JPH04305087A - Method and device for producing single crystal - Google Patents

Method and device for producing single crystal

Info

Publication number
JPH04305087A
JPH04305087A JP9341491A JP9341491A JPH04305087A JP H04305087 A JPH04305087 A JP H04305087A JP 9341491 A JP9341491 A JP 9341491A JP 9341491 A JP9341491 A JP 9341491A JP H04305087 A JPH04305087 A JP H04305087A
Authority
JP
Japan
Prior art keywords
single crystal
heater
melt
crucible
peak
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
Application number
JP9341491A
Other languages
Japanese (ja)
Other versions
JP3099403B2 (en
Inventor
Yukio Suga
菅 有希雄
Hiroshi Sakai
酒井 弘
Masamitsu Oguchi
小口 政充
Nobuto Harai
原井 宣人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KYUSHU ELECTRON METAL CO Ltd
Osaka Titanium Co Ltd
Original Assignee
KYUSHU ELECTRON METAL CO Ltd
Osaka Titanium Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by KYUSHU ELECTRON METAL CO Ltd, Osaka Titanium Co Ltd filed Critical KYUSHU ELECTRON METAL CO Ltd
Priority to JP03093414A priority Critical patent/JP3099403B2/en
Publication of JPH04305087A publication Critical patent/JPH04305087A/en
Application granted granted Critical
Publication of JP3099403B2 publication Critical patent/JP3099403B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PURPOSE:To provide a device capable of producing a single crystal low in oxygen concentration, without the lifting speed being lowered with respect to the conventional process and without the single crystal being normalized. CONSTITUTION:The peak of the produced heat distribution of a heater 8 is positioned above the surface of a melt 6, the amt. of oxygen dissolved into the melt 6 from the peripheral wall of a crucible 4 is reduced, and the oxygen concn. in a single crystal 3 pulled up from the melt 6 is diminished.

Description

【発明の詳細な説明】[Detailed description of the invention]

【0001】0001

【産業上の利用分野】本発明は、シリコン単結晶等の単
結晶製造方法及び該方法に使用する装置に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a single crystal, such as a silicon single crystal, and an apparatus used in the method.

【0002】0002

【従来の技術】単結晶製造方法としてはチョクラルスキ
ー(CZ)法が広く知られている。図4はCZ法による
従来の単結晶製造の実施状態を示す模式図であり、図中
4は石英坩堝である。石英坩堝4の外周にはカーボン坩
堝5が配設され、さらにその外周側にはカーボン坩堝5
全体を囲むようにカーボン製のヒータ7が配置されてい
る。そして石英坩堝4内に結晶用原料を投入し、これを
ヒータ7にて加熱溶融せしめた後、この溶融液6中に引
上げ軸1にて吊り下げた種結晶2を浸し、これを回転さ
せつつ上方に引き上げると、種結晶2の下端に単結晶3
が成長せしめられる。
2. Description of the Related Art The Czochralski (CZ) method is widely known as a single crystal manufacturing method. FIG. 4 is a schematic diagram showing the state of implementation of conventional single crystal production by the CZ method, and 4 in the figure is a quartz crucible. A carbon crucible 5 is disposed on the outer periphery of the quartz crucible 4, and a carbon crucible 5 is further disposed on the outer periphery of the quartz crucible 4.
A heater 7 made of carbon is arranged so as to surround the whole. Then, the raw material for crystal is put into the quartz crucible 4, and after heating and melting it with the heater 7, the seed crystal 2 suspended by the pulling shaft 1 is immersed in the molten liquid 6, and while it is being rotated. When pulled upward, the single crystal 3 is placed at the bottom end of the seed crystal 2.
is made to grow.

【0003】0003

【発明が解決しようとする課題】以上の如く構成された
単結晶成長装置においては、ヒータ7はその上端及び下
端部では熱が逃げ、上下方向の中心部では熱が逃げない
ので、ヒータ7の発熱量は破線で示したように中心部、
即ち溶融液6の液面より少し下の位置でピークに達する
。この発熱分布により矢符に示した如く石英坩堝4の側
周壁中央部から単結晶3の引上げ領域へ向かう熱対流が
生じる。そしてヒータ7の加熱により石英坩堝4が溶け
出し、酸素が溶融液6中に供給され、前記熱対流によっ
て単結晶3の引上げ領域に運ばれ、酸素が単結晶3中に
取り込まれる。従って、この装置では単結晶3に供給さ
れる酸素量が多いので、略13.0×1018atms
/cc 以下の低酸素濃度の単結晶を製造することは不
可能であった。
[Problems to be Solved by the Invention] In the single crystal growth apparatus constructed as described above, heat escapes from the heater 7 at its upper and lower ends, but does not escape from the center in the vertical direction. The calorific value is in the center as shown by the broken line,
That is, it reaches a peak at a position slightly below the liquid level of the melt 6. Due to this heat generation distribution, heat convection occurs from the center of the side peripheral wall of the quartz crucible 4 toward the pulling region of the single crystal 3, as shown by the arrow. Then, the quartz crucible 4 begins to melt due to heating by the heater 7, oxygen is supplied into the melt 6, is carried to the pulling region of the single crystal 3 by the thermal convection, and is taken into the single crystal 3. Therefore, in this device, the amount of oxygen supplied to the single crystal 3 is large, so approximately 13.0 x 1018 atms
It has been impossible to produce single crystals with low oxygen concentrations below /cc.

【0004】そこでヒータ7をその中央部が石英坩堝4
の上端位置と略一致するように高く配置し、ヒータ7の
発熱が溶融液6の液面の上側でピークに達するようにす
ると、石英坩堝4の側周壁から単結晶3の引上げ領域へ
向かう熱対流が小さくなり、石英坩堝4から溶け出す酸
素量が減少して単結晶3に供給される酸素量が少なくな
り、低酸素濃度の単結晶を製造することが可能になる。 しかし単結晶3の引上げ領域の加熱量が大きくなり、単
結晶3の引上げを継続して行うためには引上げ速度を低
下させなければならず、また単結晶の有転位化を伴うと
いう問題があった。
Therefore, the center of the heater 7 is a quartz crucible 4.
By arranging the heater 7 at a high position so as to substantially coincide with the upper end position so that the heat generated by the heater 7 reaches its peak above the surface of the melt 6, the heat flowing from the side peripheral wall of the quartz crucible 4 toward the pulling region of the single crystal 3 is Convection is reduced, the amount of oxygen dissolved from the quartz crucible 4 is reduced, and the amount of oxygen supplied to the single crystal 3 is reduced, making it possible to produce a single crystal with a low oxygen concentration. However, the amount of heating in the pulling region of the single crystal 3 increases, and in order to continue pulling the single crystal 3, the pulling speed must be reduced, and there is a problem that the single crystal becomes dislocated. Ta.

【0005】本発明は斯かる事情に鑑みなされたもので
あり、ヒータの発熱分布のピークが溶融液の液面より上
に位置するようにして坩堝の側周壁から溶融液へ溶け込
む酸素量を減少させて、単結晶の引上げ領域に供給され
る酸素量を減少させることにより、引上げ速度の従来よ
りの低下及び単結晶の有転位化を伴なわずに低酸素濃の
単結晶を得ることができる単結晶製造方法及び該方法に
使用する単結晶製造装置を提供することを目的とする。
The present invention was developed in view of the above circumstances, and aims to reduce the amount of oxygen that dissolves into the melt from the side wall of the crucible by locating the peak of the heat distribution of the heater above the liquid level of the melt. By reducing the amount of oxygen supplied to the pulling region of the single crystal, it is possible to obtain a single crystal with a low oxygen concentration without reducing the pulling speed compared to the conventional method and without causing dislocations in the single crystal. An object of the present invention is to provide a single crystal manufacturing method and a single crystal manufacturing apparatus used in the method.

【0006】[0006]

【課題を解決するための手段】第1発明の単結晶製造方
法は、周囲に配置したヒータで坩堝内にて結晶用原料を
溶融し、溶融液から単結晶を引き上げる単結晶製造方法
において、前記ヒータの発熱分布のピークが前記溶融液
の液面の上側に位置するようにして単結晶を製造するこ
とを特徴とする。第2発明の単結晶製造装置は、周囲に
ヒータを配置した坩堝内にて結晶用原料を溶融し、溶融
液から単結晶を引き上げて成長させる単結晶製造装置に
おいて、前記ヒータの発熱分布のピークが前記溶融液の
液面の上側に位置するようにしてあることを特徴とする
[Means for Solving the Problems] A method for producing a single crystal according to a first aspect of the present invention is a method for producing a single crystal in which a raw material for crystal is melted in a crucible by a heater disposed around the crucible, and a single crystal is pulled from the melt. The method is characterized in that the single crystal is manufactured such that the peak of the heat generation distribution of the heater is located above the liquid level of the melt. A single crystal manufacturing apparatus according to a second aspect of the present invention is a single crystal manufacturing apparatus in which a raw material for crystal is melted in a crucible around which a heater is arranged, and a single crystal is pulled up and grown from the melt. is located above the liquid level of the melt.

【0007】[0007]

【作用】本発明においては、ヒータの発熱分布のピーク
が溶融液の液面より上に位置するようにしているので、
ヒータの発熱分布のピークが溶融液の液面より下に位置
する場合と異なり、溶融液に生じる熱対流は坩堝の側周
壁上側から単結晶の引上げ領域に向かうのみの規模の小
さいものであり、また坩堝の側周壁から溶融液へ溶け込
む酸素量が少ない。従って単結晶の引上げ領域に供給さ
れる酸素量が減少して低酸素濃度の単結晶を製造するこ
とができる。そしてヒータをその中央部が石英坩堝の上
端位置と略一致するように高く配置する場合と比較して
単結晶の引上げ領域の加熱量が小さいので、引上げ速度
を低下させなくても引上げを実施でき、また単結晶の有
転位化を伴なわない。
[Operation] In the present invention, since the peak of the heat generation distribution of the heater is located above the liquid level of the melt,
Unlike the case where the peak of the heat generation distribution of the heater is located below the liquid level of the melt, the thermal convection that occurs in the melt is small and only flows from the upper side of the side peripheral wall of the crucible toward the pulling region of the single crystal. Also, the amount of oxygen that dissolves into the melt from the side wall of the crucible is small. Therefore, the amount of oxygen supplied to the pulling region of the single crystal is reduced, making it possible to produce a single crystal with a low oxygen concentration. In addition, since the amount of heating in the pulling region of the single crystal is small compared to when the heater is placed high so that its central part approximately coincides with the top position of the quartz crucible, pulling can be carried out without reducing the pulling speed. , and does not involve formation of dislocations in the single crystal.

【0008】[0008]

【実施例】以下、本発明をその実施例を示す図面に基づ
き具体的に説明する。図1は本発明に係る単結晶製造装
置の模式的縦断面図であり、図中4は石英坩堝である。 石英坩堝4の外周にはカーボン坩堝5が配設され、さら
にその外周側にはカーボン製のヒータ8がカーボン坩堝
5を囲むようにして配置されている。そして石英坩堝4
内に結晶用原料を投入し、これをヒータ8にて加熱溶融
せしめた後、この溶融液6中に引上げ軸1にて吊り下げ
た種結晶2を浸し、これを回転させつつ上方に引き上げ
ると、種結晶2の下端に単結晶3が成長せしめられる。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below with reference to drawings showing embodiments thereof. FIG. 1 is a schematic vertical cross-sectional view of a single crystal manufacturing apparatus according to the present invention, and 4 in the figure is a quartz crucible. A carbon crucible 5 is disposed on the outer periphery of the quartz crucible 4, and a carbon heater 8 is further disposed on the outer periphery side so as to surround the carbon crucible 5. And quartz crucible 4
After putting the raw material for crystal into the tank and heating and melting it with the heater 8, the seed crystal 2 suspended by the pulling shaft 1 is immersed in the molten liquid 6 and pulled upward while rotating. , a single crystal 3 is grown on the lower end of the seed crystal 2.

【0009】図2はヒータ8の斜視図である。ヒータ8
には、上端から切り込まれた上方スリット8b,8b,
8b,…と下端から切り込まれた下方スリット8c,8
c,8c,…とが周方向に交互に設けられている。ヒー
タ8の下端には周方向に180℃隔てて電極8a,8a
が設けられており、通電されるようになっている。通電
されたときヒータ8には電流が矢符で示したように上下
方向に向きを変えながら流れる。ヒータ8の厚みは上、
中、下の3段で異なる。中段部の厚みt2 は下段部の
厚みt3 の略1/2であり、上段部の厚みt1 は中
段部の厚みt2 より少し厚くしてある。そして上段部
の長さl1 、中段部の長さl2 、下段部の長さl3
 の比は略1:2:5である。
FIG. 2 is a perspective view of the heater 8. Heater 8
have upper slits 8b, 8b, cut from the upper end.
8b,... and lower slits 8c, 8 cut from the lower end
c, 8c, . . . are provided alternately in the circumferential direction. At the lower end of the heater 8, electrodes 8a, 8a are spaced apart by 180 degrees in the circumferential direction.
is provided and is energized. When energized, current flows through the heater 8 while changing its direction in the vertical direction as shown by the arrow. The thickness of heater 8 is above,
The middle and bottom three levels are different. The thickness t2 of the middle part is approximately 1/2 of the thickness t3 of the lower part, and the thickness t1 of the upper part is slightly thicker than the thickness t2 of the middle part. The length of the upper part is l1, the length of the middle part is l2, and the length of the lower part is l3.
The ratio is approximately 1:2:5.

【0010】抵抗は抵抗体の厚み、即ち断面積に反比例
し、発熱量は抵抗に比例する。上述した如くヒータ8は
上段部及び中段部の厚みを下段部より薄くしているので
上段部及び中段部の発熱量は下段部より大きい。従って
ヒータ8の中段部の中央より少し下に溶融液6の液面が
位置するようにしたとき、ヒータ8の発熱は破線で示し
たように中段部の略中央、即ち溶融液6の液面より少し
上の位置でピークに達する。この発熱分布により溶融液
6には矢符に示した如く、ヒータの発熱分布のピークが
溶融液の液面より下に位置する場合と異なり、石英坩堝
4の側周壁上側から単結晶3の引上げ領域へ向かうのみ
の小規模の熱対流が生じる。そしてヒータ8の加熱によ
り石英坩堝4が溶け出す量は少ない。従って前記熱対流
によって、石英坩堝4の側周壁から単結晶3の引上げ領
域に運ばれる酸素量は少なく、その結果、単結晶3の酸
素濃度を低くすることができる。
[0010] Resistance is inversely proportional to the thickness of the resistor, that is, the cross-sectional area, and the amount of heat generated is proportional to the resistance. As described above, since the thickness of the upper and middle parts of the heater 8 is thinner than that of the lower part, the amount of heat generated in the upper and middle parts is larger than that of the lower part. Therefore, when the liquid level of the melt 6 is positioned slightly below the center of the middle part of the heater 8, the heat generated by the heater 8 is located approximately at the center of the middle part, that is, the liquid level of the melt 6, as shown by the broken line. It reaches its peak at a slightly higher position. Due to this heat generation distribution, the single crystal 3 is pulled from the upper side of the side peripheral wall of the quartz crucible 4, unlike when the peak of the heat generation distribution of the heater is located below the liquid level of the melt, as shown by the arrow. Small-scale heat convection occurs only towards the area. The amount of quartz crucible 4 that melts due to heating by heater 8 is small. Therefore, the amount of oxygen carried from the side wall of the quartz crucible 4 to the pulling region of the single crystal 3 by the thermal convection is small, and as a result, the oxygen concentration of the single crystal 3 can be lowered.

【0011】図3は発熱ピークの位置を変えたときの引
上げ長と酸素濃度との関係を示したグラフである。図中
□は発熱ピークが溶融液6の液面上にある本発明例、△
は発熱ピークが溶融液6の液面と同位置にある比較例、
○は発熱ピークが溶融液6の液面下にある従来例である
。図3より本発明方法によると7.0〜13.0×10
18atms/cc 程度の低酸素濃度の単結晶を製造
することができることが判る。
FIG. 3 is a graph showing the relationship between the pulling length and the oxygen concentration when the position of the exothermic peak is changed. In the figure, □ indicates an example of the present invention in which the exothermic peak is above the liquid surface of the melt 6, and △
is a comparative example in which the exothermic peak is at the same position as the liquid level of melt 6,
○ is a conventional example in which the exothermic peak is below the surface of the melt 6. From FIG. 3, according to the method of the present invention, 7.0 to 13.0×10
It can be seen that single crystals with a low oxygen concentration of about 18 atms/cc can be produced.

【0012】本発明の実施例においてはヒータ8の厚み
を3段階にし、上段部の厚みをその下の中段部より少し
厚くして単結晶3の引上げ領域上側に対する加熱量を抑
制しているが、引上げ速度の低下及び単結晶の有転位化
等の問題が生じない場合は、ヒータ8の厚みを上部で薄
く、下部で厚くする2段構造にしてもよい。またヒータ
8の薄厚部分の設置位置、長さ及び厚みは、単結晶3の
目標酸素濃度に応じ、この目標酸素濃度が得られるよう
に発熱分布を想定して設定すれはよい。
In the embodiment of the present invention, the thickness of the heater 8 is set in three stages, and the thickness of the upper stage is slightly thicker than that of the middle stage below, thereby suppressing the amount of heating to the upper side of the pulling region of the single crystal 3. If problems such as a reduction in the pulling speed and formation of dislocations in the single crystal do not occur, the heater 8 may have a two-stage structure in which the thickness is thinner at the upper part and thicker at the lower part. Further, the installation position, length, and thickness of the thin portion of the heater 8 may be set according to the target oxygen concentration of the single crystal 3, assuming a heat generation distribution so as to obtain the target oxygen concentration.

【0013】[0013]

【発明の効果】以上の如く本発明においては、ヒータの
発熱分布のピークが溶融液の液面より上に位置するよう
にし、坩堝の側周壁から溶融液へ溶け込む酸素量を減少
させているので、単結晶の引上げ領域に供給される酸素
量が減少し、低酸素濃度の単結晶を得ることができる。 そして単結晶の引上げ領域上側の加熱量が、ヒータを坩
堝より上側にずらして配置した場合と比較して少ないの
で、引上げ速度を低下させる必要がなく、また単結晶の
有転位化を伴なわない等、本発明は優れた効果を奏する
ものである。
As described above, in the present invention, the peak of the heat generation distribution of the heater is positioned above the liquid level of the melt, thereby reducing the amount of oxygen that dissolves into the melt from the side peripheral wall of the crucible. , the amount of oxygen supplied to the pulling region of the single crystal is reduced, and a single crystal with a low oxygen concentration can be obtained. Furthermore, since the amount of heating above the single crystal pulling region is smaller than when the heater is placed above the crucible, there is no need to reduce the pulling speed, and the single crystal does not become dislocated. etc., the present invention has excellent effects.

【図面の簡単な説明】[Brief explanation of drawings]

【図1】本発明に係る単結晶製造装置の模式的縦断面図
である。
FIG. 1 is a schematic vertical cross-sectional view of a single crystal manufacturing apparatus according to the present invention.

【図2】ヒータの斜視図である。FIG. 2 is a perspective view of a heater.

【図3】発熱ピークの位置を変えたときの引上げ長と酸
素濃度との関係を示したグラフである。
FIG. 3 is a graph showing the relationship between the pulling length and oxygen concentration when the position of the exothermic peak is changed.

【図4】従来の単結晶製造装置の模式的縦断面図である
FIG. 4 is a schematic vertical cross-sectional view of a conventional single crystal manufacturing apparatus.

【符号の説明】[Explanation of symbols]

1  引上げ軸 2  種結晶 3  単結晶 4  石英坩堝 5  カーボン坩堝 6  溶融液 8  ヒータ 1 Pulling shaft 2 Seed crystal 3 Single crystal 4 Quartz crucible 5 Carbon crucible 6 Melt liquid 8 Heater

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】  周囲に配置したヒータで坩堝内にて結
晶用原料を溶融し、溶融液から単結晶を引き上げる単結
晶製造方法において、前記ヒータの発熱分布のピークが
前記溶融液の液面の上側に位置するようにして単結晶を
製造することを特徴とする単結晶製造方法。
1. A method for producing a single crystal in which a raw material for crystal is melted in a crucible using heaters arranged around the crucible and a single crystal is pulled from the melt, wherein the peak of the heat generation distribution of the heater is at a level below the liquid level of the melt. A method for producing a single crystal, characterized in that the single crystal is produced so as to be located on the upper side.
【請求項2】  周囲にヒータを配置した坩堝内にて結
晶用原料を溶融し、溶融液から単結晶を引き上げて成長
させる単結晶製造装置において、前記ヒータの発熱分布
のピークが前記溶融液の液面の上側に位置するようにし
てあることを特徴とする単結晶製造装置。
2. In a single crystal manufacturing apparatus in which a raw material for crystal is melted in a crucible around which a heater is arranged, and a single crystal is pulled up and grown from the melt, the peak of the heat distribution of the heater is the same as that of the melt. A single crystal production device characterized by being positioned above a liquid level.
JP03093414A 1991-03-29 1991-03-29 Single crystal manufacturing method and single crystal manufacturing apparatus Expired - Lifetime JP3099403B2 (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5911825A (en) * 1997-09-30 1999-06-15 Seh America, Inc. Low oxygen heater
WO1999063133A1 (en) * 1998-06-05 1999-12-09 Memc Electronic Materials, Inc. Electrical resistance heater for crystal growing apparatus
US6053974A (en) * 1997-09-30 2000-04-25 Memc Electronic Materials, Inc. Heat shield for crystal puller
US6285011B1 (en) 1999-10-12 2001-09-04 Memc Electronic Materials, Inc. Electrical resistance heater for crystal growing apparatus
JP2010254487A (en) * 2009-04-21 2010-11-11 Sumco Corp Method for growing single crystal
KR101105526B1 (en) * 2008-12-30 2012-01-13 주식회사 엘지실트론 Heater used for manufacturing single crystal ingot and single crystal ingot manufacturing apparatus having the same
KR101105593B1 (en) * 2003-12-23 2012-01-17 주식회사 엘지실트론 A Silicon Single Crystal Grower

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5911825A (en) * 1997-09-30 1999-06-15 Seh America, Inc. Low oxygen heater
US6053974A (en) * 1997-09-30 2000-04-25 Memc Electronic Materials, Inc. Heat shield for crystal puller
WO1999063133A1 (en) * 1998-06-05 1999-12-09 Memc Electronic Materials, Inc. Electrical resistance heater for crystal growing apparatus
US6093913A (en) * 1998-06-05 2000-07-25 Memc Electronic Materials, Inc Electrical heater for crystal growth apparatus with upper sections producing increased heating power compared to lower sections
US6285011B1 (en) 1999-10-12 2001-09-04 Memc Electronic Materials, Inc. Electrical resistance heater for crystal growing apparatus
KR101105593B1 (en) * 2003-12-23 2012-01-17 주식회사 엘지실트론 A Silicon Single Crystal Grower
KR101105526B1 (en) * 2008-12-30 2012-01-13 주식회사 엘지실트론 Heater used for manufacturing single crystal ingot and single crystal ingot manufacturing apparatus having the same
JP2010254487A (en) * 2009-04-21 2010-11-11 Sumco Corp Method for growing single crystal

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