JPH05339090A - Method for growing single crystal - Google Patents
Method for growing single crystalInfo
- Publication number
- JPH05339090A JPH05339090A JP14949792A JP14949792A JPH05339090A JP H05339090 A JPH05339090 A JP H05339090A JP 14949792 A JP14949792 A JP 14949792A JP 14949792 A JP14949792 A JP 14949792A JP H05339090 A JPH05339090 A JP H05339090A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- container
- crystal
- melted
- polycrystalline
- 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]
【産業上の利用分野】本発明は溶融試料を一方向固化さ
せて単結晶を得る方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for unidirectionally solidifying a molten sample to obtain a single crystal.
【０００２】[0002]
【従来の技術】近年、ロケットなどを利用して無重力状
態を作り出して地上では得られない理想的な結晶を作る
という試みがなされている。この種の無重力実験の際に
は通常、ブリッジマン法と呼ばれる結晶成長法が採用さ
れる。2. Description of the Related Art In recent years, attempts have been made to create an ideal crystal that cannot be obtained on the ground by creating a weightless state using a rocket or the like. A crystal growth method called Bridgman method is usually adopted in this kind of weightlessness experiment.
【０００３】ブリッジマン法は本来、結晶化させようと
する試料を入れた容器を複数のヒ−タから成る適当な温
度勾配をもたせた炉内で動かすか、または容器を固定し
て炉を動かすことによって、容器の一方の端から結晶化
を開始させて他方の端の方へ結晶成長させていく方法で
ある。しかし、この種の実験では打上げ能力の小さい小
型ロケットが使用されため搭載できる実験装置の重量に
は厳しい制約があり、実験装置を簡略化せざるを得な
い。また、結晶成長に適した無重力状態が達成されるの
は約６分間程度でしかないため、その限られた短い時間
の間に試料の溶融開始から冷却・結晶化までの工程を全
て完了させなければならない。The Bridgman method essentially involves moving a container containing a sample to be crystallized in a furnace having a suitable temperature gradient consisting of a plurality of heaters, or fixing the container and moving the furnace. In this way, crystallization is started from one end of the container and the crystal is grown toward the other end. However, since a small rocket with a small launch capability is used in this type of experiment, the weight of the experimental device that can be mounted is severely limited, and the experimental device must be simplified. In addition, the weightless state suitable for crystal growth is achieved for only about 6 minutes, so all the steps from the start of melting the sample to the cooling and crystallization must be completed within the limited short time. I have to.
【０００４】そこで、試料の加熱は一個の均熱ヒ−タを
用いた一様な加熱とし、試料の溶融後ヒ−タを切って容
器の一方の端のみをヘリウムなどの冷却ガスで冷やすこ
とによって試料に温度勾配をもたせて冷却端側から結晶
を成長させていく方法が提案された。この方法によれ
ば、ヒ−タの温度を制御するための装置や試料容器と加
熱炉とを相対移動させるための駆動機構および相対移動
速度の制御装置を省略することができ、実験装置の大幅
な簡略化、軽量化が可能である。また、冷却ガスを用い
て溶融試料を強制的に冷却するので短時間で結晶成長を
完了させることができる。Therefore, the sample is heated uniformly by using one soaking heater, and after the sample is melted, the heater is cut and only one end of the container is cooled with a cooling gas such as helium. Proposed a method of growing a crystal from the cooling end side by giving a temperature gradient to the sample. According to this method, a device for controlling the temperature of the heater, a drive mechanism for relatively moving the sample container and the heating furnace, and a control device for the relative moving speed can be omitted, and thus the experimental apparatus can be greatly improved. It can be simplified and lightened. Further, since the molten sample is forcibly cooled by using the cooling gas, the crystal growth can be completed in a short time.
【０００５】[0005]
【発明が解決しようとする課題】ところが、均熱ヒ−タ
を用いた上述の方法では、ヒ−タを切ったのち容器の一
方の端のみを強制冷却することによって、溶融した試料
を一方の端から先に凝固点以下に冷却してそこから順次
凝固させていき、ある程度までは一方向に結晶を成長さ
せていくことができるが、その結晶成長の途中の時点で
溶融試料のもう一方の端も凝固点以下に冷えてしまうこ
とがある。そうなると両端からの結晶成長となるため、
最終的に得られる結晶の中間部に不純物層や欠陥が生じ
てしまうことになり、所望の大きさで理想的な結晶を得
ることができない。However, in the above-mentioned method using the soaking heater, the molten sample is removed from the molten sample by forcibly cooling only one end of the container after cutting the heater. It is possible to grow the crystal in one direction up to a certain degree by cooling it below the freezing point first and then solidifying it sequentially from the end, but at the point during the crystal growth, the other end of the molten sample May cool below the freezing point. In that case, crystal growth from both ends,
Impurity layers and defects will occur in the intermediate portion of the finally obtained crystal, and an ideal crystal with a desired size cannot be obtained.
【０００６】この発明は上記課題を解消すべく創案され
たものであり、その目的は一様な加熱によって溶融させ
た試料をその一方の端から順次結晶化させていって確実
にもう一方の端で結晶化を完了させることのできる結晶
成長法を提供することにある。The present invention was devised in order to solve the above-mentioned problems, and its purpose is to successively crystallize a sample melted by uniform heating from one end thereof to ensure the other end. The purpose of the present invention is to provide a crystal growth method capable of completing crystallization.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するため
にこの発明の結晶成長法においては、多結晶試料を封入
した容器をその一方の端に高輻射率材を配した状態で周
囲から加熱し、当該試料が溶融したのち加熱を止め、そ
の溶融した試料を当該容器のもう一方の端から冷却して
結晶化させていく。In order to achieve the above object, in the crystal growth method of the present invention, a container enclosing a polycrystalline sample is heated from the surroundings with a high emissivity material arranged at one end thereof. Then, after the sample is melted, heating is stopped, and the melted sample is cooled from the other end of the container and crystallized.
【０００８】[0008]
【作用】多結晶試料の傍らに高輻射率材を配しておけば
これらを同時に一様に加熱した場合でも一般に多結晶試
料よりも高輻射率材の方がかなり温度が高くなる。多結
晶試料よりも高輻射率材料の方が熱を吸収しやすいから
である。したがって、上記手段のように多結晶試料を封
入した容器をその一方の端に高輻射率材を配した状態で
周囲から加熱すれば、高輻射率材を配していない側より
もこれを配した側の温度を高くした状態で多結晶試料を
加熱することができる。そして試料が溶融したのち加熱
を止め、その溶融した試料を容器の高輻射率材を配して
いない方の端から冷却すれば、試料の両端間の温度勾配
を高くとることができるので、一方の端からもう一方の
端へ確実に一方向に結晶化が進行していく。When a high emissivity material is arranged beside the polycrystalline sample, the high emissivity material generally has a considerably higher temperature than the polycrystalline sample even when they are heated uniformly at the same time. This is because the high emissivity material absorbs heat more easily than the polycrystalline sample. Therefore, if the container in which the polycrystalline sample is sealed as in the above means is heated from the surroundings with the high emissivity material being arranged at one end of the container, the container is placed more than the side without the high emissivity material. The polycrystalline sample can be heated with the temperature on the heating side increased. Then, after the sample is melted, the heating is stopped, and if the melted sample is cooled from the end of the container where the high emissivity material is not arranged, the temperature gradient between both ends of the sample can be made high. Crystallization surely proceeds in one direction from one end to the other end.
【０００９】[0009]
【実施例】図１にこの発明の方法によって単結晶を製造
するための装置の概念図を示す。DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows a conceptual diagram of an apparatus for producing a single crystal by the method of the present invention.
【００１０】同図において、１は試料容器である石英ア
ンプルであり、石英アンプル１の周囲にはコイル型の均
熱ヒ−タ２が設けられている。石英アンプル１は均熱ヒ
−タ２と同軸的に設けられた円筒状のガラス管３と、ガ
ラス管３の途中を閉塞しこの石英アンプル１の結晶成長
室の底を構成する隔壁４と、ガラス管３内に多結晶試料
６を入れた後にこれを密封するためのカップ状の内蓋５
とからなる。隔壁４並びに内蓋５の材質はガラス管３と
同質で、隔壁４は多結晶試料６を入れる前に、内蓋５は
多結晶試料６を入れた後にガラス管３に気密に溶接され
たものである。この例では、多結晶試料６と共に種子結
晶７が石英アンプル１内に封入されている。種子結晶７
は多結晶試料６と同じ構成元素の単結晶で、この装置に
よって単結晶を作成するに際し別途作成されたものであ
る。ただしこの場合、図のように多結晶試料６を内蓋５
側に、種子結晶７を隔壁４側に配置しておく必要があ
る。この装置では石英アンプル１内で溶融させた試料を
種子結晶７側から冷却して結晶を成長させていくことに
なるからである。そのためにガラス管３の隔壁４側端部
はヘリウムガスなどの冷却ガス９を導入するための冷却
ガス供給源（図示せず）に接続されている。また、内蓋
５の中には高輻射率材であるカ−ボン材８が詰め込まれ
ている。このカ−ボン材８としてはカ−ボン繊維を編ん
だもの又はカ−ボン棒が使用される。In FIG. 1, reference numeral 1 denotes a quartz ampoule which is a sample container, and a coil-type soaking heater 2 is provided around the quartz ampoule 1. The quartz ampoule 1 has a cylindrical glass tube 3 provided coaxially with the heat equalizing heater 2, and a partition wall 4 which closes the glass tube 3 to form the bottom of the crystal growth chamber of the quartz ampoule 1. A cup-shaped inner lid 5 for sealing the polycrystalline sample 6 after putting it in the glass tube 3
Consists of. The material of the partition wall 4 and the inner lid 5 is the same as that of the glass tube 3, and the partition wall 4 is hermetically welded to the glass tube 3 after putting the polycrystalline sample 6 in the inner lid 5 before putting the polycrystalline sample 6 in it. Is. In this example, a seed crystal 7 together with a polycrystalline sample 6 is enclosed in a quartz ampoule 1. Seed crystal 7
Is a single crystal having the same constituent elements as the polycrystalline sample 6, and was separately prepared when the single crystal was prepared by this apparatus. However, in this case, the polycrystalline sample 6 is placed on the inner lid 5 as shown in the figure.
, It is necessary to arrange the seed crystal 7 on the partition 4 side. This is because in this apparatus, the sample melted in the quartz ampoule 1 is cooled from the seed crystal 7 side to grow the crystal. Therefore, the end of the glass tube 3 on the side of the partition wall 4 is connected to a cooling gas supply source (not shown) for introducing a cooling gas 9 such as helium gas. The inner lid 5 is filled with a carbon material 8 which is a high emissivity material. As the carbon material 8, a knitted carbon fiber or a carbon rod is used.
【００１１】この装置をロケットに搭載して打ち上げる
ことによって無重力状態で結晶成長を行うことができ
る。ただし、通常この種の無重力実験に使用される小型
ロケットの場合、打ち上げから落下の間で結晶成長に適
した無重力状態（１０-5Ｇ程度）になるのは高々６分間
程度である。その短時間の間に、試料の溶融開始から冷
却・結晶化までの工程を全て完了させなければならな
い。したがって、試料が完全に溶融するまでの所用時間
を差し引くと、冷却開始から結晶化完了にあてることの
できる時間は６分間のうちのさらに限られた時間とな
る。この装置は、このように極めて限られた時間内で、
溶融試料を隔壁４側から内蓋５側へ確実に一方向に凝固
させいって結晶化させることを可能とする。By mounting this device on a rocket and launching it, crystals can be grown in a weightless state. However, in the case of a small rocket that is usually used for this kind of weightlessness experiment, the weightlessness suitable for crystal growth (about 10 -5 G) between launch and fall is about 6 minutes at most. In the short time, all the steps from the start of melting the sample to the cooling and crystallization must be completed. Therefore, when the time required until the sample is completely melted is subtracted, the time that can be devoted to the completion of crystallization from the start of cooling is a further limited time of 6 minutes. This device, in this very limited time,
It is possible to surely solidify the molten sample from the partition wall 4 side to the inner lid 5 side in one direction and crystallize it.
【００１２】以下に、ゲルマニウムの単結晶を作成する
場合を例にとり説明する。The case of forming a germanium single crystal will be described below as an example.
【００１３】まず、ゲルマニウムの多結晶試料６と種子
結晶７とを石英アンプル１内に封入し、ロケットの打ち
上げ前から均熱ヒ−タ２に通電して試料を予め８００℃
程度に加熱しておく。ヒ−タ加熱によって、内蓋５から
種子結晶７の多結晶試料６との境目部分にかけての領域
が主に加熱される。First, a germanium polycrystal sample 6 and a seed crystal 7 were enclosed in a quartz ampoule 1, and the soaking heater 2 was energized before the rocket was launched to preheat the sample to 800 ° C.
Heat to a degree. Due to the heater heating, the region from the inner lid 5 to the boundary between the seed crystal 7 and the polycrystalline sample 6 is mainly heated.
【００１４】ロケット打上げ後しばらくの間はヒ−タ温
度を８００℃程度に保ち、無重力状態となる少し手前で
再びヒ−タ温度を上げて１２００℃程度を目標温度とし
て試料を加熱していく。無重力状態となった直後に加熱
温度はゲルマニウムの融点である９３６℃に達し、多結
晶試料６が溶融し始める。その際、多結晶試料６の溶融
は内蓋５に近い方から始まる。内蓋５に詰め込まれてい
るカ−ボン材８の温度が多結晶試料６よりも先にかなり
高温になるからである。The temperature of the heater is kept at about 800 ° C. for a while after the launch of the rocket, the heater temperature is raised again just before the weightless state is reached, and the sample is heated with a target temperature of about 1200 ° C. Immediately after the weightless state, the heating temperature reaches 936 ° C., which is the melting point of germanium, and the polycrystalline sample 6 begins to melt. At that time, the melting of the polycrystalline sample 6 starts from the side closer to the inner lid 5. This is because the temperature of the carbon material 8 packed in the inner lid 5 becomes considerably higher than that of the polycrystalline sample 6.
【００１５】そして、多結晶試料６が完全に溶融したの
ち直ちに均熱ヒ−タ２の通電を絶ち、ガラス管３内への
冷却ガス９の導入を開始する。これにより、溶融試料は
隔壁４を介して種子結晶７側から冷却されて急速に凝固
結晶化していく。溶融試料の温度は内蓋５に近いほど高
温になっているので、種子結晶７側から内蓋５側へ確実
に一方向に結晶が成長していくことになり、理想的な結
晶が得られる。Immediately after the polycrystalline sample 6 is completely melted, the soaking heater 2 is immediately de-energized, and the introduction of the cooling gas 9 into the glass tube 3 is started. As a result, the molten sample is cooled from the seed crystal 7 side through the partition wall 4 and rapidly solidified and crystallized. The temperature of the melted sample becomes higher as it gets closer to the inner lid 5, so that the crystal surely grows in one direction from the seed crystal 7 side to the inner lid 5 side, and an ideal crystal is obtained. .
【００１６】この実施例の方法によれば、溶融試料が凝
固する際の膨脹によって石英アンプル１が割れてしまう
危険性は極めて少ない。これは上述したように溶融試料
が種子結晶７側から内蓋５側へ確実に一方向に凝固し結
晶化していくため、凝固の際の膨脹による体積増加分が
順次結晶成長方向（内蓋５側）へ逃げていくことになる
ためである。これに対しカ−ボン材８がない場合には、
ヒ−タ２を切ると種子結晶７側からの結晶成長の途中で
溶融試料がその外周部からも固まり始める。そのため、
拡径方向への膨脹となり石英アンプル１を割ってしまう
危険性がある。According to the method of this embodiment, the risk of the quartz ampoule 1 cracking due to expansion when the molten sample solidifies is extremely low. This is because, as described above, the melted sample surely solidifies and crystallizes in one direction from the seed crystal 7 side to the inner lid 5 side. This is because it will run away to the side). On the other hand, if there is no carbon material 8,
When the heater 2 is cut, the molten sample begins to solidify also from the outer peripheral portion during the crystal growth from the seed crystal 7 side. for that reason,
There is a risk of expanding the quartz ampoule 1 due to expansion in the diameter expanding direction.
【００１７】[0017]
【発明の効果】以上要するに本発明によれば、試料の両
端間の温度勾配を大きくとることができるので、溶融さ
せた試料をその一方の端から順次結晶化させていって確
実にもう一方の端で結晶化を完了させて理想的な結晶を
得ることができる。In summary, according to the present invention, since the temperature gradient between both ends of the sample can be made large, the melted sample is successively crystallized from one end thereof to ensure the other Crystallization can be completed at the edges to obtain ideal crystals.
【図１】本発明の方法によって単結晶を製造するための
装置構成例を示す概念図である。FIG. 1 is a conceptual diagram showing a structural example of an apparatus for producing a single crystal by the method of the present invention.
１ 石英アンプル（容器） ２ 均熱ヒ−タ ３ ガラス管 ４ 隔壁 ５ 内蓋 ６ 多結晶試料 ７ 種子結晶 ８ カ−ボン材（高輻射率材） ９ 冷却ガス 1 Quartz Ampoule (Container) 2 Soaking Heater 3 Glass Tube 4 Partition 5 Inner Lid 6 Polycrystalline Sample 7 Seed Crystal 8 Carbon Material (High Emissivity Material) 9 Cooling Gas
Claims (1)
端に高輻射率材を配した状態で周囲から加熱し、当該試
料が溶融したのち加熱を止め、その溶融した試料を当該
容器のもう一方の端から冷却して結晶化させるようにし
たことを特徴とする単結晶成長法。1. A container enclosing a polycrystalline sample is heated from the surroundings in a state where a high emissivity material is arranged at one end of the container, the heating is stopped after the sample is melted, and the molten sample is stored in the container. A single crystal growth method characterized by cooling from the other end to crystallize.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04149497A JP3144058B2 (en) | 1992-06-09 | 1992-06-09 | Single crystal growth method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04149497A JP3144058B2 (en) | 1992-06-09 | 1992-06-09 | Single crystal growth method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05339090A true JPH05339090A (en) | 1993-12-21 |
| JP3144058B2 JP3144058B2 (en) | 2001-03-07 |
Family
ID=15476446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP04149497A Expired - Fee Related JP3144058B2 (en) | 1992-06-09 | 1992-06-09 | Single crystal growth method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3144058B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002080291A (en) * | 2000-09-07 | 2002-03-19 | Ishikawajima Harima Heavy Ind Co Ltd | Testing cartridge for space laboratory for manufacturing apparatus of single crystal |
-
1992
- 1992-06-09 JP JP04149497A patent/JP3144058B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002080291A (en) * | 2000-09-07 | 2002-03-19 | Ishikawajima Harima Heavy Ind Co Ltd | Testing cartridge for space laboratory for manufacturing apparatus of single crystal |
| JP4641600B2 (en) * | 2000-09-07 | 2011-03-02 | 株式会社Ｉｈｉエアロスペース | Cartridge for space experiment of single crystal manufacturing equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3144058B2 (en) | 2001-03-07 |
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