JPS6036399A - Fixing of seed crystal - Google Patents
Fixing of seed crystalInfo
- Publication number
- JPS6036399A JPS6036399A JP14415183A JP14415183A JPS6036399A JP S6036399 A JPS6036399 A JP S6036399A JP 14415183 A JP14415183 A JP 14415183A JP 14415183 A JP14415183 A JP 14415183A JP S6036399 A JPS6036399 A JP S6036399A
- Authority
- JP
- Japan
- Prior art keywords
- seed crystal
- crystal
- seed
- fixing
- single crystal
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（技術分野）
本発明はチョクラルスキー法（以下、ＣＺ法と称す）又
は液体カプセルチョクラルスキー法（以下、ＬＥＣ法と
称す）によシ単結晶を引上ける際、種結晶（シード）を
固定する方法に関するものである。Detailed Description of the Invention (Technical Field) The present invention involves pulling a single crystal using the Czochralski method (hereinafter referred to as the CZ method) or the liquid capsule Czochralski method (hereinafter referred to as the LEC method). The invention relates to a method for fixing seed crystals (seeds).
（背景技術）
ＣＺ法は、第１図に例を示すように、ヒータ５によシ加
熱されるるつぼ６に原料融液１ｅ収容し、必要によりそ
の表面’ｋ Ｂ２０ｇ融液２でおおい（ＬＥＣ法の場合
）、融液１表面に種結晶３を浸漬し、なじませた後、種
結晶３を回転しながら引上げて単結晶４全引上げる方法
である。この場合、種結晶は引上軸の下端に取付けられ
た・Ｚ−ド棒７に固定される。(Background Art) In the CZ method, as shown in FIG. 1, a raw material melt 1e is placed in a crucible 6 heated by a heater 5, and if necessary, the surface is covered with a 20 g melt 2 (LEC method), the seed crystal 3 is immersed in the surface of the melt 1, and after being blended, the seed crystal 3 is pulled up while rotating, and the entire single crystal 4 is pulled up. In this case, the seed crystal is fixed to a Z-rod 7 attached to the lower end of the pulling shaft.
従来、この種結晶を固定する方法として第１図（イ）〜
（ト）に例を示すような種々の方法が採られており、そ
れぞれ次のような欠点がある。図において３は種結晶、
７はンード棒である。Conventionally, methods for fixing this seed crystal are shown in Figure 1 (a) -
Various methods have been adopted, as shown in (g) below, and each method has the following drawbacks. In the figure, 3 is a seed crystal,
7 is the nd bar.
（イ）図に示す方法は、種結晶３を小型チャック又はピ
ンバイス８により固定する方法で、種結晶の大きさによ
シ各種サイズを必要とする。(a) The method shown in the figure is a method in which the seed crystal 3 is fixed with a small chuck or pin vise 8, and various sizes are required depending on the size of the seed crystal.
（ロ）図に示す方法は、種結晶３を挿入孔９に挿入し、
通常例えはステンレス鋼、ＭＯ製等のねじ１０の３〜８
個によシ固定する方法である。(b) The method shown in the figure is to insert the seed crystal 3 into the insertion hole 9,
Usually screws 10-3 to 8 are made of stainless steel, MO, etc.
This is a method of fixing it individually.
（ハ）図に示す方法は、種結晶８に半円状切欠を設けて
挿入孔９に挿入し、丸ピン１１で止める方法で、かなシ
高精度の加工を要する。(c) The method shown in the figure is a method in which a semicircular notch is provided in the seed crystal 8, the seed crystal 8 is inserted into the insertion hole 9, and the seed crystal 8 is fixed with a round pin 11, which requires high-precision machining.
に）図に示す方法は、種結晶３を２つ割シチャック１２
により挾持する方法で、種結晶の大きさにより各種寸法
のものを必要とする。) The method shown in the figure is to split the seed crystal 3 into two parts.
This method requires seed crystals of various sizes depending on the size of the seed crystal.
０９図に示す方法は、種結晶３の上部をテーパー状に加
工し、テーパー付き挿入孔１３に挿入し、固定する方法
で、結晶の加工が必要である。The method shown in FIG. 09 involves processing the upper part of the seed crystal 3 into a tapered shape, inserting it into the tapered insertion hole 13, and fixing it, which requires processing the crystal.
（へ）図に示す方法は、種結晶３を挿入孔Ｉ４に挿入し
、セメント止めする方法で、不用意なセメント使用は種
結晶を落とすことがある。(f) The method shown in the figure is a method of inserting the seed crystal 3 into the insertion hole I4 and fixing it with cement. Careless use of cement may cause the seed crystal to fall.
（ト）図に示す方法は、種結晶３をシード棒７に耐熱ワ
イヤ１５によりしばる方法で、簡便であるが、しばしば
結晶の落下、ぐらつきがある。(g) The method shown in the figure is a method in which the seed crystal 3 is tied to the seed rod 7 with a heat-resistant wire 15, and is simple, but the crystal often falls and wobbles.
又このような種結晶の固定部分は高温の外気にさらされ
ているため次のような問題がある。Furthermore, since the fixed portion of such a seed crystal is exposed to high temperature outside air, there are the following problems.
例えば、ＧａＡｓ等の蒸発し易い物質を含む単結晶を、
転位密度を減らせるために低温度勾配で成長させようと
すると、第３図に例を示すようにＡｓ等が種結晶３から
抜け、種結晶固定が不完全になり、ついには脱落するに
至る。図に示すように、最初様れ、右図に示すように脱
落する。For example, a single crystal containing a substance that evaporates easily, such as GaAs,
When trying to grow at a low temperature gradient in order to reduce the dislocation density, as shown in Figure 3, As and the like fall out of the seed crystal 3, making the seed crystal fixation incomplete and eventually causing it to fall off. . As shown in the figure, it first disintegrates and falls off as shown in the figure on the right.
本発明は、」二連の問題点全解決するため成されたもの
で、単結晶引上げ中、種結晶の把持部をＢ２Ｏ３融液に
より保護して蒸発し易い物質（例、Ａｓ。The present invention has been made to solve both of the two problems. During single crystal pulling, the gripping part of the seed crystal is protected by a B2O3 melt to prevent substances that easily evaporate (eg, As).
Ｐ、 Ｓ、 Ｓｅ等）の蒸発全防いで、種結晶の損傷に
よる脱落全防止する種結晶の固定方法を提供せんとする
ものである。The present invention aims to provide a method for fixing seed crystals that completely prevents evaporation of P, S, Se, etc.) and completely prevents seed crystals from falling off due to damage.
本発明は、チョクラルスキー法により単結晶を引上げる
際、種結晶をシード棒に固定する方法において、前記種
結晶の少なくとも把持される部分の一部をＢ２Ｏ３′融
液でおおうことを特徴とする種結晶の固定方法である。The present invention is characterized in that in a method of fixing a seed crystal to a seed rod when pulling a single crystal by the Czochralski method, at least a part of the gripped portion of the seed crystal is covered with a B2O3' melt. This is a method of fixing seed crystals.
本発明によシ引上げる単結晶は、例えばＧａＡｓ 。The single crystal to be pulled according to the present invention is, for example, GaAs.
Ｇａｐ、 ＩｎＳｂ＋ ＴｎＰ、 ＩｎＡｓ等の周期律
表のＩ−Ｖ族化合物半導体、例えばＺｎＳ、 Ｚｎ５ｅ
、 ＣｄＳ、 ｃｄｓｅ等の１ｔ−ｖｉ族化合物、例え
ばＳｉ、Ｇｅ等の第■族半導体、酸化物、窒化物、硼化
物、炭化物などより成るものである。Group IV compound semiconductors of the periodic table such as Gap, InSb+TnP, InAs, etc., such as ZnS, Zn5e
, CdS, Cdse, etc., Group I semiconductors such as Si, Ge, etc., oxides, nitrides, borides, carbides, etc.
以下、本発明を図面を用いて実施例により説明する。第
４図は本発明方法の実施例における種結晶の把持部を示
す縦断面図（中央）およびチャックの斜視図であり、第
５図は同じく種結晶を示す斜視図である。Hereinafter, the present invention will be explained by examples using the drawings. FIG. 4 is a longitudinal cross-sectional view (center) showing a gripping portion for a seed crystal and a perspective view of a chuck in an embodiment of the method of the present invention, and FIG. 5 is a perspective view similarly showing a seed crystal.
本発明方法では、第５図に示すように種結晶３の上方の
角を削って切欠部１８を作る。又種結晶３を挾持するチ
ャックは、第４図に示すように、２つ割りのチャック１
９．２０とし、合せてねじ孔２＋、２２にねじを挿入し
て締付けるようになっている。一方のチャック１９は長
く、７字型の溝２３が切られ、他方のチャック２０は短
かく、下方には奥の平らになった部分２５を有するＶ字
型の溝２４が切られ、上方にはＢ２Ｏ３融液２６を収容
するＢ２Ｏ３溜め２７が設けられている。このようなチ
ャック１９，２．−０によシ種結晶３を把持するには、
種結晶３の切欠部１８をチャック２０の溝２４Ｉ：
の奥の平らになった部分２５寺嵌合するようにしてチャ
ック１９．２０ではさみ、ねじで締付けた後、Ｂ２Ｏ３
溜め２７にはじめはＢ２Ｏ３固体の小片を入れる。炉中
熱する過程でこれが軟化し、上端部をおおう。In the method of the present invention, the upper corner of the seed crystal 3 is cut to form a notch 18, as shown in FIG. The chuck that holds the seed crystal 3 is a chuck 1 divided into two parts, as shown in FIG.
9.20, and screws are inserted into screw holes 2+ and 22 and tightened. One chuck 19 is long and has a 7-shaped groove 23 cut in it, while the other chuck 20 is short and has a V-shaped groove 24 cut in it with a flattened part 25 at the bottom and a flattened part 25 in the upper part. A B2O3 reservoir 27 containing a B2O3 melt 26 is provided. Such a chuck 19,2. To grasp the seed crystal 3 by -0,
The notch 18 of the seed crystal 3 is held in the chuck 19.20 so that it fits into the flattened part 25 at the back of the groove 24I of the chuck 20, and after tightening with a screw, the B2O3
Reservoir 27 is initially filled with a small piece of B2O3 solid. During the heating process in the oven, this softens and covers the upper end.
こうして種結晶３の上端部２８をＢ２Ｏ３融液２６でお
おう。In this way, the upper end 28 of the seed crystal 3 is covered with the B2O3 melt 26.
このようにすると、種結晶３の切欠部１８はチャック２
０の溝の奥の部分２５で抑えられ、切欠部１８のＡ部で
脱落が防がれ、かつ外気にさらされる上端部２８がＢ２
Ｏ３融液２６におおわれて蒸発し易い物質（例、Ａｓ等
）の蒸発を防ぐため、種結晶３の把持される部分が損傷
せず、単結晶成長中脱落することがない。In this way, the notch 18 of the seed crystal 3 is removed from the chuck 2.
The upper end 28 is held down by the deep part 25 of the groove 0, is prevented from falling off by the part A of the notch 18, and is exposed to the outside air.
Since it is covered with the O3 melt 26 and prevents evaporation of easily evaporated substances (eg, As, etc.), the gripped portion of the seed crystal 3 is not damaged and does not fall off during single crystal growth.
なお、本発明においてＢ２Ｏ３融液でおおう部分は、種
結晶の少なくとも把持される部分の一部又は全部であり
、特に種結晶の支持に不可欠の部分であり、又廁結晶の
固定方法は第４図に示すものに限定されるものではなく
、例えば第２図（ロ）〜（ホ）に示す形式のものにＢ２
Ｏ３溜めを設ければ適用可能である。In addition, in the present invention, the part covered with the B2O3 melt is at least a part or all of the part of the seed crystal that is gripped, and is particularly an essential part for supporting the seed crystal, and the method of fixing the crystal is the fourth part. B2 is not limited to those shown in the figure, and for example, B2
It can be applied if an O3 reservoir is provided.
（実施例）
本発明方法には第４図に示すようなチャックを用い、従
来法には第６図に示すようなチャックを用い、ＧａＡｓ
単結晶’６ｃｚ法によシ引上げた。(Example) A chuck as shown in FIG. 4 was used for the method of the present invention, and a chuck as shown in FIG. 6 was used for the conventional method.
It was pulled by the single crystal '6cz method.
第６図において、第５図に示すような切欠部１８を設け
た種結晶３全挾持するチャック２９．８０は、第４図に
示すようなＶ字型の溝のみな切ったもので、Ｂ２Ｏ３溜
めのないものである。In FIG. 6, the chucks 29 and 80 that hold the entire seed crystal 3 provided with a notch 18 as shown in FIG. 5 are made by cutting only a V-shaped groove as shown in FIG. It is something that does not accumulate.
第７図に示するつぽ６にＧａＡｓ多結晶４ Ｋｇ、 、
Ｂ２０８ｉチヤージし、融解した後、雰囲気Ｎ２ガス
圧５気圧とし、温度勾配Ｔｉ第７図に示すように保持し
、引上速度１０ｍｍ１時、引上軸回転数ＩＱｒｐｍ、る
つぼ回転数１Ｏｒｐｍとして単結晶を引上げ、直径７５
〜８０ｍｍ、直胴部長約１４０ ｍｍの単結晶を得た。GaAs polycrystal 4 kg, , at the point 6 shown in Figure 7.
After charging and melting B208i, the atmosphere was N2 gas pressure 5 atm, the temperature gradient Ti was maintained as shown in Fig. 7, the pulling speed was 10 mm, 1 hour, the pulling shaft rotation speed was IQ rpm, and the crucible rotation speed was 1 Orpm to form a single crystal. Pull up, diameter 75
A single crystal with a diameter of ~80 mm and a straight body length of approximately 140 mm was obtained.
従来法による場合は、５回の引上げのうち３回種結晶ご
と単結晶が脱落した。In the case of the conventional method, the single crystal fell off along with the seed crystal three times out of five times of pulling.
これに対し、本発明方法による場合は、１３回の引上げ
のうち、１回の脱落もなかった。On the other hand, in the case of the method of the present invention, not one dropout occurred among the 13 pullings.
（発明の効果）
上述のように構成された本発明の種結晶の固定方法は次
のような効果がある。(Effects of the Invention) The seed crystal fixing method of the present invention configured as described above has the following effects.
種結晶の少なくとも把持される部分の一部’ｉｉ Ｂ２
Ｏ３融液でおおうため、単結晶引上中、種結晶の支持さ
れる部分がＢ２Ｏ３融液におおわれ、蒸気し易い物質（
例、Ａｓ、Ｐ等）の蒸発を防ぐので、種結晶が損傷せず
、脱落を防ぐ。At least a part of the part of the seed crystal to be held 'ii B2
Because it is covered with O3 melt, the supported part of the seed crystal is covered with B2O3 melt during single crystal pulling, and substances that easily vaporize (
For example, As, P, etc.) are prevented from evaporating, so the seed crystal is not damaged and is prevented from falling off.
第１図は単結晶引上げ法の例を説明するだめの縦断面図
である。
第２図（イ）〜（ト）はそれぞれ従来の種結晶の固定方
法の例を説明する図である。
第３図は従来法における種結晶の脱落の状態の例を示す
断面図である。
第４図は本発明方法の実施例における種結晶の把持部を
示す縦断面図およびチャックの斜視図であり、第５図は
同じく種結晶を示す斜視図である。
第６図は従来法の例における種結晶の把持部を示す縦断
面図である。
第７図は本発明方法の実施例におけるるつぼおよび温度
分布を示す図である。
１ ・反別融液、２，２６・・・Ｂ２Ｏ３融液、３・・
種結晶、４ ・単結晶、５・・ヒーター、６ るつぼ、
７・・・シード棒、８・・・小型チャック又はピンバイ
ス、９゜１４・・・挿入孔、１０・・・ねじ、１１・・
・丸ピア１．１２゜１９．２０，２９．３０ チャック
、１３・・テーパー付き挿入孔、１５ ・耐熱ワイヤ、
ｌ６−Ａｓ抜け、１７ ＝−Ｇａ融解、１８ 切欠部、
２１．２２−・・ねじ孔、２３．２４ ・Ｖ字型の溝、
２５ 奥の平らになった部分、２７・Ｂ２Ｏ３溜め、２
８・・・上端部、Ａ・・・部分。
許１図
官３図
芳４図
大７図FIG. 1 is a longitudinal sectional view illustrating an example of a single crystal pulling method. FIGS. 2(A) to 2(G) are diagrams each illustrating an example of a conventional method of fixing a seed crystal. FIG. 3 is a sectional view showing an example of a state in which a seed crystal falls off in a conventional method. FIG. 4 is a longitudinal sectional view showing a gripping portion for a seed crystal and a perspective view of a chuck in an embodiment of the method of the present invention, and FIG. 5 is a perspective view similarly showing a seed crystal. FIG. 6 is a longitudinal sectional view showing a gripping portion of a seed crystal in an example of the conventional method. FIG. 7 is a diagram showing a crucible and temperature distribution in an example of the method of the present invention. 1 ・Tanbetsu melt, 2,26...B2O3 melt, 3...
Seed crystal, 4.Single crystal, 5..Heater, 6. Crucible,
7... Seed rod, 8... Small chuck or pin vise, 9°14... Insertion hole, 10... Screw, 11...
・Round pier 1.12゜19.20, 29.30 Chuck, 13...Tapered insertion hole, 15 ・Heat-resistant wire,
16-As missing, 17 =-Ga melting, 18 notch,
21.22-...screw hole, 23.24 ・V-shaped groove,
25 Flat part at the back, 27・B2O3 reservoir, 2
8...Top end, A...part. Xu 1 Zukan 3 Zu Fang 4 Dai 7
Claims (1)
種結晶を７−ド棒に固定する方法において、前記種結晶
の少なくとも把持される部分の一部をＢ２Ｏ３融液でお
おうことを特徴とする種結晶の固定方法。(1) When pulling a single crystal using the Czochralski method,
A method for fixing a seed crystal to a 7-rod rod, the method comprising: covering at least a portion of the seed crystal to be gripped with a B2O3 melt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14415183A JPS6036399A (en) | 1983-08-06 | 1983-08-06 | Fixing of seed crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14415183A JPS6036399A (en) | 1983-08-06 | 1983-08-06 | Fixing of seed crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6036399A true JPS6036399A (en) | 1985-02-25 |
Family
ID=15355398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14415183A Pending JPS6036399A (en) | 1983-08-06 | 1983-08-06 | Fixing of seed crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6036399A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6814242B2 (en) | 2001-07-26 | 2004-11-09 | Satake Corporation | Rotatively oscillating separator |
-
1983
- 1983-08-06 JP JP14415183A patent/JPS6036399A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6814242B2 (en) | 2001-07-26 | 2004-11-09 | Satake Corporation | Rotatively oscillating separator |
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