JPH09249494A - Crucible for melting silicon - Google Patents
Crucible for melting siliconInfo
- Publication number
- JPH09249494A JPH09249494A JP252197A JP252197A JPH09249494A JP H09249494 A JPH09249494 A JP H09249494A JP 252197 A JP252197 A JP 252197A JP 252197 A JP252197 A JP 252197A JP H09249494 A JPH09249494 A JP H09249494A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- carbon
- silicon
- melting
- quartz
- 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
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、シリコン単結晶
の引上げに用いられるシリコン溶融用坩堝に関し、さら
に詳しくは引上げ中における坩堝上部の変形を防止した
シリコン溶融用坩堝に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silicon melting crucible used for pulling a silicon single crystal, and more particularly to a silicon melting crucible which prevents deformation of the upper part of the crucible during pulling.
【０００２】[0002]
【従来の技術】シリコン単結晶を製造するには、高純度
シリコン原料を減圧下のアルゴン雰囲気で溶融し、種結
晶を用いて上方に引き上げながら凝固させる方法が多用
されている。2. Description of the Related Art In order to manufacture a silicon single crystal, a method of melting a high-purity silicon raw material in an argon atmosphere under reduced pressure and solidifying it while pulling it upward with a seed crystal is widely used.
【０００３】図５は、引き上げながら原料溶融液を凝固
させるシリコン単結晶製造装置を示す図である。図中の
符号６はシリコン単結晶の引上げ雰囲気を減圧するチャ
ンバーであり、チャンバーの内部には溶融坩堝１が配置
され、坩堝の外側にはこれを囲んで誘導加熱コイルなど
で構成された加熱用ヒーター４が、更にその外側に断熱
材で円筒状に構成された保温筒５が配設されている。溶
融坩堝１内には加熱用ヒーター４により溶融された結晶
形成用材料、つまりシリコン原料の溶融液７が収容され
ている。その溶融液の表面に引上げ棒またはワイヤ10の
先に取り付けた種結晶８の下端を接触させ、この種結晶
を上方に引き上げることによって、その下端に溶融液が
凝固したシリコン単結晶９を成長させていく。FIG. 5 is a view showing a silicon single crystal production apparatus for solidifying a raw material melt while pulling it up. Reference numeral 6 in the figure is a chamber for depressurizing the pulling atmosphere of the silicon single crystal. The melting crucible 1 is arranged inside the chamber, and the induction crucible for heating is formed outside the crucible by surrounding it. The heater 4 is further provided on the outside thereof with a heat insulating cylinder 5 formed of a heat insulating material in a cylindrical shape. In the melting crucible 1, the crystal forming material melted by the heater 4 for heating, that is, the melt 7 of the silicon raw material is contained. The lower end of a seed crystal 8 attached to the tip of a pulling rod or wire 10 is brought into contact with the surface of the melt, and the seed crystal is pulled upward to grow a silicon single crystal 9 in which the melt solidifies at the lower end. To go.
【０００４】このとき溶融坩堝１は回転軸13で支持され
て回転し、一方、シリコン単結晶９は引上げ棒の上部に
設けた回転機構（図示せず）によって駆動され、お互い
に反対方向に回転させられる。また、ガス供給口11から
アルゴンガスを供給し、ガス排気口12から排出する。At this time, the melting crucible 1 is supported by a rotating shaft 13 to rotate, while the silicon single crystal 9 is driven by a rotating mechanism (not shown) provided on the upper part of the pulling rod to rotate in opposite directions. To be made. Further, argon gas is supplied from the gas supply port 11 and discharged from the gas exhaust port 12.
【０００５】使用される溶融坩堝１は二重構造であり、
内側が石英製の容器２（以下、これを「石英坩堝」とい
う）、外側がカーボン製の容器３（以下、これを「カー
ボン坩堝」という）から構成されており、シリコン単結
晶の引上げ直径が大きくなるにしたがい、石英坩堝２の
直径も大きくなり、加熱のために投入される熱量も増加
し、坩堝の表面温度も高くなる。The melting crucible 1 used has a double structure,
It is composed of a container 2 made of quartz on the inside (hereinafter referred to as "quartz crucible") and a container 3 made of carbon on the outside (hereinafter referred to as "carbon crucible"), and has a pulling diameter of a silicon single crystal. As the size of the quartz crucible 2 increases, the diameter of the quartz crucible 2 also increases, the amount of heat input for heating also increases, and the surface temperature of the crucible also increases.
【０００６】通常、溶融坩堝の上端部は、石英坩堝の側
壁の方がカーボン坩堝の側壁よりも上方に高くなるよう
に構成されている。このため、シリコン単結晶の引上げ
中に高温に曝されたとき、石英坩堝の上部が内側に倒れ
込む変形が生じたり、石英坩堝の自重によって座屈が発
生したりすることがあるが、このような場合にはシリコ
ンの引上げの中止を余儀なくされる。また、シリコン単
結晶の製造中は、その溶融液の表面からSiO ガスが発生
していることから、石英坩堝とカーボン坩堝との間にSi
O ガスが侵入し、カーボン（Ｃ）が珪化反応（SiO ＋Ｃ
→SiC ）してカーボン坩堝の寿命が低下する。Usually, the upper end of the melting crucible is constructed such that the side wall of the quartz crucible is higher than the side wall of the carbon crucible. Therefore, when the silicon single crystal is exposed to a high temperature during pulling, the upper part of the quartz crucible may be deformed to fall inward or buckling may occur due to the weight of the quartz crucible. In some cases, the pulling of silicon will be stopped. In addition, since SiO gas is generated from the surface of the molten liquid during the production of the silicon single crystal, the Si gas is generated between the quartz crucible and the carbon crucible.
O gas invades and carbon (C) reacts with silicidation (SiO + C
→ SiC) and the life of the carbon crucible decreases.
【０００７】図６および図７は、シリコン単結晶の引上
げ中に発生する石英坩堝の変形やカーボン坩堝の珪化部
について説明する図である。図６は、シリコン溶融坩堝
の石英坩堝の上部が内部に倒れ込んだ状態（左側図面）
とカーボン坩堝に珪化部が発生した状態（右側図面）を
示す溶融坩堝の縦断面図である。また、図７は、シリコ
ン溶融坩堝の石英坩堝の自重によって発生した座屈の状
態（左側図面）と湾曲した状態（右側図面）を示す溶融
坩堝の縦断面図である。FIGS. 6 and 7 are views for explaining the deformation of the quartz crucible and the silicified portion of the carbon crucible which occur during the pulling of the silicon single crystal. FIG. 6 shows a state in which the upper part of the quartz crucible of the silicon melting crucible falls inside (left side drawing).
FIG. 4 is a vertical cross-sectional view of a molten crucible showing a state (a right side drawing) in which a silicified portion is generated in the carbon crucible. FIG. 7 is a longitudinal sectional view of the melting crucible showing a buckling state (left side drawing) and a curved state (right side drawing) caused by the weight of the quartz crucible of the silicon melting crucible.
【０００８】図６において、左側が石英坩堝の上部が内
部に倒れ込んだ倒れ込み部18を示し、右側がカーボン坩
堝の珪化部19を示ている。左側図面に示したように、石
英坩堝の倒れ込んだ内面18' が形成されると、その部分
にSiO ガスが付着し易くなり、SiO ガスが酸化され粒状
のSiO2となってシリコン溶融液に落下する。落下したSi
O2はシリコン単結晶の成長界面まで移動し、やがて単結
晶内に浸入し有転位の要因となるので、無転位結晶の引
上げが困難となる。また、同図の右側に示したように、
カーボン坩堝の上部の石英坩堝との界面19' にが浸入す
ると、カーボン坩堝が珪化され、損傷が著しく再利用が
できなくなる。In FIG. 6, the left side shows the collapsed portion 18 in which the upper part of the quartz crucible falls down, and the right side shows the silicified portion 19 of the carbon crucible. As shown in the drawing on the left, when the inner surface 18 'of the quartz crucible that has collapsed is formed, SiO gas easily adheres to the inner surface 18', and the SiO gas is oxidized and becomes granular SiO 2 that falls into the silicon melt. To do. Si dropped
O 2 moves to the growth interface of the silicon single crystal and eventually penetrates into the single crystal to cause dislocations, which makes it difficult to pull up the dislocation-free crystal. Also, as shown on the right side of the figure,
If the interface 19 'with the quartz crucible at the upper part of the carbon crucible penetrates, the carbon crucible is silicified, and the damage becomes remarkable, and the carbon crucible cannot be reused.
【０００９】図７では、左側に石英坩堝の自重によって
発生した座屈部20を示し、右側に高温下での軟化にとも
なって発生した湾曲部21を示ている。このような石英坩
堝の変形が生じた場合であっても、図６に示す倒れ込み
変形と同様に、SiO 付着および粒状SiO2落下にともなっ
て無転位結晶の引上げが困難となる。In FIG. 7, a buckling portion 20 caused by the weight of the quartz crucible is shown on the left side, and a bending portion 21 caused by softening at high temperature is shown on the right side. Even when such a deformation of the quartz crucible occurs, it is difficult to pull up the dislocation-free crystal due to the SiO 2 adhesion and the granular SiO 2 drop, as in the collapse deformation shown in FIG.
【００１０】このような問題を解決するため特開昭63-3
15263 号報には、石英坩堝の円筒状側壁の上端に、外側
に広がるフランジが一体に設けられた溶融坩堝が提案さ
れている。しかし、外側に広がるフランジを一体に設け
る加工は煩雑であり、コスト高になる。また、特開平3-
290393号公報には、溶融坩堝の円筒状側壁上端に、これ
を被う石英リングが設けられた溶融坩堝が提案されてい
る。しかし、高温に曝されたとき、石英リングは石英坩
堝と融合し、取り外しできなくなり、この石英リングの
再利用ができないという問題がある。In order to solve such a problem, Japanese Patent Laid-Open No. 63-3
No. 15263 proposes a melting crucible in which a flange extending outward is integrally provided on the upper end of a cylindrical side wall of a quartz crucible. However, the process of integrally forming the flange that spreads to the outside is complicated and the cost is high. In addition, JP-A-3-
JP-A-290393 proposes a melting crucible in which a quartz ring covering the cylindrical side wall of the melting crucible is provided on the upper end of the side wall. However, when exposed to high temperatures, the quartz ring fuses with the quartz crucible and cannot be removed, and this quartz ring cannot be reused.
【００１１】また、特開平６−32692号公報には、シリ
コン単結晶の製造において高速引上げを可能とし生産性
の向上を図ることが重要なことから、結晶原料である多
結晶シリコンの充填量を増加させるため、石英坩堝の側
壁上端部に上方が拡大したテーパを設けたシリコン溶融
用坩堝が提案され、特に側壁上端部のテーパ角度は45°
が適しているとされている。しかし、提案された石英坩
堝は、結晶原料の充填量を向上させることだけを意図し
ており、何ら石英坩堝の倒れ込み、座屈等の変形やカー
ボン坩堝の珪化部の発生を防止することを考慮するもの
ではない。例えば、ここで採用するテーパ角度45°の条
件でシリコン単結晶の引上げを実施すると、前記図７の
右側に示すように、石英坩堝の上部が坩堝の内側に向か
って激しく変形し、湾曲部21を形成する。その結果、単
結晶の引上げ領域でのアルゴンガスの流れに乱れが生
じ、溶融液の表面から発生したSiO ガスを効率的に排出
できず、変形した部分に付着した粒状のSiO2が溶融液に
落下し製造される単結晶が有転位化するという問題があ
る。Further, in Japanese Unexamined Patent Publication No. 6-32692, it is important to enable high-speed pulling and improve productivity in the production of a silicon single crystal. In order to increase the number, a silicon melting crucible with a tapered upper part on the upper end of the side wall of the quartz crucible has been proposed. In particular, the taper angle of the upper end of the side wall is 45 °.
Is said to be suitable. However, the proposed quartz crucible is intended only to improve the filling amount of the crystal raw material, and considers how to prevent the quartz crucible from collapsing, deforming such as buckling, and forming a silicified portion of the carbon crucible. Not something to do. For example, when the silicon single crystal is pulled up under the condition of the taper angle of 45 ° adopted here, the upper portion of the quartz crucible is severely deformed toward the inside of the crucible as shown on the right side of FIG. To form. As a result, the flow of the argon gas in the pulling region of the single crystal is disturbed, the SiO gas generated from the surface of the melt cannot be discharged efficiently, and the granular SiO 2 attached to the deformed part becomes the melt. There is a problem that the single crystal that is dropped and produced has dislocation.
【００１２】[0012]
【発明が解決しようとする課題】本発明の目的は、シリ
コン単結晶の引上げでの高温雰囲気中においても石英坩
堝上部の倒れ込み、座屈等の変形がなく、またカーボン
坩堝の寿命の延長を可能としたシリコン溶融用坩堝を提
供することにある。SUMMARY OF THE INVENTION The object of the present invention is to prevent the upper portion of a quartz crucible from being collapsed or buckled even in a high temperature atmosphere during pulling of a silicon single crystal, and to extend the life of the carbon crucible. To provide a crucible for melting silicon.
【００１３】[0013]
【課題を解決するための手段】本発明の要旨は、下記
(1)から(4)のシリコン溶融用坩堝にある。The gist of the present invention is as follows.
It is located in the silicon melting crucible of (1) to (4).
【００１４】(1) 石英坩堝をカーボン坩堝の内部に挿
入した二重構造のシリコン溶融用坩堝であって、前記石
英坩堝の上部が逆円錐帯状の傾斜部を有するシリコン溶
融用坩堝である（図１参照）。(1) A silicon melting crucible having a double structure in which a quartz crucible is inserted into a carbon crucible, and the upper part of the quartz crucible is a silicon melting crucible having an inclined portion having an inverted conical band shape (Fig. 1).
【００１５】ここで、逆円錐帯状の傾斜部の角度αを５
〜40°とするのが望ましい。Here, the angle α of the inclined portion of the inverted cone band is 5
It is desirable to set it to -40 °.
【００１６】(2) 石英坩堝をカーボン坩堝の内部に挿
入したシリコン溶融用坩堝であって、前記石英坩堝およ
びカーボン坩堝の上部に、断面鈎状のカーボン製リング
が石英坩堝に挿入されているシリコン溶融用坩堝である
（図２参照）。(2) A silicon melting crucible in which a quartz crucible is inserted into a carbon crucible, wherein a carbon ring having a hook-shaped cross section is inserted into the quartz crucible above the quartz crucible and the carbon crucible. It is a melting crucible (see FIG. 2).
【００１７】(3) 石英坩堝をカーボン坩堝の内部に挿
入させたシリコン溶融用坩堝であって、前記石英坩堝お
よびカーボン坩堝の上部に、断面が下方に開いたコの字
形のカーボン製リングが両者に被さって挿入されている
シリコン溶融用坩堝である（図３参照）。(3) A silicon melting crucible in which a quartz crucible is inserted into a carbon crucible, wherein a carbon ring having a U-shaped cross-section with a downward opening is provided on both of the quartz crucible and the carbon crucible. It is a crucible for melting silicon which is inserted to cover (see FIG. 3).
【００１８】(4) 石英坩堝をカーボン坩堝の内部に挿
入したシリコン溶融用坩堝であって、前記石英坩堝およ
びカーボン坩堝の上部に、断面が下方に開いたコの字形
のカーボン製クリップが両者に跨がって断続的に挿入さ
れているシリコン溶融用坩堝である（図４参照）。(4) A silicon melting crucible in which a quartz crucible is inserted into a carbon crucible, wherein a carbon clip having a U-shaped cross-section with a downward opening is formed on both of the quartz crucible and the carbon crucible. It is a crucible for melting silicon, which is inserted intermittently across the ground (see FIG. 4).
【００１９】[0019]
【発明の実施の態様】図１は、本発明のシリコン溶融用
坩堝の縦断面を示す図である。本発明の溶融坩堝１は、
同図に示すように、外側のカーボン坩堝３の内部に内側
の石英坩堝２が挿入された二重構造である。そして石英
坩堝２の上部を、外側に開いた傾斜部14として側壁と一
体に設けることによって石英坩堝の剛性が増し、坩堝内
部への倒れ込みをなくすことができ、しかも石英坩堝の
自重によって発生する座屈や湾曲を抑制することができ
る。このとき、傾斜部の角度αは石英坩堝の座屈部およ
び湾曲部の発生状況に影響を与えることから、所定の範
囲で選択すればよく、５〜40°とするのが望ましい。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 is a view showing a vertical section of a crucible for melting silicon according to the present invention. The melting crucible 1 of the present invention is
As shown in the figure, it has a double structure in which an inner quartz crucible 2 is inserted inside an outer carbon crucible 3. By providing the upper portion of the quartz crucible 2 integrally with the side wall as the inclined portion 14 opened to the outside, the rigidity of the quartz crucible can be increased, and it is possible to prevent the quartz crucible from falling into the inside of the crucible, and moreover, the seat generated by the weight of the quartz crucible. Bending and bending can be suppressed. At this time, the angle α of the inclined portion affects the occurrence of the buckling portion and the curved portion of the quartz crucible, so it may be selected within a predetermined range, and is preferably 5 to 40 °.
【００２０】石英坩堝の逆円錐帯状の傾斜部角度αが５
°未満であると、石英坩堝の剛性を増して倒れ込みを防
止することが困難になる。さらに、前記図７の左側に示
すように、石英坩堝の中央部において自重によって座屈
部20を発生し易くなる。一方、前述の特開平６−32692
号公報で提案された石英坩堝のように、傾斜部の角度α
が40°を超えると、石英坩堝の曲げ加工が困難になりコ
スト高を招く。しかも、自重による石英坩堝の変形は軽
減できるものの、傾斜部の角度αの増加にともなって引
上げ中の高温条件の下で軟化した石英坩堝の上部が坩堝
の内側に向かって変形することによって、湾曲部21を形
成することがある。したがって、後述する実施例１で示
すように、傾斜部の角度αを５〜40°とすることによっ
て、前記図７の変形量Ｌで示される石英坩堝の変形を最
小とし、坩堝の変形に起因する有転位化の問題を解消す
ることができる。The angle α of the inverted conical band of the quartz crucible is 5
If it is less than °, it becomes difficult to increase the rigidity of the quartz crucible and prevent the quartz crucible from falling. Further, as shown on the left side of FIG. 7, the buckling portion 20 is easily generated due to its own weight in the central portion of the quartz crucible. On the other hand, the above-mentioned JP-A-6-32692
Like the quartz crucible proposed in Japanese Patent Publication, the angle α of the inclined part is
If it exceeds 40 °, it becomes difficult to bend the quartz crucible, resulting in high cost. Moreover, although the deformation of the quartz crucible due to its own weight can be reduced, the upper part of the quartz crucible softened under the high temperature condition during the pulling due to the increase of the angle α of the inclined part is deformed toward the inside of the crucible, so that The part 21 may be formed. Therefore, as described in Example 1 described later, by setting the angle α of the inclined portion to 5 to 40 °, the deformation of the quartz crucible indicated by the deformation amount L in FIG. 7 is minimized and the deformation of the crucible is caused. It is possible to solve the problem of causing dislocation.
【００２１】図２は、本発明の別態様のシリコン溶融用
坩堝の縦断面を示す図である。本発明の溶融坩堝１は、
同図に示すように、溶融坩堝側壁の上部には、石英坩堝
２とカーボン坩堝３とが共に平行に立ち上がっており、
その上端部に断面が鈎状に開いたカーボンリング15が石
英坩堝の内部に挿入されている。カーボンリングの外径
は、カーボン坩堝の外径よりも大きくするのが望まし
い。カーボンリングを挿入することによって、石英坩堝
の剛性が増し、坩堝内部への倒れ込みをなくすことがで
きる。また、カーボンは石英に比べ加工性がよいので、
図１に示すような傾斜をもったカーボンリングでもよ
い。FIG. 2 is a view showing a vertical cross section of a crucible for melting silicon according to another embodiment of the present invention. The melting crucible 1 of the present invention is
As shown in the figure, the quartz crucible 2 and the carbon crucible 3 both stand in parallel on the upper portion of the side wall of the melting crucible,
A carbon ring 15 having a hook-shaped cross section opened at its upper end is inserted inside the quartz crucible. The outer diameter of the carbon ring is preferably larger than the outer diameter of the carbon crucible. By inserting the carbon ring, the rigidity of the quartz crucible is increased and it is possible to prevent the quartz crucible from falling into the inside of the crucible. Also, since carbon has better workability than quartz,
A carbon ring having an inclination as shown in FIG. 1 may be used.
【００２２】図３は、本発明の別態様のシリコン溶融用
坩堝の縦断面を示す図である。本発明の溶融坩堝１は、
同図に示すように、溶融坩堝の側壁上部に断面コの字形
のカーボンリング16を、石英坩堝２とカーボン坩堝３と
の側壁上部を挟み被せて挿入し、構成する。コの字形の
カーボンリングを挿入することによって、石英坩堝の剛
性が増し、坩堝内部への倒れ込みをなくすことができ、
またカーボン坩堝の珪化反応を防止することができる。FIG. 3 is a view showing a vertical cross section of a crucible for melting silicon according to another embodiment of the present invention. The melting crucible 1 of the present invention is
As shown in the figure, a carbon ring 16 having a U-shaped cross section is inserted into the upper portion of the side wall of the melting crucible so as to sandwich the upper side walls of the quartz crucible 2 and the carbon crucible 3 therebetween. By inserting the U-shaped carbon ring, the rigidity of the quartz crucible is increased and it is possible to prevent the quartz crucible from falling into the inside of the crucible.
Further, it is possible to prevent the silicidation reaction of the carbon crucible.
【００２３】図４は、本発明の別態様のシリコン溶融用
坩堝の縦断面を示す図である。本発明の溶融坩堝１は、
同図に示すように、溶融坩堝の側壁上部に断面コの字形
のカーボンクリップ17を、石英坩堝２とカーボン坩堝３
との側壁上部を断続的に挟み、構成する。カーボンクリ
ップを断続的に挿入することによって、石英坩堝の剛性
が増し、坩堝内部への倒れ込みをなくすことができる。FIG. 4 is a diagram showing a vertical cross section of a crucible for melting silicon according to another embodiment of the present invention. The melting crucible 1 of the present invention is
As shown in the figure, a carbon clip 17 having a U-shaped cross section is provided on the upper side wall of the melting crucible, a quartz crucible 2 and a carbon crucible 3 are provided.
The upper part of the side wall of and is intermittently sandwiched and configured. By intermittently inserting the carbon clip, the rigidity of the quartz crucible is increased, and it is possible to prevent the quartz crucible from falling into the inside of the crucible.
【００２４】カーボンクリップの長さは、使用する坩堝
寸法によって異なるが、例えば直径22 インチ坩堝の場
合には長さを 50 mm程度とし、円周に６個程度設けるの
が望ましい。The length of the carbon clip varies depending on the size of the crucible to be used. For example, in the case of a 22-inch diameter crucible, the length is preferably about 50 mm, and it is desirable to provide about 6 on the circumference.
【００２５】[0025]
（実施例１）図１に示す本発明の溶融用坩堝を配置した
図５に示すシリコン単結晶製造装置を用い、直径８イン
チの単結晶を製造した。内径560 mm、高さ360 mmの石英
坩堝を使用し、100 kgの多結晶シリコンを溶融し、 100
0 mm長さの単結晶を製造した。このとき、逆円錐帯状の
傾斜部の角度αを２〜60°の範囲で変動させ、各条件で
それぞれ10本の単結晶の製造を行い、石英坩堝の変形量
Ｌ（図７参照）および無転位化率（％）を測定した。そ
の測定結果を表１に示す。ただし、無転位化率（％）は
単結晶の直胴部の引上げ量に対する無転位単結晶量の比
率を示す。Example 1 A single crystal having a diameter of 8 inches was manufactured using the silicon single crystal manufacturing apparatus shown in FIG. 5 in which the melting crucible of the present invention shown in FIG. 1 is arranged. Using a quartz crucible with an inner diameter of 560 mm and a height of 360 mm, melt 100 kg of polycrystalline silicon,
A 0 mm long single crystal was produced. At this time, the angle α of the inverted conical strip-shaped inclined portion was varied within the range of 2 to 60 °, and 10 single crystals were produced under each condition, and the deformation amount L of the quartz crucible (see FIG. 7) and The dislocation rate (%) was measured. Table 1 shows the measurement results. However, the dislocation-free rate (%) indicates the ratio of the dislocation-free single crystal amount to the pulling amount of the straight body portion of the single crystal.
【００２６】[0026]
【表１】 [Table 1]
【００２７】表１の結果から明らかなように、傾斜部の
角度αを５〜40°の範囲で選択するのが望ましい。これ
にによって、石英坩堝の変形を低減させて、引上げられ
る単結晶の有転位化を防止することができる。As is clear from the results shown in Table 1, it is desirable to select the angle α of the inclined portion within the range of 5 to 40 °. This can reduce the deformation of the quartz crucible and prevent dislocation of the pulled single crystal.
【００２８】（実施例２）図２に示す本発明の溶融用坩
堝を配置した図５に示すシリコン単結晶製造装置を用
い、直径８インチの単結晶を製造した。実施例１と同様
に、内径560 mm、高さ360 mmの石英坩堝を使用し、100
kgの多結晶シリコンを溶融し、 1000 mm長さの単結晶を
製造した。また、比較例として図５に示すような従来の
溶融坩堝を用い、同様のシリコン単結晶を製造した。Example 2 A single crystal having a diameter of 8 inches was manufactured using the silicon single crystal manufacturing apparatus shown in FIG. 5 in which the melting crucible of the present invention shown in FIG. 2 was arranged. As in Example 1, a quartz crucible having an inner diameter of 560 mm and a height of 360 mm was used.
1,000 kg of single crystal was manufactured by melting kg of polycrystalline silicon. As a comparative example, a conventional silicon crucible as shown in FIG. 5 was used to manufacture the same silicon single crystal.
【００２９】図２に示す石英坩堝およびカーボン坩堝の
上部に、断面鈎状のカーボン製リングが挿入されている
溶融用坩堝を用いると、25回の引上げのうち石英坩堝の
変形、座屈が認められたものはなかった。 これに対
し、従来の溶融用坩堝を用いた比較例では、25回の引上
げのうち18回に石英坩堝の変形、座屈が認められ、18回
のうち引上げを中止したものは３回に及んだ。したがっ
て、鈎状リングを挿入することによって、石英坩堝側壁
の内部への倒れ込みがなくなることが分かる。When a melting crucible in which a carbon ring having a hook-shaped cross section is inserted in the upper part of the quartz crucible and the carbon crucible shown in FIG. 2, deformation and buckling of the quartz crucible are recognized after pulling 25 times. Nothing was given. On the other hand, in the comparative example using the conventional melting crucible, deformation and buckling of the quartz crucible were observed in 18 of the 25 pulls, and pulling was stopped in 3 of the 18 pulls. I see. Therefore, it can be seen that by inserting the hook-shaped ring, the collapse of the side wall of the quartz crucible is prevented.
【００３０】（実施例３）図３または図４に示す本発明
の溶融用坩堝を配置した図５に示すシリコン単結晶製造
装置を用い、直径８インチの単結晶を製造した。内径56
0 mm、高さ360 mmの石英坩堝を使用し、100 kgの多結晶
シリコンを溶融し、 1000 mm長さの単結晶を製造した。Example 3 A single crystal having a diameter of 8 inches was manufactured using the silicon single crystal manufacturing apparatus shown in FIG. 5 in which the melting crucible of the present invention shown in FIG. 3 or 4 was arranged. Inner diameter 56
A quartz crucible having a height of 0 mm and a height of 360 mm was used to melt 100 kg of polycrystalline silicon to produce a single crystal having a length of 1000 mm.
【００３１】図３に示すように石英坩堝およびカーボン
坩堝の上部に、断面が下方に開いたコの字形のカーボン
製リングが挿入されている溶融坩堝を用いると、25回の
引上げのうち石英坩堝の変形、座屈が認められたものは
なかった。また、図４に示す石英坩堝およびカーボン坩
堝の上部に、断面が下方に開いた長さ 60 mmのコの字形
のカーボン製クリップ６個を円周に挿入した溶融坩堝を
用いると、25回の引上げのうち石英坩堝の変形、座屈が
認められたものはなかった。As shown in FIG. 3, when a fused crucible in which a carbon ring having a U-shaped cross section is inserted in the upper part of the quartz crucible and the carbon crucible is used, the quartz crucible is pulled out 25 times. No deformation or buckling was observed. In addition, when the fused crucible in which six U-shaped carbon clips with a length of 60 mm and a cross section opened downward are inserted into the circumference on the upper part of the quartz crucible and the carbon crucible shown in FIG. No deformation or buckling of the quartz crucible was observed in the pulling.
【００３２】石英坩堝およびカーボン坩堝の上部に、断
面が下方に開いたコの字形のカーボン製リングを挿入す
ることによって、石英坩堝側壁の内部への倒れ込みがな
くなり、さらに石英坩堝とカーボン坩堝との間へのSiO
ガスの侵入がなく、カーボン坩堝の珪化（ＣがSiC とな
る）を防止してカーボン坩堝の寿命を延長させることが
できた。By inserting a carbon ring having a U-shaped cross-section that opens downward in the upper part of the quartz crucible and the carbon crucible, the quartz crucible side wall is prevented from falling into the inside of the quartz crucible and the carbon crucible. SiO between
It was possible to extend the life of the carbon crucible by preventing gas from entering and preventing silicidation of the carbon crucible (C becomes SiC).
【００３３】[0033]
【発明の効果】本発明のシリコン溶融坩堝を使用したシ
リコンの単結晶製造装置によれば、石英坩堝側壁の倒れ
込み、座屈、湾曲等の変形や石英坩堝とカーボン坩堝と
の間にSiO ガスが侵入することがなくなり、溶融坩堝当
たりのシリコン単結晶の製造本数を増加させることがで
きる。According to the apparatus for producing a silicon single crystal using the silicon melting crucible of the present invention, the side wall of the quartz crucible collapses, is deformed such as buckling, curved, or SiO gas is generated between the quartz crucible and the carbon crucible. It is possible to increase the number of silicon single crystals produced per molten crucible, since no invasion occurs.
【図１】本発明のシリコン溶融用坩堝の縦断面を示す図
である。FIG. 1 is a view showing a vertical cross section of a silicon melting crucible of the present invention.
【図２】本発明の別態様のシリコン溶融用坩堝の縦断面
を示す図である。FIG. 2 is a view showing a longitudinal section of a silicon melting crucible according to another embodiment of the present invention.
【図３】本発明の別態様のシリコン溶融用坩堝の縦断面
を示す図である。FIG. 3 is a view showing a vertical cross section of a crucible for melting silicon according to another embodiment of the present invention.
【図４】本発明の別態様のシリコン溶融用坩堝の縦断面
を示す図である。FIG. 4 is a view showing a vertical cross section of a crucible for melting silicon according to another embodiment of the present invention.
【図５】引き上げながら凝固させるシリコン単結晶製造
装置を示す縦断面図である。FIG. 5 is a vertical cross-sectional view showing a silicon single crystal production apparatus for solidifying while pulling.
【図６】従来のシリコン溶融用坩堝の変形状態であっ
て、シリコン溶融坩堝の石英坩堝の上部が内部に倒れ込
んだ状態（左側図面）とカーボン坩堝に珪化部が発生し
た状態（右側図面）を示す溶融坩堝の縦断面図である。FIG. 6 shows a deformed state of a conventional silicon melting crucible, showing a state in which the upper part of the quartz crucible of the silicon melting crucible falls inside (left side drawing) and a state in which a silicified portion has occurred in the carbon crucible (right side drawing). It is a longitudinal cross-sectional view of the melting crucible shown.
【図７】従来のシリコン溶融用坩堝の変形状態であっ
て、シリコン溶融坩堝の石英坩堝の自重によって発生し
た座屈の状態（左側図面）と湾曲した状態（右側図面）
を示す溶融坩堝の縦断面図である。FIG. 7 shows a deformed state of a conventional crucible for melting silicon, which is a buckling state (left side drawing) and a curved state (right side drawing) caused by the self-weight of the quartz crucible of the silicon melting crucible.
FIG. 4 is a vertical cross-sectional view of the melting crucible.
１．溶融坩堝 ２．石英坩堝 ３．カーボン坩堝 ４．加熱用ヒータ ５．保温筒 ６．減圧チャンバー ７．シリコン溶融液 ８．種結晶 ９．シリコン単結晶 10．引上げ棒 11．ガス供給口 12．ガス排出口 13．回転軸 14．傾斜部 15．鈎状カーボンリング 16．コの字形カーボンリング 17．コの字形カーボンクリップ 18．石英坩堝の倒れ込み部 18'.倒れ込んだ内面 19．カーボン坩堝の珪化部 19'.石英坩堝とカーボン坩堝との界面 20.石英坩堝の座屈部 21.石英坩堝の湾曲部 1. 1. melting crucible Quartz crucible 3. Carbon crucible 4. Heater for heating 5. Insulation cylinder 6. Decompression chamber 7. Silicon melt 8. Seed crystal 9. Silicon single crystal 10. Pull bar 11. Gas supply port 12. Gas outlet 13． Rotating shaft 14． Inclined part 15. Hook-shaped carbon ring 16. U-shaped carbon ring 17. U-shaped carbon clip 18. Falling part of quartz crucible 18 '. Falling inside 19. Silicified part of carbon crucible 19 '. Interface between quartz crucible and carbon crucible 20. Buckling part of quartz crucible 21. Curved part of quartz crucible
Claims (5)
二重構造のシリコン溶融用坩堝であって、前記石英坩堝
の上部に逆円錐帯状の傾斜部を有するシリコン溶融用坩
堝。1. A crucible for melting silicon having a double structure in which a quartz crucible is inserted inside a carbon crucible, wherein the crucible for melting silicon has an inverted conical band-shaped inclined portion on an upper portion of the crucible.
あることを特徴とする請求項１記載のシリコン溶融用坩
堝。2. The crucible for melting silicon according to claim 1, wherein the angle α of the inclined portion in the shape of an inverted conical strip is 5 to 40 °.
シリコン溶融用坩堝であって、前記石英坩堝およびカー
ボン坩堝の上部に、断面鈎状のカーボン製リングが石英
坩堝に挿入されているシリコン溶融用坩堝。3. A crucible for melting silicon in which a quartz crucible is inserted inside a carbon crucible, wherein a silicon ring having a hook-shaped cross section is inserted into the quartz crucible above the quartz crucible and the carbon crucible. A crucible.
シリコン溶融用坩堝であって、前記石英坩堝およびカー
ボン坩堝の上部に、断面が下方に開いたコの字形のカー
ボン製リングが両者に被さって挿入されているシリコン
溶融用坩堝。4. A silicon melting crucible in which a quartz crucible is inserted into a carbon crucible, wherein a carbon ring having a U-shaped cross-section with a downward opening is provided on both of the quartz crucible and the carbon crucible. The silicon melting crucible that has been inserted.
シリコン溶融用坩堝であって、前記石英坩堝およびカー
ボン坩堝の上部に、断面が下方に開いたコの字形のカー
ボン製クリップが両者にまたがって断続的に挿入されて
いるシリコン溶融用坩堝。5. A silicon melting crucible in which a quartz crucible is inserted into a carbon crucible, wherein a carbon clip having a U-shaped cross-section with a downward opening is provided on both of the quartz crucible and the carbon crucible. Crucible for melting silicon, which is inserted intermittently.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9002521A JP3011114B2 (en) | 1996-01-12 | 1997-01-10 | Silicon melting crucible |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP370696 | 1996-01-12 | ||
| JP8-3706 | 1996-01-12 | ||
| JP9002521A JP3011114B2 (en) | 1996-01-12 | 1997-01-10 | Silicon melting crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09249494A true JPH09249494A (en) | 1997-09-22 |
| JP3011114B2 JP3011114B2 (en) | 2000-02-21 |
Family
ID=26335914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9002521A Expired - Fee Related JP3011114B2 (en) | 1996-01-12 | 1997-01-10 | Silicon melting crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3011114B2 (en) |
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| JP2010163311A (en) * | 2009-01-15 | 2010-07-29 | Japan Siper Quarts Corp | Mold for producing silica crucible |
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| JP2010163311A (en) * | 2009-01-15 | 2010-07-29 | Japan Siper Quarts Corp | Mold for producing silica crucible |
| JP2010163312A (en) * | 2009-01-15 | 2010-07-29 | Japan Siper Quarts Corp | Mold for producing silica crucible |
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