JP4161296B2 - Method for producing quartz glass crucible - Google Patents
Method for producing quartz glass crucible Download PDFInfo
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- JP4161296B2 JP4161296B2 JP2002157228A JP2002157228A JP4161296B2 JP 4161296 B2 JP4161296 B2 JP 4161296B2 JP 2002157228 A JP2002157228 A JP 2002157228A JP 2002157228 A JP2002157228 A JP 2002157228A JP 4161296 B2 JP4161296 B2 JP 4161296B2
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- crucible
- quartz glass
- quartz
- glass
- melted
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
- C03B2201/03—Impurity concentration specified
Description
【０００１】
【発明の属する技術分野】
本発明は、半導体材料となるシリコン単結晶の引き上げに使用する石英ガラスルツボとその製造方法に関する。
【０００２】
【従来技術】
シリコン単結晶の引き上げに使用される石英ガラスルツボは、シリコン溶体と接触する内表面の品質が、引き上げ歩留まりや、引き上げた結晶の品質に大きな影響を与える。このため、石英ガラスルツボの内面はできる限り気泡および不純物の少ない透明な高純度のガラス層であることが求められ、不純物の少ない合成石英によって形成されているものが多い。
【０００３】
現在の石英ルツボの製造方法はいわゆる回転モールド法が主流であり、この方法は原料となる石英粉を回転しているルツボ形状のモールドの内面に遠心力を利用して堆積させ、回転するモールドに堆積した石英粉をアーク放電熱によって溶融し、ガラス化してルツボの形状に成形する。この場合、ルツボの内表面に気泡の少ない高純度の透明石英層を形成する方法として次の２つの方法が知られている。第一の方法は、石英粉のアーク溶融中にモールド側から石英層の真空引きを行う方法であり、石英粉が溶融してガラス化する際に石英層を減圧して内部の気泡を外部に吸引除去することにより、気泡を殆ど含まない透明なガラス層を形成する（特開平01−157426号、特開平01−160836号など）。第二の方法は、アーク中に石英粉を通過させて溶融し、この溶融した石英粉を、すでに成形した石英ルツボの内面に積層させて透明ガラス層を形成する方法である（特開平01−148718号など）。何れの方法でも、内表面層の原料石英粉として高純度の合成石英粉を使用すれば内表面が高純度の合成石英層を有する石英ルツボを製造することができる。
【０００４】
【発明が解決しようとする課題】
上記真空溶融法は、石英層内の空気を吸引して減圧した状態で石英粉を溶融するため、不純物や気泡の少ないガラス層を得ることができるが、多少は周囲からのガス流入があり、完全な真空中での溶融ではないので、透明ガラス層中に微量の気泡が残留することは避けられない。一方、溶融した石英粉をルツボ内表面に堆積させる方法はアークを通過させて石英粉を溶融する際に、例えば電極から飛散したカーボンが付着し、あるいは周囲の窒素ガスが取り込まれるなどして、ガス成分が透明ガラス層に混入し、ルツボを単結晶引き上げ時のような高温下に長時間保持すると、これがガス化して大きな気泡を生じる原因になる。また、溶融雰囲気中で金属等の不純物を巻き込む懸念がある。
【０００５】
本発明は、ルツボ内表面に透明ガラス層を形成する場合における従来の上記問題を解決したものであり、石英粉を溶融して堆積させる方法に代え、予め高真空下で溶融することによって精製した石英ガラスを用い、この精製石英ガラスからなるガラス片をルツボ内表面に一体に溶着させることによって、内部気泡および不純物を殆ど含まない高純度の透明ガラス層を形成した石英ガラスルツボとその製造方法を提供するものである。
【０００６】
【課題を解決する手段】
すなわち、本発明は（１）石英原料粉を不活性ガス雰囲気下で溶融し、さらに２０００℃以上、０.０５torr以上の真空度に５時間以上保持して精製して得た石英ガラスを、石英ガラスルツボの内表面に張り合せ、加熱溶融して一体化したことを特徴とする石英ガラスルツボの製造方法に関する。
【０００７】
本発明の製造方法は、（２）上記[１]の製造方法において、高温高真空下で溶融精製した石英ガラスインゴットからルツボ内表面に形状に合わせてガラス片を切り出し、このガラス片をルツボ内表面に隙間なく並べて張り合わせ、加熱溶融して一体化する石英ガラスルツボの製造方法を含む。
【０００８】
本発明の製造方法は、（３）上記[１]または上記[２]の製造方法において、高温高真空下で溶融精製した石英ガラスインゴットから石英ガラス板および石英ガラスリングを切り出し、この石英ガラス板および石英ガラスリングをフッ酸で洗浄してルツボの底部とコーナー部に張り合わせ、加熱溶融して一体化する石英ガラスルツボの製造方法を含む。
【０００９】
本発明の製造方法は、（４）上記[１]または上記[２]の製造方法において、ルツボの底部曲率に合わせた底部形状の溶融容器を用い、該溶融容器に石英原料粉を入れて加熱溶融して高温高真空下で溶融精製した石英ガラスインゴットにし、該石英ガラスインゴットをルツボ底部に設置して加熱溶融して一体化する石英ガラスルツボの製造方法、（５）石英ガラスルツボを回転しながら、ルツボ内表面に設けた石英ガラス片を加熱溶融してルツボ内表面と一体に溶着させる上記[１]〜上記[４]の何れかに記載する製造方法。
【００１０】
本発明の石英ガラスルツボは、高純度の合成石英粉等を用い、これを予め真空溶融して更に不純物とガス成分を除去した精製石英ガラスインゴットとし、この精製石英ガラスからなるガラス片を用いてルツボ内表面の透明ガラス層を形成しているので、ルツボ内表面層の純度が極めて高く、しかも実質的に気泡を含まない。このため、シリコン単結晶引き上げに用いた場合、高い引き上げ歩留まりで高品質のシリコン単結晶を得ることができる。
【００１１】
【発明の実施の形態】
以下、本発明を実施形態に基づいて具体的に説明する。
本発明の石英ガラスルツボは、真空溶融して精製した石英ガラスからなるガラス片を、石英ガラスルツボ内表面の全体または一部に張り合わせ、これを加熱溶融して一体に溶着させることにより、ルツボ内表面に透明ガラス層を形成したことを特徴とする石英ガラスルツボである。具体的には、例えば、真空溶融して精製した合成石英からなるガラス片をルツボ内表面に加熱溶融して一体に溶着させて形成した透明ガラス層を有し、この透明ガラス層に含まれるＡｌ、Ｔｉ、Ｆｅ、Ｃａ、Ｃｕ、Ｎａ、Ｋ、Ｌｉ、Ｍｇ、Ｂａ、Ｎｉ、Ｃｒが何れも０.１ppm以下であり、気泡含有率が０.０１vol％以下の石英ガラスルツボである。
【００１２】
透明ガラス層を形成するガラス材料としては不純物が少ない合成石英を原料とし、これを更に真空溶融して精製したものを用いる。合成石英粉を真空下で加熱溶融してガラス化すると、真空下での加熱溶融によって、石英粉に含まれる揮発性の不純物およびガス成分は系外に吸引され、石英粉から除去される。この真空溶融によって石英中のＡｌ、Ｔｉ、Ｆｅ、Ｃａ、Ｃｕ、Ｎａ、Ｋ、Ｌｉ、Ｍｇ、Ｂａ、Ｎｉ、Ｃｒが何れも０.１ppm以下であって気泡含有率が０.０１vol％以下の実質的に無気泡で高純度な石英ガラスインゴットを得ることができる。
【００１３】
上記真空溶融は、例えば、高純度合成石英原料粉をグラファイト製の溶融容器に入れ、カーボンヒータ等を加熱源とする高温真空炉内にセットし、不活性ガス雰囲気下で、１５００〜２０００℃以上に加熱して石英原料粉を溶融し、さらに２０００℃以上の高温下で容器内を排気して０.０５torr以上の真空度とし、この状態を５時間以上保持して揮発性の不純物を除去し、脱泡させる。なお、この真空溶融によって得られる石英ガラスインゴットの形状は石英原料粉を入れた溶融容器の形状によって定まるので、石英ガラスインゴットからガラス片を切り出す際に、その加工が容易になる形状の溶融容器を使用するのが好ましい。
【００１４】
高純度で実質的に無気泡の石英ガラスインゴットをルツボ内表面の形状に合わせて切り出し、この切り出したガラス片をルツボ内表面に張り合わせて加熱溶融し、ルツボ内表面に一体に溶着させる。ガラス片はルツボ内表面の形状に応じて複数個切り出し、これを隙間なくルツボ内表面全体または所定範囲に並べて溶着させると良い。この溶着は、石英ガラスルツボを回転しながら、ルツボ内表面に設置したガラス片を加熱溶融すれば遠心力によって溶融した石英ガラスがルツボ内表面に広がって溶着し、均一な透明ガラス層が形成される。具体的には、例えば、ルツボの底部からコーナ部の範囲において、加熱溶融された石英ガラスがルツボの底部からコーナ上部にかけて広がり、均一な層厚の透明ガラス層を形成することができる。
【００１５】
上記透明ガラス層の層厚は０.５mm以上が適当であり、０.５〜１mm程度が好ましい。ルツボにチャージした溶融シリコンから単結晶シリコンを引き上げる際、ルツボ内表面は溶融シリコンによって概ね０.５mm程度溶損するので、この溶損厚さ以上に透明ガラス層を形成するのが好ましい。
【００１６】
上記ガラス片を加熱溶融する手段は限定されない。アーク放電や酸水素炎バーナ等を用いることができる。例えば、ルツボ内表面に上記石英ガラス片を張り付けた後に、アーク電極や酸水素炎バーナをルツボの内側に挿入し、石英ルツボを回転しながらルツボ内表面に設置した上記ガラス片を加熱して溶融させ、ルツボ内表面に溶着させる。溶着後、自然冷却すれば良い。
【００１７】
【発明の効果】
上記製造方法によれば、実質的に無気泡で高純度の透明ガラス層を内表面に有する石英ガラスルツボを得ることができる。具体的には、Ａｌ、Ｔｉ、Ｆｅ、Ｃａ、Ｃｕ、Ｎａ、Ｋ、Ｌｉ、Ｍｇ、Ｂａ、Ｎｉ、Ｃｒが何れも０.１ppm以下であって、気泡含有率が０.０１vol％以下の透明ガラス層を内表面に有する石英ガラスルツボを得ることができる。この石英ガラスルツボはシリコン単結晶の引き上げに長時間使用しても内表面の品質が良好であり、高い引き上げ歩留まりを達成することができる。また、引き上げた単結晶シリコンの品質にも優れる。
【００１８】
【実施例１】
市販の高純度非晶質合成シリカ粉末（合成石英粉）５kgを高純度グラファイト製円柱容器（内径400mm×深さ100mm）に入れ、カーボンヒータを備えた高温真空炉内に設置し、炉内をＡｒガス雰囲気で１気圧とし、炉内を１８００℃に加熱して合成石英粉を溶融した後、炉内を排気して０.０２torrの真空度まで真空引きし、温度２０３０℃で７時間保持した後に冷却して、石英ガラスインゴット（長さ400mm、厚さ35mm）を得た。この石英ガラスインゴットには、目視観察において気泡は認められず、透明石英ガラスであった。この石英ガラスインゴットを切り出して不純物含有量を分析したところ、Ａｌ、Ｔｉが０.１ppm、Ｆｅが０.０２ppm、Ｃａ、Ｃｕ、Ｎａ、Ｋ、Ｌｉ、Ｍｇ、Ｂａ、Ｎｉ、Ｃｒは０.０１ppm以下であり、非常に高純度な石英ガラスであった。
【００１９】
【実施例２】
実施例１と同様の条件で石英ガラスインゴット（長さ200mm×厚さ50mm）を製造し、この石英ガラスインゴットから石英ガラス板（長さ200mm、厚さ5mm）を切り出した。さらに、実施例１と同様の条件で円柱状の石英ガラスインゴット（外径440mm×高さ50mm）を製造し、この石英ガラスインゴットから石英ガラスリング（外形440mm×厚さ5mm×高さ40mm）を切り出した。切り出した石英ガラス板および石英ガラスリングの表面をフツ酸で洗浄した後に、シリコン単結晶引き上げに使用されている天然石英ルツボの底部とコーナー上部に張り合わせ、これをカーボン製ルツボ回転支持台に載せ、回転させながらアーク電極を用いて加熱溶融し、上記石英ガラス板と石英ガラスリングをルツボ内表面に溶着させた。
加熱溶融終了後、冷却したルツボの内表面を確認すると、天然石英ルツボと完全に密着した無気泡の透明石英ガラス層がルツボ内表面に形成されていた。この無気泡の透明ガラス層は加熱溶融時の回転による遠心力によってルツボのボトム部からコーナ上部全体に広がり、均一な層厚の透明ガラス層を形成していた。さらに、この石英ガラスルツボ（口径１８インチ）を用いてシリコン単結晶の引き上げを行ったところ、従来の天然石英ルツボを使用した引き上げに対し、引き上げ中の転位発生率が７０％減少し、単結晶化率が１８％向上した。
【００２０】
【実施例３】
合成石英原料粉を入れるグラファイト製の溶融容器の底部形状をルツボ（口径24インチ）の底部曲率に合わせた球面状にし、この球面を有する無気泡の高純度石英ガラスインゴット（外径300mm×厚さ5〜8mm）を実施例１と同じ条件で製造した。この球面を有する石英ガラスインゴットをフッ酸洗浄した後に、天然石英ルツボ(口径24インチ)の底部に設置し、実施例２と同様の方法でアーク電極を用いて溶融加熱した。加熱溶融終了後、冷却したルツボの底部からコーナ上部にかけて無気泡の透明石英ガラス層が均一に形成されていた。この石英ガラスルツボをシリコン単結晶の引き上げに使用したところ、従来の天然石英ルツボを使用した引き上げに対し、引き上げ中の転位発生率は６０％減少し、単結晶化率も１５％向上した。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a quartz glass crucible used for pulling a silicon single crystal as a semiconductor material and a method for manufacturing the same.
[0002]
[Prior art]
In the quartz glass crucible used for pulling up a silicon single crystal, the quality of the inner surface that comes into contact with the silicon solution greatly affects the pulling yield and the quality of the pulled crystal. For this reason, the inner surface of the quartz glass crucible is required to be a transparent high-purity glass layer with as few bubbles and impurities as possible, and is often formed of synthetic quartz with few impurities.
[0003]
The current method for producing a quartz crucible is the so-called rotary mold method. This method deposits quartz powder, which is a raw material, on the inner surface of a rotating crucible-shaped mold using centrifugal force, and forms a rotating mold. The deposited quartz powder is melted by arc discharge heat, vitrified and formed into a crucible shape. In this case, the following two methods are known as a method for forming a high-purity transparent quartz layer with few bubbles on the inner surface of the crucible. The first method is a method of evacuating the quartz layer from the mold side during the arc melting of the quartz powder. When the quartz powder is melted and vitrified, the quartz layer is decompressed so that the internal bubbles are exposed to the outside. By removing by suction, a transparent glass layer containing almost no bubbles is formed (Japanese Patent Laid-Open Nos. 01-157426 and 01-160836, etc.). The second method is a method in which quartz powder is passed through an arc and melted, and this fused quartz powder is laminated on the inner surface of an already formed quartz crucible to form a transparent glass layer (Japanese Patent Laid-Open No. 01-1). 148718). In any method, if high-purity synthetic quartz powder is used as the raw material quartz powder for the inner surface layer, a quartz crucible having an inner surface having a high-purity synthetic quartz layer can be produced.
[0004]
[Problems to be solved by the invention]
In the vacuum melting method, the quartz powder is melted in a state where the air in the quartz layer is sucked and decompressed, so that a glass layer with few impurities and bubbles can be obtained, but there is a slight gas inflow from the surroundings, Since melting is not complete in vacuum, it is inevitable that a small amount of bubbles remain in the transparent glass layer. On the other hand, the method of depositing the fused quartz powder on the inner surface of the crucible is that when the quartz powder is melted by passing an arc, for example, carbon scattered from the electrode adheres or the surrounding nitrogen gas is taken in, When gas components are mixed in the transparent glass layer and the crucible is kept at a high temperature for a long time, such as when pulling a single crystal, this causes gasification and causes large bubbles. Further, there is a concern that impurities such as metals are involved in the molten atmosphere.
[0005]
The present invention solves the above-mentioned conventional problems in the case of forming a transparent glass layer on the inner surface of the crucible, and has been purified by previously melting under high vacuum instead of a method of melting and depositing quartz powder. A quartz glass crucible having a high-purity transparent glass layer containing almost no internal bubbles and impurities by integrally welding a glass piece made of this purified quartz glass to the inner surface of the crucible and a method for producing the same. It is to provide.
[0006]
[Means for solving the problems]
That is, the present invention provides (1) quartz glass obtained by melting quartz raw material powder in an inert gas atmosphere and further purifying it by maintaining it in a vacuum degree of 2000 ° C. or higher and 0.05 torr or higher for 5 hours or more. The present invention relates to a method for producing a quartz glass crucible characterized in that it is laminated on the inner surface of a glass crucible and integrated by heating and melting.
[0007]
The production method of the present invention is (2) in the production method of [1] above, a glass piece is cut out from a quartz glass ingot melt-purified under high temperature and high vacuum according to the shape of the inner surface of the crucible, and the glass piece is cut into the crucible It includes a method for producing a quartz glass crucible that is laminated and bonded to the surface without any gaps, and is fused by heating and melting.
[0008]
The production method of the present invention includes (3) a quartz glass plate and a quartz glass ring cut out from a quartz glass ingot melt-purified under high temperature and high vacuum in the production method of [1] or [2] above, and this quartz glass plate And a method for producing a quartz glass crucible in which the quartz glass ring is washed with hydrofluoric acid and bonded to the bottom and corners of the crucible, and heated to melt.
[0009]
The manufacturing method of the present invention is (4) in the manufacturing method of [1] or [2] described above, using a melting vessel having a bottom shape matching the curvature of the bottom of the crucible, and heating the quartz raw material powder in the melting vessel A quartz glass crucible that is melted and melted and purified under high temperature and high vacuum, and the quartz glass ingot is placed at the bottom of the crucible and heated and melted to be integrated. (5) The quartz glass crucible is rotated. However, the manufacturing method according to any one of [1] to [4] above, wherein the quartz glass piece provided on the inner surface of the crucible is heated and melted and welded integrally with the inner surface of the crucible.
[0010]
The quartz glass crucible of the present invention uses a high-purity synthetic quartz powder or the like, which is previously purified by vacuum melting to obtain a purified quartz glass ingot from which impurities and gas components are further removed, and a glass piece made of this purified quartz glass is used. Since the transparent glass layer on the inner surface of the crucible is formed, the purity of the inner surface layer of the crucible is extremely high and substantially free of bubbles. Therefore, when used for pulling a silicon single crystal, a high-quality silicon single crystal can be obtained with a high pulling yield.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be specifically described based on embodiments.
The quartz glass crucible of the present invention is obtained by laminating a glass piece made of quartz glass vacuum-melted and purified on the whole or a part of the inner surface of the quartz glass crucible, and heat-melting and fusing them together to integrally weld them. A quartz glass crucible characterized in that a transparent glass layer is formed on the surface. Specifically, for example, it has a transparent glass layer formed by heating and melting a glass piece made of synthetic quartz purified by vacuum melting on the inner surface of the crucible and integrally welding, and Al contained in this transparent glass layer , Ti, Fe, Ca, Cu, Na, K, Li, Mg, Ba, Ni, Cr are quartz glass crucibles each having a content of 0.1 ppm or less and a bubble content of 0.01 vol% or less.
[0012]
As a glass material for forming the transparent glass layer, a synthetic quartz containing few impurities is used as a raw material, which is further purified by vacuum melting. When synthetic quartz powder is heated and melted under vacuum to be vitrified, volatile impurities and gas components contained in the quartz powder are sucked out of the system and removed from the quartz powder by heating and melting under vacuum. By this vacuum melting, Al, Ti, Fe, Ca, Cu, Na, K, Li, Mg, Ba, Ni, Cr in the quartz are all 0.1 ppm or less and the bubble content is 0.01 vol% or less. A quartz glass ingot that is substantially bubble-free and highly pure can be obtained.
[0013]
The above-mentioned vacuum melting is performed, for example, by placing high-purity synthetic quartz raw material powder in a graphite melting vessel, setting it in a high-temperature vacuum furnace using a carbon heater or the like as a heating source, and 1500 to 2000 ° C. or higher in an inert gas atmosphere. To melt the quartz raw material powder, and then evacuate the container at a high temperature of 2000 ° C. or higher to obtain a vacuum level of 0.05 torr or higher and maintain this state for 5 hours or more to remove volatile impurities. , Defoam. Note that the shape of the quartz glass ingot obtained by this vacuum melting is determined by the shape of the melting container containing the quartz raw material powder. Therefore, when a glass piece is cut out from the quartz glass ingot, It is preferred to use.
[0014]
A high-purity, substantially bubble-free quartz glass ingot is cut out in accordance with the shape of the inner surface of the crucible, and the cut glass piece is attached to the inner surface of the crucible and heated and melted to be integrally welded to the inner surface of the crucible. A plurality of glass pieces may be cut out according to the shape of the inner surface of the crucible, and the glass pieces may be welded by arranging them on the entire inner surface of the crucible or in a predetermined range without any gaps. In this welding, if the glass piece placed on the inner surface of the crucible is heated and melted while rotating the quartz glass crucible, the fused quartz glass is spread and welded to the inner surface of the crucible by the centrifugal force, and a uniform transparent glass layer is formed. The Specifically, for example, in the range from the bottom of the crucible to the corner, the heated and melted quartz glass spreads from the bottom of the crucible to the top of the corner, so that a transparent glass layer having a uniform layer thickness can be formed.
[0015]
The thickness of the transparent glass layer is suitably 0.5 mm or more, preferably about 0.5 to 1 mm. When pulling up the single crystal silicon from the molten silicon charged in the crucible, the inner surface of the crucible is melted by about 0.5 mm by the molten silicon. Therefore, it is preferable to form a transparent glass layer with a thickness greater than this melted thickness.
[0016]
The means for heating and melting the glass piece is not limited. An arc discharge or an oxyhydrogen flame burner can be used. For example, after the quartz glass piece is attached to the inner surface of the crucible, an arc electrode or an oxyhydrogen flame burner is inserted inside the crucible, and the glass piece placed on the inner surface of the crucible is heated and melted while rotating the quartz crucible. And welded to the inner surface of the crucible. After welding, it may be naturally cooled.
[0017]
【The invention's effect】
According to the above production method, a quartz glass crucible having a substantially glass-free and high-purity transparent glass layer on the inner surface can be obtained. Specifically, Al, Ti, Fe, Ca, Cu, Na, K, Li, Mg, Ba, Ni, and Cr are all 0.1 ppm or less and the bubble content is 0.01 vol% or less. A quartz glass crucible having a glass layer on the inner surface can be obtained. Even if this quartz glass crucible is used for pulling a silicon single crystal for a long time, the quality of the inner surface is good and a high pulling yield can be achieved. In addition, the quality of the pulled single crystal silicon is excellent.
[0018]
[Example 1]
Place 5 kg of commercially available high-purity amorphous synthetic silica powder (synthetic quartz powder) in a high-purity graphite cylindrical container (inner diameter 400 mm x depth 100 mm) and place it in a high-temperature vacuum furnace equipped with a carbon heater. The atmosphere was set to 1 atm in an Ar gas atmosphere, and the interior of the furnace was heated to 1800 ° C. to melt the synthetic quartz powder. Then, the interior of the furnace was evacuated to a vacuum of 0.02 torr and held at 2030 ° C. for 7 hours. After cooling, a quartz glass ingot (length 400 mm, thickness 35 mm) was obtained. The quartz glass ingot was transparent quartz glass with no bubbles observed by visual observation. When this quartz glass ingot was cut out and analyzed for impurity content, 0.1 ppm for Al and Ti, 0.02 ppm for Fe, 0.01 ppm for Ca, Cu, Na, K, Li, Mg, Ba, Ni, and Cr. It was the following and was a very high purity quartz glass.
[0019]
[Example 2]
A quartz glass ingot (length 200 mm × thickness 50 mm) was produced under the same conditions as in Example 1, and a quartz glass plate (length 200 mm, thickness 5 mm) was cut out from the quartz glass ingot. Furthermore, a cylindrical quartz glass ingot (outside diameter 440 mm × height 50 mm) is manufactured under the same conditions as in Example 1, and a quartz glass ring (outside diameter 440 mm × thickness 5 mm × height 40 mm) is produced from this quartz glass ingot. Cut out. After the surfaces of the cut quartz glass plate and quartz glass ring are washed with hydrofluoric acid, they are pasted on the bottom and corner top of a natural quartz crucible used for pulling a silicon single crystal, and this is placed on a carbon crucible rotating support base. The quartz glass plate and the quartz glass ring were welded to the inner surface of the crucible by heating and melting using an arc electrode while rotating.
When the inner surface of the cooled crucible was confirmed after completion of heating and melting, a bubble-free transparent quartz glass layer completely in close contact with the natural quartz crucible was formed on the inner surface of the crucible. This bubble-free transparent glass layer spreads from the bottom of the crucible to the entire upper corner of the crucible due to the centrifugal force generated by rotation during heating and melting, forming a transparent glass layer having a uniform layer thickness. Further, when the silicon single crystal was pulled using this quartz glass crucible (18-inch diameter), the dislocation occurrence rate during the pulling was reduced by 70% compared to the conventional pulling using the natural quartz crucible, and the single crystal The conversion rate improved by 18%.
[0020]
[Example 3]
The bottom of the graphite melting vessel containing synthetic quartz raw material powder is shaped into a spherical shape that matches the curvature of the bottom of the crucible (24 inch diameter), and this bubble-free high-purity quartz glass ingot (outer diameter 300mm x thickness) 5-8 mm) was produced under the same conditions as in Example 1. The quartz glass ingot having this spherical surface was washed with hydrofluoric acid, then placed on the bottom of a natural quartz crucible (24 inch diameter), and melted and heated using an arc electrode in the same manner as in Example 2. After completion of heating and melting, a bubble-free transparent quartz glass layer was uniformly formed from the bottom of the cooled crucible to the top of the corner. When this quartz glass crucible was used for pulling up a silicon single crystal, the rate of dislocation generation during pulling was reduced by 60% and the single crystallization rate was improved by 15% compared to pulling using a conventional natural quartz crucible.
Claims (5)
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| JP2002157228A JP4161296B2 (en) | 2002-05-30 | 2002-05-30 | Method for producing quartz glass crucible |
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| JP2002157228A JP4161296B2 (en) | 2002-05-30 | 2002-05-30 | Method for producing quartz glass crucible |
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| JP4161296B2 true JP4161296B2 (en) | 2008-10-08 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20050120945A1 (en) * | 2003-12-03 | 2005-06-09 | General Electric Company | Quartz crucibles having reduced bubble content and method of making thereof |
| JP4931106B2 (en) * | 2005-09-29 | 2012-05-16 | コバレントマテリアル株式会社 | Silica glass crucible |
| KR101312999B1 (en) * | 2007-07-28 | 2013-10-01 | 쟈판 스파 쿼츠 가부시키가이샤 | Method and apparatus for manufacturing vitreous silica crucible |
| JP5121760B2 (en) * | 2009-03-16 | 2013-01-16 | ジャパンスーパークォーツ株式会社 | Method of pulling a silicon single crystal |
| JP5191003B2 (en) * | 2009-09-28 | 2013-04-24 | コバレントマテリアル株式会社 | Silica glass crucible for silicon single crystal pulling |
| JP4951057B2 (en) | 2009-12-10 | 2012-06-13 | 信越石英株式会社 | Silica container and method for producing the same |
| JP5685894B2 (en) | 2010-11-05 | 2015-03-18 | 信越半導体株式会社 | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal |
| JP5500688B2 (en) * | 2010-12-03 | 2014-05-21 | 株式会社Ｓｕｍｃｏ | Method for producing silica glass crucible |
| JP5488519B2 (en) * | 2011-04-11 | 2014-05-14 | 信越半導体株式会社 | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal |
| JP5741163B2 (en) * | 2011-04-11 | 2015-07-01 | 信越半導体株式会社 | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal |
| JP5791497B2 (en) * | 2011-12-29 | 2015-10-07 | 株式会社Sumco | Determination method of silica powder suitable for production of silica glass crucible for pulling silicon single crystal |
| JP6208080B2 (en) * | 2014-05-22 | 2017-10-04 | クアーズテック株式会社 | Quartz glass crucible |
| RU2731764C1 (en) * | 2019-12-30 | 2020-09-08 | Акционерное общество "Научно-производственное предприятие "Медикон" (АО "НПП "Медикон") | Melting method of quartz glass |
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