JP3798849B2 - Quartz crucible manufacturing apparatus and method - Google Patents

Quartz crucible manufacturing apparatus and method Download PDF

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Publication number
JP3798849B2
JP3798849B2 JP17953696A JP17953696A JP3798849B2 JP 3798849 B2 JP3798849 B2 JP 3798849B2 JP 17953696 A JP17953696 A JP 17953696A JP 17953696 A JP17953696 A JP 17953696A JP 3798849 B2 JP3798849 B2 JP 3798849B2
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Prior art keywords
mold
hollow
hollow mold
quartz crucible
quartz
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JPH1025184A (en
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龍弘 佐藤
光男 松村
繁夫 水野
博行 渡辺
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Shin Etsu Quartz Products Co Ltd
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Shin Etsu Quartz Products Co Ltd
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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

【０００１】
【発明の属する技術分野】
本発明は、石英ルツボの製造装置及び方法に関し、特に単結晶半導体材料、例えばシリコン単結晶の引き上げに用いられる石英ルツボの製造装置及び方法に関する。
【０００２】
【従来の技術】
単結晶半導体材料、例えばシリコン単結晶の製造には、チョクラルスキー法（ＣＺ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漬けて回転させながら引き上げるもので、種結晶上に種結晶と同一の結晶方位の単結晶が成長する。この単結晶の引き上げの容器には、石英ルツボが一般的に使用されている。
【０００３】
この石英ルツボを製造するには、回転可能な中空型に石英粉体を投入して該中空型を回転しながら石英粉体をアーク放電手段等の加熱手段によって加熱溶融し、遠心力の作用により溶融又は半溶融の石英粉体層を中空型の内周面に押圧してルツボの形状に焼結する方法が知られている。
【０００４】
上記方法によって製造された石英ルツボの壁体内部には気泡が多数残留する。石英ルツボの壁体に気泡が多いとルツボの強度が低下する上に、石英ルツボの加熱時にルツボ内周面付近の気泡が熱膨張して該内周面を部分的に剥離させ、剥離した石英小片が溶融シリコンに混入して単結晶化率を低下させるという問題があった。
【０００５】
そこで、内部気泡の少ない石英ルツボが求められ、その製造法として、中空型に充填した石英粉体を減圧下で加熱溶融する方法が知られている（特公昭５９−３４６５９号公報）。しかし、この方法によっても石英ルツボの壁体の内部気泡を完全に除去することは困難であった。また、その後も上記した内部気泡を除去するための提案が種々なされたが満足のいく結果を得られるものはなかった。
【０００６】
一方、近年、引き上げられるシリコン単結晶の大口径化が進むと同時に石英ルツボ並びに石英ルツボ製造用の中空型の大口径化も進行している。大口径の中空型の加工の困難性は、小口径の中空型に比べて格段に増大する。また、中空型の上部面は、熱で酸化消耗し易いが、大口径石英ルツボの製造に際しては、石英粉体の溶融時の被爆熱量が増し、かつ製造時間が延長するため、中空型の上面の消耗はさらに促進される。その結果、中空型の全体を交換する頻度が増大し、それだけ製造コストが高くなる欠点がある。
【０００７】
石英粉体を溶融している時には、中空型の直胴部には、内面から外面へ向けて温度差が生じる。内面が１０００℃程度のとき、外面は数１００℃と推定される。このような温度差が生じているとき、中空型の外表面には、強い引っ張り応力が発生し割れ易くなるという問題があった。
【０００８】
【発明が解決しようとする課題】
本発明は、上記した従来技術の問題点に鑑みなされたもので、石英ルツボの壁体の内部気泡を効率よく除去することを可能とした石英ルツボの製造装置及び方法を提供することを目的とする。
【０００９】
【課題を解決するための手段】
上記課題を解決するために、本発明の石英ルツボの製造装置は、水平回転自在な中空型と、該中空型の外周を減圧吸引する減圧吸引手段と、該中空型内を加熱する加熱手段とを具備した石英ルツボの製造装置であって、該中空型の内面に臨むように設けられた通気性部材と、一端が該通気性部材に接続し他端が該中空型の外周面と連通するように該中空型の壁体内部に穿設された吸引通路とを有し、前記中空型がカーボン質材料によって形成されるとともに、前記通気性部材が通気性カーボン質材料によって形成され、前記通気性部材のガス透過率が前記中空型のガス透過率よりも大きいことを特徴とする。
【００１０】
前記中空型を形成する材料としては、黒鉛やグラファイト等のカーボン質材料が好適である。
【００１１】
前記通気性部材は、前記中空型の内面に均一に多数配設されるものである。この通気性部材の配設の方法としては、各々の通気性部材の吸引範囲が交叉しないように配設するのが効率的であり、格子状の交点に通気性部材を配置する他に、吸引効率の観点からは、千鳥状（ジクザグ状）に通気性部材を配置するのが好適である。
【００１２】
該通気性部材を形成する材料としては、黒鉛やグラファイト等のカーボン質材料が好適である。該通気性部材はガスが透過可能であれば使用可能であり、中空型のガス透過率よりも大きいガス透過率を有することが必要であるが、好ましいガス透過率は平均圧力１ｋｇｆ／ｃｍ2 で１〜１０ｍ2 ／ｓ程度の範囲である。
【００１３】
前記中空型としては、上部型と下部型とからなり、該上部型と下部型とを接合することによって構成される、いわゆる２分割型の中空型を用いることもできる。この２分割型の中空型の場合には、中空型の内面と外面との温度差によって生ずる強い引っ張り応力は分散され、中空型の割れが回避される利点がある。
【００１４】
この２分割型の中空型の場合には、前記通気性部材及び吸引通路は、上部型及び下部型の双方に設けることが可能であるが、この場合上部型と下部型の吸引通路の接続部分の漏れを密封する作業を行なう必要がある。下部型のみに通気性部材及び吸引通路を設けた場合には石英ルツボの上部の気泡の除去効率は多少低下するが、上部型と下部型の接続部分には吸引通路は存在せず、それだけ製造が容易となる利点がある。
【００１５】
本発明の石英ルツボの製造方法は、上記石英ルツボの製造装置を用い、回転する前記中空型の内周面に原料石英粉体を投入して石英粉体層を形成し、該石英粉体層をその内周面側から加熱溶融し、該加熱溶融時に該中空型の外面を減圧吸引して該石英粉体層内の内部ガスを前記通気性部材及び吸引通路を介して吸引排気しながら該石英粉体層をルツボ形状に焼結させることを特徴とする。該中空型としては、非分割型及び２分割型のいずれもが使用できる。
【００１６】
【発明の実施の形態】
以下に本発明の１つの実施の形態を添付図面に基いて説明する。図１は本発明の石英ルツボの製造装置の１例を示す縦断面図、図２は同上の横断面図及び図３は図１の要部を示す摘示断面図である。
【００１７】
図中、２は本発明に係る石英ルツボの製造装置で、水平回転自在な中空型４を有している。該中空型４は、黒鉛又はグラファイト等のカーボン質材料によって形成される。該中空型４は、不図示の回転駆動手段によって水平回転せしめられる。該中空型４の外周は、真空ポンプ等の減圧吸引手段Ｐに接続され、その外周が減圧吸引されるようになっている。６は、該中空型４の内面を加熱するための加熱手段、例えばアーク放電手段である。
【００１８】
８は、通気性部材で、該中空型４の内面に臨むように設けられている。該通気性部材８は、上記中空型４の内面に均一に多数配設されるものである。この通気性部材８の配設方法としては、各々の通気性部材８の吸引範囲が交叉しないように配設するのが効率的であり、格子状の交点に通気性部材８を配置すればよいが、吸引効率の観点からは千鳥状（ジグザグ状）に通気性部材８を配置するのが好適である。
【００１９】
該通気性部材８は、黒鉛又はグラファイト等の通気性カーボン質材料によって形成されている。１０は、該中空型４の壁体４ａの内部に穿設された吸引通路である。該吸引通路１０の一端は該通気性部材８に接続し、その他端は該中空型４の外周面と連通している。
【００２０】
Ｂは、前記中空型４の外周面に設けられた支持枠体で、該支持枠体Ｂの内底面に配置されたパッキン部材Ｃを介して該中空型４を支持するものである。
【００２１】
上記した製造装置を用いて石英ルツボを製造するに際しては、まず前記中空型４を回転しながら原料石英粉体を該中空型４の内周面に投入する。該石英粉体は、回転する中空型４の遠心力の作用により、該中空型４の内周面に押し付けられ、該内周面に沿って推積し、石英粉体層Ａが形成される。
【００２２】
次に、アーク放電手段等の加熱手段６により、該石英粉体層Ａをその内周面側から加熱溶融する。この加熱溶融とともに、該中空型４の外面、図示の例では底部外面を真空ポンプ等の減圧吸引手段Ｐによって減圧吸引し、該石英粉体層Ａ内の内部ガスを前記通気性部材８及び吸引通路１０を介して吸引排気する。
【００２３】
上記加熱溶融により、石英粉体層Ａはその内周面から外表面付近まで次第に溶融し、ルツボ状に焼結する。
【００２４】
図示した実施例においては、多数の通気性部材８としては、小円板状部材を多数独立して配設した場合を示したが、長方形状部材、正方形状部材、三角形状部材等を用いることができる他、該中空型４の内周面を一周する環状又はリング状部材を多数配設することも可能である。
【００２５】
次いで、本発明の別の実施の形態を添付図面に基いて説明する。図４は本発明の石英ルツボの別の例を示す縦断面図、図５は通気性部材の設置状態を示す図４の摘示拡大断面図である。
【００２６】
図４において、１２は石英ルツボ製造用中空型である。該中空型１２は上部型１４及び下部型１６から構成されている。
【００２７】
該上部型１４は円筒壁１４ａを有し、その下端部には上部接合段部壁１８が形成されている。該下部型１６は該上部型１４の円筒壁１４ａと同一径を有する円筒部１６ａと該円筒部１６ａの下部に連設された丸椀状の底部１６ｂとを有している。該円筒壁１４ａの上端部には下部接合段部壁２０が該上部接合段部壁１８に当接可能に形成されている。
【００２８】
３６は、通気性部材で、該下部型１６の内面に臨むように設けられている。該通気性部材３６は、上記下部型１６の内面に均一に多数配設されるものである。この通気性部材３６の配設方法としては、各々の通気性部材３６の吸引範囲が交叉しないように配設するのが効率的であり、格子状の交点に通気性部材３６を配置すればよいが、吸引効率の観点からは千鳥状（ジグザグ状）に通気性部材３６を配置するのが好適である。
【００２９】
該通気性部材３６は、黒鉛又はグラファイト等の通気性カーボン質材料によって形成されている。３８は、該下部型１６の壁体の内部に穿設された吸引通路である。該吸引通路３８の一端は該通気性部材３６に接続し、その他端は該下部型１６の外周面と連通している。
【００３０】
図４において、４０は本発明に係る石英ルツボの製造装置で、上記した中空型１２を有している。該中空型１２は、不図示の回転駆動手段によって水平回転せしめられる。該中空型１２の外周は、真空ポンプ等の減圧吸引手段Ｐに接続され、その外周が減圧吸引されるようになっている。４２は、該中空型１２の内面を加熱するための加熱手段、例えばアーク放電手段である。
【００３１】
４４は、該中空型１２の外周面を囲みかつ該中空型１２を支持するように設けられた支持枠体である。
【００３２】
上記した製造装置を用いて石英ルツボを製造するに際しては、まず前記中空型１２を回転しながら原料石英粉体を該中空型１２の内周面に投入する。該石英粉体は、回転する中空型１２の遠心力の作用により、該中空型１２の内周面に押し付けられ、該内周面に沿って推積し、石英粉体層４６が形成される。
【００３３】
次に、アーク放電手段等の加熱手段４２により、該石英粉体層４６をその内周面側から加熱溶融する。この加熱溶融とともに、該中空型１２の外面、図示の例では底部外面を真空ポンプ等の減圧吸引手段Ｐによって減圧吸引し、該石英粉体層４６内の内部ガスを前記通気性部材３６及び吸引通路３８を介して吸引排気する。
【００３４】
上記加熱溶融により、石英粉体層４６はその内周面から外表面付近まで次第に溶融し、ルツボ状に焼結する。
【００３５】
図示した実施の形態においては、多数の通気性部材３６としては、小円板状部材を多数独立して配設した場合を示したが、長方形状部材、正方形状部材、三角形状部材等を用いることができる他、該中空型１２の内周面を一周する環状又はリング状部材を多数配設することも可能である。
【００３６】
図示した例では、下部型１６にのみ通気性材料３６及び吸引通路３８を設けた構成を示したが、上部型１４にも通気性材料３６及び吸引通路３８を形成する構成を採用することも勿論可能である。
【００３７】
上記別の実施の形態で用いられる中空型１２は、上部型１４と下部型１６とによって２分割可能に構成されているため、材料となるカーボン塊のサイズが小さくて済み、材料の入手が簡単で、製造容易となりカーボン材料の純化も容易に行なうことができる。また、中空型の上部の酸化消耗が進んだ場合、上部型を交換すれば下部型をそのまま継続して使用でき、それだけコストダウンとなる。
【００３８】
【発明の効果】
以上述べた如く、本発明によれば、石英ルツボの壁体の内部気泡を効率よく除去することができるという大きな効果を奏する。また、本発明は２分割型の中空型に対しても適用可能である。
【図面の簡単な説明】
【図１】本発明の石英ルツボの製造装置の一例を示す縦断面図である。
【図２】同上の横断面図である。
【図３】図１の要部を示す摘示断面図である。
【図４】本発明の石英ルツボの製造装置の別の例を示す縦断面図である。
【図５】通気性部材の設置状態を示す図４の摘示拡大断面図である。
【符号の説明】
２，４０ 石英ルツボの製造装置
４，１２ 中空型
６，４２ 加熱手段
８，３６ 通気性部材
１０，３８ 吸引通路
１４ 上部型
１４ａ 壁体、円筒壁
１６ 下部型
１６ａ 円筒部
１６ｂ 底部
１８ 上部接合段部壁
２０ 下部接合段部壁
４４，Ｂ 支持枠体
４６，Ａ 石英粉体層
Ｃ パッキン部材
Ｐ 減圧吸引手段[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a quartz crucible manufacturing apparatus and method, and more particularly to a quartz crucible manufacturing apparatus and method used for pulling a single crystal semiconductor material such as a silicon single crystal.
[0002]
[Prior art]
A method called the Czochralski method (CZ method) is widely used for manufacturing a single crystal semiconductor material, for example, a silicon single crystal. In this method, polycrystalline silicon is melted in a container, and the end of the seed crystal is immersed in this melting bath and pulled up while rotating, and a single crystal having the same crystal orientation as the seed crystal grows on the seed crystal. . A quartz crucible is generally used for this single crystal pulling container.
[0003]
In order to manufacture this quartz crucible, quartz powder is charged into a rotatable hollow mold, and the quartz powder is heated and melted by a heating means such as an arc discharge means while rotating the hollow mold. A method is known in which a molten or semi-molten quartz powder layer is pressed against a hollow inner peripheral surface and sintered into the shape of a crucible.
[0004]
Many bubbles remain inside the wall of the quartz crucible manufactured by the above method. If the quartz crucible wall contains a large number of bubbles, the strength of the crucible decreases, and when the quartz crucible is heated, the bubbles near the inner peripheral surface of the crucible thermally expand, causing the inner peripheral surface to partially peel off. There has been a problem that small pieces are mixed with molten silicon to reduce the single crystallization rate.
[0005]
Therefore, a quartz crucible with few internal bubbles is required, and as a method for producing the quartz crucible, a method is known in which quartz powder filled in a hollow mold is heated and melted under reduced pressure (Japanese Patent Publication No. 59-34659). However, even with this method, it is difficult to completely remove the internal bubbles in the wall of the quartz crucible. In addition, various proposals for removing the above-mentioned internal bubbles have been made thereafter, but none of them has obtained satisfactory results.
[0006]
On the other hand, in recent years, the diameter of the silicon single crystal to be pulled has been increased, and at the same time, the diameter of the quartz crucible and the hollow type for manufacturing the quartz crucible has been increased. The difficulty in processing a large-diameter hollow mold is significantly increased compared to a small-diameter hollow mold. In addition, the upper surface of the hollow mold is easily oxidized and consumed by heat. However, when manufacturing a large-diameter quartz crucible, the amount of heat exposed to the explosion of the quartz powder is increased and the manufacturing time is extended. Consumption is further promoted. As a result, there is a disadvantage that the frequency of replacing the entire hollow mold increases and the manufacturing cost increases accordingly.
[0007]
When the quartz powder is melted, a temperature difference is generated from the inner surface toward the outer surface of the hollow straight body. When the inner surface is about 1000 ° C., the outer surface is estimated to be several 100 ° C. When such a temperature difference is generated, there is a problem that a strong tensile stress is generated on the outer surface of the hollow mold and is easily cracked.
[0008]
[Problems to be solved by the invention]
The present invention has been made in view of the above-described problems of the prior art, and an object thereof is to provide a quartz crucible manufacturing apparatus and method capable of efficiently removing internal bubbles in a quartz crucible wall. To do.
[0009]
[Means for Solving the Problems]
In order to solve the above problems, a quartz crucible manufacturing apparatus of the present invention includes a horizontally rotatable hollow mold, a vacuum suction means for vacuum suction of the outer periphery of the hollow mold, and a heating means for heating the inside of the hollow mold. A quartz crucible manufacturing apparatus comprising: a breathable member provided so as to face the inner surface of the hollow mold, one end connected to the breathable member, and the other end communicated with the outer peripheral surface of the hollow mold have a suction passage which is formed in the inside wall of the hollow type as said with hollow type is formed by the carbon material, the air-permeable member is formed by a breathable carbonaceous material, the vent The gas permeability of the conductive member is larger than the gas permeability of the hollow type .
[0010]
As the material for forming the hollow mold, a carbonaceous material such as graphite or graphite is suitable.
[0011]
A large number of the air-permeable members are uniformly arranged on the inner surface of the hollow mold. As a method of disposing the air-permeable member, it is efficient to dispose the air-absorbing members so that the suction ranges of the air-permeable members do not intersect with each other. From the viewpoint of efficiency, it is preferable to arrange the breathable members in a zigzag shape.
[0012]
As a material for forming the air-permeable member, a carbonaceous material such as graphite or graphite is suitable. The gas permeable member can be used as long as it allows gas to pass through. The gas permeable member needs to have a gas permeability larger than that of the hollow gas, but the preferred gas permeability is an average pressure of 1 kgf / cm 2 . The range is about 1 to 10 m 2 / s.
[0013]
As the hollow mold, a so-called two-divided hollow mold composed of an upper mold and a lower mold and configured by joining the upper mold and the lower mold may be used. In the case of this two-divided hollow type, the strong tensile stress generated by the temperature difference between the inner surface and the outer surface of the hollow mold is dispersed, and there is an advantage that cracking of the hollow mold is avoided.
[0014]
In the case of the two-divided hollow type, the air-permeable member and the suction passage can be provided in both the upper die and the lower die, but in this case, the connection portion between the upper die and the lower die suction passage. It is necessary to work to seal the leak. When a breathable member and a suction passage are provided only in the lower mold, the efficiency of removing the air bubbles at the top of the quartz crucible is somewhat reduced, but there is no suction passage in the connection part between the upper mold and the lower mold, and it is manufactured as much There is an advantage that becomes easy.
[0015]
The method for producing a quartz crucible of the present invention uses the quartz crucible production apparatus to form a raw material quartz powder on the inner peripheral surface of the rotating hollow mold to form a quartz powder layer. Is heated and melted from the inner peripheral surface side, and the outer surface of the hollow mold is sucked under reduced pressure at the time of heating and melting, and the internal gas in the quartz powder layer is sucked and exhausted through the breathable member and the suction passage. The quartz powder layer is sintered into a crucible shape. As the hollow type, both a non-divided type and a two-divided type can be used.
[0016]
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a longitudinal sectional view showing an example of a quartz crucible manufacturing apparatus according to the present invention, FIG. 2 is a transverse sectional view of the same, and FIG. 3 is a cutaway sectional view showing an essential part of FIG.
[0017]
In the figure, reference numeral 2 denotes a quartz crucible manufacturing apparatus according to the present invention, which has a hollow mold 4 that can be rotated horizontally. The hollow mold 4 is formed of a carbonaceous material such as graphite or graphite. The hollow mold 4 is horizontally rotated by a rotation driving means (not shown). The outer periphery of the hollow mold 4 is connected to a vacuum suction means P such as a vacuum pump, and the outer periphery thereof is sucked under reduced pressure. Reference numeral 6 denotes a heating means for heating the inner surface of the hollow mold 4, for example, an arc discharge means.
[0018]
Reference numeral 8 denotes a breathable member that is provided so as to face the inner surface of the hollow mold 4. A large number of the air-permeable members 8 are uniformly arranged on the inner surface of the hollow mold 4. As a method for disposing the air permeable members 8, it is efficient to dispose the air permeable members 8 so that the suction ranges of the air permeable members 8 do not cross each other, and the air permeable members 8 may be disposed at lattice-shaped intersections. However, from the viewpoint of suction efficiency, it is preferable to arrange the breathable members 8 in a zigzag shape (zigzag shape).
[0019]
The breathable member 8 is made of a breathable carbonaceous material such as graphite or graphite. Reference numeral 10 denotes a suction passage formed in the wall 4 a of the hollow mold 4. One end of the suction passage 10 is connected to the breathable member 8, and the other end communicates with the outer peripheral surface of the hollow mold 4.
[0020]
B is a support frame provided on the outer peripheral surface of the hollow mold 4, and supports the hollow mold 4 via a packing member C disposed on the inner bottom surface of the support frame B.
[0021]
When manufacturing a quartz crucible using the manufacturing apparatus described above, first, raw material quartz powder is put into the inner peripheral surface of the hollow mold 4 while rotating the hollow mold 4. The quartz powder is pressed against the inner peripheral surface of the hollow mold 4 by the action of the centrifugal force of the rotating hollow mold 4, and is accumulated along the inner peripheral surface to form a quartz powder layer A. .
[0022]
Next, the quartz powder layer A is heated and melted from the inner peripheral surface side by a heating means 6 such as an arc discharge means. Along with this heating and melting, the outer surface of the hollow mold 4, in the illustrated example, the bottom outer surface is sucked under reduced pressure by a vacuum suction means P such as a vacuum pump, and the internal gas in the quartz powder layer A is sucked into the breathable member 8 and the suction member 8. Suction exhaust is performed through the passage 10.
[0023]
By the heating and melting, the quartz powder layer A is gradually melted from the inner peripheral surface to the vicinity of the outer surface, and sintered into a crucible shape.
[0024]
In the illustrated embodiment, the case where a large number of small disk-shaped members are independently arranged is shown as the large number of breathable members 8, but a rectangular member, a square member, a triangular member, or the like is used. In addition, it is also possible to arrange a large number of annular or ring-shaped members that go around the inner peripheral surface of the hollow mold 4.
[0025]
Next, another embodiment of the present invention will be described with reference to the accompanying drawings. FIG. 4 is a longitudinal sectional view showing another example of the quartz crucible of the present invention, and FIG. 5 is an enlarged enlarged sectional view of FIG. 4 showing an installation state of a breathable member.
[0026]
In FIG. 4, 12 is a hollow mold for producing a quartz crucible. The hollow mold 12 includes an upper mold 14 and a lower mold 16.
[0027]
The upper die 14 has a cylindrical wall 14a, and an upper joint step wall 18 is formed at the lower end thereof. The lower die 16 has a cylindrical portion 16a having the same diameter as the cylindrical wall 14a of the upper die 14 and a round bowl-shaped bottom portion 16b provided continuously to the lower portion of the cylindrical portion 16a. A lower joint step wall 20 is formed at the upper end of the cylindrical wall 14a so as to be able to contact the upper joint step wall 18.
[0028]
Reference numeral 36 denotes a gas permeable member provided so as to face the inner surface of the lower mold 16. A large number of the air-permeable members 36 are uniformly arranged on the inner surface of the lower mold 16. As a method for disposing the air permeable members 36, it is efficient to dispose the air permeable members 36 so that the suction ranges of the air permeable members 36 do not cross each other. The air permeable members 36 may be disposed at lattice-shaped intersections. However, from the viewpoint of suction efficiency, it is preferable to dispose the air-permeable member 36 in a zigzag shape.
[0029]
The breathable member 36 is made of a breathable carbonaceous material such as graphite or graphite. Reference numeral 38 denotes a suction passage drilled in the wall of the lower mold 16. One end of the suction passage 38 is connected to the air-permeable member 36, and the other end communicates with the outer peripheral surface of the lower mold 16.
[0030]
In FIG. 4, reference numeral 40 denotes a quartz crucible manufacturing apparatus according to the present invention, which has the hollow mold 12 described above. The hollow mold 12 is horizontally rotated by a rotation driving means (not shown). The outer periphery of the hollow mold 12 is connected to a decompression suction means P such as a vacuum pump, and the outer periphery thereof is sucked under reduced pressure. Reference numeral 42 denotes a heating means for heating the inner surface of the hollow mold 12, for example, an arc discharge means.
[0031]
Reference numeral 44 denotes a support frame provided so as to surround the outer peripheral surface of the hollow mold 12 and to support the hollow mold 12.
[0032]
When a quartz crucible is manufactured using the above-described manufacturing apparatus, first, raw material quartz powder is introduced into the inner peripheral surface of the hollow mold 12 while rotating the hollow mold 12. The quartz powder is pressed against the inner peripheral surface of the hollow mold 12 by the action of the centrifugal force of the rotating hollow mold 12, and is accumulated along the inner peripheral surface to form a quartz powder layer 46. .
[0033]
Next, the quartz powder layer 46 is heated and melted from the inner peripheral surface side by a heating means 42 such as an arc discharge means. Along with this heating and melting, the outer surface of the hollow mold 12, in the illustrated example, the bottom outer surface is sucked under reduced pressure by a vacuum suction means P such as a vacuum pump, and the internal gas in the quartz powder layer 46 is sucked into the breathable member 36 and the suction member 36. Suction exhaust is performed through the passage 38.
[0034]
By the heating and melting, the quartz powder layer 46 is gradually melted from the inner peripheral surface to the vicinity of the outer surface and sintered in a crucible shape.
[0035]
In the illustrated embodiment, a case where a large number of small disk-shaped members are independently arranged is shown as the large number of air-permeable members 36, but a rectangular member, a square member, a triangular member, or the like is used. In addition, a large number of annular or ring-shaped members that circulate around the inner peripheral surface of the hollow mold 12 can be provided.
[0036]
In the illustrated example, the configuration in which the air-permeable material 36 and the suction passage 38 are provided only in the lower mold 16 is shown, but it is needless to say that the configuration in which the air-permeable material 36 and the suction passage 38 are formed also in the upper mold 14 is adopted. Is possible.
[0037]
Since the hollow mold 12 used in the other embodiment is configured to be divided into two parts by the upper mold 14 and the lower mold 16, the size of the carbon lump used as the material can be small, and the material can be easily obtained. Thus, it becomes easy to manufacture and the carbon material can be easily purified. In addition, when the oxidation consumption of the upper part of the hollow mold progresses, if the upper mold is replaced, the lower mold can be used as it is, and the cost is reduced accordingly.
[0038]
【The invention's effect】
As described above, according to the present invention, there is a great effect that the internal bubbles of the wall of the quartz crucible can be efficiently removed. The present invention can also be applied to a two-part hollow type.
[Brief description of the drawings]
FIG. 1 is a longitudinal sectional view showing an example of a quartz crucible manufacturing apparatus according to the present invention.
FIG. 2 is a cross-sectional view of the above.
FIG. 3 is a cutaway cross-sectional view showing a main part of FIG. 1;
FIG. 4 is a longitudinal sectional view showing another example of the quartz crucible manufacturing apparatus of the present invention.
FIG. 5 is an enlarged cross-sectional view taken along the line in FIG. 4 showing an installation state of the breathable member.
[Explanation of symbols]
2,40 Quartz crucible manufacturing apparatus 4,12 Hollow mold 6,42 Heating means 8,36 Breathable member 10,38 Suction passage 14 Upper mold 14a Wall body, cylindrical wall 16 Lower mold 16a Cylindrical section 16b Bottom 18 Upper joint stage Part wall 20 Lower joint step part wall 44, B Support frame body 46, A Quartz powder layer C Packing member P Vacuum suction means

Claims (5)

水平回転自在な中空型と、該中空型の外周を減圧吸引する減圧吸引手段と、該中空型内を加熱する加熱手段とを具備した石英ルツボの製造装置であって、該中空型の内面に臨むように設けられた通気性部材と、一端が該通気性部材に接続し他端が該中空型の外周面と連通するように該中空型の壁体内部に穿設された吸引通路とを有し、前記中空型がカーボン質材料によって形成されるとともに、前記通気性部材が通気性カーボン質材料によって形成され、前記通気性部材のガス透過率が前記中空型のガス透過率よりも大きいことを特徴とする石英ルツボの製造装置。A quartz crucible manufacturing apparatus comprising a horizontally rotatable hollow mold, a vacuum suction means for vacuum suction of the outer periphery of the hollow mold, and a heating means for heating the inside of the hollow mold, the inner surface of the hollow mold being A breathable member provided so as to face, and a suction passage formed in the hollow wall so that one end is connected to the breathable member and the other end communicates with the outer peripheral surface of the hollow mold. Yes, and the with hollow type is formed by the carbon material, the air-permeable member is formed by a breathable carbonaceous material, the gas permeability of the permeable member is greater than the gas permeability of the hollow An apparatus for producing a quartz crucible. 前記通気性部材が前記中空型の内面に均一に多数配設されることを特徴とする請求項１記載の石英ルツボの製造装置。The quartz crucible manufacturing apparatus according to claim 1, wherein a large number of the air-permeable members are uniformly disposed on the inner surface of the hollow mold. 前記中空型が上部型と下部型とからなり、該上部型と下部型とを接合することによって構成されていることを特徴とする請求項１又は２記載の石英ルツボの製造装置。The quartz crucible manufacturing apparatus according to claim 1 or 2, wherein the hollow mold includes an upper mold and a lower mold, and the upper mold and the lower mold are joined to each other. 前記通気性部材及び吸引通路を前記下部型のみに設けたことを特徴とする請求項３記載の石英ルツボの製造装置。4. The quartz crucible manufacturing apparatus according to claim 3, wherein the breathable member and the suction passage are provided only in the lower mold. 請求項１〜４のいずれか１項記載の装置を用い、回転する前記中空型の内周面に原料石英粉体を投入して石英粉体層を形成し、該石英粉体層をその内周面側から加熱溶融し、該加熱溶融時に該中空型の外面を減圧吸引して該石英粉体層内の内部ガスを前記通気性部材及び吸引通路を介して吸引排気しながら該石英粉体層をルツボ形状に焼結させることを特徴とする石英ルツボの製造方法。Using the apparatus according to any one of claims 1 to 4 , a raw material quartz powder is introduced into an inner peripheral surface of the rotating hollow mold to form a quartz powder layer, and the quartz powder layer is contained therein. The quartz powder is heated and melted from the peripheral surface side, and the outer surface of the hollow mold is sucked under reduced pressure at the time of heating and melting, and the internal gas in the quartz powder layer is sucked and exhausted through the breathable member and the suction passage. A method for producing a quartz crucible, wherein the layer is sintered into a crucible shape.
JP17953696A 1996-07-09 1996-07-09 Quartz crucible manufacturing apparatus and method Expired - Lifetime JP3798849B2 (en)

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