JPS5957984A - Method for contacting seed crystal or substrate - Google Patents
Method for contacting seed crystal or substrateInfo
- Publication number
- JPS5957984A JPS5957984A JP17204082A JP17204082A JPS5957984A JP S5957984 A JPS5957984 A JP S5957984A JP 17204082 A JP17204082 A JP 17204082A JP 17204082 A JP17204082 A JP 17204082A JP S5957984 A JPS5957984 A JP S5957984A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- resistance
- seed crystal
- melt
- moment
- 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
- C30B15/20—Controlling or regulating
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ｕ、Ｂ１１２ＳｉＯ３０（ビスマス、ンリコン、
オキサイド）、Ｂｉ＋２ＧｅＯ２ｏ （ビスマス、ゲ
ルマニウム、オキサイド）又はその他の酸化物単結晶を
育成又はエピタキシャル成長させる方法において、！１
！１″に種結晶（シード）又は基板と原註融液が接触し
た瞬間を・検知する方法に関するものである。Detailed Description of the Invention (Technical Field) The present invention u, B112SiO30 (bismuth,
oxide), Bi+2GeO2o (bismuth, germanium, oxide) or other oxide single crystals in a method for growing or epitaxially growing it! 1
! This invention relates to a method of detecting the moment when a seed crystal or a substrate and a melt contact each other.
（背景技術）
従来、Ｂ１１２Ｓｉ０２（１（以下、ＢＳＯと称す）単
結晶を育成又はエピタキシャル成長させるには、第１図
に例を示すよう外方法を採っていた。（２）において、
外周にヒーター４を設けた結晶育成炉（又はエピタキシ
ャル炉）３内のるつは２に原刺融／？り】が収容されて
いる。上部カバー１５の開口１６より炉３内に支持棒７
が挿入され、支持棒７の下端にはシード（又は基板）８
が取付けられる。この／−ド（又は基板）８を徐々に下
降させ、それを融′Ｄ、１に接触させた後、シード８全
引」二げてＢＳＯ単結晶を育成するか、又は基板８上に
ＢＳＯエピタキシャル成長させた後、基板８を引上ける
ものである。この場合、シード（又は基板）８と融ｍｌ
とが接触した瞬間を知ることが重要であるが、従来亀
は支持棒７と上部カバー１５の開口１６の隙間から目視
によって行なうか、又は炉３内に石英ロッドを挿入し、
これ全通して観察することにより行なりていた。(Background Art) Conventionally, in order to grow or epitaxially grow a B112Si02 (1 (hereinafter referred to as BSO)) single crystal, a method as shown in FIG. 1 has been adopted. In (2),
The crystal growth furnace (or epitaxial furnace) 3 has a heater 4 installed around its outer periphery. ] is accommodated. The support rod 7 is inserted into the furnace 3 through the opening 16 of the upper cover 15.
is inserted, and a seed (or substrate) 8 is inserted at the lower end of the support rod 7.
is installed. After gradually lowering the seed (or substrate) 8 and bringing it into contact with the melt, the seed 8 is completely withdrawn to grow a BSO single crystal, or the BSO single crystal is grown on the substrate 8. After epitaxial growth, the substrate 8 is pulled up. In this case, the seed (or substrate) 8 and the melted ml
It is important to know the moment when the two contact each other. Conventionally, this is done by visually observing from the gap between the support rod 7 and the opening 16 of the upper cover 15, or by inserting a quartz rod into the furnace 3.
This was done by observing the entire process.
しかし、この炉３では、炉内の温度分布が外気の影響を
受けにくいように、上部カバー１５の開口１６を極力小
さくしているため、目視による場合、視野が狭く、又炉
３内の暖ためられた空気が上昇気流として、開１月６よ
り流出するだめ、目視では熱くて長時間の観察が不可能
である欠点がある。However, in this furnace 3, the opening 16 of the upper cover 15 is made as small as possible so that the temperature distribution inside the furnace is less affected by the outside air. The accumulated air flows out in the form of updrafts starting from January 6, which has the disadvantage that it is too hot to observe with the naked eye for a long period of time.
又イ」英ロット全使用した場合は、融液１中がらＢｉ２
Ｏ３の蒸気が絶えず蒸発しており、石英ロッドの主成分
である５１０２と反応するため、表面がくもり、長期に
わたり使用した場合、透明度が悪くなり、観察しにくい
欠点があった。In addition, if all British lots are used, melt 1 and Bi2
O3 vapor constantly evaporates and reacts with 5102, the main component of the quartz rod, resulting in a cloudy surface and poor transparency when used for a long period of time, making it difficult to observe.
（発明の開示）
本発明は、上述の欠点を解消するため成されたもので、
種結晶又は基板と原料融液が接触した瞬間を電気的に検
知することにより、単結晶育成炉又はエピタキシャル炉
全密閉した状態で使用でき、長時間の観察が容易で、疲
労少なく、かつ長期間精度良く、検知可能な種結晶又は
基板の接触方法を提供せんとするものである。(Disclosure of the Invention) The present invention has been made in order to eliminate the above-mentioned drawbacks.
By electrically detecting the moment when the seed crystal or substrate comes into contact with the raw material melt, the single crystal growth furnace or epitaxial furnace can be used in a completely sealed state, making long-term observation easy, reducing fatigue, and providing long-term operation. It is an object of the present invention to provide a method of contacting a seed crystal or a substrate that can be detected with high precision.
本発明は、Ｂｌ １２ｓ１０２ ｏ、Ｂｌ １２Ｇｅ０
２ｇ又はその他の酸化物ｔ１つ結晶を育成又はエピタキ
シャル成長させる方法において、種結晶又は基板が原訃
ｌ酵１！液に４と）（］・１１した瞬間を、前記種結晶
又は前記基板と前記原第１融液との間の抵抗を測定する
ことにより、検知すること庖・特徴とする種結晶又は基
板の接触方法である。The present invention provides Bl 12s102 o, Bl 12Ge0
In a method for growing or epitaxially growing 2g or other oxide crystals, a seed crystal or substrate is used as a source for fermentation. Detecting the moment when the liquid enters the liquid by measuring the resistance between the seed crystal or the substrate and the original first melt. This is a contact method.
本発明における単結晶を育成する方法は、（」１１結晶
（ソート）ヲ用いて単結晶を育成する方法で、例えばチ
ョクラルスキー法、ブリッジマン法（ボート成長法）な
どである。又エピタキシャル成長させる方法は、基板を
原相融液中に浸漬し、液相エピタキシャル成長させるも
のである。The method of growing a single crystal in the present invention is a method of growing a single crystal using 11 crystals (sorting), such as the Czochralski method and Bridgman method (boat growth method).Also, epitaxial growth The method involves immersing the substrate in an original phase melt and performing liquid phase epitaxial growth.
以下、本発明を図面を用いて実施例により説明する。第
２図は本発明方法の実施例を説明する縦断面図である。Hereinafter, the present invention will be explained by examples using the drawings. FIG. 2 is a longitudinal sectional view illustrating an embodiment of the method of the present invention.
図において第１図と同一の符号はそれぞれ同一の部分を
示す。図において、支持棒７の下端に取付けられた種結
晶（シード）又は基板８の一部に白金線９の一端が固定
され、白金線９ｉｌ−１：支持棒７を伝って結晶育成炉
（又はエピタキシャル炉）３外に出て、他端が抵抗言１
１１に接１１’ｊ’１″、されている。In the figure, the same reference numerals as in FIG. 1 indicate the same parts. In the figure, one end of the platinum wire 9 is fixed to a seed crystal (seed) attached to the lower end of the support rod 7 or to a part of the substrate 8, and the platinum wire 9il-1: The platinum wire 9il-1 is passed through the support rod 7 to the crystal growth furnace (or epitaxial furnace) 3, and the other end is the resistance word 1.
11 and 11'j'1''.
又るつは２（例、白金るつぼ）の外壁に他の白金＃ＩＩ
Ｉ Ｏの一端が接続され、その他端は炉３外に取出され
、抵抗泪１１に接続されている。Another platinum #II is placed on the outer wall of 2 (e.g. platinum crucible)
One end of the IO is connected, and the other end is taken out of the furnace 3 and connected to the resistor 11.
このように構成された単結晶育成又はエピタキシャル成
長装置によると、シート又は基板８が原オ′１融ｄ久１
に接触する寸では、固自金線９．１０の間は空気層１２
によって絶縁されて抵抗計ＩＩは極太抵抗を示すが、シ
ート又は基板８が下降し、融ｉｌと接触すると、固自金
線９．１０の間は融液１、るつぼ２を介して接続され、
１３＋１２３ｉ０２０ は溶融状態では低抵抗である
ので、抵抗計１１による抵抗値は空気層１２の抵抗たけ
減少し、著しく低下する。従ってシート又は基板８を下
降しながら、抵抗計１１による抵抗値の読み全観測し、
抵抗が急激に低下するｊμｍ間全間知検知ことにより、
シート又は基板８が融＃！ｌに接触した瞬間を精度良く
瞬時に検知することができる。According to the single crystal growth or epitaxial growth apparatus configured in this way, the sheet or substrate 8 is
There is an air layer 12 between the solid gold wires 9 and 10 at the contact point.
When the sheet or substrate 8 descends and comes into contact with the molten metal, the solid gold wires 9 and 10 are connected via the melt 1 and the crucible 2.
Since 13+123i020 has a low resistance in a molten state, the resistance value measured by the resistance meter 11 is reduced by the resistance of the air layer 12, and is significantly lowered. Therefore, while lowering the sheet or substrate 8, read all the resistance values with the resistance meter 11, and
By detecting the entire distance between jμm where the resistance suddenly decreases,
The sheet or substrate 8 is melted! It is possible to instantly detect the moment of contact with l with high precision.
この場合、従来のように、目視又は石英ロッドにより／
−ト又は基板８の接触を観察するための上１°（ＩＸカ
バー１５の開口１６と支持棒７の間の大きな隙間（第１
図）を要しないので、上部力・・−５の開口６と支持棒
７の間（第２図）を密閉状態にして単結晶の育成又はエ
ピタキシャル成長を行なうことが可能である。In this case, as in the past, / by visual inspection or by a quartz rod.
- upper 1° (large gap between the opening 16 of the IX cover 15 and the support rod 7 (the first
(Fig. 2), it is possible to grow a single crystal or epitaxially grow the space between the opening 6 of -5 and the support rod 7 (Fig. 2) in a sealed state.
実施例：
第２図に示すようなエピタキシャル成長装置を使用して
、本発明方法によりＢＳＯ基板上にＢＳＯエピタキシャ
ル層を成長させた。Example: Using an epitaxial growth apparatus as shown in FIG. 2, a BSO epitaxial layer was grown on a BSO substrate by the method of the present invention.
基板８として１３ Ｓ Ｏ基板を用い、支持棒７の下端
に取付け、その一部に白金線９の一端を固定した。A 13 SO substrate was used as the substrate 8, and was attached to the lower end of the support rod 7, and one end of the platinum wire 9 was fixed to a part of the support rod 7.
原木１融液１は約９００°Ｃに保持された。Log 1 melt 1 was maintained at approximately 900°C.
２本の白金線９，１０の終端間の抵抗は、基板８が原料
融液１に接触するまでは、２本の白金線するつぼ十融液
＋空気層→−ＢＳＯ基板の直列抵抗となり、抵抗ｉ１１
１による抵抗値は２０ＭΩ以上を示していたが、基板８
が下降し、融液１に接触した瞬間、空気層１２による最
大の抵抗が無くなった結果、抵抗値は数百にΩまで急激
に低下したので、この瞬間を基板と原料融液の接触開始
点と認め、これより１０〜３０分間浸漬した後、基板８
を融液１より引１−け／へ。基板８−にには所望の厚さ
１〜５μｍのＢＳＯエヒ゛クキ／ヤル成長層が精度良く
得られた。The resistance between the ends of the two platinum wires 9 and 10 is the series resistance of the two platinum wires, melt + air layer → -BSO substrate, until the substrate 8 comes into contact with the raw material melt 1. resistance i11
The resistance value of 1 was more than 20MΩ, but the resistance value of substrate 8
At the moment when the substrate descended and came into contact with the melt 1, the maximum resistance due to the air layer 12 disappeared, and the resistance value rapidly decreased to several hundred ohms. After dipping for 10 to 30 minutes, the substrate 8
is drawn from melt 1 to page 1. On the substrate 8-, a BSO cavity/dial growth layer having a desired thickness of 1 to 5 μm was obtained with high accuracy.
これより、本発明によれば通常の抵抗ｉｔ ｋ使って容
易に観測１」能であり、炉の内部を監視しなくても、基
板が原料融液に接触する瞬間を検知することがｒｉＪ能
であることが分った。From this, according to the present invention, it is possible to easily observe using a normal resistor, and it is possible to detect the moment when the substrate comes into contact with the raw material melt without monitoring the inside of the furnace. It turned out to be.
なお、上述の実施例ではＢＳＯのエピタキシャル成艮の
場合について説明したが、ＢＳＯ単結晶育成の場合にも
全く同様に実施し得ることは明らかである。Incidentally, in the above-mentioned embodiments, the case of epitaxial growth of BSO was explained, but it is clear that the same method can be applied to the case of BSO single crystal growth.
又抵抗を測定する装置は、第２図に示す抵抗計のみに限
定されるものではなく、例えば２本の白金＆Ｑ９．１０
に一定の電圧を印加しておき、シード又は基板と原オニ
・１融澄の接触により流れる電流を検知するものであっ
ても良い。Furthermore, the device for measuring resistance is not limited to the resistance meter shown in Fig. 2, for example, two platinum &Q9.10
It may also be possible to apply a constant voltage to the substrate and detect the current flowing due to contact between the seed or the substrate and the raw oni-1 melt.
（発明の効果）
以」二のように＋１６成された本発明方法は次のような
効果を有する。(Effects of the Invention) The method of the present invention, which has been achieved as described above, has the following effects.
（イｌ １３！ ＋２５１０２０．Ｂｉ １２ＧｅＯ
２０又はその他の酸化物単結晶を育成又（はエピタキシ
ャル成長させる方法において１１棟結晶又は基板が原料
融液に接触したＲ間を、前記種結晶又は前記基板と前記
原料融液との間の抵抗を測定することにより、検知する
だめ、従来のような観１１１１しにくい目視等全心安と
ぜす、抵抗計の指示の変化を読み取るたけであるので、
前記接触の検知が極めて容易で、精度が良く、かつ肉体
的疲労が少ないので、長期間精度の良い観察が可能であ
る。(Il 13! +251020.Bi 12GeO
In the method of growing or (epitaxially growing) 20 or other oxide single crystals, the resistance between the seed crystal or the substrate and the raw material melt is increased between R where the crystal or substrate is in contact with the raw material melt. By measuring, you can simply read the change in the resistance meter's indication, without having to detect it or visually inspecting it, which is difficult to do in the past.
Since the contact detection is extremely easy, highly accurate, and requires little physical fatigue, long-term, highly accurate observation is possible.
（ロ）抵抗測定のためのリート線（例、２本の白金線）
を取出す口を炉に設けるたけて良いため、炉全密閉（〜
だ状態で使用できるので、炉内の熱の放散が小なく、か
つ炉内の温度分布が外気の影響を受けず、規定の温度分
布に保持し易い。(b) Riet wire for resistance measurement (e.g., two platinum wires)
The furnace can be completely sealed (~
Since it can be used in the open state, heat dissipation inside the furnace is not small, and the temperature distribution inside the furnace is not affected by outside air, making it easy to maintain a specified temperature distribution.
シ］ リード線（例、白金線）、るつぼ、原オー１融散
の抵抗値の経時変化は、殆んど無視できる程度に僅かで
あるから、経時変化による測定精度の劣化は非常に小さ
いので、測定装置４の寿命が非常に長い。C] Changes over time in the resistance values of the lead wire (e.g., platinum wire), crucible, and original O1 melt are negligible, so the deterioration in measurement accuracy due to changes over time is extremely small. , the life of the measuring device 4 is very long.
第１商は従来の単結晶育成装置又ｄ：エビクキシャル成
長装置の例を示す縦断伯ｊ図である。
第２図は本発明方法の実施例を説り」１″るための縦断
面図である。
１・原Ｆｌ醐）液、２・・るつは、３・・・結晶育Ｊ戊
炉又はエビクキ／キル炉、４・・・ヒーター、５．１５
・・」−音ＩＳカバー、６．１６・・・ｌ１Ｐ４ Ｄ、
７・・・支持棒、８・・（耳支綻ｉ晶（７−ド）又は基
板、９．１０・・白金線、１１ 抵抗泪、１２・空気
層。
″７１関The first quotient is a vertical sectional diagram showing an example of a conventional single crystal growth apparatus or d: eviaxial growth apparatus. Fig. 2 is a vertical cross-sectional view for explaining an embodiment of the method of the present invention. Ebikuki/Kill Furnace, 4...Heater, 5.15
..."-Sound IS Cover, 6.16...l1P4 D,
7...Support rod, 8...(ear split i crystal (7-board) or substrate, 9.10...platinum wire, 11. resistance layer, 12. air layer. ``71 section
Claims (1)
０又はその他の酸化物単結晶を育成又はエピタキシャル
成長させる方法において、イΦ結晶又は基板が原料融液
に接触した瞬間を、前記種結晶又は前記基板と前配原刺
融敵との間の抵抗を測定することにより、検知すること
を特徴とする種結晶又は基板の接触方法。(υ J3+ 1251020. Bl 126eo2
In the method of growing or epitaxially growing a single crystal of 0 or other oxides, the moment when the Φ crystal or the substrate comes into contact with the raw material melt, the resistance between the seed crystal or the substrate and the pre-distribution material is A method of contacting a seed crystal or a substrate, characterized by detecting by measuring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17204082A JPS5957984A (en) | 1982-09-29 | 1982-09-29 | Method for contacting seed crystal or substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17204082A JPS5957984A (en) | 1982-09-29 | 1982-09-29 | Method for contacting seed crystal or substrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5957984A true JPS5957984A (en) | 1984-04-03 |
Family
ID=15934409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17204082A Pending JPS5957984A (en) | 1982-09-29 | 1982-09-29 | Method for contacting seed crystal or substrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5957984A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002092885A1 (en) * | 2001-05-15 | 2002-11-21 | Memc Electronic Materials, Inc. | Electrically conductive crystal seed chuck assembly |
| CN107523869A (en) * | 2017-09-21 | 2017-12-29 | 浙江晶盛机电股份有限公司 | A kind of single crystal growing furnace can lift water cooling heat shield arrangement |
-
1982
- 1982-09-29 JP JP17204082A patent/JPS5957984A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002092885A1 (en) * | 2001-05-15 | 2002-11-21 | Memc Electronic Materials, Inc. | Electrically conductive crystal seed chuck assembly |
| CN107523869A (en) * | 2017-09-21 | 2017-12-29 | 浙江晶盛机电股份有限公司 | A kind of single crystal growing furnace can lift water cooling heat shield arrangement |
| CN107523869B (en) * | 2017-09-21 | 2024-03-05 | 浙江晶盛机电股份有限公司 | Single crystal furnace device capable of lifting water-cooling heat shield |
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