JP5611904B2 - Silica glass crucible for pulling silicon single crystal and method for producing the same - Google Patents
Silica glass crucible for pulling silicon single crystal and method for producing the same Download PDFInfo
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- JP5611904B2 JP5611904B2 JP2011174509A JP2011174509A JP5611904B2 JP 5611904 B2 JP5611904 B2 JP 5611904B2 JP 2011174509 A JP2011174509 A JP 2011174509A JP 2011174509 A JP2011174509 A JP 2011174509A JP 5611904 B2 JP5611904 B2 JP 5611904B2
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Description
本発明は、チョクラルスキー法（以下、ＣＺ法と言う。）によりシリコン単結晶を引上げる際に用いられる、原料シリコン融液を収容するための石英ガラスルツボ及びその製造方法に関する。 The present invention relates to a quartz glass crucible for containing a raw material silicon melt used when pulling up a silicon single crystal by the Czochralski method (hereinafter referred to as CZ method) and a method for producing the same.
シリコン単結晶の製造においては、ＣＺ法が広く用いられている。この方法は、ルツボ内に収容された原料シリコン融液の表面に種結晶を接触させ、ルツボを回転させるとともに、前記種結晶を反対方向に回転させながら上方へ引上げることにより、種結晶の下端に単結晶インゴットを育成していくものである。
上記方法において、シリコン融液を収容するためのルツボには、一般に、内層が高純度の合成石英ガラスの透明層からなり、外層が内層よりも純度が低く、安価な、天然石英ガラスの不透明層からなる石英ガラスルツボが用いられている。
The CZ method is widely used in the production of silicon single crystals. In this method, the seed crystal is brought into contact with the surface of the raw material silicon melt contained in the crucible, the crucible is rotated, and the seed crystal is pulled upward while rotating the seed crystal in the opposite direction. Single crystal ingots are nurtured.
In the above method, the crucible for containing the silicon melt is generally an opaque layer of natural quartz glass whose inner layer is made of a transparent layer of high-purity synthetic quartz glass and whose outer layer is lower in purity and cheaper than the inner layer. A quartz glass crucible made of is used.
しかしながら、安価な天然石英ガラス層中には、一般的に、Ｎａ、Ｋ、Ｌｉ等のアルカリ金属が多く含まれており、このような高温で拡散しやすい不純物がルツボ外層に多く含まれていると、シリコン単結晶の引上げ初期にルツボ内表面に拡散し、引上げ中に内表面の劣化が進行しやすくなり、引上げられるシリコン単結晶に転位が発生する要因となる。また、前記不純物は、ルツボ内表面の石英ガラスとともにシリコン融液中に溶出するため、引上げられるシリコン単結晶の品質低下の要因にもなり得るため、シリコン単結晶引上げの歩留低下を招くこととなる。 However, an inexpensive natural quartz glass layer generally contains a large amount of alkali metals such as Na, K, and Li, and a large amount of such impurities that are likely to diffuse at high temperatures are contained in the outer layer of the crucible. Then, the silicon single crystal is diffused to the inner surface of the crucible at the initial stage of pulling, and the inner surface is easily deteriorated during the pulling, which causes dislocation in the pulled silicon single crystal. In addition, since the impurities are eluted into the silicon melt together with the quartz glass on the inner surface of the crucible, it may cause a decrease in the quality of the silicon single crystal to be pulled up. Become.
これに対しては、特許文献１に、外層の添加Ａｌを５０〜１２０ｐｐｍの高濃度とする一方、この外層と高純度合成石英層の内層との間に、天然石英層又は高純度合成石英層の中間層を形成し、３層構造とすることにより、内層へのアルカリ金属の拡散を防止することができ、シリコン融液のアルカリ金属汚染が防止される旨記載されている。 For this, in Patent Document 1, the additive Al in the outer layer is set to a high concentration of 50 to 120 ppm, while a natural quartz layer or a high purity synthetic quartz layer is provided between the outer layer and the inner layer of the high purity synthetic quartz layer. It is described that the intermediate layer is formed to have a three-layer structure, whereby diffusion of alkali metal into the inner layer can be prevented, and alkali metal contamination of the silicon melt is prevented.
しかしながら、上記特許文献１に記載された外層のように高濃度のＡｌを添加すると、ルツボ使用時の高温下において、ルツボ外層の結晶化が急速に進行し、厚い結晶層が形成され、特に、底部の湾曲部において、冷却時にルツボにクラックが生じ、湯漏れを招くおそれがあった。 However, when a high concentration of Al is added as in the outer layer described in Patent Document 1, the crucible outer layer rapidly crystallizes at a high temperature when the crucible is used, and a thick crystal layer is formed. In the curved portion at the bottom, there was a risk that cracks would occur in the crucible during cooling, leading to hot water leakage.
したがって、高品質のシリコン単結晶を歩留よく引上げるためには、該ルツボの構成材料である石英ガラスに含まれるアルカリ金属等によるルツボ内のシリコン融液の汚染が防止され、しかも、湯漏れ等を生じることのない十分な強度を保持することができるルツボが求められる。 Therefore, in order to increase the yield of high-quality silicon single crystals with good yield, contamination of the silicon melt in the crucible by alkali metal contained in quartz glass, which is a constituent material of the crucible, is prevented, and hot water leaks. There is a need for a crucible that can maintain sufficient strength without causing any other problems.
本発明は、上記技術的課題を解決するためになされたものであり、ルツボの構成材料に含まれるアルカリ金属によってルツボ内のシリコン融液が汚染されるのを防止することができ、しかも、シリコン融液の保持のための十分な強度を備えており、シリコン単結晶引上げの歩留向上を図ることができるシリコン単結晶引上げ用石英ガラスルツボを提供することを目的とするものである。 The present invention has been made to solve the above technical problem, and can prevent the silicon melt in the crucible from being contaminated by an alkali metal contained in the constituent material of the crucible. An object of the present invention is to provide a quartz glass crucible for pulling a silicon single crystal that has sufficient strength for holding a melt and can improve the yield of pulling the silicon single crystal.
本発明に係るシリコン単結晶引上げ用石英ガラスルツボは、ルツボ内層が合成石英ガラスからなり、ルツボ外層が２〜１０ｐｐｍの添加Ａｌが固溶した天然石英ガラスからなり、前記添加Ａｌの濃度が、外表面付近よりも前記ルツボ内層との界面付近の方が高く、該天然石英ガラス中のアルカリ金属の濃度の総和と同等以上であることを特徴とする。
このように、ルツボ外層に所定量のＡｌを添加して固溶させることにより、ルツボの強度を十分に保持しつつ、ルツボの構成材料に含まれるアルカリ金属が拡散してルツボ内のシリコン融液を汚染することを抑制することができる。
The quartz glass crucible for pulling up a silicon single crystal according to the present invention has a crucible inner layer made of synthetic quartz glass and a crucible outer layer made of natural quartz glass in which 2 to 10 ppm of added Al is dissolved, and the concentration of the added Al is outside. than near the surface it is rather high in the vicinity of the interface with the crucible inner layer, and characterized in that the sum equal to or greater than the concentration of the alkali metal of the natural quartz glass.
In this way, by adding a predetermined amount of Al to the outer layer of the crucible and dissolving it, the alkali metal contained in the material constituting the crucible diffuses and the silicon melt in the crucible diffuses while maintaining the strength of the crucible sufficiently. It is possible to suppress contamination.
前記ルツボ外層の添加Ａｌの濃度は、アルカリ金属を十分にトラップさせる観点から、該天然石英ガラス中のアルカリ金属の濃度の総和と同等以上であることが好ましい。 The concentration of added Al of the crucible outer layer, from the viewpoint of sufficiently trapped alkali metal is preferably Ru der sum equal to or greater than the concentration of the alkali metal of the natural quartz glass.
また、本発明に係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は、上記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おいて、前記添加Ａｌが硝酸アルミニウム九水和物水溶液として天然石英ガラス原料粉末に添加されることを特徴とする。
このような硝酸塩の水溶液によれば、天然石英ガラスに固溶させるＡｌを容易に添加することができる。
The method for producing a quartz glass crucible for pulling up a silicon single crystal according to the present invention is the method for producing a quartz glass crucible for pulling up a silicon single crystal, wherein the additive Al is a natural quartz glass raw material powder as an aluminum nitrate nonahydrate aqueous solution. It is characterized by being added to.
According to such an aqueous solution of nitrate, Al to be dissolved in natural quartz glass can be easily added.
本発明に係るシリコン単結晶引上げ用石英ガラスルツボによれば、ルツボ使用時の高温下においても、シリコン融液を収容保持可能な十分な強度が維持され、かつ、ルツボ外層に含まれるアルカリ金属が拡散し、ルツボ内のシリコン融液が汚染されることを抑制することができる。
したがって、本発明に係る石英ガラスルツボは、シリコン単結晶引上げの歩留向上に寄与し得るものである。
According to the silica glass crucible for pulling up a silicon single crystal according to the present invention, sufficient strength is maintained that can hold and hold a silicon melt even under high temperature when the crucible is used, and the alkali metal contained in the outer layer of the crucible is Diffusion and contamination of the silicon melt in the crucible can be suppressed.
Therefore, the quartz glass crucible according to the present invention can contribute to the improvement of the yield of pulling the silicon single crystal.
以下、本発明をより詳細に説明する。
本発明に係るシリコン単結晶引上げ用石英ガラスルツボは、ルツボ内層が合成石英ガラスであり、ルツボ外層が２〜１０ｐｐｍの添加Ａｌが固溶した天然石英ガラスである。
すなわち、本発明においては、ルツボ外層の天然石英ガラスに所定量のＡｌを添加して固溶させることを特徴とする。
このように、ルツボ外層におけるＡｌ濃度を従来のように過度にすることなく、少量の添加によって、ルツボ使用時の高温下においても、ルツボの構成材料である石英ガラスからのアルカリ金属が拡散することを効果的に抑制することができる。しかも、過度なＡｌ添加によるルツボ表面の結晶化やそれに起因するクラックの発生等を生じることなく、ルツボの強度を十分に保持することができる。
The present invention will be described in detail below.
The quartz glass crucible for pulling a silicon single crystal according to the present invention is a natural quartz glass in which the inner layer of the crucible is a synthetic quartz glass and the outer layer of the crucible is solid-solved with 2 to 10 ppm of added Al.
That is, the present invention is characterized in that a predetermined amount of Al is added to the natural quartz glass of the outer layer of the crucible and dissolved therein.
In this way, the alkali metal from the quartz glass, which is the constituent material of the crucible, diffuses even at high temperatures when using the crucible by adding a small amount without excessively increasing the Al concentration in the outer layer of the crucible as in the past. Can be effectively suppressed. Moreover, the strength of the crucible can be sufficiently maintained without causing crystallization of the crucible surface due to excessive addition of Al or generation of cracks resulting therefrom.
天然石英ガラス中に添加されたＡｌは、溶融時に置換固溶する形態でガラスネットワーク内に取り込まれ、このとき、Ａｌイオンの正電荷が１個不足した状態となる。このため、石英ガラス中にＡｌを固溶させることにより、Ｎａ、Ｋ、Ｌｉ等のアルカリ金属がトラップされ、拡散することを抑制することができる。
なお、石英ガラス原料には、元々、数ｐｐｍ〜数十ｐｐｍ程度のＡｌが含まれているが、この元々含まれているＡｌは、すでにアルカリ金属を取り込んだ状態であるため、ルツボを構成する石英ガラス中に拡散するアルカリ金属を新たに取り込むことはできない。
したがって、本発明においては、ルツボ外層を構成する天然石英ガラス原料に元々含まれているＡｌ濃度にかかわらず、この天然石英ガラス原料に２〜１０ｐｐｍの濃度でＡｌを新たに添加する。
Al added to the natural quartz glass is taken into the glass network in a form of substitutional solid solution at the time of melting, and at this time, one Al ion has a shortage of positive charge. For this reason, it can suppress that alkali metals, such as Na, K, and Li, are trapped and diffused by making Al dissolve in quartz glass.
Note that the quartz glass raw material originally contains about several ppm to several tens of ppm of Al, but this originally contained Al is already in the state of taking in an alkali metal, and thus constitutes a crucible. Alkali metals that diffuse into quartz glass cannot be newly taken up.
Therefore, in the present invention, Al is newly added to the natural quartz glass raw material at a concentration of 2 to 10 ppm regardless of the Al concentration originally contained in the natural quartz glass raw material constituting the crucible outer layer.
前記ルツボ外層の添加Ａｌの濃度は、少なくとも、ルツボ内のシリコン融液に対する不純物となる前記アルカリ金属の濃度の総和と同等以上である必要がある。
一方、多すぎると、ルツボの使用中に外面から過度に結晶化が進行し、結晶層が厚く形成されることとなる。これにより、特に、ルツボ底部において、冷却中にクラックが発生し、湯漏れの原因となりやすい。
したがって、添加Ａｌ濃度は２〜１０ｐｐｍとする。
The concentration of added Al in the outer layer of the crucible needs to be at least equal to or higher than the total concentration of the alkali metals that become impurities with respect to the silicon melt in the crucible.
On the other hand, when the amount is too large, crystallization proceeds excessively from the outer surface during use of the crucible, and the crystal layer is formed thick. As a result, cracks are generated during cooling, particularly at the bottom of the crucible, which is likely to cause hot water leakage.
Therefore, the additive Al concentration is 2 to 10 ppm.
また、前記添加Ａｌの濃度は、外表面付近よりも前記ルツボ内層との界面付近の方が高いことが好ましい。
このように、前記ルツボ外層の添加Ａｌの濃度を内層側の方が高くなるようにすることによって、少量の添加にもかかわらず、ルツボ使用時の高温下においても、ルツボ外層の天然石英ガラスからルツボ内層の合成石英ガラスへのアルカリ金属の拡散をより効果的に抑制することができる。
The concentration of the added Al is preferably higher in the vicinity of the interface with the crucible inner layer than in the vicinity of the outer surface.
In this way, by making the concentration of added Al in the outer layer of the crucible higher on the inner layer side, the natural silica glass of the outer layer of the crucible is used even at a high temperature when the crucible is used, despite the addition of a small amount. Alkali metal diffusion into the synthetic quartz glass in the inner crucible layer can be more effectively suppressed.
なお、一般に、ルツボ外層の天然石英ガラス層は、純度は低いものの、耐熱性に優れた不透明層であり、ルツボ内層の合成石英ガラス層は、シリコンアルコキシドの加水分解等により得られる高純度の合成シリカ原料により形成される透明層である。 In general, the natural silica glass layer of the outer crucible layer is an opaque layer with excellent heat resistance although the purity is low. The synthetic silica glass layer of the inner crucible layer is a high-purity synthetic material obtained by hydrolysis of silicon alkoxide or the like. It is a transparent layer formed from a silica raw material.
合成石英ガラスからなる前記ルツボ内層の厚さは１〜５ｍｍとすることが好ましい。
前記厚さが１ｍｍ未満の場合、薄すぎて、溶出によりルツボ内表面にルツボ外層が露出したり、シリコン融液の液面振動を生じさせたりするおそれがある。
一方、前記厚さが５ｍｍを超えても、厚さに見合った液面振動の発生の抑制等の効果の向上は図られず、また、ルツボの強度が不十分となるおそれがあるため、厚さは５ｍｍ以下で十分である。
The thickness of the inner crucible layer made of synthetic quartz glass is preferably 1 to 5 mm.
When the thickness is less than 1 mm, it is too thin and the outer layer of the crucible may be exposed on the inner surface of the crucible due to elution, or the liquid level vibration of the silicon melt may occur.
On the other hand, even if the thickness exceeds 5 mm, the effect of suppressing the occurrence of liquid level vibration corresponding to the thickness cannot be improved, and the strength of the crucible may be insufficient. A thickness of 5 mm or less is sufficient.
一方、天然石英ガラスからなる前記ルツボ外層の厚さは９〜１８ｍｍとすることが好ましい。
前記厚さが９ｍｍ未満の場合、薄すぎてルツボの強度を十分に保持することが困難となり、また、上述したアルカリ金属の拡散を抑制する効果が十分に得られない。
一方、前記厚さが１８ｍｍを超えても、厚さに見合ったアルカリ金属の拡散抑制効果が得られず、また、ルツボの重量増加によりルツボの支持が困難となるため、厚さは１８ｍｍ以下で十分である。
On the other hand, the thickness of the crucible outer layer made of natural quartz glass is preferably 9 to 18 mm.
When the thickness is less than 9 mm, it is too thin to sufficiently maintain the strength of the crucible, and the effect of suppressing the alkali metal diffusion described above cannot be sufficiently obtained.
On the other hand, even if the thickness exceeds 18 mm, the effect of suppressing the diffusion of alkali metal corresponding to the thickness cannot be obtained, and the crucible is difficult to support due to the increase in the weight of the crucible. It is enough.
前記内層及び外層を含むルツボ全体の厚さは、ルツボの強度や重量等を考慮して、１０〜２３ｍｍ程度であることが好ましい。通常は１５ｍｍ程度とする。 The thickness of the entire crucible including the inner layer and the outer layer is preferably about 10 to 23 mm in consideration of the strength and weight of the crucible. Usually about 15 mm.
上記のような本発明に係る石英ガラスルツボの製造においては、ルツボ外層を形成する際に、前記添加Ａｌを硝酸アルミニウム九水和物（Ａｌ(ＮＯ3)3・９Ｈ2Ｏ）の水溶液として天然石英ガラス原料粉末に添加した混合粉を用いることが好ましい。
このような硝酸塩の水溶液によれば、天然石英ガラスに固溶させるＡｌを容易に添加することができる。また、過剰の水分及び硝酸分は、乾燥、加熱により容易に除去することができ、取扱い容易である。
In the production of the silica glass crucible according to the present invention as described above, when the crucible outer layer is formed, the added Al is used as an aqueous solution of aluminum nitrate nonahydrate (Al (NO 3 ) 3 · 9H 2 O). It is preferable to use a mixed powder added to the British glass raw material powder.
According to such an aqueous solution of nitrate, Al to be dissolved in natural quartz glass can be easily added. Excess water and nitric acid can be easily removed by drying and heating, and is easy to handle.
本発明に係る石英ガラスルツボの製造方法は、上記のように天然石英ガラス原料に別途Ａｌを添加すること以外は、特に限定されるものではない。一般的には、回転モールド法及びアーク溶融法により製造される。
具体的には、回転するルツボ成形用型内に、外層を構成するための天然シリカ原料粉及び添加Ａｌの混合粉を所定の層厚さで装填し、その内側に内層を構成するための合成シリカ原料粉末を所定厚さで装填して、成形する。そして、この中にアーク電極を挿入し、減圧アーク溶融にてガラス化することにより、本発明に係る石英ガラスルツボを製造することができる。
なお、外層形成後、火炎溶融法により内層を直接堆積させて形成することもできる。
The method for producing a quartz glass crucible according to the present invention is not particularly limited except that Al is separately added to the natural quartz glass raw material as described above. Generally, it is manufactured by a rotary molding method and an arc melting method.
Specifically, in a rotating crucible molding die, a natural silica raw material powder for constituting the outer layer and a mixed powder of added Al are loaded with a predetermined layer thickness, and a synthesis for constituting the inner layer inside thereof. The silica raw material powder is charged at a predetermined thickness and molded. And the quartz glass crucible which concerns on this invention can be manufactured by inserting an arc electrode in this and vitrifying by low pressure arc melting.
In addition, after forming the outer layer, the inner layer can be directly deposited by a flame melting method.
以下、本発明を実施例に基づきさらに具体的に説明するが、本発明は下記の実施例により制限されるものではない。
回転モールド法及びアーク溶融法により、ルツボ内層が厚さ２ｍｍの合成石英ガラス層からなり、ルツボ外層が下記表１に示す各濃度の添加Ａｌが固溶した厚さ１４ｍｍの天然石英ガラス層からなる外径３２インチ、高さ４５０ｍｍの石英ガラスルツボを作製した。
天然石英ガラス原料粉末にＡｌを添加した混合粉末は、０．１〜０．９％の範囲の濃度で適宜調製した硝酸アルミニウム九水和物水溶液を、天然石英ガラス原料粉末１ｋｇ当たり１８ｇ添加して均一に分散させて乾燥させることにより調製した。
また、前記アーク溶融は、約２０００℃で１時間未満で行った。
EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
The inner layer of the crucible is made of a synthetic quartz glass layer having a thickness of 2 mm by the rotary molding method and the arc melting method, and the outer layer of the crucible is made of a natural quartz glass layer having a thickness of 14 mm in which additive Al of each concentration shown in Table 1 below is dissolved. A quartz glass crucible having an outer diameter of 32 inches and a height of 450 mm was produced.
The mixed powder obtained by adding Al to the natural quartz glass raw material powder is obtained by adding 18 g of an aluminum nitrate nonahydrate aqueous solution appropriately prepared at a concentration in the range of 0.1 to 0.9% per 1 kg of the natural quartz glass raw material powder. It was prepared by uniformly dispersing and drying.
The arc melting was performed at about 2000 ° C. for less than 1 hour.
作製した石英ガラスルツボ各１０個を、カーボンルツボに嵌め込んでセットし、ルツボ外周からヒータ加熱して、ルツボ内で約３００ｋｇの原料シリコンを溶融させ、ＣＺ法により、直径１２インチのシリコン単結晶の引上げを２回行った。
そして、シリコン単結晶引上げ後のルツボ内表面を観察した。
また、シリコン単結晶引上げにおける無転位化率（ＤＦ率）を求めた。無転位化率は、原料シリコンの量から理論的に求められる単結晶長さに対して実際に無転位で引上げられた単結晶長さの割合である。表１においては、各ルツボのＤＦ率の平均値を示した。また、引上げ後のルツボ内層のアルカリ金属の含有量をＩＣＰ質量分析により測定した。
これらの評価結果を表１にまとめて示す。
Each 10 quartz glass crucibles that were produced were fitted and set in a carbon crucible, heated by a heater from the outer periphery of the crucible, about 300 kg of raw silicon was melted in the crucible, and a silicon single crystal having a diameter of 12 inches was obtained by the CZ method. Was raised twice.
Then, the inner surface of the crucible after pulling the silicon single crystal was observed.
Further, the dislocation-free rate (DF rate) in pulling the silicon single crystal was determined. The dislocation-free rate is the ratio of the single crystal length actually pulled up without dislocation to the single crystal length theoretically determined from the amount of raw silicon. In Table 1, the average value of the DF ratio of each crucible is shown. Further, the content of alkali metal in the crucible inner layer after the pulling was measured by ICP mass spectrometry.
These evaluation results are summarized in Table 1.
上記評価の結果、本発明に係る石英ガラスルツボ（実施例１〜３）によれば、ルツボ内表面の面荒れの発生はなく、また、無転位のシリコン単結晶をほぼ確実に引き上げることができた。
一方、外層の添加Ａｌ濃度が低い場合（比較例１）は、ルツボの直胴部から底部にかけての湾曲部におけるルツボ内表面の面荒れの発生が目立ち、また、引上げるシリコン単結晶のＤＦ率も低下した。
また、外層の添加Ａｌ濃度が高い場合（比較例２）は、ルツボ使用後のルツボ内表面の面状態は良好であったが、長時間の使用により、ルツボ２個の底部外面に結晶化層が厚く成長し、冷却時に湯漏れが発生した。
As a result of the above evaluation, according to the quartz glass crucible (Examples 1 to 3) according to the present invention, there is no surface roughness of the inner surface of the crucible, and the dislocation-free silicon single crystal can be pulled up almost certainly. It was.
On the other hand, when the added Al concentration in the outer layer is low (Comparative Example 1), the surface roughness of the inner surface of the crucible in the curved portion from the straight body portion to the bottom portion of the crucible is conspicuous, and the DF ratio of the silicon single crystal to be pulled up Also declined.
In addition, when the additive Al concentration in the outer layer is high (Comparative Example 2), the surface state of the inner surface of the crucible after the use of the crucible was good, but the crystallization layer was formed on the outer surface of the bottom of the two crucibles after a long period of use. Grew thick and leaked during cooling.
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