JP5344767B2 - Method for manufacturing a silicon single crystal pulling quartz glass crucible for - Google Patents

Method for manufacturing a silicon single crystal pulling quartz glass crucible for Download PDF

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JP5344767B2
JP5344767B2 JP2010140335A JP2010140335A JP5344767B2 JP 5344767 B2 JP5344767 B2 JP 5344767B2 JP 2010140335 A JP2010140335 A JP 2010140335A JP 2010140335 A JP2010140335 A JP 2010140335A JP 5344767 B2 JP5344767 B2 JP 5344767B2
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crucible
silica powder
quartz glass
silicon single
glass crucible
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JP2010202515A (en
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康生 大浜
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信越石英株式会社
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    • 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

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a quartz glass crucible for pulling up silicon single crystals in which silica powder released from the outermost layer in which unmelted or semi-melted silica powder is unevenly distributed in a crucible is properly controlled without grinding, on the other hand, the crystalline part in the outermost layer is largely left, heat resistance at high temperature is maintained, and silicon single crystals can be produced at a high yield. <P>SOLUTION: The method for producing a quartz glass crucible for pulling up silicon single crystals is characterized in that raw material powder is fed into a rotating die, so as to form a crucible-shaped raw material powder layer, from the inside thereof, arc discharge heating is performed, and melting is caused so as to produce a quartz glass crucible having a smooth inner surface, an opaque or translucent external layer and the outermost layer in which unmelted or semi-melted silica powder is unevenly distributed at the outside thereof, solid silica powder is sprayed on the outer surface thereof under the spraying pressure of 0.1 to 5 MPa, thereafter, high pressure water is sprayed under the spraying pressure of 24 to 40 MPa, and next, hydrofluoric acid aqueous solution treatment is performed. <P>COPYRIGHT: (C)2010,JPO&amp;INPIT

Description

本発明は、シリコン単結晶引上げに用いられる石英ガラスルツボの製造方法に関し、さらに詳しくは、石英ガラスルツボの最外層の未溶融ないし半溶融のシリカ粉の離脱粉を最適に制御することで、シリコン単結晶を高歩留りで製造でき、かつ高温における耐熱性に優れ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 manufacturing a silica glass crucible used in a silicon single crystal pulling, and more particularly, by optimally controlling the disengagement powder of the outermost layer of unmelted or semi-molten silica powder of the quartz glass crucible, a silicon the single crystal can be manufactured at high yield, and a method for producing a quartz glass crucible having excellent heat resistance at high temperatures.

シリコン単結晶の製造には、いわゆる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が、この製造方法では、石英ガラスルツボが一般的に用いられている。 The production of a silicon single crystal, a method referred to as so-called Czochralski method (CZ method) has been widely adopted, but this production method, the quartz glass crucible is generally used. このシリコン単結晶引上げ用石英ガラスルツボは、回転している型内に原料粉を供給しルツボ状の原料粉体層を形成し、その内側からアーク放電加熱し溶融する方法で製造され、平滑な内表面と不透明又は半透明な外層と、未溶融ないし半溶融の石英粉が偏在する最外層とを有している。 The silicon single crystal for pulling up the quartz glass crucible, the raw material powder is supplied to form a crucible-like raw material powder layer in the mold which is rotating, it is manufactured by a method of melting and arcing heated from the inside, smooth an inner surface and an opaque or semi-transparent outer layer, quartz powder unmelted or semi-molten has a outermost layer ubiquitous. 前記石英ガラスルツボを用いてシリコン単結晶の引上げを行うと、最外層の未溶融ないし半溶融の石英粉がシリコン単結晶の引上げ時に離脱し、シリコン融液に混入し、それが溶け残ってシリコン単結晶の歩留まりを低下する欠点があった。 Doing pulling a silicon single crystal using the quartz glass crucible, quartz powder unmelted or partially melted in the outermost layer is disengaged when pulling the silicon single crystal, mixed into the silicon melt, it remains melted silicon It has a disadvantage of reducing the yield of the single crystal.

この欠点を解決するため最外層を研削して未溶融ないし半溶融の石英粉を除去する方法が特許文献1で提案されている。 Method for removing silica powder unmelted or partially melted by grinding the outermost layer to solve this drawback is proposed in Patent Document 1. しかし、この方法ではルツボの結晶質部分が全て取り除かれ高温における熱耐性が低下する欠点があった。 However, the heat resistance in a high temperature removes all the crystalline portion of the crucible has a disadvantage to decrease in this way.
特許第2962976号公報 Patent No. 2962976 Publication

こうした現状に鑑み、本発明者らは鋭意研究を続けた結果、回転する型内に原料粉を供給しルツボ状の原料粉体層を形成し、その内側からアーク放電加熱し溶融して平滑な内表面と不透明又は半透明な外層と、その外側に未溶融ないし半溶融のシリカ粉が偏在する最外層を有する石英ガラスルツボを製造し、その外表面に固体シリカ粉を吹き付けたのち、高圧水を吹き付け、次いでフッ酸水溶液処理を施こすことで、離脱シリカ粉のシリコン融液への混入を抑え結晶転位を少なくする上に、最外層に結晶質部分を多く残し、これを核として外表面全体を容易に結晶化し高温における耐熱性を維持し、シリコン単結晶を安定して高歩留りで製造できる石英ガラスルツボが製造できることを見出した。 In view of these circumstances, the present inventors have found that continued intensive studies to supply the raw material powder into a rotating mold to form a crucible-like raw material powder layer, smooth and arc discharge heated and melted from the inside an inner surface and an opaque or semi-transparent outer layer, after which the silica powder unmelted or partially melted manufactures a quartz glass crucible having an outermost layer unevenly distributed on the outside, sprayed with solid silica powder on its outer surface, high pressure water spraying, followed by straining facilities hydrofluoric acid aqueous solution treatment, in order to reduce the the suppressing crystal dislocation contamination of the silicon melt leaving the silica powder, leaving a lot of crystalline portions in the outermost layer, the outer surface of this as nuclei the whole maintaining heat resistance in easily crystallized hot, the silicon single crystal stably quartz glass crucible can be produced with a high yield has been found that can be produced. すなわち、 That is,

本発明は、研削なしでルツボの未溶融ないし半溶融のシリカ粉が偏在する最外層から離脱するシリカ粉が抑えられる上に、最外層の結晶質部分が多く残り、高温における耐熱性が維持されシリコン単結晶を高歩留りで製造でき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を提供することを目的とする。 The present invention, on the silica powder to be separated from the outermost layer is suppressed to silica powder unmelted or partially melted in the crucible without grinding is unevenly distributed, remaining many crystalline portion of the outermost layer, the heat resistance is maintained at elevated temperatures and to provide a method for manufacturing a silicon single crystal pulling quartz glass crucible for the silicon single crystal can be produced in high yield.

上記目的を達成する本発明は、回転する型内に原料粉を供給しルツボ状の原料粉体層を形成し、その内側からアーク放電加熱し溶融して平滑な内表面と不透明又は半透明な外層と、その外側に未溶融ないし半溶融のシリカ粉が偏在する最外層を有する石英ガラスルツボを製造し、その外表面に固体シリカ粉を吹付け圧が0.1〜5MPaで吹き付けたのち、高圧水を吹付け圧が24〜40MPaで吹き付け、次いでフッ酸水溶液処理を施こす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に係る。 The present invention to achieve the above object, supplies raw material powder into a rotating mold to form a crucible-like raw material powder layer, and the opaque or translucent arc discharge heating to melt to a smooth inner surface from the inside and an outer layer, then to produce a quartz glass crucible having an outermost layer silica powder unmelted or partially melted in its outer is unevenly distributed, the spray pressure of the solid silica powder on its outer surface was sprayed with 0.1 to 5 MPa, pressure water spray pressure is blown in 24~40MPa and then according to the method for manufacturing a silicon single crystal for pulling up the quartz glass crucible is characterized by straining facilities hydrofluoric acid aqueous solution treatment.

上述のように本発明の製造方法で得られたシリコン単結晶引上げ用石英ガラスルツボは、平滑な内表面と不透明又は半透明な外層と、その外側に未溶融ないし半溶融のシリカ粉が偏在する最外層を有するシリコン単結晶引上げ用石英ガラスルツボであって、ルツボ内表面に離脱シリカ粉がなく、かつ少なくとも直胴部における最外層から離脱するシリカ粉が粘着テープ法で0.1〜1.0個/cm の石英ガラスルツボである。 A silicon single crystal for pulling up the quartz glass crucible obtained by the manufacturing method of the present invention as described above, a smooth inner surface and an opaque or semi-transparent outer layer, silica powder unmelted or partially melted in its outer unevenly distributed a silicon single crystal for pulling up the quartz glass crucible having the outermost layer, without leaving the silica powder in the surface crucible, and silica powder to leave the outermost layer in at least the straight body portion is an adhesive tape method 0.1. 0 is quartz glass crucible / cm 2. 通常、石英ガラスルツボは異物が混入しないようにルツボの開口部にシート状の蓋をかぶせられ、さらに袋で梱包させているが、ルツボの使用のためこれらの梱包から開封する際に、或はルツボをカーボンの型にセットする際等に、ルツボの外表面からシリカ粉が離脱し、これがルツボ内部に入り込み、シリコン単結晶の引上げ時にシリコン単結晶に付着して、結晶の転位を引き起こしシリコン単結晶の生産性を低下させることがあるが、離脱するシリカ粉が前記範囲にあると最外層から離脱するシリカ粉がシリコン融液へ混入することが抑えられ、結晶の転位が少なくなりシリコン単結晶を高歩留りで製造できるようになる。 Usually, a quartz glass crucible was covered with a sheet-like lid to the opening of the crucible so as foreign material is not mixed, when it is then further packed in a bag, for opening these packing for use of the crucible, or when such setting the crucible in a mold of carbon, silica powder is disengaged from the outer surface of the crucible, which enters inside the crucible, attached to the silicon single crystal during pulling of the silicon single crystal, a silicon single cause dislocation of the crystal While it may reduce the productivity of the crystal, the silica powder to leave is in the range that is suppressed to the silica powder to be separated from the outermost layer is mixed into the silicon melt, a silicon dislocations of the crystal is reduced monocrystalline the so can be manufactured at high yield. 最外層から離脱するシリカ粉の個数が0.1〜1.0個/cm であると、最外層からの離脱シリカ粉がシリコン融液へ混入することがほとんどなくシリコン単結晶の歩留りが一段と向上するとともに結晶質部分が残るため、高温時の耐熱性に優れる。 If the number of silica powder to be separated from the outermost layer is 0.1 to 1.0 pieces / cm 2, more hardly yield of the silicon single crystal be disengaged silica powder from the outermost layer is mixed into the silicon melt to remain the crystalline portion with enhanced, excellent heat resistance at high temperature. 最外層からの離脱シリカ粉を0.1個/cm 未満にすると結晶質部分が十分でなく石英ガラスルツボの高温における熱耐性が低下するため、使用条件によっては変形が生じ易く、注意が必要である。 Since the crystalline portions detachment silica powder to be less than 0.1 / cm 2 or from the outermost layer is lowered heat resistance at high temperature of the quartz glass crucible not sufficient, easy deformation occurs in the use condition, caution it is. その一方、最外層から離脱するシリカ粉が1.5個/cm を超えると離脱シリカ粉がルツボ内に混入し易く、シリコン単結晶の歩留りが著しく低下する。 Meanwhile, the silica powder and leaving the silica powder exceeds 1.5 / cm 2, which leaves the outermost easily mixed into the crucible, the yield of the silicon single crystal is remarkably reduced. 本発明で使用する粘着テープ法とは、回転モールド法で製造した石英ガラスルツボの外表面に粘着テープ((株)共和製、商品名ミリオンビニルテープ黒)を貼り付け、その粘着テープに付着する100μm以上の石英粉の個数を目視でカウントして測定する方法である。 The adhesive tape method for use in the present invention, paste adhesive on the outer surface tape of the quartz glass crucible manufactured by the rotating mold method (Co. Kyowa Ltd., trade name Million vinyl tape, black), 100 [mu] m to adhere to the adhesive tape a method for measuring by counting visually the number of the above quartz powder.

上記の石英ガラスルツボの製造方法では、回転する型であって少なくともルツボの直胴部を形成する部分がステンレス鋼製の型内に原料粉を供給しルツボ状の原料粉体層を形成し、その内側からアーク放電加熱し溶融するいわゆる回転モールド法で製造した石英ガラスルツボの外表面に、吹付け圧0.1〜5MPaで固体シリカ粉を吹付け、次いで24〜40MPaの高圧水を、ルツボと高圧水噴射ノズルとの距離を10〜60mmに保って吹き付け、さらに内表面のエッチング量が1〜50μmに、外表面のエッチング量が1〜10μmとなるようにフッ酸水溶液処理を制御し、純水で濯ぎ、乾燥して製造される。 In the manufacturing method of the quartz glass crucible, a mold rotating supplying raw powder portion forming the straight body portion of the at least crucible into a mold made of stainless steel to form a crucible-like raw material powder layer, on the outer surface of the quartz glass crucible produced in the so-called rotational molding of molten arcing heated from the inside, only spraying the solid silica powder with spray pressure 0.1 to 5 MPa, then the high pressure water 24~40MPa, crucible and sprayed while maintaining the distance between the high-pressure water jet nozzles 10 to 60 mm, further etching of the inner surface of 1 to 50 [mu] m, and controls the hydrofluoric acid aqueous solution treated as the etching amount of the outer surface is 1 to 10 [mu] m, rinsed with pure water, it is prepared by drying. 前記処理によりルツボ内表面の離脱シリカ粉は十分に除去される上に、最外層からの離脱シリカ粉が粘着テープ法で0.1〜1.0個/cm となる。 On leaving the silica powder crucible inner surface that is sufficiently removed by the process, leaving the silica powder from the outermost layer is 0.1 to 1.0 pieces / cm 2 with adhesive tape method. 前記固体シリカ粉の吹付圧が0.1MPa未満では未溶融ないし半溶融のシリカ粉の除去が十分でなく、高圧水やフッ酸水溶液処理後の排水に離脱シリカ粉が溜りやすくなりその処理のため作業性の低下が懸念され、5MPaを超えると外表面の半溶融の結晶質部分まで削られ高温における耐熱性が低下する。 It said solid spraying pressure silica powder removal of unmelted or semi-molten silica powder is less than 0.1MPa is insufficient, leaving silica powder drainage after high pressure water or an aqueous solution of hydrofluoric acid treatment tends pool for that process is concerned a decrease in workability, heat resistance is lowered at high temperatures trimmed to the semi-molten crystalline portion of the outer surface exceeds 5 MPa. 使用する固体シリカ粉としては、天然シリカ粉、合成シリカ粉又はそれらの混合シリカ粉が用いられる。 The solid silica powder to be used, natural silica powder, synthetic silica powder or a mixed silica powder thereof is used. また、高圧水の圧力が24MPa未満では離脱シリカ粉の除去が十分に行われず、40MPaを超えると結晶質部分まで除去されルツボの高温における耐熱性が低下する。 The pressure of the high pressure water is not sufficiently removed leaving the silica powder is less than 24 MPa, the heat resistance is lowered at high temperatures of the crucible is removed until the crystalline portion exceeds 40 MPa.

上記フッ酸水溶液処理は、ルツボの内外表面にフッ酸水溶液を吹き付けても、またルツボをフッ酸水溶液に浸漬してもよいが、内表面のエッチング量を1〜50μm、外表面のエッチング量を1〜10μmとすることが重要である。 The hydrofluoric acid treatment, be sprayed hydrofluoric acid solution in the inner and outer surfaces of the crucible, also may be immersed the crucible in an aqueous solution of hydrofluoric acid, the etching amount of the inner surface 1 to 50 [mu] m, the amount of etching of the outer surface it is important to 1~10μm. 内表面のエッチング量が1μm未満では表面の不純物及び離脱シリカ粉の除去が十分でなく、エッチング量が50μmを超えると内表面が肌荒れを起し、シリコン単結晶の結晶化率が低下する。 Etching of the inner surface is not sufficient removal of impurities and leaving the silica powder surface is less than 1 [mu] m, the amount of etching caused the inner surface rough exceeds 50 [mu] m, the crystallization rate of the silicon single crystal is lowered. さらに、最外層のエッチング量が1μm未満では表面の不純物及び離脱シリカ粉の除去が十分でなく、エッチング量が10μmを超えると、外表面の半溶融部分が剥離し易くなり離脱シリカ粉が増大する。 Furthermore, it is less than the amount of etching of the outermost layer is 1μm removal of impurities and leaving the silica powder surface is not sufficient, an etching amount exceeds 10 [mu] m, leaving the silica powder tends semi-molten portion of the outer surface is separated increases . この状態から更にエッチング処理を行い、半溶融部分を全て除去すれば離脱シリカ粉を少なくできるが、この場合は外表面の結晶質部分が除去され高温における耐熱性が低下する。 And performing additional etching process from this state, can be reduced withdrawal silica powder If all the semi-molten portion removed, in this case heat resistance at high temperatures is removed crystalline portion of the outer surface is reduced.

上記の製造方法において、回転する型の少なくとも直胴部を形成する部分がステンレス鋼製であることでルツボ最外層の未溶融ないし半溶融のシリカ粉の層が好ましい範囲に形成される。 In the above manufacturing method, the portion forming at least the straight body portion of a rotating mold a layer of silica powder unmelted or partially melted in the crucible outermost layer is formed in a preferable range by a stainless steel. カーボン型を使用すると未溶融ないし半溶融のシリカ粉の層が薄くなり耐熱性が低下し易くなる。 Layer becomes thin heat resistance of the silica powder unmelted or partially melted by using the carbon mold tends to decrease. また、回転する型と溶融された石英ガラスルツボの最外層の間に残る原料粉の厚さを、少なくとも直胴部において3〜7mmとすることで、同様に、未溶融ないし半溶融のシリカ粉の層が最適化される。 Further, the thickness of the raw material powder remaining between the outermost layer of the mold and the molten quartz glass crucible is rotated, by a 3~7mm at least the straight body part, similarly, unmelted or semi-molten silica powder layer of is optimized. 前記範囲未満では未溶融ないし半溶融のシリカ粉の層が少なくなり、前記範囲を超えるとルツボの寸法を制御することが難しくなるため好ましくない。 Wherein the amount is less than the range decreases the layer of silica powder unmelted or partially melted, is not preferable because it becomes difficult to control the size of the crucible when exceeding the above range.

本発明は、回転モールド法で得たルツボの外表面に固体シリカ粉を吹き付けたのち高圧水を吹き付け、さらに内・外表面をフッ酸水溶液処理で施すという簡便な方法で石英ガラスルツボの内表面に離脱するシリカ粉がない上に、最外層から離脱するシリカ粉が少なく、離脱シリカ粉のシリコン融液への混入による結晶転位を抑え、されに、最外層の結晶質部分を多く残し高温における耐熱性を高く維持できシリコン単結晶を高歩留りで製造できるという効果を奏します。 The present invention, the inner surface of the quartz glass crucible in a simple method of rotating the outer surface of the obtained crucible molding blowing high pressure water After spraying the solid silica powder is subjected to inner and outer surfaces with hydrofluoric acid aqueous solution treatment further on no silica powder to leave the less silica powder leaves the outermost suppressing crystal dislocation due to contamination of the silicon melt leaving the silica powder, to be, at high temperatures, leaving a lot of crystalline portion of the outermost layer This provide an advantage that a silicon single crystal can maintain a high heat resistance can be produced in high yield.

以下に実施例を挙げて本発明を更に具体的に説明するが、本発明はこれに限定されるものではない。 The following examples further illustrate the invention, but the present invention is not limited thereto.

回転するステンレス鋼の型内に純化処理した高純度の天然シリカ粉を投入し、遠心力によりルツボ状成形体を形成し、その内にアーク電極を挿入し、開口部を板状の蓋体で覆い、アーク電極により内部キャビティー内を高温ガス雰囲気とし、溶融ガラス化して不透明な外層を作成し、次いで合成シリカ粉をシリカ粉供給手段から100g/minで供給し、溶融して合成石英ガラスからなる内層を形成し24インチの石英ガラスルツボを製造した。 And purification treatment into a mold of stainless steel that rotates a high-purity natural silica powder was charged, to form a crucible-shaped molded product by centrifugal force, to insert the arc electrode to them, the opening with a plate-shaped lid from cover, the inside of the internal cavity to a high temperature gas atmosphere by the arc electrode, and the molten vitrified to create an opaque outer layer, then synthetic silica powder was fed at 100 g / min from the silica powder supply means, melted and synthetic quartz glass inner layer was formed composed to produce a quartz glass crucible 24 inch. 前記石英ガラスルツボの外表面に固体シリカ粉を吹付圧1MPaで吹き付けたのち、高圧水を吹付圧30MPaで、かつルツボと高圧水噴射ノズルの距離を50mmに保って吹き付け、次いで、25質量%のフッ酸水溶液を内表面は40分間、外表面は10分間吹付け、内表面のエッチング量を20μm、外表面のエッチング量を5μmとし、純水で20分間濯ぎ、乾燥して石英ガラスルツボを製造した。 After spraying solid silica powder on the outer surface of the quartz glass crucible by spraying pressure 1 MPa, at a spraying pressure 30MPa high-pressure water, and sprayed while maintaining a distance of the crucible and the high-pressure water jet nozzle 50 mm, then 25% by weight inner surface 40 min hydrofluoric acid aqueous solution, the outer surface is spraying 10 minutes, the amount of etching of the inner surface 20 [mu] m, and 5μm etching amount of the external surface, rinsed with pure water for 20 minutes, producing a quartz glass crucible and dried did. 得られた石英ガラスルツボについて粘着テープ法で直胴部外表面の離脱シリカ粉の個数を測定したところ0.5個/cm2であった。 The number of withdrawal silica powder of the obtained quartz glass crucible with adhesive tape method straight barrel outer surface was 0.5 pieces / cm2 was measured. この石英ガラスルツボに多結晶シリコンを充填し、溶融してCZ法で単結晶の引上げを行ったところシリコン単結晶を乱れなく引き上げることができた。 The quartz glass crucible filled with polycrystalline silicon, could be raised without turbulence the melted and the silicon single crystal was subjected to pulling of the single crystal in the CZ method.
(比較例1) (Comparative Example 1)

実施例1において、外表面を内表面と同じ40分間のフッ酸水溶液処理を行った以外、実施例1と同様にして石英ガラスルツボを製造し、その最外層の離脱シリカ粉の個数を粘着テープ法で測定したところ2.3個/cm3であった。 In Example 1, except that was hydrofluoric acid treatment of the same 40 minutes the inner surface of the outer surface, to produce a quartz glass crucible in the same manner as in Example 1, the adhesive and the number of withdrawal silica powder of the outermost tape was 2.3 cells / cm3 was measured by law. この石英ガラスルツボを用いてシリコン単結晶を引き上げたところ、転位が数回発生し付け直しを行って引上げを継続したが、最終歩留りは設定の75%であった。 The quartz glass crucible using was pulled silicon single crystal, but dislocation was continued pulling performed renumbered occurs several times, the final yield was 75% of the set.
(比較例2) (Comparative Example 2)

実施例1と同様にして製造した石英ガラスルツボの外表面を研削加工した以外、実施例1と同様にして石英ガラスルツボを製造した。 Except that the outer surface of the quartz glass crucible produced in the same manner as in Example 1 were grinding, to produce a quartz glass crucible in the same manner as in Example 1. 得られた石英ガラスルツボの離脱石英粉の個数を粘着テープ法で測定したところ0.02個/cm3であった。 The number of withdrawal quartz powder obtained quartz glass crucible was 0.02 / cm3 was measured by adhesive tape method. この石英ガラスルツボを用いてシリコン単結晶を引き上げたところ、引上げの途中でルツボに変形が起こり単結晶の引上げを中止せざるを得なかった。 The quartz glass crucible using was pulled silicon single crystal, is deformed in the crucible during the pulling occurred had to discontinue the pulling of the single crystal.

本発明はシリコン単結晶を高歩留りで製造できシリコン単結晶の引上げ分野において有用な製造方法である。 The present invention is a useful method for producing in pulling the field of silicon single crystal can be produced a silicon single crystal at high yield.

Claims (2)

  1. 回転する少なくとも直胴部がステンレス鋼製である型内に原料粉を供給しルツボ状の原料粉体層を形成し、その内側からアーク放電加熱し溶融して平滑な内表面と不透明又は半透明な外層と、その外側に未溶融ないし半溶融のシリカ粉が偏在する最外層を有する石英ガラスルツボを製造し、その外表面に固体シリカ粉を吹付け圧0.1〜5MPaで吹き付けたのち、高圧水を吹付け圧24〜40M Paで、かつルツボと高圧水噴射ノズルとの距離を10〜60mmに保って吹き付け、次いでフッ酸水溶液処理を施し、内表面のエッチング量を1〜50μm、外表面のエッチング量を1〜10μmと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。 At least the straight body section rotates supplies the raw material powder in a mold made of stainless steel to form a crucible-like raw material powder layer, opaque or translucent and the arc discharge heating to melt to a smooth inner surface from the inside and an outer layer, such, after its manufacture unfused or fused silica crucible having an outermost layer of the silica powder of semi-molten is unevenly distributed on the outside, a solid silica powder was sprayed with spray pressure 0.1~5MPa on its outer surface, in high-pressure water spraying pressure 24~40M Pa, and sprayed while maintaining a distance between the crucible and the high-pressure water jet nozzles 10 to 60 mm, then facilities hydrofluoric acid aqueous solution treatment, the etching amount of the inner surface 1 to 50 [mu] m, method for manufacturing a silicon single crystal for pulling up the quartz glass crucible, characterized in that the etching amount of the external surface and the 1 to 10 [mu] m.
  2. 回転する型と溶融された石英ガラスルツボの最外層の間に残る原料粉の厚さが、少なくとも直胴部において3〜7mmであることを特徴とする請求項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。 The thickness of the raw material powder remaining between the outermost layer of the melt and the mold rotating quartz glass crucible, a silicon single crystal for pulling quartz according to claim 1, characterized in that the 3~7mm at least in the straight body portion manufacturing method of a glass crucible.



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