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JP5352245B2 - Compound semiconductor single crystal manufacturing method and crystal growth apparatus - Google Patents
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JP5352245B2 - Compound semiconductor single crystal manufacturing method and crystal growth apparatus - Google Patents

Compound semiconductor single crystal manufacturing method and crystal growth apparatus Download PDF

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JP5352245B2
JP5352245B2 JP2008558096A JP2008558096A JP5352245B2 JP 5352245 B2 JP5352245 B2 JP 5352245B2 JP 2008558096 A JP2008558096 A JP 2008558096A JP 2008558096 A JP2008558096 A JP 2008558096A JP 5352245 B2 JP5352245 B2 JP 5352245B2
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聰明 朝日
孝幸 清水
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JX Nippon Mining and Metals Corp
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B27/00Single-crystal growth under a protective fluid
    • C30B27/02Single-crystal growth under a protective fluid by pulling from a melt
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te

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Description

本発明は、化合物半導体単結晶の製造方法および結晶成長装置に関し、特に、液体封止チョクラルスキー(LEC)法により、例えばZnTe系化合物半導体単結晶を製造する方法に適用して有用な技術に関する。   The present invention relates to a method of manufacturing a compound semiconductor single crystal and a crystal growth apparatus, and more particularly to a technique useful when applied to a method of manufacturing, for example, a ZnTe-based compound semiconductor single crystal by a liquid-sealed Czochralski (LEC) method. .

従来、ZnTe系化合物半導体単結晶の成長には、気相成長法や垂直ブリッジマン法(VB法)、垂直温度勾配徐冷法(VGF法)が利用されていた。   Conventionally, a vapor phase growth method, a vertical Bridgman method (VB method), and a vertical temperature gradient annealing method (VGF method) have been used for the growth of a ZnTe-based compound semiconductor single crystal.

ところが、気相成長法によるZnTe系化合物半導体結晶の成長においては成長途中に所望の不純物を添加することは難しく、ZnTe系化合物半導体単結晶の抵抗率を制御するのは困難であるという不具合があった。また、気相成長法ではZnTe結晶の成長速度が著しく遅いために十分な大きさの単結晶を得ることが困難であり、生産性が低いという欠点があった。   However, in the growth of ZnTe-based compound semiconductor crystals by the vapor phase growth method, it is difficult to add a desired impurity during the growth, and it is difficult to control the resistivity of the ZnTe-based compound semiconductor single crystal. It was. Further, the vapor phase growth method has a drawback that the growth rate of ZnTe crystal is extremely slow, so that it is difficult to obtain a sufficiently large single crystal, and the productivity is low.

また、VB法やVGF法によるZnTe系化合物半導体単結晶の製造は、大型の結晶が成長できる反面、成長後に封止材に覆われた状態で室温まで冷却するので、封止剤と成長結晶との熱膨張差により結晶が割れてしまうという事態がしばしば生じた。   In addition, while manufacturing a ZnTe-based compound semiconductor single crystal by the VB method or the VGF method, a large crystal can be grown, but after cooling, it is cooled to room temperature in a state of being covered with a sealing material. Often, the crystal cracked due to the difference in thermal expansion.

そこで、本発明者等は、VB法やVGF法と同様に、結晶成長時に不純物を添加することが可能な液体封止チョクラルスキー法(LEC法)を利用して、大型で良質なZnTe系化合物半導体単結晶を成長させる技術を提案している(例えば、特許文献1)。   Therefore, the present inventors use a liquid-sealed Czochralski method (LEC method) in which impurities can be added during crystal growth, like the VB method and the VGF method, to provide a large and high-quality ZnTe system. A technique for growing a compound semiconductor single crystal has been proposed (for example, Patent Document 1).

図5は、LEC法に用いられる従来の結晶成長装置の概略構成図である。
結晶成長装置100’は、密閉可能な高圧容器1と、有底円筒状したpBN製の外ルツボ8と、底部に外ルツボ8との連通孔を有するpB製の内ルツボ6と、内ルツボ6に収容された原料融液12の上方に昇降自在に設けられ、下端部に種結晶保持部を有する結晶引き上げ軸4と、高圧容器1と同心円状に配置され、外ルツボ8および内ルツボ6に収容された原料12を加熱溶融する多段型加熱ヒータ3と、を備えて構成される。
FIG. 5 is a schematic configuration diagram of a conventional crystal growth apparatus used in the LEC method.
The crystal growth apparatus 100 ′ includes a hermetically sealed high-pressure vessel 1, a bottomed cylindrical pBN outer crucible 8, a pB inner crucible 6 having a communication hole with the outer crucible 8 at the bottom, and an inner crucible 6. The crystal pulling shaft 4 having a seed crystal holding portion at the lower end and the high pressure vessel 1 are arranged concentrically with the lower portion of the raw material melt 12 accommodated in the outer crucible 8 and the inner crucible 6. And a multistage heater 3 that heats and melts the contained raw material 12.

また、高圧容器1の中央部には回転軸7が配置され、回転軸7の上端には外ルツボホルダ5が載置される。外ルツボ8は、例えば、この外ルツボホルダ5に嵌合された状態で保持される。一方、内ルツボ6は、内ルツボホルダ2に保持され、内ルツボホルダ2は内ルツボ6が外ルツボ8の内側となるように配置される。例えば、内ルツボホルダ2は、一端に高圧容器1と係合されるフランジ2aを有するとともに、内壁に内ルツボ6を保持するための係合部2bを有し、フランジ2aを高圧容器1の天板にボトル止めされることにより固定される。   A rotating shaft 7 is disposed at the center of the high-pressure vessel 1, and an outer crucible holder 5 is placed on the upper end of the rotating shaft 7. The outer crucible 8 is held in a state of being fitted to the outer crucible holder 5, for example. On the other hand, the inner crucible 6 is held by the inner crucible holder 2, and the inner crucible holder 2 is arranged so that the inner crucible 6 is inside the outer crucible 8. For example, the inner crucible holder 2 has a flange 2 a that is engaged with the high-pressure vessel 1 at one end, and an engagement portion 2 b that holds the inner crucible 6 on the inner wall, and the flange 2 a is a top plate of the high-pressure vessel 1. It is fixed by being bottled.

また、結晶引き上げ軸4は高圧容器1外に配置された駆動部(図示しない)に連結され回転引き上げ機構を構成する。回転軸7は高圧容器1外に配置された駆動部(図示しない)に連結されルツボ回転機構を構成するとともに、外ルツボホルダ5の昇降機構を構成する。なお、結晶引き上げ軸4および回転軸7の回転並びに昇降移動の運動は、それぞれ独立に設定・制御される。   Further, the crystal pulling shaft 4 is connected to a drive unit (not shown) disposed outside the high-pressure vessel 1 to constitute a rotary pulling mechanism. The rotating shaft 7 is connected to a drive unit (not shown) disposed outside the high-pressure vessel 1 to constitute a crucible rotating mechanism and to constitute an elevating mechanism for the outer crucible holder 5. Note that the rotation of the crystal pulling shaft 4 and the rotating shaft 7 and the movement of the lifting and lowering movement are independently set and controlled.

図6A〜図6Cは、図5に示す結晶成長装置の原料収容部(ルツボ周辺)の拡大図であり、LEC法による結晶成長の過程を示している。   6A to 6C are enlarged views of the raw material container (around the crucible) of the crystal growth apparatus shown in FIG. 5, and show the process of crystal growth by the LEC method.

すなわち、LEC法ではまず、内ルツボ6および外ルツボ8に原料12を入れ、その表面を封止剤11で覆った状態で加熱ヒータ3により原料12を融解し、融解した状態で一定時間保持した後、種結晶9を原料融液の表面に接触させる(図6A)。   That is, in the LEC method, first, the raw material 12 is put in the inner crucible 6 and the outer crucible 8, and the raw material 12 is melted by the heater 3 in a state where the surface is covered with the sealant 11, and the melted state is held for a certain time. Thereafter, the seed crystal 9 is brought into contact with the surface of the raw material melt (FIG. 6A).

その後、結晶引き上げ軸4を回転させながら引き上げ、結晶の肩部・胴体部を形成する(図6B)。このとき、成長結晶13の胴体部の直径は内ルツボ6の内径と略同一となる。次いで、結晶成長後は、結晶引き上げ軸4を上昇させて成長結晶13を引き上げ、所定の時間だけ冷却する(図6C)。   Thereafter, the crystal pulling shaft 4 is rotated to form a shoulder portion / body portion of the crystal (FIG. 6B). At this time, the diameter of the body portion of the growth crystal 13 is substantially the same as the inner diameter of the inner crucible 6. Next, after the crystal growth, the crystal pulling shaft 4 is raised to pull the growth crystal 13 and cooled for a predetermined time (FIG. 6C).

特許文献1によれば、図5に示す結晶成長装置100’を用いて、図6A〜図6Cに示すLEC法を利用することで、大型のZnTe系化合物半導体単結晶を成長させることが可能となっている。
特開2004−99333号公報
According to Patent Document 1, it is possible to grow a large ZnTe-based compound semiconductor single crystal by using the LEC method shown in FIGS. 6A to 6C using the crystal growth apparatus 100 ′ shown in FIG. It has become.
JP 2004-99333 A

しかしながら、上記先願技術を利用してZnTe単結晶を成長させた場合、結晶成長装置の性能(例えば、加熱ヒータの周方向の均一性)によっては単結晶歩留まりが変動することがあり、安定して良質なZnTe単結晶を成長させることは困難であることが判明した。具体的には、(110)と(100)のZnTe単結晶を成長させた場合に、成長結晶中の単結晶が90%以上となることもあれば、全く単結晶とならないこともあった。   However, when a ZnTe single crystal is grown using the prior application technique, the yield of the single crystal may fluctuate depending on the performance of the crystal growth apparatus (for example, the uniformity in the circumferential direction of the heater). It has been found that it is difficult to grow a high quality ZnTe single crystal. Specifically, when (110) and (100) ZnTe single crystals are grown, the single crystals in the grown crystals may be 90% or more, or may not be single crystals at all.

本発明は、LEC法を利用した結晶成長に適用できる技術であって、大型のZnTe系化合物半導体単結晶を歩留まりよく製造できる化合物半導体単結晶の製造方法および結晶成長装置を提供することを目的とする。   The present invention is a technique applicable to crystal growth utilizing the LEC method, and an object thereof is to provide a compound semiconductor single crystal manufacturing method and a crystal growth apparatus capable of manufacturing a large ZnTe-based compound semiconductor single crystal with high yield. To do.

本発明は、上記目的を達成するために、有底円筒形の第1のルツボと、該第1のルツボの内側に配置され底部に前記第1のルツボとの連通孔を設けた第2のルツボと、から構成された原料融液収容部に、半導体原料と封止剤を収容し、前記原料収容部を加熱して原料を溶融させ、この状態で前記原料融液表面に種結晶を接触させて、該種結晶を引き上げながら結晶成長させる液体封止チョクラルスキー法による化合物半導体単結晶の製造方法であって、前記第1のルツボと前記第2のルツボを、共に6rpm以上10rpm以下の同一回転数で同一周方向に回転させるとともに、結晶成長に伴う原料融液の減少に合わせて、前記第1のルツボを前記第2のルツボに対して上昇させながら結晶成長を行うことを特徴とする。 In order to achieve the above object, the present invention provides a second crucible having a bottomed cylindrical shape, and a second crucible disposed inside the first crucible and provided with a communication hole for the first crucible at the bottom. A raw material melt containing part composed of a crucible contains a semiconductor raw material and a sealant, and the raw material containing part is heated to melt the raw material, and in this state, the seed crystal contacts the surface of the raw material melt A compound semiconductor single crystal manufacturing method by a liquid-sealed Czochralski method in which the seed crystal is grown while pulling up the seed crystal, wherein both the first crucible and the second crucible are 6 rpm or more and 10 rpm or less. characterized Rutotomoni rotate in the same circumferential direction at the same rotational speed, in accordance with the decrease of the raw material melt by crystal growth, the crystal growth is performed while increasing the first crucible to the second crucible And

上述した化合物半導体単結晶の製造方法は、例えば、密閉可能な高圧容器と、前記高圧容器の中央部に回転可能かつ昇降可能に配置された第1のルツボと、前記第1のルツボの内側に配置され、底部に前記第1のルツボとの連通孔を有する第2のルツボと、前記第2のルツボに収容された原料融液の上方に昇降自在に設けられ、下端部に種結晶保持部を有する結晶引き上げ軸と、前記高圧容器と同心円状に配置され、前記第1のルツボおよび第2のルツボに収容された原料を加熱溶融する加熱ヒータと、前記第1のルツボまたは前記第2のルツボの何れかを回転駆動する回転駆動手段と、前記第1のルツボの昇降を制御する制御手段と、を備えた結晶成長装置において、前記第1のルツボまたは前記第2のルツボの一方は前記回転駆動手段によって回転駆動され、他方は前記一方のルツボの回転動作に連動して回転するように構成され、前記制御手段は、前記第1のルツボが、前記第2のルツボに対し、結晶成長に伴う原料融液の減少に合わせて上昇するよう制御するようにしたことを特徴とする結晶成長装置を利用することで実現される。 Production method of the above-mentioned compound semiconductor single crystal, for example, a dense closed possible high pressure vessel, a first crucible which is rotatably and vertically movably disposed in a central portion of the high pressure vessel, the inside of the first crucible And a second crucible having a communication hole with the first crucible at the bottom and a material crucible accommodated in the second crucible are provided so as to be movable up and down, and a seed crystal is held at the lower end. A crystal pulling shaft having a portion, a heater arranged concentrically with the high-pressure vessel, for heating and melting the raw materials contained in the first crucible and the second crucible, the first crucible or the second crucible One of the first crucible and the second crucible is a crystal growth apparatus comprising: a rotation driving unit that rotationally drives any one of the crucibles; and a control unit that controls raising and lowering of the first crucible. In the rotation drive means Is rotated I and the other is configured to rotate in conjunction with rotation of the one of the crucible, said control means, said first crucible, relative to the second crucible, by crystal growth is realized by utilizing the crystal growth apparatus is characterized in that the so that controls so as to increase in accordance with the decrease of the raw material melt.

これにより、加熱ヒータの周方向の温度が十分に均一でない場合であっても、加熱溶融された原料融液の温度差を低減させることができる。   Thereby, even if it is a case where the temperature of the circumferential direction of a heater is not sufficiently uniform, the temperature difference of the raw material melt melted by heating can be reduced.

なお、第1のルツボと第2のルツボが連動するための伝達機構は特に限定しないが、例えば、第1のルツボと第2のルツボの一方に爪(凸部)、他方に爪(凸部)または爪受け(凹部)を設けたり、一方に歯車、他方に歯止めを設けたりすることで、容易に連動させることができる。   The transmission mechanism for interlocking the first crucible and the second crucible is not particularly limited. For example, one of the first crucible and the second crucible is a nail (convex portion), and the other is a nail (convex portion). ) Or a claw support (concave portion), or a gear on one side and a pawl on the other, can be easily interlocked.

以下に、本発明を完成するに至った経緯について説明する。
まず、本発明者等が、上記特許文献1に記載の技術を利用してZnTe単結晶を成長させたところ、単結晶歩留まりが変動し、安定して良質なZnTe単結晶を成長させることは困難であることが判明した。
Below, the background that led to the completion of the present invention will be described.
First, when the present inventors grew a ZnTe single crystal using the technique described in Patent Document 1, it was difficult to stably grow a good quality ZnTe single crystal because the single crystal yield fluctuated. It turned out to be.

そして、ZnTe単結晶の単結晶歩留まりが変動する原因を突き止めるべく、内ルツボ内の原料融液の温度を測定したところ、周方向で4℃程度の温度差が生じており均一となっていないことが判明した。   Then, in order to find out the cause of the fluctuation of the single crystal yield of the ZnTe single crystal, the temperature of the raw material melt in the inner crucible was measured, and a temperature difference of about 4 ° C. occurred in the circumferential direction, and was not uniform. There was found.

この原料融液の温度差が生じる要因としては、(1)加熱ヒータの周方向の温度ばらつき、(2)高圧容器内のガスの流れの不均一、(3)内ルツボ、外ルツボ、加熱ヒータの位置関係(時崩れなど)などがあるが、特に、(1)加熱ヒータの周方向の温度ばらつきは、通常使われるヒータの足(裾)部分で±15℃、中央部でも±10℃となっているため、原料融液の温度差に最も大きく影響していると考えられた。   Factors causing the temperature difference of the raw material melt include (1) temperature variation in the circumferential direction of the heater, (2) non-uniform gas flow in the high-pressure vessel, (3) inner crucible, outer crucible, heater In particular, (1) The temperature variation in the circumferential direction of the heater is ± 15 ° C at the foot (hem) part of the heater normally used, and ± 10 ° C at the center. Therefore, it was considered that the temperature difference of the raw material melt had the largest influence.

そこで、原料融液を溶融させる際に、加熱ヒータの周方向の温度ばらつきの影響を低減させ、原料融液の温度差が生じないようにする手法について検討し、ルツボを回転させることで原料融液の周方向の温度を均一化できるのではないかと考えた。また、外ルツボ(外ルツボホルダ)はもともと回転軸に載置されているので、外ルツボの回転を有効に利用する方法を考えた。   Therefore, when melting the raw material melt, we studied a method to reduce the effect of temperature variations in the circumferential direction of the heater and prevent the temperature difference of the raw material melt from occurring, and by rotating the crucible, We thought that the temperature in the circumferential direction of the liquid could be made uniform. Further, since the outer crucible (outer crucible holder) is originally placed on the rotating shaft, a method of effectively using the rotation of the outer crucible was considered.

そして、外ルツボを回転させたときの原料融液の温度差を調べたところ、回転させない場合に比べると原料融液の温度差は低減された。しかしながら、それでも3℃程度の温度差は残ってしまい、ZnTe単結晶の単結晶歩留まりを向上させるには不十分であると考えられた。   And when the temperature difference of the raw material melt when the outer crucible was rotated was examined, the temperature difference of the raw material melt was reduced as compared with the case where the outer crucible was not rotated. However, a temperature difference of about 3 ° C. still remains, which is considered insufficient to improve the single crystal yield of the ZnTe single crystal.

さらに、結晶成長装置が複雑化するのを回避するため、外ルツボの回転を利用して内ルツボも回転させたところ(つまり、外ルツボと内ルツボの回転数は同一となる)、原料融液の温度差を1℃以下に低減することができ、単結晶歩留まりを格段に改善することもできた。   Furthermore, in order to avoid complication of the crystal growth apparatus, when the inner crucible is rotated using the rotation of the outer crucible (that is, the rotation speed of the outer crucible and the inner crucible becomes the same), the raw material melt The temperature difference of 1 ° C. could be reduced to 1 ° C. or less, and the single crystal yield could be remarkably improved.

具体的には、回転数を5rpm以上にすることで温度差を1℃以下に低減することができた。一方、回転数が20rpmを越えると原料融液の流れが生じてしまい、好ましくないことがわかった。   Specifically, the temperature difference could be reduced to 1 ° C. or less by setting the rotation speed to 5 rpm or more. On the other hand, it was found that when the rotational speed exceeds 20 rpm, the raw material melt flows, which is not preferable.

また、回転数を6−10rpmの範囲としたときは、原料融液の温度差を1℃以下に低減できる上、成長結晶中の単結晶は常に70%以上となり、単結晶歩留まりを安定させることができた。   Moreover, when the rotational speed is in the range of 6-10 rpm, the temperature difference of the raw material melt can be reduced to 1 ° C. or less, and the single crystal in the grown crystal is always 70% or more, and the single crystal yield is stabilized. I was able to.

なお、内ルツボだけを回転させた場合も同様の効果が得られる可能性がある。ただし、内ルツボだけを回転させるためには、内ルツボを回転駆動させるための駆動手段を新規に設ける必要があり、結晶成長装置の複雑化につながる点で望ましくないと考えられる。   Note that the same effect may be obtained when only the inner crucible is rotated. However, in order to rotate only the inner crucible, it is necessary to newly provide a driving means for rotationally driving the inner crucible, which is undesirable from the viewpoint of complicating the crystal growth apparatus.

本発明は、上記知見に基づいて完成されたもので、液体封止チョクラルスキー法による化合物半導体単結晶の製造方法において、外ルツボと内ルツボを、所定の回転数で周方向に回転させながら結晶成長を行うことを特徴とするものである。   The present invention has been completed on the basis of the above knowledge, and in a method for producing a compound semiconductor single crystal by a liquid-sealed Czochralski method, while rotating an outer crucible and an inner crucible in a circumferential direction at a predetermined rotational speed. It is characterized by crystal growth.

本発明によれば、有底円筒形の第1のルツボと、該第1のルツボの内側に配置され底部に前記第1のルツボとの連通孔を設けた第2のルツボと、から構成された原料融液収容部に、半導体原料と封止剤を収容し、前記原料収容部を加熱して原料を溶融させ、この状態で前記原料融液表面に種結晶を接触させて、該種結晶を引き上げながら結晶成長させる液体封止チョクラルスキー法による化合物半導体単結晶の製造方法において、前記第1のルツボと前記第2のルツボを、所定の回転数で周方向に回転させながら結晶成長を行うようにしたので、内ルツボに収容された原料融液に周方向の温度差が生じるのを効率よく低減できる。その結果、ZnTe系化合物半導体単結晶の単結晶化率を向上できるとともに、単結晶歩留まりを安定させることができる。   According to the present invention, the first crucible having a bottomed cylindrical shape and a second crucible disposed inside the first crucible and provided with a communication hole with the first crucible at the bottom are configured. In the raw material melt container, the semiconductor raw material and the sealant are accommodated, the raw material container is heated to melt the raw material, and in this state, the seed crystal is brought into contact with the surface of the raw material melt, In the method of manufacturing a compound semiconductor single crystal by the liquid-sealed Czochralski method in which crystal growth is performed while pulling up the crystal, crystal growth is performed while rotating the first crucible and the second crucible in a circumferential direction at a predetermined rotational speed. Since it performed, it can reduce efficiently that the temperature difference of the circumferential direction arises in the raw material melt accommodated in the inner crucible. As a result, the single crystallization rate of the ZnTe-based compound semiconductor single crystal can be improved, and the single crystal yield can be stabilized.

また、加熱ヒータ自身に周方向の温度ばらつきがあっても、原料融液の温度差を小さくできるので、均一性の良い加熱ヒータに取り替える必要はなく、装置改良に伴うコストを最小限に抑えることができる。
更に、結晶成長に伴う原料融液の減少に合わせて第1のルツボが上昇することにより、第2のルツボが原料融液に所定深さで浸漬された状態が維持されるので、原料融液の温度差が小さくなった状態を維持することができる。
In addition, even if the heater itself has temperature variations in the circumferential direction, the temperature difference of the raw material melt can be reduced, so there is no need to replace it with a heater with good uniformity, minimizing costs associated with equipment improvements. Can do.
Furthermore, since the first crucible rises with the decrease in the raw material melt accompanying the crystal growth, the second crucible is maintained immersed in the raw material melt at a predetermined depth. It is possible to maintain a state in which the temperature difference is small.

本実施形態に使用される結晶成長装置の概略構成図である。It is a schematic block diagram of the crystal growth apparatus used for this embodiment. 内ルツボホルダ2と外ルツボホルダ5の係合状態の一例を示す上面図である。FIG. 6 is a top view showing an example of an engagement state between the inner crucible holder 2 and the outer crucible holder 5. 本実施形態に係る結晶成長装置(図1)を用いたときの内ルツボ6内の原料融液について、周方向の温度を測定した結果である。It is the result of having measured the temperature of the circumferential direction about the raw material melt in the inner crucible 6 when using the crystal growth apparatus (FIG. 1) which concerns on this embodiment. 従来の結晶成長装置(図5)を用いたときの内ルツボ6内の原料融液について、周方向の温度を測定した結果である。It is the result of having measured the temperature of the circumferential direction about the raw material melt in the inner crucible 6 when using the conventional crystal growth apparatus (FIG. 5). 従来の結晶成長装置の概略構成図である。It is a schematic block diagram of the conventional crystal growth apparatus. LEC法による結晶成長過程を示す説明図である。It is explanatory drawing which shows the crystal growth process by LEC method. LEC法による結晶成長過程を示す説明図である。It is explanatory drawing which shows the crystal growth process by LEC method. LEC法による結晶成長過程を示す説明図である。It is explanatory drawing which shows the crystal growth process by LEC method.

符号の説明Explanation of symbols

1 高圧容器
2 内ルツボホルダ
2aフランジ
2b内ルツボ保持部
21爪(係合片)
3 多段型加熱ヒータ
4 結晶引き上げ軸
5 外ルツボホルダ
51爪(係合片)
6 内ルツボ(第2のルツボ)
7 回転軸
8 外ルツボ(第1のルツボ)
9 種結晶
10 ベアリング
11 封止剤
12 原料融液
100結晶成長装置
DESCRIPTION OF SYMBOLS 1 High pressure vessel 2 Inner crucible holder 2a flange 2b Crucible holding part 21 Claw (engagement piece)
3 Multi-stage heater 4 Crystal pulling shaft 5 Outer crucible holder 51 Claw (engagement piece)
6 Inner crucible (second crucible)
7 Rotating shaft 8 Outer crucible (first crucible)
9 Seed crystal 10 Bearing 11 Sealant 12 Raw material melt 100 Crystal growth device

以下、本発明の好適な実施の形態を図面に基づいて説明する。
図1は本実施形態に係る結晶成長装置の概略構成図である。本実施形態に示す結晶成長装置100は、図5に示す従来の結晶成長装置100’と内ルツボホルダ2の設置方法が異なっており、外ルツボホルダ5が回転することに連動して内ルツボホルダ2も回転するようになっている。なお、ルツボの回転機構の詳細については後述する。
DESCRIPTION OF EXEMPLARY EMBODIMENTS Hereinafter, preferred embodiments of the invention will be described with reference to the drawings.
FIG. 1 is a schematic configuration diagram of a crystal growth apparatus according to this embodiment. The crystal growth apparatus 100 shown in the present embodiment is different from the conventional crystal growth apparatus 100 ′ shown in FIG. 5 in the installation method of the inner crucible holder 2, and the inner crucible holder 2 rotates in conjunction with the rotation of the outer crucible holder 5. It is supposed to be. The details of the crucible rotation mechanism will be described later.

結晶成長装置100は、密閉可能な高圧容器1と、有底円筒状したpBN製の外ルツボ8と、底部を開放されて外ルツボ8と連通されたpB製の内ルツボ6と、内ルツボ6に収容された原料融液12の上方に昇降自在に設けられ、下端部に種結晶保持部を有する結晶引き上げ軸4と、高圧容器1と同心円状に配置され、外ルツボ8および内ルツボ6に収容された原料12を加熱溶融する多段型加熱ヒータ3と、を備えて構成される。   The crystal growth apparatus 100 includes a hermetically sealed high-pressure vessel 1, a bottomed cylindrical outer crucible 8 made of pBN, an inner crucible 6 made of pB open at the bottom and communicated with the outer crucible 8, and an inner crucible 6. The crystal pulling shaft 4 having a seed crystal holding portion at the lower end and the high pressure vessel 1 are arranged concentrically with the lower portion of the raw material melt 12 accommodated in the outer crucible 8 and the inner crucible 6. And a multistage heater 3 that heats and melts the contained raw material 12.

また、高圧容器1の中央部には回転軸7が配置され、回転軸7の上端には外ルツボホルダ5が載置される。外ルツボ8は、例えば、この外ルツボホルダ5に嵌合された状態で保持される。一方、内ルツボ6は、内ルツボホルダ2に保持され、内ルツボホルダ2は内ルツボ6が外ルツボ8の内側となるように配置される。   A rotating shaft 7 is disposed at the center of the high-pressure vessel 1, and an outer crucible holder 5 is placed on the upper end of the rotating shaft 7. The outer crucible 8 is held in a state of being fitted to the outer crucible holder 5, for example. On the other hand, the inner crucible 6 is held by the inner crucible holder 2, and the inner crucible holder 2 is arranged so that the inner crucible 6 is inside the outer crucible 8.

ここで、内ルツボホルダ2は、一端に高圧容器1と係合されるフランジ2aを有するとともに、内壁に内ルツボ6を保持するための係合部2bを有する。また、高圧容器1の天板には円環状にボールベアリング10が敷き詰められている。内ルツボホルダ2のフランジ2aの所定部位をベアリング10と係合させることで、内ルツボホルダ2は高圧容器1に回転可能に取り付けられる。   Here, the inner crucible holder 2 has a flange 2a engaged with the high-pressure vessel 1 at one end and an engaging portion 2b for holding the inner crucible 6 on the inner wall. Further, a ball bearing 10 is laid in an annular shape on the top plate of the high-pressure vessel 1. By engaging a predetermined portion of the flange 2 a of the inner crucible holder 2 with the bearing 10, the inner crucible holder 2 is rotatably attached to the high-pressure vessel 1.

さらに、内ルツボホルダ2は、外ルツボホルダ5の回転動作に連動して回転するように、外ルツボホルダ5と係合されている。すなわち、内ルツボホルダ2と外ルツボホルダ5が連動するための伝達機構が設けられている。   Further, the inner crucible holder 2 is engaged with the outer crucible holder 5 so as to rotate in conjunction with the rotation operation of the outer crucible holder 5. That is, a transmission mechanism for interlocking the inner crucible holder 2 and the outer crucible holder 5 is provided.

図2は、内ルツボホルダ2と外ルツボホルダ5の係合状態の一例を示す上面図である。
図2に示すように、外ルツボホルダ5の外壁面の2箇所には外側に向けて爪51が凸設されており、内ルツボホルダ2の内壁面の2箇所には内側に向けて爪21が凸設されている。図2において、外ルツボホルダ5が反時計回りに回転すると、爪51と爪21が係合状態となり、内ルツボホルダ2も反時計回りに回転することとなる。
FIG. 2 is a top view showing an example of an engaged state of the inner crucible holder 2 and the outer crucible holder 5.
As shown in FIG. 2, claws 51 protrude outwardly at two locations on the outer wall surface of the outer crucible holder 5, and claws 21 protrude toward the inner side at two locations on the inner wall surface of the inner crucible holder 2. It is installed. In FIG. 2, when the outer crucible holder 5 rotates counterclockwise, the claw 51 and the claw 21 are engaged, and the inner crucible holder 2 also rotates counterclockwise.

なお、外ルツボ8は、外ルツボホルダ5に特別な係合手段を用いずに載置されているだけであるが、外ルツボホルダ5の回転に伴って回転する。また、内ルツボ6は、内ルツボホルダ2に設けられた係合部2bにより固着されるので、内ルツボホルダ2の回転に伴い回転することとなる。   The outer crucible 8 is merely placed on the outer crucible holder 5 without using any special engagement means, but rotates with the rotation of the outer crucible holder 5. Further, since the inner crucible 6 is fixed by the engaging portion 2 b provided in the inner crucible holder 2, the inner crucible 6 rotates with the rotation of the inner crucible holder 2.

つまり、内ルツボホルダ2が外ルツボホルダ5の回転動作に連動して回転するということは、内ルツボ6が外ルツボ8の回転動作に連動して回転すると言い換えることができる。このように、本実施形態の結晶成長装置100では、従来から設けられていた回転軸7を利用して、外ルツボ8および内ルツボ6を回転させることができるので、内ルツボ6を回転させる駆動源を新たに設ける等、装置構成が複雑化されることもなく、比較的低コストで外ルツボ8と内ルツボ6を回転させる機構を実現できる。   That is, the fact that the inner crucible holder 2 rotates in conjunction with the rotating operation of the outer crucible holder 5 can be rephrased as the inner crucible 6 rotates in conjunction with the rotating operation of the outer crucible 8. As described above, in the crystal growth apparatus 100 of the present embodiment, the outer crucible 8 and the inner crucible 6 can be rotated by using the rotary shaft 7 provided conventionally, so that the inner crucible 6 is rotated. A mechanism for rotating the outer crucible 8 and the inner crucible 6 can be realized at a relatively low cost without complicating the apparatus configuration, such as providing a new source.

また、結晶引き上げ軸4は高圧容器1外に配置された駆動部(図示しない)に連結され回転引き上げ機構を構成する。回転軸7は高圧容器1外に配置された駆動部(図示しない)に連結されルツボ回転機構を構成するとともに、外ルツボホルダ5の昇降機構を構成する。なお、結晶引き上げ軸4および回転軸7の回転並びに昇降移動の運動は、それぞれ独立に設定・制御される。   Further, the crystal pulling shaft 4 is connected to a drive unit (not shown) disposed outside the high-pressure vessel 1 to constitute a rotary pulling mechanism. The rotating shaft 7 is connected to a drive unit (not shown) disposed outside the high-pressure vessel 1 to constitute a crucible rotating mechanism and to constitute an elevating mechanism for the outer crucible holder 5. Note that the rotation of the crystal pulling shaft 4 and the rotating shaft 7 and the movement of the lifting and lowering movement are independently set and controlled.

図3は、本実施形態に係る結晶成長装置(図1)を用いたときの内ルツボ6内の原料融液について、周方向の温度を測定した結果である。例えば、外ルツボ8と内ルツボ6の両方を回転数5〜10rpmで回転させたときの原料融液の周方向の温度差を示している。具体的には、内ルツボ6の内壁から5mm離れた位置の温度を、周方向に45℃刻みで測定している。   FIG. 3 shows the result of measuring the temperature in the circumferential direction of the raw material melt in the inner crucible 6 when the crystal growth apparatus (FIG. 1) according to the present embodiment is used. For example, the temperature difference in the circumferential direction of the raw material melt when both the outer crucible 8 and the inner crucible 6 are rotated at a rotational speed of 5 to 10 rpm is shown. Specifically, the temperature at a position 5 mm away from the inner wall of the inner crucible 6 is measured in increments of 45 ° C. in the circumferential direction.

図3に示すように、外ルツボ8と内ルツボ6を、回転数5〜20rpmで回転させることで、原料融液の周方向の温度差を1℃以下に制御でき、均一化することができた。例えば、加熱ヒータ3の周方向の温度差が30℃程度の場合には、回転数を上記範囲とすることで効果的に対応することができる。   As shown in FIG. 3, by rotating the outer crucible 8 and the inner crucible 6 at a rotational speed of 5 to 20 rpm, the temperature difference in the circumferential direction of the raw material melt can be controlled to 1 ° C. or less and can be made uniform. It was. For example, when the temperature difference in the circumferential direction of the heater 3 is about 30 ° C., it is possible to effectively cope with the rotation speed within the above range.

図4は、従来の結晶成長装置(図5)を用いたときの内ルツボ6内の原料融液について、周方向の温度を測定した結果である。なお、■の凡例は外ルツボ8も回転させない場合で、▲の凡例は外ルツボ8のみを回転数5rpmで回転させた場合の原料融液の周方向の温度差を示している。   FIG. 4 shows the results of measuring the temperature in the circumferential direction of the raw material melt in the inner crucible 6 when the conventional crystal growth apparatus (FIG. 5) is used. Note that the legend of ■ indicates the case where the outer crucible 8 is not rotated, and the legend of ▲ indicates the temperature difference in the circumferential direction of the raw material melt when only the outer crucible 8 is rotated at a rotational speed of 5 rpm.

図4に示すように、外ルツボ8を回転させた場合は、回転させない場合に比べると原料融液の温度差は低減されることがわかる。ただし、3℃程度の温度差は残ってしまい、外ルツボ8に連動させて内ルツボ6も回転させた場合に比較すると、原料融液の温度差は大きく、ZnTe単結晶の単結晶歩留まりを向上させるには不十分である。   As shown in FIG. 4, it can be seen that when the outer crucible 8 is rotated, the temperature difference of the raw material melt is reduced as compared with the case where the outer crucible 8 is not rotated. However, a temperature difference of about 3 ° C. remains, and the temperature difference of the raw material melt is larger than when the inner crucible 6 is rotated in conjunction with the outer crucible 8 and the single crystal yield of the ZnTe single crystal is improved. It is not enough to make it happen.

上述したように、結晶成長装置100を用いることで、内ルツボ6内の原料融液の温度差を有効に低減させることができ、さらに、LEC法により大型のZnTe系化合物半導体単結晶を歩留まりよく成長させることができる。   As described above, by using the crystal growth apparatus 100, the temperature difference of the raw material melt in the inner crucible 6 can be effectively reduced, and a large ZnTe-based compound semiconductor single crystal can be obtained with a high yield by the LEC method. Can be grown.

次に、結晶成長装置100を用いて、化合物半導体の一例としてZnTe単結晶を製造する方法について具体的に説明する。   Next, a method for manufacturing a ZnTe single crystal as an example of a compound semiconductor using the crystal growth apparatus 100 will be specifically described.

本実施形態では、外ルツボ8として内径100mmφ×高さ100mm×肉厚1mmのpBN製ルツボを使用し、内ルツボ6として内径54mmφ(底部)〜56mmφ(上部)×高さ100mm×肉厚1mmのテーパー構造をしたpBN製ルツボを使用した。このとき、内ルツボ6の側面の傾斜角θは鉛直方向に対して約0.57°となる。   In this embodiment, a pBN crucible having an inner diameter of 100 mmφ × height of 100 mm × thickness of 1 mm is used as the outer crucible 8, and an inner crucible 6 of inner diameter of 54 mmφ (bottom) to 56 mmφ (top) × height of 100 mm × thickness of 1 mm. A pBN crucible having a tapered structure was used. At this time, the inclination angle θ of the side surface of the inner crucible 6 is about 0.57 ° with respect to the vertical direction.

まず、原料として純度6NのZnと6NのTeを、外ルツボ8および内ルツボ内にZnとTeが等モル比となるように合計1.5kg入れ、その上を400gの封止剤(B)11で覆い、封止剤層の厚さが35mmとなるようにした。なお、内ルツボ6は、加熱ヒータ3により原料を融解した後、原料融液の液面から20mmの深さで浸漬した状態となるように保持具で固定した。First, Zn of a purity of 6N and Te of 6N as raw materials are put in a total of 1.5 kg in the outer crucible 8 and the inner crucible so that Zn and Te are in an equimolar ratio, and 400 g of a sealing agent (B 2 It was covered with O 3 ) 11 so that the thickness of the sealant layer was 35 mm. The inner crucible 6 was fixed with a holder so that the raw material was melted by the heater 3 and then immersed at a depth of 20 mm from the surface of the raw material melt.

なお、結晶成長に伴い原料融液は徐々に減少するが、回転軸7の昇降駆動により外ルツボホルダサセプタ5(外ルツボ8)を上昇させることにより内ルツボ6の浸漬状態を制御した。例えば、内ルツボ6が原料融液の液面から10mm〜40mmの範囲で浸漬された状態で保持するようにした。   Although the raw material melt gradually decreases as the crystal grows, the immersion state of the inner crucible 6 was controlled by raising the outer crucible holder susceptor 5 (outer crucible 8) by driving the rotary shaft 7 up and down. For example, the inner crucible 6 is held in a state of being immersed in a range of 10 mm to 40 mm from the liquid surface of the raw material melt.

次に、高圧容器1内を不活性ガス(例えばAr)で満たして所定の圧力となるように調整した。そして、封止剤11で原料12の表面を抑えながら加熱ヒータ3を用いて所定の温度で加熱し、ZnとTeを融解して直接合成させた。   Next, the inside of the high-pressure vessel 1 was filled with an inert gas (for example, Ar) and adjusted so as to have a predetermined pressure. And while suppressing the surface of the raw material 12 with the sealing agent 11, it heated at predetermined temperature using the heater 3, and melt | dissolved Zn and Te directly and synthesize | combined them.

このとき、回転軸7を回転させることで、外ルツボを回転させた。また、外ルツボ8の回転動作に連動して内ルツボ6を同一回転数で回転させた。このように、内ルツボ6および外ルツボ8を同一速度で回転させることで、原料融液12の周方向の温度差を1℃以下とすることができた(例えば、図3)。   At this time, the outer crucible was rotated by rotating the rotating shaft 7. Further, the inner crucible 6 was rotated at the same rotational speed in conjunction with the rotation operation of the outer crucible 8. Thus, by rotating the inner crucible 6 and the outer crucible 8 at the same speed, the temperature difference in the circumferential direction of the raw material melt 12 could be 1 ° C. or less (for example, FIG. 3).

その後、原料を融解した状態で一定時間保持した後、種結晶9を原料融液12の表面に接触させた。ここで、種結晶として結晶方位が(100)の種結晶を使用した。また、種結晶9が分解するのを防止するためにモリブデン製のカバー(図示しない)で種結晶を覆うようにした。   Thereafter, after the raw material was melted and held for a certain time, the seed crystal 9 was brought into contact with the surface of the raw material melt 12. Here, a seed crystal having a crystal orientation of (100) was used as the seed crystal. Further, in order to prevent the seed crystal 9 from being decomposed, the seed crystal was covered with a molybdenum cover (not shown).

そして、結晶引き上げ軸4を1〜2rpmの回転数で回転させ、2.5mm/hの速度で引き上げながら結晶の肩部を形成した。続いて、肩部が形成された後、2.5mm/hの速度で引き上げながら胴体部を形成した。このとき、回転軸7は0〜10rpmで回転させた。   Then, the crystal pulling shaft 4 was rotated at a rotational speed of 1 to 2 rpm, and a shoulder portion of the crystal was formed while pulling up at a speed of 2.5 mm / h. Subsequently, after the shoulder portion was formed, the body portion was formed while being pulled up at a speed of 2.5 mm / h. At this time, the rotating shaft 7 was rotated at 0 to 10 rpm.

以上のようにして、液体封止チョクラルスキー法による結晶成長を行い、結晶成長後に封止剤11から成長結晶を切り離して割れのないZnTe化合物半導体結晶を得た。得られたZnTe化合物半導体結晶は、多結晶や双晶の発生していない極めて良好な単結晶であった。   As described above, crystal growth was performed by the liquid-sealed Czochralski method, and after the crystal growth, the grown crystal was separated from the encapsulant 11 to obtain a ZnTe compound semiconductor crystal having no cracks. The obtained ZnTe compound semiconductor crystal was a very good single crystal free of polycrystals or twins.

また、成長した結晶の大きさは直径54mmφ×長さ60mmであり、従来困難とされていたZnTe系化合物半導体単結晶の大型化を実現することができた。さらに、同じ結晶成長装置を用いて繰り返しZnTe単結晶を成長させたところ、成長結晶中の90%以上は単結晶となり、単結晶歩留まりが格段に向上することが確認できた。   Further, the size of the grown crystal was 54 mmφ × 60 mm in length, and it was possible to realize the enlargement of the ZnTe-based compound semiconductor single crystal, which was conventionally considered difficult. Furthermore, when ZnTe single crystals were repeatedly grown using the same crystal growth apparatus, 90% or more of the grown crystals became single crystals, and it was confirmed that the single crystal yield was greatly improved.

以上本発明者によってなされた発明を実施例に基づき具体的に説明したが、本発明は上記実施例に限定されるものではない。
例えば、上記実施形態では、外ルツボ8と内ルツボ6に爪(凸部)を設けるようにしているが、外ルツボ8と内ルツボ6が連動するための伝達機構はこれに限定されない。例えば、外ルツボ8と内ルツボ6の一方に爪(凸部)、他方に爪受け(凹部)を設けたり、一方に歯車、他方に歯止めを設けたりすることで、容易に連動させることができる。
Although the invention made by the present inventor has been specifically described based on the embodiments, the present invention is not limited to the above embodiments.
For example, in the above embodiment, the outer crucible 8 and the inner crucible 6 are provided with claws (projections), but the transmission mechanism for interlocking the outer crucible 8 and the inner crucible 6 is not limited to this. For example, a claw (convex portion) is provided on one of the outer crucible 8 and the inner crucible 6, a claw receptacle (concave portion) is provided on the other side, a gear is provided on one side, and a pawl is provided on the other side. .

また、上記実施の形態では内ルツボ6の底部を開放して外ルツボ8と連通させるようにしたが、内ルツボ6の底面に所定の大きさの連通孔を一つ形成するようにしてもよいし、連通孔の数は一つに制限されず複数の連通孔を設けるようにしてもよい。   In the above embodiment, the bottom of the inner crucible 6 is opened to communicate with the outer crucible 8, but one communication hole of a predetermined size may be formed on the bottom surface of the inner crucible 6. However, the number of communication holes is not limited to one, and a plurality of communication holes may be provided.

また、内ルツボ6だけを回転させた場合や、外ルツボ8と内ルツボ6の回転数を異ならせた場合でも同様の効果が得られる可能性がある。ただし、内ルツボ6だけを回転させるためには、内ルツボを回転駆動させるための駆動手段を新規に設ける必要があり、結晶成長装置の複雑化・高コスト化につながる虞がある。   In addition, the same effect may be obtained even when only the inner crucible 6 is rotated or when the rotational speeds of the outer crucible 8 and the inner crucible 6 are different. However, in order to rotate only the inner crucible 6, it is necessary to newly provide a driving means for rotationally driving the inner crucible, which may lead to the complexity and cost increase of the crystal growth apparatus.

また、ZnTe単結晶に限らず、ZnTeを含む三元以上のZnTe系化合物半導体単結晶やその他の化合物半導体単結晶の製造においても本発明を適用することにより大型で高品質の化合物半導体単結晶を得ることができる。   In addition, not only ZnTe single crystals but also ternary or higher ZnTe-based compound semiconductor single crystals containing ZnTe and other compound semiconductor single crystals can be applied to produce large and high quality compound semiconductor single crystals. Can be obtained.

Claims (2)

有底円筒形の第1のルツボと、該第1のルツボの内側に配置され底部に前記第1のルツボとの連通孔を設けた第2のルツボと、から構成された原料融液収容部に、半導体原料と封止剤を収容し、前記原料収容部を加熱して原料を溶融させ、この状態で前記原料融液表面に種結晶を接触させて、該種結晶を引き上げながら結晶成長させる液体封止チョクラルスキー法による化合物半導体単結晶の製造方法であって、
前記第1のルツボと前記第2のルツボを、共に6rpm以上10rpm以下の同一回転数で同一周方向に回転させるとともに、
結晶成長に伴う原料融液の減少に合わせて、前記第1のルツボを前記第2のルツボに対して上昇させながら結晶成長を行うことを特徴とする化合物半導体単結晶の製造方法。
A raw material melt container comprising a first cylindrical crucible with a bottom, and a second crucible disposed inside the first crucible and provided with a communication hole with the first crucible at the bottom. Next, the semiconductor raw material and the sealant are accommodated, the raw material accommodating portion is heated to melt the raw material, and in this state, the seed crystal is brought into contact with the surface of the raw material melt, and crystal growth is performed while pulling up the seed crystal. A method for producing a compound semiconductor single crystal by a liquid-sealed Czochralski method,
Said first crucible and said second crucible is rotated in the same circumferential direction together with 10rpm following the same rotational speed or 6rpm Rutotomoni,
A method for producing a compound semiconductor single crystal, wherein crystal growth is performed while raising the first crucible relative to the second crucible in accordance with a decrease in raw material melt accompanying crystal growth .
密閉可能な高圧容器と、
前記高圧容器の中央部に回転可能かつ昇降可能に配置された第1のルツボと、
前記第1のルツボの内側に配置され、底部に前記第1のルツボとの連通孔を有する第2のルツボと、
前記第2のルツボに収容された原料融液の上方に昇降自在に設けられ、下端部に種結晶保持部を有する結晶引き上げ軸と、
前記高圧容器と同心円状に配置され、前記第1のルツボおよび第2のルツボに収容された原料を加熱溶融する加熱ヒータと、
前記第1のルツボまたは前記第2のルツボの何れかを回転駆動する回転駆動手段と、
前記第1のルツボの昇降を制御する制御手段と、
を備えた結晶成長装置において、
前記第1のルツボまたは前記第2のルツボの一方は前記回転駆動手段によって回転駆動され、他方は前記一方のルツボの回転動作に連動して回転するように構成され、
前記制御手段は、前記第1のルツボが、前記第2のルツボに対し、結晶成長に伴う原料融液の減少に合わせて上昇するよう制御することを特徴とする結晶成長装置
A sealable high-pressure vessel;
A first crucible disposed at the center of the high-pressure vessel so as to be rotatable and movable up and down;
A second crucible disposed inside the first crucible and having a communication hole with the first crucible at the bottom;
A crystal pulling shaft provided so as to be movable up and down above the raw material melt contained in the second crucible and having a seed crystal holding portion at the lower end;
A heater arranged concentrically with the high-pressure vessel, for heating and melting the raw materials contained in the first crucible and the second crucible;
Rotation driving means for rotating and driving either the first crucible or the second crucible;
Control means for controlling raising and lowering of the first crucible;
A crystal growth apparatus comprising:
One of the first crucible or the second crucible is rotationally driven by the rotational drive means, and the other is configured to rotate in conjunction with the rotational operation of the one crucible,
The crystal growth apparatus characterized in that the control means controls the first crucible to rise with the decrease in the raw material melt accompanying the crystal growth with respect to the second crucible .
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Citations (3)

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Publication number Priority date Publication date Assignee Title
JPS63282187A (en) * 1987-05-11 1988-11-18 Sumitomo Electric Ind Ltd Method and device for producing single crystal
JP2004099333A (en) * 2002-02-13 2004-04-02 Nikko Materials Co Ltd Method of manufacturing compound semiconductor single crystal
JP2004196591A (en) * 2002-12-18 2004-07-15 Nikko Materials Co Ltd Method of manufacturing compound semiconductor single crystal and crystal growth system

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63282187A (en) * 1987-05-11 1988-11-18 Sumitomo Electric Ind Ltd Method and device for producing single crystal
JP2004099333A (en) * 2002-02-13 2004-04-02 Nikko Materials Co Ltd Method of manufacturing compound semiconductor single crystal
JP2004196591A (en) * 2002-12-18 2004-07-15 Nikko Materials Co Ltd Method of manufacturing compound semiconductor single crystal and crystal growth system

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