JPH082932A - Quartz glass crucible and its production - Google Patents
Quartz glass crucible and its productionInfo
- Publication number
- JPH082932A JPH082932A JP15960294A JP15960294A JPH082932A JP H082932 A JPH082932 A JP H082932A JP 15960294 A JP15960294 A JP 15960294A JP 15960294 A JP15960294 A JP 15960294A JP H082932 A JPH082932 A JP H082932A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- group
- glass crucible
- crucible
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、シリコン単結晶を長時
間引上げることができる石英ガラスルツボとその製造方
法、さらに詳しくはマルチ引上げ法や連続充填引上げ法
等でシリコン単結晶を長時間に亘って引上げることがで
きる大口径石英ガラスルツボおよびその製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a quartz glass crucible capable of pulling a silicon single crystal for a long time and a method for manufacturing the same, and more specifically, a multi-pulling method or a continuous filling pulling method for pulling a silicon single crystal for a long time. The present invention relates to a large-diameter quartz glass crucible that can be pulled over and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】近年、シリコンウエーハの大口径化に伴
い、単結晶引上用石英ガラスルツボの口径も１８インチ
（４５７．２ｍｍ）から２２〜２４インチ（５５８．８
〜６０９．６ｍｍ）と大きくなりそれが今日では主流と
なりつつある。前記単結晶引上用石英ガラスルツボの内
表面は、シリコン溶融液に接し、シリコンと反応し溶解
したり、あるいは外部のカーボンヒーターからの熱をシ
リコン融液に伝熱する機能を有している。この単結晶引
上用石英ガラスルツボの大口径化に伴い、ルツボの内壁
が単結晶から離れその熱負荷が大きくなり、例えば８イ
ンチ結晶の引上げには６インチ結晶の時より接湯面の温
度が５℃以上高くなり、ルツボ内表面の溶損速度は５割
増し以上となる等、溶損量が増え、ルツボ内表面が荒
れ、ルツボの長期使用が困難となり、単結晶のコスト高
を招いていた。こうした問題点を解決するため、ルツボ
の内表面を炭化物やチッ化物のセラミックスで被覆する
方法が特開平１ー１４１７０号公報で、また石英ガラス
にクリストバライトを混入したいわゆるガラスセラミッ
クスルツボが特開平５ー２４８７０号公報で提案され
た。しかしながら、前者のルツボは単結晶の引き上げ時
に被覆セラミックスが剥離し、満足のいく溶損量の低減
を図ることができなかった。また後者のルツボにおいて
は溶損量が従来のルツボとほとんど変わるところがない
という欠点があった。2. Description of the Related Art In recent years, as the diameter of silicon wafers has increased, the diameter of quartz glass crucibles for pulling single crystals has increased from 18 inches (457.2 mm) to 22 to 24 inches (558.8).
Up to 609.6 mm), which is becoming the mainstream today. The inner surface of the quartz glass crucible for pulling a single crystal has a function of coming into contact with a silicon melt and melting by reacting with silicon, or transferring heat from an external carbon heater to the silicon melt. . With the increase in diameter of this quartz glass crucible for pulling a single crystal, the inner wall of the crucible separates from the single crystal and its heat load becomes large. For example, when pulling an 8-inch crystal, the temperature of the molten surface is higher than that of a 6-inch crystal. Is higher than 5 ° C and the melting rate of the inner surface of the crucible is increased by 50% or more. The amount of melting loss is increased, the inner surface of the crucible is roughened, the long-term use of the crucible becomes difficult, and the cost of the single crystal is increased. It was In order to solve these problems, a method of coating the inner surface of the crucible with a ceramic of carbide or nitride is disclosed in JP-A-1-14170, and a so-called glass-ceramic crucible in which cristobalite is mixed in quartz glass is disclosed in JP-A-5-170. It was proposed in Japanese Patent No. 24870. However, in the former crucible, the coating ceramics were peeled off when pulling the single crystal, and it was not possible to satisfactorily reduce the melting loss amount. Further, the latter crucible has a drawback that the amount of melting loss is almost the same as that of the conventional crucible.
【０００３】[0003]
【発明が解決しようとする課題】こうした現状に鑑み、
本発明者らは鋭意研究を重ねた結果、ルツボ内表面をそ
の使用時に結晶化させることにより石英ガラスルツボの
溶損量を少なくできることを見出し、本発明を完成した
ものである。すなわち、In view of the current situation,
As a result of earnest studies, the present inventors have found that the amount of melting loss of the quartz glass crucible can be reduced by crystallizing the inner surface of the crucible at the time of its use, and completed the present invention. That is,
【０００４】本発明は、溶損量が少なく長時間の使用に
耐える石英ガラスルツボを提供することを目的とする。An object of the present invention is to provide a quartz glass crucible which has a small amount of melting loss and can be used for a long time.
【０００５】また、本発明は、ルツボの使用時に内表面
が結晶化する耐熱性の高い石英ガラスルツボを提供する
ことを目的とする。Another object of the present invention is to provide a quartz glass crucible having a high heat resistance whose inner surface is crystallized when the crucible is used.
【０００６】さらに、本発明は、耐熱性の高い石英ガラ
スルツボの製造方法を提供することを目的とする。A further object of the present invention is to provide a method for manufacturing a quartz glass crucible having high heat resistance.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成する本発
明は、石英ガラスルツボ内表面の厚さ１ｍｍ以内に結晶
化促進剤含有塗布膜または固溶層が形成されていること
を特徴とする石英ガラスルツボおよび該ルツボの製造方
法に係る。The present invention for achieving the above object is characterized in that a coating film or a solid solution layer containing a crystallization accelerator is formed within a thickness of 1 mm on the inner surface of the quartz glass crucible. The present invention relates to a quartz glass crucible and a method for manufacturing the crucible.
【０００８】上記結晶化促進剤とは、ルツボがシリコン
融液と接触した時ルツボ内表面に結晶を生成させる結晶
化剤をいい、２ａ族元素または３ｂ族元素からなる。前
記２ａ族元素としては、マグネシウム、ストロンチウ
ム、カルシウムまたはバリウムが挙げられ、また３ｂ族
元素としてはアルミニウムが挙げられる。前記結晶化促
進剤はルツボ内表面に塗布膜または固溶層として存在す
る。The above-mentioned crystallization accelerator is a crystallization agent which produces crystals on the inner surface of the crucible when the crucible comes into contact with the silicon melt, and is composed of a 2a group element or a 3b group element. The group 2a element may be magnesium, strontium, calcium or barium, and the group 3b element may be aluminum. The crystallization accelerator exists as a coating film or a solid solution layer on the inner surface of the crucible.
【０００９】上記結晶化促進剤が２ａ族元素の場合に
は、その化合物の溶液をルツボ内表面に２ａ族元素濃度
が塗布膜１ｃｍ2当り１〜１００μｇ、好ましくは１０
〜５０μｇの範囲となるように塗布して塗布膜を形成す
る。これにより単結晶引上げの加熱時に前記２ａ族元素
がルツボ内部に拡散浸透し深さ０．５〜１ｍｍの範囲に
結晶層を形成し、ルツボ内壁の溶損量を少なくし、ルツ
ボの長時間の使用を可能とする。２ａ族元素の存在量が
前記範囲未満では結晶の生成が少なく効果がなく、また
前記範囲以上では結晶が多過ぎ、シリコン単結晶の引上
げ中に該結晶が剥離し、単結晶の結晶化率を低下させ
る。When the crystallization accelerator is a group 2a element, a solution of the compound is added to the inner surface of the crucible so that the concentration of the group 2a element is 1 to 100 μg, preferably 10 per cm 2 of the coating film.
A coating film is formed by coating so as to be in the range of 50 μg. As a result, the group 2a element diffuses and permeates into the crucible at the time of heating for pulling the single crystal to form a crystal layer in a depth range of 0.5 to 1 mm, thereby reducing the amount of melting damage on the inner wall of the crucible, and for a long time of the crucible. Enables use. If the abundance of the 2a group element is less than the above range, there is little effect of crystal formation, and if it is more than the above range, the number of crystals is too large and the crystals are separated during pulling of the silicon single crystal, and the crystallization rate of the single crystal is increased. Lower.
【００１０】上記２ａ族元素化合物としては水に溶ける
硝酸塩または炭酸塩がよく、これを水、好ましくはアル
コールを２０重量％以上含む水に溶解した塗布液が好適
である。前記アルコールとしては、メチルアルコールま
たはエチルアルコールを挙げることができる。The group 2a element compound is preferably a nitrate or carbonate soluble in water, and a coating solution prepared by dissolving this in water, preferably water containing 20% by weight or more of alcohol, is suitable. Examples of the alcohol include methyl alcohol and ethyl alcohol.
【００１１】また、結晶化促進剤が３ｂ族元素の場合に
は、前記元素を含む塗布液で塗布しても加熱による拡散
浸透が起こらないため、固溶状態で層中に存在させるの
がよい。固溶層としては、例えば特開平１ー１４８７１
８号公報に記載するように、回転する型内にシリカ粉末
をルツボ状に充填しそれを溶融すると同時に、ゾルゲル
法で得られた高純度のゾルゲルシリカ粉にドープした３
ｂ族元素ドープトシリカ粉をルツボ内に供給し、それを
ルツボ内表面上に溶融・飛散させ形成した０．５〜１ｍ
ｍの厚さの透明層とするのがよい。前記透明層に０．１
〜２重量％の範囲で３ｂ族元素が存在するとシリコン単
結晶の引上げ等の加熱時に結晶層が形成されルツボ内壁
の溶損量が少なくなる。３ｂ族元素としてはアルミニウ
ムが好適である。前記固溶層中の３ｂ族元素が前記範囲
以下では結晶の形成が少なく効果がなく、また前記範囲
を超える量であると、結晶が多過ぎルツボとの熱膨張率
の差による剥離が起こり、シリコン単結晶の結晶化率を
阻害する。When the crystallization accelerator is a Group 3b element, it does not cause diffusion and permeation by heating even if it is coated with a coating liquid containing the above element, so it is preferable to make it exist in the layer in a solid solution state. . As the solid solution layer, for example, JP-A-1-14871.
As described in Japanese Unexamined Patent Publication No. 8-8, silica powder was charged into a rotating mold in a crucible shape and melted, and at the same time, high-purity sol-gel silica powder obtained by a sol-gel method was doped with 3
0.5 to 1 m formed by supplying the b-group element-doped silica powder into the crucible and melting and scattering it on the inner surface of the crucible
It is preferable that the transparent layer has a thickness of m. 0.1 in the transparent layer
If the Group 3b element is present in the range of up to 2% by weight, a crystal layer is formed during heating such as pulling of the silicon single crystal, and the amount of melting damage on the inner wall of the crucible decreases. Aluminum is preferable as the Group 3b element. If the group 3b element in the solid solution layer is less than the above range, there is little effect of crystal formation, and if the amount exceeds the above range, the amount of crystals is too large and peeling occurs due to the difference in the coefficient of thermal expansion from the crucible, It hinders the crystallization rate of silicon single crystals.
【００１２】本発明の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、約１４００℃でルツボ内表
面に結晶層が形成され、その耐熱性によりルツボ内壁の
平滑さが維持され例えばマルチ引上げ法や連続充填法等
の長時間の引上げによっても溶損することが少なくてす
む。When a silicon single crystal is pulled up using the quartz glass crucible of the present invention, a crystal layer is formed on the inner surface of the crucible at about 1400 ° C., and the heat resistance thereof keeps the inner wall of the crucible smooth, for example, multi-pulling. It is less likely to be melted down even by a long-time pulling method such as a method or a continuous filling method.
【００１３】[0013]
【実施例】以下に実施例に基づいて具体的に説明する
が、本発明はこれに限定されるものではない。EXAMPLES The present invention will be specifically described below based on examples, but the present invention is not limited thereto.
【００１４】実施例１ シリコンテトラエトキシドを主原料として塩化アルミニ
ウムの水溶液を加え、濃度とＰＨを調節しながら、シリ
カゾルを作った。これを１，０００℃で焼成後、粉砕整
粒して平均粒径１２５μｍの、重量濃度で１％のアルミ
ニウム元素を含む二酸化珪素粉を得た。高純度天然水晶
粉を垂直軸の周りに回転するモールド中に成型し、内面
から電気アークで加熱して口径が１８インチの石英ガラ
スルツボ基体を製造し、引き続いてアーク火炎中に、前
記アルミニウムドープ二酸化珪素粉を徐々に供給してル
ツボ基体の内側に１ｍｍの厚さの石英ガラス層を形成し
た。該ガラス層はわずかに白濁しているが強固に基体に
融着した石英ガラス層であった。このルツボを用いてシ
リコン単結晶を引上げたところ、アルミニウム元素がド
ープされている厚さ（１ｍｍ）だけ結晶化し、このため
溶融シリコンに殆ど溶けなかった。多結晶シリコンを追
加し再び結晶を引上げる操作を繰り返す、いわゆるマル
チ引上げ法を用いて１０回の引上げが実施できた。Example 1 A silica sol was prepared by adding an aqueous solution of aluminum chloride using silicon tetraethoxide as a main raw material and adjusting the concentration and PH. This was baked at 1,000 ° C. and then pulverized and sized to obtain silicon dioxide powder having an average particle diameter of 125 μm and containing 1% by weight of aluminum element. High-purity natural quartz powder is molded in a mold rotating around a vertical axis and heated from the inner surface by an electric arc to produce a quartz glass crucible substrate with an 18-inch diameter. Subsequently, the aluminum dope is added to the arc flame. The silicon dioxide powder was gradually supplied to form a quartz glass layer having a thickness of 1 mm inside the crucible substrate. The glass layer was a slightly opaque quartz glass layer which was firmly fused to the substrate. When a silicon single crystal was pulled up using this crucible, it was crystallized by a thickness (1 mm) doped with aluminum element, and thus was hardly melted in the molten silicon. It was possible to carry out pulling 10 times by using the so-called multi-pulling method in which the operation of adding polycrystalline silicon and pulling the crystal again was repeated.
【００１５】実施例２ 口径が１８インチの高純度石英ガラスルツボに、表１に
示した配合の溶液を徐々に注ぎ入れた。この時、ルツボ
を回転軸の傾きを変えながら回転して、いわゆるごます
り運動させて、内表面全体に溶液を塗布した。溶液は始
めは透明であるが乾燥する前にわずかに濁っていた。空
気中の炭酸ガスと反応して炭酸バリウムに一部変化する
ためと思われる。このまま温風を送り込みながら石英ガ
ラスルツボのごますり運動を続けて完全に乾燥させ、バ
リウム元素を内表面にもつ石英ガラスルツボを作成し
た。塗布量は１ｃｍ2当り５０μｇであった。このルツ
ボに多結晶シリコン塊を入れた後加熱してシリコンを溶
融し、融液からシリコン単結晶を引上げた。１０回のマ
ルチ引上げ法を実施することができた。後にルツボの内
表面を観察したところ、０．８ｍｍの厚さの厚い結晶層
が内面全体を覆っており、ルツボ全体の厚みも殆ど減少
していなかった。Example 2 A solution having the composition shown in Table 1 was gradually poured into a high-purity quartz glass crucible having a diameter of 18 inches. At this time, the crucible was rotated while changing the inclination of the rotation axis, and was subjected to a so-called "rubbing motion" to apply the solution to the entire inner surface. The solution was initially clear but slightly cloudy before drying. This is probably because it reacts with carbon dioxide in the air and partly changes to barium carbonate. While continuing to blow warm air, the quartz glass crucible was continuously rubbed and completely dried to form a quartz glass crucible having an elemental surface of barium. The coating amount was 50 μg per cm 2 . A polycrystalline silicon block was put into this crucible and then heated to melt the silicon, and a silicon single crystal was pulled from the melt. It was possible to carry out the multi-pulling method 10 times. Later, when the inner surface of the crucible was observed, a thick crystal layer having a thickness of 0.8 mm covered the entire inner surface, and the thickness of the entire crucible was hardly reduced.
【００１６】[0016]
【表１】 [Table 1]
【００１７】[0017]
【発明の効果】本発明の石英ガラスルツボは、その使用
時にルツボの内側に結晶層が形成され、耐熱性が向上
し、例えば減圧下でシリコン単結晶の引上げを行って
も、内表面が荒れず、平滑さが維持される。前記本発明
の石英ガラスルツボはその内表面に２ａ族元素含有塗布
膜または３ｂ族元素含有固溶層を形成するという簡便な
方法で製造でき、工業的に有利な製造方法である。EFFECTS OF THE INVENTION The quartz glass crucible of the present invention has a crystal layer formed inside the crucible at the time of use and has improved heat resistance. For example, even if a silicon single crystal is pulled up under reduced pressure, the inner surface becomes rough. Instead, the smoothness is maintained. The quartz glass crucible of the present invention can be manufactured by a simple method of forming a 2a group element-containing coating film or a 3b group element-containing solid solution layer on the inner surface thereof, which is an industrially advantageous manufacturing method.
Claims (9)
に結晶化促進剤含有塗布膜または固溶層が形成されてい
ることを特徴とする石英ガラスルツボ。1. A quartz glass crucible characterized in that a coating film containing a crystallization accelerator or a solid solution layer is formed within a thickness of 1 mm on the inner surface of the quartz glass crucible.
素であることを特徴とする請求項１記載の石英ガラスル
ツボ。2. The quartz glass crucible according to claim 1, wherein the crystallization accelerator is a group 2a element or a group 3b element.
ム、カルシウムまたはバリウムであることを特徴とする
請求項２記載の石英ガラスルツボ。3. The quartz glass crucible according to claim 2, wherein the Group 2a element is magnesium, strontium, calcium or barium.
を特徴とする請求項２記載の石英ガラスルツボ。4. The quartz glass crucible according to claim 2, wherein the Group 3b element is an aluminum element.
ｍ2当り２ａ族元素を１〜１００μｇの範囲で含有する
ことを特徴とする請求項１記載の石英ガラスルツボ。5. The coating film formed on the inner surface of the crucible is 1c.
The quartz glass crucible according to claim 1, wherein the group 2a element is contained in the range of 1 to 100 µg per m 2 .
ｍｍの固溶層中の３ｂ族元素濃度が０．１〜２重量％の
範囲であることを特徴とする請求項２記載の石英ガラス
ルツボ。6. A thickness of 0.5 to 1 formed on the inner surface of the crucible.
The quartz glass crucible according to claim 2, wherein the concentration of the Group 3b element in the solid solution layer having a thickness of mm is in the range of 0.1 to 2% by weight.
塗布し、乾燥することを特徴とする石英ガラスルツボの
製造方法。7. A method for producing a quartz glass crucible, which comprises applying a solution of a Group 2a element compound to the inner surface of the crucible and drying the solution.
物をアルコール２０重量％以上を含む水に溶解した溶液
であることを特徴とする請求項７記載の石英ガラスルツ
ボの製造方法。8. The method for producing a quartz glass crucible according to claim 7, wherein the solution of the 2a group element compound is a solution in which the 2a group element compound is dissolved in water containing 20% by weight or more of an alcohol.
リカ粉充填層を形成し、それをアーク加熱で溶融すると
共に、３ｂ族元素ドープトシリカ粉を供給し溶融・散布
させ厚さ０．５〜１ｍｍの層に３ｂ族元素を固溶させる
ことを特徴とする石英ガラスルツボの製造方法。9. A high-purity silica powder is fed into a rotating mold to form a silica powder filling layer, which is melted by arc heating, and at the same time, a 3b group element-doped silica powder is supplied and melted / sprayed to a thickness of 0. A method for producing a quartz glass crucible, characterized in that a Group 3b element is solid-dissolved in a layer of 5 to 1 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06159602A JP3100836B2 (en) | 1994-06-20 | 1994-06-20 | Quartz glass crucible and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06159602A JP3100836B2 (en) | 1994-06-20 | 1994-06-20 | Quartz glass crucible and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH082932A true JPH082932A (en) | 1996-01-09 |
| JP3100836B2 JP3100836B2 (en) | 2000-10-23 |
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| JP06159602A Expired - Lifetime JP3100836B2 (en) | 1994-06-20 | 1994-06-20 | Quartz glass crucible and its manufacturing method |
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