, and then the arc electrode The quartz glass crucible is produced by lowering or raising the mold and heating and melting the lower portion from the rim end.

回転モールドに充填した石英粉成形体の加熱溶融による石英ルツボ製造の概略を図１に示す。図示するように、回転するモールド１０の内面に石英粉１１が所定の厚さに充填されている。該モールド１０には真空引き用の通気孔１２が設けられており、該通気孔１２はモールド内面に開口している。上記モールド１０の中心線Ｌの線上にはアーク加熱用の電極１３が設けられている。さらに、上記モールド１０または電極１３を上下左右移動させる手段（図示省略）が設けられており、電極１３はモールド１０の中心線上において任意の位置に設定することができる。   FIG. 1 shows an outline of the production of a quartz crucible by heating and melting a quartz powder compact filled in a rotary mold. As shown in the drawing, the inner surface of the rotating mold 10 is filled with quartz powder 11 to a predetermined thickness. The mold 10 is provided with a vent hole 12 for evacuation, and the vent hole 12 opens on the inner surface of the mold. On the line of the center line L of the mold 10, an arc heating electrode 13 is provided. Furthermore, means (not shown) for moving the mold 10 or the electrode 13 up and down, left and right is provided, and the electrode 13 can be set at an arbitrary position on the center line of the mold 10.

本発明の製造方法は、モールド１０の石英粉成形体１２を真空引きしながら加熱溶融する場合、加熱開始時には電極１３をリム端１５の上方に設定しておき、リム端１５から石英粉の加熱溶融を開始する。リム端１５を所定時間加熱して溶融した後に、モールド１０を上げ、または電極１３を下げて、リム端１５の下側部分を加熱溶融する。下側部分の加熱はリム端１５に引き続いてルツボ側壁部１６から湾曲部１７および底部１８の順に加熱して溶融するのが好ましい。なお、ルツボの側壁部１６とはルツボの縦壁の部分であり、湾曲部１７とは側壁部１６に続き底部１８に至る部分、底部１８とは湾曲部１７に続く横に広がる部分である。また、リム端１５は側壁部１６の上端面である。   In the manufacturing method of the present invention, when the quartz powder molded body 12 of the mold 10 is heated and melted while evacuating, the electrode 13 is set above the rim end 15 at the start of heating, and the quartz powder is heated from the rim end 15. Start melting. After the rim end 15 is heated and melted for a predetermined time, the mold 10 is raised or the electrode 13 is lowered to heat and melt the lower portion of the rim end 15. It is preferable that the lower portion is heated and melted in this order from the crucible side wall 16 to the curved portion 17 and the bottom 18 following the rim end 15. The crucible side wall 16 is a portion of the crucible vertical wall, the curved portion 17 is a portion extending to the bottom 18 following the side wall 16, and the bottom 18 is a portion extending laterally following the curved portion 17. The rim end 15 is the upper end surface of the side wall portion 16.

上記リム端１５から加熱溶融する本発明の製造方法において、加熱時間の配分はアーク溶融開始からアーク総時間の１０％以内の時間内に石英粉成形体のリム端から側壁部、湾曲部、および底部を加熱溶融して内表面全体をシールするのが好ましい。なお、アーク温度およびアーク総時間はルツボの大きさによって設定される。具体的には、例えば、外径３０インチの石英ルツボについては、概ね、ルツボの温度１６００〜２５００℃であり、アーク総時間は６０分である。この場合、リム端１５からアーク溶融を開始し、アーク溶融開始から６分以内に、側壁部１６から湾曲部１７および底部１８の順に加熱溶融してルツボ内表面全体をシールするのが好ましい。   In the manufacturing method of the present invention in which the rim end 15 is heated and melted, the heating time is distributed within 10% of the total arc time from the start of arc melting, from the rim end of the quartz powder molded body to the side wall portion, the curved portion, and It is preferable to heat and melt the bottom to seal the entire inner surface. The arc temperature and the total arc time are set according to the size of the crucible. Specifically, for example, for a quartz crucible having an outer diameter of 30 inches, the temperature of the crucible is generally 1600 to 2500 ° C., and the total arc time is 60 minutes. In this case, it is preferable to start the arc melting from the rim end 15 and seal the entire crucible inner surface by heating and melting in order from the side wall portion 16 to the curved portion 17 and the bottom portion 18 within 6 minutes from the start of the arc melting.

上記製造方法において、ルツボ内表面がシールされるまでに溶融した石英ガラス層厚（シール厚）は３mm以下であることが好ましい。ルツボ内表面がシールされる前に溶融された石英ガラス層は多くの気泡を含んでいる。この気泡を取り除くには、石英ガラスを高温に加熱して、気泡のガスを脱気させ、気泡を消滅ないし小さくする必要がある。しかし、経済的に成り立つ製造条件において、高温加熱によって気泡を消滅ないし小さくする範囲は表面から深さ３mm程度までの範囲なので、それ以上にシール厚さを増すことは得策ではない。   In the above manufacturing method, the thickness of the fused silica glass layer (seal thickness) until the inner surface of the crucible is sealed is preferably 3 mm or less. The quartz glass layer melted before the inner surface of the crucible is sealed contains many bubbles. In order to remove the bubbles, it is necessary to heat the quartz glass to a high temperature to degas the bubbles, thereby eliminating or reducing the bubbles. However, in manufacturing conditions that are economically feasible, the range in which bubbles are eliminated or reduced by high-temperature heating is the range from the surface to a depth of about 3 mm, so it is not a good idea to increase the seal thickness beyond that.

アーク溶融開始からアーク溶融総時間の１０％以内の時間内に石英粉成形体のリム端から側壁部、湾曲部、および底部を加熱溶融してルツボ内表面全体をシールした後に、引き続き、真空引きしながら残りのアーク溶融時間を通じてアーク溶融を行い、石英粉成形体を加熱溶融しガラス化する。なお、真空引きはアーク溶融開始と共に行ってもよく、アーク溶融開始後の任意の時間、例えば、ルツボ内表面のシール後に開始してもよい。   Within 10% of the total arc melting time from the start of arc melting, the side wall, curved portion, and bottom are heated and melted from the rim end of the quartz powder compact to seal the entire crucible inner surface. While performing the remaining arc melting time, arc melting is performed, and the quartz powder compact is heated and melted to be vitrified. The evacuation may be performed simultaneously with the start of arc melting, or may be started at any time after the start of arc melting, for example, after sealing of the inner surface of the crucible.

以下に本発明の実施例を比較例と共に示す。
回転モールド法によって真空引きしながら石英粉成形体を加熱溶融し、外径３０インチの石英ルツボを製造する場合に、アーク総時間５０分において、表１に示す条件下で加熱溶融を行った。製造した石英ガラスルツボの内部気泡を測定した。この気泡含有率の測定は、例えば、光源から供給される光を被検体である石英ルツボに照射し、これを光学カメラ等の画像取り込み光学系によって撮影・観察し、この画像情報に基づいて、二値化、包括四角形計算、輪郭抽出等の画像処理を施し、内表面近傍に存在する気泡を検出する方法を利用すると良い（特開平11-228283号参照）。この結果を加熱条件と共に表１に示した。 Examples of the present invention are shown below together with comparative examples.
When producing a quartz crucible with an outer diameter of 30 inches by heating and melting the quartz powder compact while evacuating by the rotary mold method, the melt was performed under the conditions shown in Table 1 for a total arc time of 50 minutes. The internal bubbles of the manufactured quartz glass crucible were measured. The measurement of the bubble content is, for example, irradiating a quartz crucible which is a subject with light supplied from a light source, photographing and observing this with an image capturing optical system such as an optical camera, and based on this image information. A method of detecting bubbles present in the vicinity of the inner surface by performing image processing such as binarization, comprehensive quadrangle calculation, contour extraction, etc. may be used (see JP-A-11-228283). The results are shown in Table 1 together with the heating conditions.

表１に示すように、本発明の方法によって製造した実施例１〜実施例３のルツボは何れも内部気泡が大幅に少ない。一方、本発明の製造条件を外れた比較例１〜６のルツボはルツボの湾曲部および底部の内部気泡が何れも著しく多く、あるいは湾曲部の内部気泡が著しく多い。   As shown in Table 1, all of the crucibles of Examples 1 to 3 manufactured by the method of the present invention have significantly less internal bubbles. On the other hand, the crucibles of Comparative Examples 1 to 6 outside the production conditions of the present invention have remarkably many internal bubbles at the crucible and bottom of the crucible, or remarkably many internal bubbles at the bend.

Figure 0005121226
Figure 0005121226

回転モールド法による石英ガラスルツボ製造の概念図Conceptual diagram of quartz glass crucible production by rotary mold method

符号の説明Explanation of symbols

１０−モールド、１１−石英粉成形体、１２−通気孔、１３−電極、Ｌ−モールド中心線 10-mold, 11-quartz powder compact, 12-vent hole, 13-electrode, L-mold center line

Claims (1)

モールド内面に充填した石英粉成形体を真空引きしながらアーク溶融するルツボの製造方法において、石英粉成形体のリム端の上方に設置されたアーク電極を用いて、前記リム端から石英粉の溶融を開始し、前記リム端が溶融した後にアーク電極を下げまたはモールドを上げて、ルツボ壁部から湾曲部および底部の順に加熱して溶融し、ルツボの内表面をシールし、
アーク溶融開始からアーク総時間の１０％以内の時間内にルツボ内表面（リム端から側壁部、湾曲部、および底部）をシールし、
ルツボ内表面がシールされるまでに溶融した石英ガラス層厚（シール厚）が３ｍｍ以下であることを特徴とする石英ガラスルツボの製造方法。 In the crucible manufacturing method for arc melting while evacuating the quartz powder molded body filled in the inner surface of the mold, the quartz powder is melted from the rim end using an arc electrode installed above the rim end of the quartz powder molded body. After the rim end is melted , the arc electrode is lowered or the mold is raised , the crucible wall is heated and melted in this order from the crucible wall, and the inner surface of the crucible is sealed.
Seal the inner surface of the crucible (from the rim end to the side wall portion, the curved portion, and the bottom portion) within 10% of the total arc time from the start of arc melting,
Method for manufacturing a silica glass crucible of quartz glass layer thickness which is melted to the inner surface of the crucible is sealed (seal thickness) is characterized and this is 3mm or less.
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