JP2538598B2 - Single crystal pulling device - Google Patents
Single crystal pulling deviceInfo
- Publication number
- JP2538598B2 JP2538598B2 JP62139831A JP13983187A JP2538598B2 JP 2538598 B2 JP2538598 B2 JP 2538598B2 JP 62139831 A JP62139831 A JP 62139831A JP 13983187 A JP13983187 A JP 13983187A JP 2538598 B2 JP2538598 B2 JP 2538598B2
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- single crystal
- refractory
- precious metal
- fixing base
- 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.)
- Expired - Lifetime
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 〔発明の目的〕 （産業上の利用分野） 本発明は、単結晶の引き上げ装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to a single crystal pulling apparatus.
（従来の技術） 単結晶、例えばLiTaO3,LiNbOa,Li2B4O7等の酸化物単
結晶は、回転引き上げ法により成長させ得ている。(Prior Art) Single crystals, for example, oxide single crystals such as LiTaO 3 , LiNbO a , and Li 2 B 4 O 7 can be grown by a rotary pulling method.
以下、LiTaOa（タンタル酸リチウム）を例にとり従来
の単結晶の引き上げ装置を第３図を参照して説明する。A conventional single crystal pulling apparatus will be described below with reference to FIG. 3 by taking LiTaO a (lithium tantalate) as an example.
LiTaO3原料が投入された白金ロジウム合金るつぼ
（２）と耐火るつぼ（１）の間には、耐火性バブル
（９）が充填され、白金ロジウム合金るつぼ（２）の上
部にアフタヒータ（７）や図示しないアルミナ保温筒が
配置される。白金ロジウム合金るつぼ（２）やアフタヒ
ータ（７）は、外周に配置される高周波ワークコイル
（３）に高周波電流を流すことにより誘導加熱され、融
液（４）の温度を制御する。そしてシードホルダ（６）
に取り付けられた種子結晶（５）を融液（４）に接触
後、回転しながら徐々に引き上げると種子結晶（５）に
融液（４）が凝固して成長が開始する。A refractory bubble (9) is filled between the platinum-rhodium alloy crucible (2) containing the LiTaO 3 raw material and the refractory crucible (1), and an afterheater (7) or An alumina heat insulating cylinder (not shown) is arranged. The platinum-rhodium alloy crucible (2) and the afterheater (7) are induction-heated by applying a high-frequency current to the high-frequency work coil (3) arranged on the outer periphery, and control the temperature of the melt (4). And seed holder (6)
After contacting the seed crystal (5) attached to the melt crystal (5) with the melt (4), the melt (4) is solidified in the seed crystal (5) and gradually grows when the seed crystal (5) is gradually pulled up while rotating.
るつぼ内は、るつぼ材の蒸発や消耗を防ぐために雰囲
気ガスを耐火るつぼ（１）の底部に設けられた10mmφ程
度の通気孔（８）から導入し、図示しないアルミナ保温
筒の孔から排出される。In the crucible, atmospheric gas is introduced from a vent hole (8) of about 10 mmφ provided at the bottom of the refractory crucible (1) in order to prevent evaporation and consumption of the crucible material, and is discharged from a hole of an alumina heat insulating tube (not shown). .
（発明が解決しようとする問題点） しかしながら、上述した従来の単結晶の引き上げ装置
によると次のような欠点を有する。(Problems to be Solved by the Invention) However, the conventional single crystal pulling apparatus described above has the following drawbacks.
即ち、白金ロジウム合金るつぼを、耐火るつぼの底部
に直接又は耐火性バブルを敷いて配置し、白金ロジウム
合金るつぼと耐火るつぼとの間に耐火性バブルを充填す
ることによって白金ロジウム合金るつぼを固定している
ため、熱膨張により白金ロジウム合金るつぼの変形を生
じ、耐火性バブルを押しつぶすことになる。これによ
り、耐火性バブルの空間が不均一となり、白金ロジウム
合金るつぼの固定が十分でなくなる。また、耐火るつぼ
の底部から導入された雰囲気ガスが耐火性バブル中を流
れるため、その流れが不均一となり、単結晶育成の温度
分布に影響を与える。さらに、耐火性バブルが白金ロジ
ウム合金るつぼの表面に付着し、白金ロジウム合金るつ
ぼの消耗の原因となっていた。That is, the platinum rhodium alloy crucible is placed directly on the bottom of the refractory crucible or with a refractory bubble laid, and the platinum rhodium alloy crucible is fixed by filling the refractory bubble between the platinum rhodium alloy crucible and the refractory crucible. Therefore, the platinum-rhodium alloy crucible is deformed by the thermal expansion, and the refractory bubbles are crushed. As a result, the space of the refractory bubble becomes non-uniform, and the platinum-rhodium alloy crucible is not sufficiently fixed. Further, since the atmospheric gas introduced from the bottom of the refractory crucible flows through the refractory bubble, the flow becomes non-uniform, which affects the temperature distribution of single crystal growth. Further, the refractory bubbles adhered to the surface of the platinum-rhodium alloy crucible, which was a cause of consumption of the platinum-rhodium alloy crucible.
そこで本発明は、貴金属るつぼの変形や消耗を少なく
し安定した単結晶の引き上げ装置を提供することを目的
とする。Therefore, an object of the present invention is to provide a stable single crystal pulling apparatus which reduces deformation and wear of the precious metal crucible.
（問題点を解決するための手段） 本発明は、上述した問題点を解決するためになされた
もので、筒部とこの筒部端縁から下方に錐状中空体部を
有する貴金属るつぼと、錐状中空体部に当接された複数
個の凸部を形成しこの凸部と錐状中空体部外面とで溝を
形成するるつぼ固定台と、この固定台および貴金属るつ
ぼを包囲しかつ貴金属るつぼの軸方向に通気孔をもって
溝に連通する構造を有する耐火るつぼとを具備し、溝に
雰囲気ガスを導入し得ることを特徴とするものである。(Means for Solving Problems) The present invention has been made to solve the above-mentioned problems, and includes a tubular portion and a precious metal crucible having a conical hollow body portion downward from an end edge of the tubular portion, A crucible fixing base that forms a plurality of convex portions that are in contact with the conical hollow body portion and forms a groove between the convex portion and the outer surface of the conical hollow body portion, and a precious metal that surrounds the crucible and the precious metal crucible. A refractory crucible having a structure in which a vent hole is provided in the axial direction of the crucible so as to communicate with the groove, and an atmospheric gas can be introduced into the groove.
（作用） 貴金属るつぼの錐状中空体部において、耐火性バブル
を使用する必要がなくなるため、貴金属るつぼの安定性
が向上し消耗が少なくなる。また、雰囲気ガスを流す
際、るつぼ固定台の溝に沿って流れるため、均一な温度
分布が得られる。(Function) Since it is not necessary to use a refractory bubble in the conical hollow body portion of the precious metal crucible, the stability of the precious metal crucible is improved and the consumption is reduced. Further, when the atmosphere gas is flown, it flows along the groove of the crucible fixing base, so that a uniform temperature distribution can be obtained.
（実 施 例） 以下、本発明の単結晶の引き上げ装置の一実施例を第
１図及び第２図を参照して説明する。(Examples) An example of a single crystal pulling apparatus of the present invention will be described below with reference to FIGS. 1 and 2.
第１図に示す如く、白金−ロジウム合金でなる貴金属
るつぼ（11）は、径大の円筒部（10−１）及びこの円筒
部（10−１）から延在し、円筒部（10−１）から離れる
ほど直径が細くなる有底の径小部（10−２）とを有して
いる。As shown in FIG. 1, a precious metal crucible (11) made of a platinum-rhodium alloy extends from the cylindrical portion (10-1) having a large diameter and the cylindrical portion (10-1), and the cylindrical portion (10-1 ) And a bottomed small-diameter portion (10-2), the diameter of which becomes smaller as the distance from) increases.
貴金属るつぼ（11）は、耐火性バブル（９）を介して
耐火るつぼ（１）の内側に置かれ、円錐台形状の固定台
（12）にのせて配置される。また、耐火るつぼ（１）の
底部には、雰囲気ガスを導入させるための通気孔（８）
を設けている。The precious metal crucible (11) is placed inside the refractory crucible (1) through the refractory bubble (9) and placed on the truncated cone-shaped fixed base (12). In addition, the bottom of the refractory crucible (1) has a vent hole (8) for introducing atmospheric gas.
Is provided.
るつぼ固定台（12）は、第２図（ａ）及び第２図
（ｂ）からわかるように、貴金属るつぼ（11）の径小部
（10−２）に対向して例えば８個の凸部を形成してお
り、径小部外側とによって、雰囲気ガスを通路となる溝
（14）が形成される。As can be seen from FIGS. 2 (a) and 2 (b), the crucible fixing base (12) faces the small diameter portion (10-2) of the precious metal crucible (11) and has, for example, eight convex portions. And a groove (14) serving as a passage for the atmospheric gas is formed by the outside of the small diameter portion.
実施例１ 本発明の単結晶の引き上げ装置によりLiTaO3を育成し
た。貴金属るつぼは、白金−ロージウム合金で、その形
状は円筒部の直径180mm、円筒部の高さ70mm、径小部は
円すい台状で高さ70mm、側面は円筒部側面に対して40゜
の角度である。また、固定台の凸部の寸法を幅10mm、高
さ5mmである。雰囲気ガスとしては、N2ガスを用い、６
/minの割合で通気孔から導入させ、導入されたN2ガス
は第２−ａ図及び第２−ｂ図に示するつぼ固定台の溝
（14）に沿って均一に流れていく。その結果、温度分布
が均一で貴金属るつぼの安定性が良いので、14kgの原料
融液から約8kgのLiTaO3を育成することができた。Example 1 LiTaO 3 was grown by the single crystal pulling apparatus of the present invention. The noble metal crucible is a platinum-rhodium alloy, and its shape is the diameter of the cylindrical part is 180 mm, the height of the cylindrical part is 70 mm, the small diameter part is a truncated cone shape and the height is 70 mm. Is. The convex portion of the fixed base has a width of 10 mm and a height of 5 mm. N 2 gas was used as the atmosphere gas, and 6
The N 2 gas introduced from the ventilation hole at a rate of / min uniformly flows along the groove (14) of the crucible fixing base shown in FIGS. 2-a and 2-b. As a result, since the temperature distribution is uniform and the stability of the precious metal crucible is good, about 8 kg of LiTaO 3 could be grown from 14 kg of the raw material melt.
実施例２ LiNbO3を本発明の単結晶の引き上げ装置で育成した。
るつぼは白金製で、寸法は円筒部の直径120mm、円筒部
の高さ80mm、径小部は、円錐台状で高さ40mm、側面は円
筒部側面と45゜の角度である。また、るつぼ固定台の凸
部の寸法を幅5mm、高さ5mmとした。この引き上げ装置を
用いて実施例１と同様に単結晶の育成を行なった。その
結果、3.8kgの原料融液から約2.8kgのLiNbO3を育成する
ことができた。Example 2 LiNbO 3 was grown by the single crystal pulling apparatus of the present invention.
The crucible is made of platinum. The dimensions of the crucible are 120 mm in diameter, the height of the cylinder is 80 mm, the small diameter is frustoconical and the height is 40 mm. Further, the dimensions of the convex portion of the crucible fixing base were 5 mm in width and 5 mm in height. Using this pulling device, a single crystal was grown in the same manner as in Example 1. As a result, about 2.8 kg of LiNbO 3 could be grown from 3.8 kg of the raw material melt.
このように、るつぼの寸法を変えたり、LiTaO3,LiNbO
3をはじめ他の酸化物単結晶においても有効である。In this way, changing the crucible size, changing the LiTaO 3 , LiNbO
It is also effective for other oxide single crystals such as 3 .
以上述べてきたように、本発明の単結晶の引き上げ装
置によれば、貴金属るつぼの変形及び消耗が少なく、温
度分布が均一になるため、安定で高歩留りの単結晶を得
ることができる。As described above, according to the apparatus for pulling a single crystal of the present invention, the deformation and wear of the precious metal crucible are small and the temperature distribution is uniform, so that a stable and high-yield single crystal can be obtained.
第１図は本発明の単結晶の引き上げ装置の一実施例を示
す要部縦断面図、第２図（ａ）は本発明の単結晶の引き
上げ装置に係るるつぼ固定台の一実施例を示す斜視図、
第２図（ｂ）は第２図（ａ）に基づくるつぼ固定台を示
す縦断面図、第３図は従来の単結晶の引き上げ装置を示
す要部縦断面図である。 １……耐火るつぼ、８……通気孔 10−１……径大部、10−２……径小部 11……貴金属るつぼ、12……るつぼ固定台 13……凸部FIG. 1 is a longitudinal sectional view of an essential part showing an embodiment of a single crystal pulling apparatus of the present invention, and FIG. 2 (a) shows an embodiment of a crucible fixing base according to the single crystal pulling apparatus of the present invention. Perspective view,
FIG. 2 (b) is a vertical cross-sectional view showing the crucible fixing base based on FIG. 2 (a), and FIG. 3 is a main-part vertical cross-sectional view showing a conventional single crystal pulling apparatus. 1 ... Fireproof crucible, 8 ... Ventilation hole 10-1 ... Large diameter part, 10-2 ... Small diameter part 11 ... Precious metal crucible, 12 ... Crucible fixing base 13 ... Convex part
Claims (1)
部を有する貴金属るつぼと、この貴金属るつぼの前記錐
状中空体部に当接された複数個の凸部を形成しこの凸部
と前記貴金属るつぼの錐状中空体部外面とで溝を形成す
るるつぼ固定台と、 この固定台および前記貴金属るつぼを包囲しかつ前記貴
金属るつぼの軸方向に通気孔をもって前記溝に連通する
構造を有する耐火るつぼとを具備し、前記溝に雰囲気ガ
スを導入し得ることを特徴とする単結晶の引き上げ装
置。1. A noble metal crucible having a tubular portion and a conical hollow body portion downward from an end edge of the tubular portion, and a plurality of convex portions abutting on the conical hollow body portion of the noble metal crucible. A crucible fixing base that forms a groove with the convex portion and the outer surface of the conical hollow body of the precious metal crucible; a crucible fixing base that surrounds the fixing base and the precious metal crucible; and a ventilation hole in the axial direction of the precious metal crucible that communicates with the groove. And a refractory crucible having the structure described above, and an atmosphere gas can be introduced into the groove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62139831A JP2538598B2 (en) | 1987-06-05 | 1987-06-05 | Single crystal pulling device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62139831A JP2538598B2 (en) | 1987-06-05 | 1987-06-05 | Single crystal pulling device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63307188A JPS63307188A (en) | 1988-12-14 |
| JP2538598B2 true JP2538598B2 (en) | 1996-09-25 |
Family
ID=15254507
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62139831A Expired - Lifetime JP2538598B2 (en) | 1987-06-05 | 1987-06-05 | Single crystal pulling device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2538598B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6726910B2 (en) * | 2016-04-21 | 2020-07-22 | 国立大学法人信州大学 | Device for producing gallium oxide crystal and method for producing gallium oxide crystal |
-
1987
- 1987-06-05 JP JP62139831A patent/JP2538598B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63307188A (en) | 1988-12-14 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |