JP2012116709A - Apparatus and method for manufacturing single crystal - Google Patents

Apparatus and method for manufacturing single crystal Download PDF

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JP2012116709A
JP2012116709A JP2010268056A JP2010268056A JP2012116709A JP 2012116709 A JP2012116709 A JP 2012116709A JP 2010268056 A JP2010268056 A JP 2010268056A JP 2010268056 A JP2010268056 A JP 2010268056A JP 2012116709 A JP2012116709 A JP 2012116709A
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single crystal
crucible
raw material
heat conductor
conductor
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Manabu Saito
学 齋藤
Tomohisa Kato
智久 加藤
Ichiro Nagai
一郎 長井
Tomonori Miura
知則 三浦
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Fujikura Ltd
National Institute of Advanced Industrial Science and Technology AIST
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National Institute of Advanced Industrial Science and Technology AIST
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Abstract

PROBLEM TO BE SOLVED: To provide a method and apparatus for manufacturing a single crystal that can improve manufacturing efficiency of the single crystal without enlarging a single crystal manufacturing apparatus.SOLUTION: The method for manufacturing the single crystal includes: a heat conductor arrangement step of arranging a heat conductor 11A on a surface 6a of a sublimable material 6 stored in a crucible 8; and a growth step of sublimating the material 6 by heating the crucible 8 and the heat conductor 11A and adhering a sublimated gas of the material 6 to a seed crystal 10 fixed to a lid body 9 for sealing the crucible 8 for recrystallization while lowering the heat conductor 11A to grow the single crystal 15.

Description

本発明は、単結晶の製造装置及び製造方法に関する。   The present invention relates to a single crystal manufacturing apparatus and manufacturing method.

窒化アルミニウム（ＡｌＮ）単結晶や炭化ケイ素（ＳｉＣ）単結晶は、バンドギャップが大きく、絶縁破壊特性に優れることから、小型で高出力の半導体等の電子デバイス材料として注目されている。またＡｌＮ単結晶やＳｉＣ単結晶は、光学的特性に優れることから、光学デバイス材料としても注目されている。   Aluminum nitride (AlN) single crystals and silicon carbide (SiC) single crystals are attracting attention as electronic device materials such as small and high output semiconductors because of their large band gap and excellent dielectric breakdown characteristics. AlN single crystals and SiC single crystals are also attracting attention as optical device materials because of their excellent optical characteristics.

このような単結晶の製造方法として、昇華法が知られている。昇華法は、一般的に成長速度が大きいため、バルク結晶の作製に対して有力な方法である。昇華法は、ルツボを加熱して、ルツボ内に配置した原料を昇華させ、その昇華ガスを、ルツボより温度の低い上部の蓋体に固定した種結晶にて再結晶させることで単結晶を成長させる方法である。   As a method for producing such a single crystal, a sublimation method is known. Since the sublimation method generally has a high growth rate, it is an effective method for producing a bulk crystal. In the sublimation method, a crucible is heated to sublimate the raw material placed in the crucible, and the sublimation gas is recrystallized with a seed crystal fixed to the upper lid, which is cooler than the crucible, to grow a single crystal. It is a method to make it.

ここで、原料は一般に、ルツボの内壁面に近い位置ほど昇華し易く、減少しやすい。即ち原料は、ルツボの内壁面に近い位置ほど減少しやすく、中央に向かうほど減少しにくくなる。このため、原料の昇華が進むと、ルツボ内に残存する原料の表面が平坦から山状（原料の表面の中央部が高く壁面に向かうにつれて低くなる形状）に変化していく。すると、成長した単結晶の温度分布が変化し、単結晶の成長速度が低下する。   Here, in general, the raw material is more likely to sublime and decrease as the position is closer to the inner wall surface of the crucible. That is, the raw material is more likely to decrease as the position is closer to the inner wall surface of the crucible, and is less likely to decrease toward the center. For this reason, as the sublimation of the raw material proceeds, the surface of the raw material remaining in the crucible changes from a flat shape to a mountain shape (a shape in which the central portion of the raw material surface is higher and lowers toward the wall surface). Then, the temperature distribution of the grown single crystal changes, and the growth rate of the single crystal decreases.

そこで、単結晶の成長速度の低下を抑えるために、下記特許文献１及び２に記載されたものが提案されている。   Therefore, in order to suppress a decrease in the growth rate of the single crystal, those described in Patent Documents 1 and 2 below have been proposed.

下記特許文献１には、ルツボの底部に、熱伝導体である棒状のグラファイトを固定して設置することにより、ＳｉＣ単結晶を安定した成長速度で形成できることが開示されている。   Patent Document 1 below discloses that a SiC single crystal can be formed at a stable growth rate by fixing and installing a rod-shaped graphite as a heat conductor at the bottom of a crucible.

下記特許文献２には、熱伝導体である棒状の黒鉛を、ルツボに配置した原料の内部に埋没させることにより、成長速度向上と原料消耗の均一化を同時に満たし、高品質単結晶を効率よく製造できることが開示されている。   In Patent Document 2 below, rod-shaped graphite, which is a heat conductor, is buried in the raw material arranged in the crucible, so that the growth rate is improved and the raw material consumption is made uniform at the same time. It is disclosed that it can be manufactured.

特開平５−５８７７４号公報JP-A-5-58774 特開２００７−７６９２８号公報JP 2007-76928 A

しかし、上記特許文献１、２に記載の単結晶の製造方法は、以下の課題を有していた。   However, the method for producing a single crystal described in Patent Documents 1 and 2 has the following problems.

即ち、上記特許文献１に記載の単結晶の製造方法では、熱伝導体である棒状のグラファイトがルツボの底部に固定して設置されている。このため、原料が減少しても熱伝導体の位置は変わらない。そのため、単結晶の成長が進むにつれて、成長する単結晶と熱伝導体とが接触することになる。このため、単結晶と熱伝導体との接触を避けるために、ルツボを大型化することが必要となり、ひいては単結晶の製造装置を大型化することが必要となる。また、単結晶の成長が進むにつれ、単結晶の先端は高温の熱伝導体に近づくため、温度分布が変化して単結晶の成長速度が低下する。その結果、単結晶の製造効率が低下する。   That is, in the method for producing a single crystal described in Patent Document 1, a bar-shaped graphite as a heat conductor is fixedly installed on the bottom of the crucible. For this reason, even if a raw material decreases, the position of a heat conductor does not change. Therefore, as the growth of the single crystal proceeds, the growing single crystal comes into contact with the thermal conductor. For this reason, in order to avoid contact between the single crystal and the heat conductor, it is necessary to enlarge the crucible, and accordingly, it is necessary to enlarge the apparatus for producing the single crystal. Further, as the growth of the single crystal proceeds, the tip of the single crystal approaches a high-temperature heat conductor, so that the temperature distribution changes and the growth rate of the single crystal decreases. As a result, the production efficiency of the single crystal is reduced.

特許文献２に記載の単結晶の製造方法では、熱伝導体が原料の内部に埋没しており、製造の初期の段階では、原料の表面が下降する。このため、成長した単結晶と熱伝導体とが接触することはない。しかし、原料の昇華が進むにつれて熱伝導体がルツボの底面に到達し熱伝導体が露出すると、上記特許文献１に記載された発明と同様の問題が生じる。   In the method for producing a single crystal described in Patent Document 2, the heat conductor is buried in the raw material, and the surface of the raw material is lowered at the initial stage of production. For this reason, the grown single crystal does not come into contact with the thermal conductor. However, if the heat conductor reaches the bottom of the crucible and the heat conductor is exposed as the sublimation of the raw material proceeds, the same problem as that of the invention described in Patent Document 1 occurs.

従って、単結晶製造装置を大型化せずに単結晶の製造効率を向上させることができる単結晶の製造方法が求められていた。   Therefore, there has been a demand for a method for producing a single crystal that can improve the production efficiency of the single crystal without increasing the size of the single crystal production apparatus.

本発明は、上記事情に鑑みてなされたものであり、単結晶製造装置を大型化せずに単結晶の製造効率を向上させることができる単結晶の製造方法及び製造装置を提供することを目的とする。   The present invention has been made in view of the above circumstances, and an object thereof is to provide a single crystal manufacturing method and a manufacturing apparatus capable of improving the manufacturing efficiency of a single crystal without increasing the size of the single crystal manufacturing apparatus. And

本発明者らは上記課題を解決するため、熱伝導体の設置位置に着目して鋭意検討した。その結果、熱伝導体を原料の表面上に置くことで、上記課題を解決し得ることを見出し、本発明を完成するに至った。   In order to solve the above-mentioned problems, the present inventors have intensively studied paying attention to the installation position of the heat conductor. As a result, it has been found that the above problems can be solved by placing the heat conductor on the surface of the raw material, and the present invention has been completed.

即ち本発明は、ルツボ内に収容した昇華性の原料の表面上に熱伝導体を配置する熱伝導体配置工程と、前記ルツボ及び前記熱伝導体を加熱して前記原料を昇華させ、前記熱伝導体を下降させながら、昇華した前記原料のガスを、前記ルツボを密閉する蓋体に固定した種結晶に付着させて再結晶させ、単結晶を成長させる成長工程とを含むことを特徴とする単結晶の製造方法である。   That is, the present invention includes a heat conductor disposing step of disposing a heat conductor on the surface of a sublimable raw material housed in a crucible, heating the crucible and the heat conductor to sublimate the raw material, and A growth step of growing a single crystal by causing the gas of the sublimated material to adhere to a seed crystal fixed to a lid that seals the crucible and recrystallizing while lowering the conductor. This is a method for producing a single crystal.

この単結晶の製造方法によれば、ルツボ及び熱伝導体を加熱してルツボ内に収容した原料を昇華させると、昇華した原料のガスが、ルツボを密閉する蓋体に固定した種結晶に付着して再結晶し、単結晶が成長する。このとき、単結晶の成長が進むにつれて原料が減少する。これに伴い、原料の表面が下降して熱伝導体が下降する。このため、成長した単結晶と熱伝導体とが過度に接近することが十分に防止される。従って、ルツボを大型化する必要がなくなる。また、成長した単結晶の先端と熱伝導体との温度差が縮小されることが十分に抑制され、温度分布が安定化され、その結果、単結晶が成長するにつれて単結晶の成長速度が低下することが十分に抑制される。よって、本発明の単結晶の製造方法によれば、単結晶の製造装置を大型化せずに、単結晶の製造効率を向上させることができる。   According to this method for producing a single crystal, when the crucible and the heat conductor are heated to sublimate the raw material contained in the crucible, the gas of the sublimated raw material adheres to the seed crystal fixed to the lid that seals the crucible. Then, recrystallization occurs and a single crystal grows. At this time, the raw material decreases as the growth of the single crystal proceeds. Along with this, the surface of the raw material descends and the thermal conductor descends. For this reason, the grown single crystal and the heat conductor are sufficiently prevented from approaching excessively. Therefore, it is not necessary to increase the size of the crucible. In addition, the temperature difference between the tip of the grown single crystal and the thermal conductor is sufficiently reduced, the temperature distribution is stabilized, and as a result, the growth rate of the single crystal decreases as the single crystal grows. Is sufficiently suppressed. Therefore, according to the method for producing a single crystal of the present invention, the production efficiency of the single crystal can be improved without increasing the size of the single crystal production apparatus.

上記単結晶の製造方法においては、前記熱伝導体が環状体を有し、前記熱伝導体配置工程において、前記熱伝導体は、前記環状体の内側の開口部を前記原料の表面に対向させるように配置されてもよい。   In the method for producing a single crystal, the thermal conductor has an annular body, and in the thermal conductor arrangement step, the thermal conductor causes an opening inside the annular body to face the surface of the raw material. May be arranged as follows.

ここで、前記熱伝導体が、前記環状体の内側の開口部を仕切る少なくとも１つの仕切り部をさらに有することが好ましい。   Here, it is preferable that the thermal conductor further includes at least one partition that partitions the opening inside the annular body.

この場合、仕切り部によって、環状体の内側の開口部に対向する原料をも十分に加熱することが可能となる。このため、熱伝導体が仕切り部を有しない場合に比べて、原料の表面における加熱ムラをより小さくすることが可能となる。従って、熱伝導体が仕切り部を有しない場合に比べて、単結晶の成長速度がより安定化され、その結果、単結晶が成長するにつれて単結晶の成長速度が低下することがより十分に抑制される。
また前記熱伝導体は、前記環状体の内周面から延び且つ前記開口部を完全には横切らない少なくとも１つの延出部をさらに有していてもよい。 In this case, the raw material facing the opening inside the annular body can be sufficiently heated by the partition portion. For this reason, compared with the case where a heat conductor does not have a partition part, it becomes possible to make the heating nonuniformity in the surface of a raw material smaller. Therefore, compared with the case where the thermal conductor does not have a partition portion, the growth rate of the single crystal is further stabilized, and as a result, the single crystal growth rate is more sufficiently suppressed from decreasing as the single crystal grows. Is done.
The thermal conductor may further include at least one extending portion that extends from the inner peripheral surface of the annular body and does not completely cross the opening.

上記単結晶の製造方法においては、前記熱伝導体が、複数の棒状部材の一端を接合部に接合してなるものであり、前記熱伝導体配置工程において、前記熱伝導体は、前記複数の棒状部材が前記原料の表面に接触するように配置されることが好ましい。   In the method for producing a single crystal, the thermal conductor is formed by joining one end of a plurality of rod-shaped members to a joint portion, and in the thermal conductor arranging step, the thermal conductor includes the plurality of thermal conductors. It is preferable that the rod-shaped member is disposed so as to contact the surface of the raw material.

この場合、熱伝導体配置工程において、複数の棒状部材が原料の表面に接触するように熱伝導体が配置されるため、熱伝導体が１つの棒状部材のみを有する場合に比べて、原料の表面における原料の加熱ムラを小さくすることが可能となる。従って、熱伝導体が１つの棒状部材のみを有する場合に比べて、単結晶の成長速度がより安定化され、その結果、単結晶が成長するにつれて単結晶の成長速度が低下することがより十分に抑制される。   In this case, in the heat conductor arranging step, since the heat conductor is arranged so that the plurality of rod-shaped members are in contact with the surface of the raw material, compared to the case where the heat conductor has only one rod-shaped member, It is possible to reduce the heating unevenness of the raw material on the surface. Therefore, compared with the case where the heat conductor has only one rod-shaped member, the growth rate of the single crystal is further stabilized, and as a result, the growth rate of the single crystal is more sufficiently decreased as the single crystal grows. To be suppressed.

また本発明は、昇華性の原料が収容されるルツボと、前記原料の上に配置される熱伝導体と、前記ルツボ及び前記熱伝導体を加熱する加熱装置と、前記ルツボを密閉し、種結晶を固定するための蓋体とを備えることを特徴とする単結晶の製造装置である。   The present invention also includes a crucible containing a sublimable raw material, a heat conductor disposed on the raw material, a heating device for heating the crucible and the heat conductor, and sealing the crucible, An apparatus for producing a single crystal, comprising: a lid for fixing the crystal.

この単結晶の製造装置によれば、ルツボに昇華性の原料を収容し、蓋体に種結晶を固定し、種結晶をルツボの内側に向けてルツボを蓋体で密閉した後、加熱装置によってルツボ及び熱伝導体を加熱すると、原料が加熱されて昇華する。すると、昇華した原料のガスが、ルツボの蓋体に固定した種結晶に付着して再結晶し、種結晶に単結晶が成長する。このとき、単結晶の成長が進むにつれて原料が減少する。これに伴い、原料の表面が下降して熱伝導体が下降する。このため、成長した単結晶と熱伝導体とが過度に接近することが十分に防止される。従って、ルツボを大型化する必要がなくなる。また、成長した単結晶の先端と熱伝導体との温度差が縮小されることが十分に抑制され、温度分布が安定化され、その結果、単結晶が成長するにつれて単結晶の成長速度が低下することが十分に抑制される。よって、本発明の単結晶の製造装置によれば、単結晶の製造装置を大型化せずに単結晶の製造効率を向上させることができる。   According to this single crystal manufacturing apparatus, a sublimable raw material is housed in a crucible, a seed crystal is fixed to a lid, the seed crystal is directed to the inside of the crucible, and the crucible is sealed with a lid, and then heated by a heating device. When the crucible and the heat conductor are heated, the raw material is heated and sublimated. Then, the sublimated raw material gas adheres to the seed crystal fixed to the crucible lid and recrystallizes, so that a single crystal grows on the seed crystal. At this time, the raw material decreases as the growth of the single crystal proceeds. Along with this, the surface of the raw material descends and the thermal conductor descends. For this reason, the grown single crystal and the heat conductor are sufficiently prevented from approaching excessively. Therefore, it is not necessary to increase the size of the crucible. In addition, the temperature difference between the tip of the grown single crystal and the thermal conductor is sufficiently reduced, the temperature distribution is stabilized, and as a result, the growth rate of the single crystal decreases as the single crystal grows. Is sufficiently suppressed. Therefore, according to the single crystal manufacturing apparatus of the present invention, the single crystal manufacturing efficiency can be improved without increasing the size of the single crystal manufacturing apparatus.

本発明によれば、単結晶の製造装置を大型化せずに単結晶の製造効率を向上させることができる単結晶の製造方法及び製造装置が提供される。   ADVANTAGE OF THE INVENTION According to this invention, the manufacturing method and manufacturing apparatus of a single crystal which can improve the manufacturing efficiency of a single crystal without enlarging the manufacturing apparatus of a single crystal are provided.

本発明に係る単結晶の製造装置の一実施形態を示す切断面端面図である。1 is a cross-sectional end view showing an embodiment of an apparatus for producing a single crystal according to the present invention. 原料の表面上に熱伝導体が置かれた状態のルツボを示す平面図である。It is a top view which shows the crucible of the state by which the heat conductor was put on the surface of a raw material. 図２のＩＩＩ−ＩＩＩ線に沿った熱伝導体の断面図である。It is sectional drawing of the heat conductor along the III-III line | wire of FIG. 熱伝導体の第１変形例を示す平面図である。It is a top view which shows the 1st modification of a heat conductor. 熱伝導体の第２変形例を示す平面図である。It is a top view which shows the 2nd modification of a heat conductor. 熱伝導体の第３変形例を示す平面図である。It is a top view which shows the 3rd modification of a heat conductor. 実施例１、比較例１及び比較例２における結晶成長時間と成長速度との関係を示すグラフである。5 is a graph showing the relationship between crystal growth time and growth rate in Example 1, Comparative Example 1 and Comparative Example 2. 実施例２、比較例３及び比較例４における結晶成長時間と成長速度との関係を示すグラフである。It is a graph which shows the relationship between the crystal growth time in Example 2, the comparative example 3, and the comparative example 4, and a growth rate.

以下、本発明の実施形態について図面を参照しながら詳細に説明する。   Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

図１は、本発明に係る単結晶の製造装置の一実施形態を示す切断面端面図である。図１に示すように、単結晶の製造装置（以下、単に「製造装置」と呼ぶ）１００は、単結晶１５の成長が行われる結晶成長部１と、結晶成長部１を収容する収容部２と、収容部２の周囲に巻回される高周波コイル（加熱装置）３とから構成されている。収容部２には、ガス導入口４と、ガス排出口５とが形成されており、不活性ガス供給装置（図示せず）からガス導入口４を通して不活性ガスが導入され、収容部２内のガスが、減圧装置（例えば真空ポンプ）によってガス排出口５を通して排出されるようになっている。また収容部２には、結晶成長部１を収容するための開口部（図示せず）も形成されている。製造装置１００によって成長される単結晶は、昇華性の単結晶であればいかなるものもよい。このような単結晶としては、ＳｉＣ単結晶、ＡｌＮ単結晶およびＧａＮ単結晶などが挙げられる。   FIG. 1 is a cross-sectional end view showing an embodiment of a single crystal manufacturing apparatus according to the present invention. As shown in FIG. 1, a single crystal manufacturing apparatus (hereinafter simply referred to as “manufacturing apparatus”) 100 includes a crystal growth unit 1 in which a single crystal 15 is grown, and a storage unit 2 that stores the crystal growth unit 1. And a high-frequency coil (heating device) 3 wound around the housing portion 2. A gas introduction port 4 and a gas discharge port 5 are formed in the storage unit 2, and an inert gas is introduced from the inert gas supply device (not shown) through the gas introduction port 4, and the inside of the storage unit 2 The gas is discharged through the gas discharge port 5 by a decompression device (for example, a vacuum pump). Further, an opening (not shown) for accommodating the crystal growth portion 1 is also formed in the accommodating portion 2. The single crystal grown by the manufacturing apparatus 100 may be any as long as it is a sublimable single crystal. Examples of such single crystals include SiC single crystals, AlN single crystals, and GaN single crystals.

結晶成長部１は、単結晶１５を成長させる成長容器７を備えており、成長容器７は、原料６が収容されるルツボ８と、ルツボ８を密閉する蓋体９とを有している。蓋体９には、ルツボ８の内壁面８ａ側の表面に種結晶１０が固定されるようになっている。成長容器７を構成する材料としては、例えばグラファイトが用いられる。成長容器７は、高周波コイル３によって高周波磁場を印加されることにより誘導電流が流され、発熱するようになっている。   The crystal growth unit 1 includes a growth vessel 7 for growing a single crystal 15, and the growth vessel 7 has a crucible 8 in which the raw material 6 is accommodated and a lid 9 that seals the crucible 8. A seed crystal 10 is fixed to the cover 9 on the inner wall surface 8 a side of the crucible 8. As a material constituting the growth vessel 7, for example, graphite is used. The growth vessel 7 generates heat when an induction current flows when a high frequency magnetic field is applied by the high frequency coil 3.

ルツボ８及び蓋体９は、熱伝導性の材料で構成されていればよく、例えばグラファイトで構成される。但し、単結晶１５がＡｌＮ等の炭素を含まない単結晶である場合には、ルツボ８の内壁面８ａ、及び蓋体９のうち種結晶１０を固定する面が、窒化タングステン等の金属窒化物で被覆されることが好ましい。   The crucible 8 and the lid 9 need only be made of a heat conductive material, for example, graphite. However, when the single crystal 15 is a single crystal containing no carbon such as AlN, the inner wall surface 8a of the crucible 8 and the surface of the lid 9 on which the seed crystal 10 is fixed is a metal nitride such as tungsten nitride. It is preferable to coat with.

成長容器７内には、原料６の表面６ａ上に熱伝導体１１Ａが配置されている。熱伝導体１１Ａは、成長容器７と同様、高周波コイル３によって高周波磁場を印加されることにより誘導電流が流され、発熱するようになっている。   In the growth vessel 7, a heat conductor 11 </ b> A is disposed on the surface 6 a of the raw material 6. As with the growth vessel 7, the heat conductor 11 </ b> A is configured to generate heat when an induction current is applied when a high-frequency magnetic field is applied by the high-frequency coil 3.

図２は、原料６の表面６ａ上に熱伝導体１１Ａが置かれた状態のルツボ８を示す平面図であり、原料６の表面６ａ上に熱伝導体１１Ａが置かれた状態を示している。図２に示すように、熱伝導体１１Ａは、複数の棒状部材１２の一端を接合部１３に接合してなるものであり、棒状部材１２は原料６の表面６ａに接触した状態で配置されている。棒状部材１２は、接合部１３からルツボ８の内壁面８ａに向かって放射状に延びている。棒状部材１２がルツボ８の内壁面８ａに向かって放射状に延びることにより、原料６の表面６ａにおける中央部からルツボ８の内壁面８ａに到るまで原料６を十分に加熱することが可能となり、原料６における加熱ムラを低減することが可能となる。棒状部材１２は、円柱状であっても四角柱状であってもよい。   FIG. 2 is a plan view showing the crucible 8 in a state where the heat conductor 11A is placed on the surface 6a of the raw material 6, and shows a state where the heat conductor 11A is placed on the surface 6a of the raw material 6. . As shown in FIG. 2, the heat conductor 11 </ b> A is formed by joining one end of a plurality of rod-shaped members 12 to the joint portion 13, and the rod-shaped members 12 are arranged in contact with the surface 6 a of the raw material 6. Yes. The rod-shaped member 12 extends radially from the joint portion 13 toward the inner wall surface 8 a of the crucible 8. By extending the rod-like member 12 radially toward the inner wall surface 8a of the crucible 8, it becomes possible to sufficiently heat the raw material 6 from the central portion of the surface 6a of the raw material 6 to the inner wall surface 8a of the crucible 8. It becomes possible to reduce heating unevenness in the raw material 6. The rod-shaped member 12 may be a columnar shape or a quadrangular prism shape.

棒状部材１２の他端部には、熱伝導体１１Ａの傾きを防止する傾き防止部１４が設けられていることが好ましい。この傾き防止部１４は、原料６が昇華により減少している間、全ての棒状部材１２がルツボ８の底面に平行な状態を維持して傾かないように下降させるためのものである。熱伝導体１１Ａの傾きを防止するために、傾き防止部１４は、ルツボ８の内壁面８ａに接触していることが好ましい。傾き防止部１４がルツボ８の内壁面８ａに接触していることで、熱伝導体１１Ａの傾きを防止することができる。一方、傾き防止部１４がルツボ８の内壁面８ａに接触しない場合、熱伝導体１１Ａは、原料６の表面６ａの状態に依存して傾きやすくなる傾向があるが、傾き防止部１４がルツボ８の内壁面８ａに接触していることで、原料６の表面６ａの状態にかかわらず、熱伝導体１１Ａの傾きを防止することができる。   It is preferable that the other end portion of the rod-shaped member 12 is provided with an inclination preventing portion 14 that prevents the inclination of the heat conductor 11A. This inclination prevention part 14 is for lowering all the rod-like members 12 so as not to incline while maintaining the state parallel to the bottom surface of the crucible 8 while the raw material 6 is reduced by sublimation. In order to prevent the inclination of the heat conductor 11 </ b> A, the inclination preventing part 14 is preferably in contact with the inner wall surface 8 a of the crucible 8. Since the inclination prevention part 14 is in contact with the inner wall surface 8a of the crucible 8, the inclination of the heat conductor 11A can be prevented. On the other hand, when the inclination preventing portion 14 does not contact the inner wall surface 8a of the crucible 8, the heat conductor 11A tends to be inclined depending on the state of the surface 6a of the raw material 6, but the inclination preventing portion 14 is likely to be inclined. By contacting the inner wall surface 8a, the inclination of the heat conductor 11A can be prevented regardless of the state of the surface 6a of the raw material 6.

傾き防止部１４は、熱伝導体１１Ａの傾きを防止できるものであれば、棒状でも板状でもよい。ここで、傾き防止部１４が棒状である場合、傾き防止部１４は、例えばその延び方向が棒状部材１２の延び方向に直交し且つルツボ８の延び方向に平行になるように棒状部材１２に設ければよい。傾き防止部１４が板状である場合は、傾き防止部１４は、例えば棒状部材１２の延び方向に直交するように設けるとよい。   The tilt prevention unit 14 may be rod-shaped or plate-shaped as long as it can prevent the thermal conductor 11A from tilting. Here, when the tilt preventing portion 14 is rod-shaped, the tilt preventing portion 14 is provided on the rod-shaped member 12 so that, for example, the extending direction thereof is orthogonal to the extending direction of the rod-shaped member 12 and parallel to the extending direction of the crucible 8. Just do it. When the inclination prevention part 14 is plate-shaped, the inclination prevention part 14 is good to provide so as to be orthogonal to the extending direction of the rod-shaped member 12, for example.

図３は、図２のＩＩＩ−ＩＩＩ線に沿った熱伝導体の断面図である。傾き防止部１４が板状である場合、傾き防止部１４は、図３に示すように、棒状部材１２の外周面１２ａよりも外側に張り出す張出し部１４ａを有していることが好ましい。この場合、棒状部材１２のルツボ８の内壁面８ａ側の端部がルツボ８の底面側に傾こうとしても、傾き防止部１４がルツボ８の内壁面８ａに接触している上、傾き防止部１４の張出し部１４ａがルツボ８の内壁面８ａに当たるため、その熱伝導体１１Ａの傾きを効果的に防止することができる。   FIG. 3 is a cross-sectional view of the heat conductor taken along line III-III in FIG. When the inclination prevention part 14 is plate-shaped, it is preferable that the inclination prevention part 14 has the overhang | projection part 14a projected outside the outer peripheral surface 12a of the rod-shaped member 12, as shown in FIG. In this case, even if the end of the rod-like member 12 on the inner wall surface 8 a side of the crucible 8 tends to tilt toward the bottom surface side of the crucible 8, the tilt preventing portion 14 is in contact with the inner wall surface 8 a of the crucible 8 and the tilt preventing portion. Since the 14 overhang | projection parts 14a contact the inner wall face 8a of the crucible 8, the inclination of the heat conductor 11A can be prevented effectively.

ここで、傾き防止部１４の形状としては、四角板状、楕円板状、円板状のいずれであってもよい。傾き防止部１４が楕円板状である場合、その長軸を、複数の棒状部材１２によって形成される平面に直交させるようにすることが好ましい。この場合、原料６の減少に伴って熱伝導体１１Ａが下降する際、傾き防止部１４がその自重により原料６に入り込みやすくなり、棒状部材１２を原料６に容易に接触させることができる。加えて、傾き防止部１４の張出し部１４ａが、傾き防止部１４の短軸を、複数の棒状部材１２によって形成される平面に直交させるようにする場合に比べて、ルツボ８の延び方向に沿った張出し部１４ａの長さを長くすることが可能となり、熱伝導体１１Ａの傾きをより有効に防止することができる。   Here, the shape of the inclination preventing portion 14 may be any of a square plate shape, an elliptic plate shape, and a disk shape. When the inclination prevention part 14 is elliptical plate shape, it is preferable to make the major axis orthogonal to the plane formed by the plurality of rod-shaped members 12. In this case, when the heat conductor 11 </ b> A descends as the raw material 6 decreases, the inclination preventing portion 14 easily enters the raw material 6 by its own weight, and the rod-shaped member 12 can be easily brought into contact with the raw material 6. In addition, the overhanging portion 14 a of the inclination preventing portion 14 is along the extending direction of the crucible 8 as compared with the case where the short axis of the inclination preventing portion 14 is orthogonal to the plane formed by the plurality of rod-shaped members 12. The length of the overhanging portion 14a can be increased, and the inclination of the heat conductor 11A can be more effectively prevented.

棒状部材１２の数は、特に制限されないが、３〜６本であることが好ましい。この場合、棒状部材１２の本数が、３本未満の場合に比べて、原料６における加熱ムラをより低減することが可能となる。また棒状部材１２の本数が、６本を超える場合に比べて、昇華した原料６をより容易に種結晶１０に付着させることができる。   The number of the rod-shaped members 12 is not particularly limited, but is preferably 3-6. In this case, the heating unevenness in the raw material 6 can be further reduced as compared with the case where the number of the rod-shaped members 12 is less than three. In addition, the sublimated raw material 6 can be attached to the seed crystal 10 more easily than when the number of the rod-shaped members 12 exceeds six.

熱伝導体１１Ａは、熱伝導性の材料で構成されていればよく、例えばグラファイトで構成される。但し、単結晶１５がＡｌＮ等の炭素を含まない単結晶である場合には、ルツボ８の内壁面８ａ、及び蓋体９のうち種結晶１０を固定する面が、窒化タングステン等の金属窒化物で被覆されることが好ましい。   The heat conductor 11A only needs to be made of a heat conductive material, for example, graphite. However, when the single crystal 15 is a single crystal containing no carbon such as AlN, the inner wall surface 8a of the crucible 8 and the surface of the lid 9 on which the seed crystal 10 is fixed is a metal nitride such as tungsten nitride. It is preferable to coat with.

次に、上記製造装置１００を用いた単結晶の製造方法について説明する。   Next, a method for manufacturing a single crystal using the manufacturing apparatus 100 will be described.

まず成長容器７内に原料６を収容する。そして、必要に応じて、原料６の表面６ａを平坦化する。原料６の表面６ａの平坦化は、例えば原料６を乳棒で押し込めることによって行うことができる。   First, the raw material 6 is accommodated in the growth vessel 7. And the surface 6a of the raw material 6 is planarized as needed. The surface 6a of the raw material 6 can be flattened, for example, by pressing the raw material 6 with a pestle.

その後、原料６の表面６ａ上に熱伝導体１１Ａを配置する（熱伝導体配置工程）。このとき、熱伝導体１１Ａの傾き防止部１４がルツボ８の内壁面８ａに接触するように且つ棒状部材１２が原料６に接触するように熱伝導体１１Ａを配置する。   Then, 11 A of thermal conductors are arrange | positioned on the surface 6a of the raw material 6 (thermal conductor arrangement | positioning process). At this time, the heat conductor 11A is disposed so that the inclination preventing portion 14 of the heat conductor 11A contacts the inner wall surface 8a of the crucible 8 and the rod-shaped member 12 contacts the raw material 6.

一方、蓋体９には、種結晶１０を固定する。種結晶１０としては通常、単結晶と同一のものが用いられる。   On the other hand, the seed crystal 10 is fixed to the lid 9. The seed crystal 10 is usually the same as the single crystal.

そして、蓋体９によってルツボ８を密閉する。このとき、蓋体９は、種結晶１０をルツボ８の内壁面８ａ側に向けてルツボ８を密閉する。   Then, the crucible 8 is sealed with the lid 9. At this time, the lid 9 seals the crucible 8 with the seed crystal 10 directed toward the inner wall surface 8 a of the crucible 8.

そして、結晶成長部１を、収容部２の開口部から内部に収容する。   And the crystal growth part 1 is accommodated in the inside from the opening part of the accommodating part 2. FIG.

次に、収容部２を減圧装置により真空引きする。その後、ガス導入口４から収容部２に不活性ガスを導入するとともにガス排出口５から収容部２内のガスを排出させる。こうして、結晶成長部１の周囲を不活性ガス雰囲気下に置く。ここで、不活性ガスとしては、例えば窒素ガス、アルゴンガスなどが挙げられる。またこのとき、収容部２の内部の圧力は、好ましくは１．３〜１０１ｋＰａとし、より好ましくは１３．３〜８０．０ｋＰａとする。   Next, the container 2 is evacuated by a decompression device. Thereafter, an inert gas is introduced from the gas introduction port 4 into the accommodation unit 2 and the gas in the accommodation unit 2 is discharged from the gas discharge port 5. Thus, the periphery of the crystal growth part 1 is placed in an inert gas atmosphere. Here, examples of the inert gas include nitrogen gas and argon gas. At this time, the internal pressure of the accommodating portion 2 is preferably 1.3 to 101 kPa, more preferably 13.3 to 80.0 kPa.

次に、高周波コイル３に高周波電流を印加し、それにより成長容器７及び熱伝導体１１Ａに高周波磁場を印加する。すると、成長容器７及び熱伝導体１１Ａに誘導電流が流れ、成長容器７及び熱伝導体１１Ａが発熱する。このとき、原料６の温度が種結晶１０の温度よりも高くなるようにする。そして、ルツボ８の熱が原料６に伝わり、原料６が加熱されて昇華される。これにより、昇華した原料のガスが、蓋体９に固定した種結晶１０に付着して再結晶し、種結晶１０に単結晶１５が成長する。   Next, a high frequency current is applied to the high frequency coil 3, thereby applying a high frequency magnetic field to the growth vessel 7 and the heat conductor 11A. Then, an induced current flows through the growth vessel 7 and the heat conductor 11A, and the growth vessel 7 and the heat conductor 11A generate heat. At this time, the temperature of the raw material 6 is set higher than the temperature of the seed crystal 10. And the heat of the crucible 8 is transmitted to the raw material 6, and the raw material 6 is heated and sublimated. As a result, the sublimated raw material gas adheres to the seed crystal 10 fixed to the lid 9 and is recrystallized, and the single crystal 15 grows on the seed crystal 10.

このとき、単結晶１５の成長が進むにつれて原料６が減少する。これに伴い、原料６の表面６ａが下降して熱伝導体１１Ａが下降する。このため、成長した単結晶１５と熱伝導体１１Ａとが過度に接近することが十分に防止される。従って、ルツボ８を大型化する必要がなくなる。また、成長した単結晶１５の先端と熱伝導体１１Ａとの温度差が縮小されることが十分に抑制され、温度分布が安定化され、その結果、単結晶１５が成長するにつれて単結晶１５の成長速度が低下することが十分に抑制される。よって、本実施形態の単結晶の製造方法によれば、製造装置１００を大型化せずに、単結晶１５の製造効率を向上させることができる。   At this time, the raw material 6 decreases as the growth of the single crystal 15 proceeds. Along with this, the surface 6a of the raw material 6 is lowered and the heat conductor 11A is lowered. For this reason, the grown single crystal 15 and the heat conductor 11A are sufficiently prevented from approaching too much. Therefore, it is not necessary to increase the size of the crucible 8. Further, the reduction in the temperature difference between the tip of the grown single crystal 15 and the thermal conductor 11A is sufficiently suppressed, the temperature distribution is stabilized, and as a result, the single crystal 15 grows as the single crystal 15 grows. A decrease in the growth rate is sufficiently suppressed. Therefore, according to the method for manufacturing a single crystal of this embodiment, the manufacturing efficiency of the single crystal 15 can be improved without increasing the size of the manufacturing apparatus 100.

本発明は、上記実施形態に限定されるものではない。例えば上記実施形態では、熱伝導体として、棒状部材１２の一端を接合部１３に接合してなる熱伝導体１１Ａが用いられているが、熱伝導体としては、図４に示す熱伝導体１１Ｂのように、環状体１６と、環状体１６の内側の開口部１６ａを仕切る仕切り部１７を設けてなるものであってもよい。ここで、環状体１６及び仕切り部１７は熱伝導性を有しており、環状体１６及び仕切り部１７は、例えばグラファイトを含む材料で構成することができる。この場合、仕切り部１７によって、環状体１６の内側の開口部１６ａに対向する原料６をも十分に加熱することが可能となる。このため、熱伝導体が仕切り部を有しない場合に比べて、原料６の表面６ａにおける加熱ムラをより小さくすることが可能となる。従って、熱伝導体が仕切り部を有しない場合に比べて、単結晶１５の成長速度がより安定化され、その結果、単結晶１５が成長するにつれて単結晶１５の成長速度が低下することがより十分に抑制される。なお、仕切り部１７は、開口部１６ａを完全に横切っているが、仕切り部１７を、環状体１６の内周面から延び且つ開口部１６ａを完全には横切らない延出部に代えることも可能である。   The present invention is not limited to the above embodiment. For example, in the above embodiment, the heat conductor 11A formed by joining one end of the rod-like member 12 to the joint portion 13 is used as the heat conductor. However, as the heat conductor, the heat conductor 11B shown in FIG. Like this, the partition part 17 which partitions off the annular body 16 and the opening part 16a inside the annular body 16 may be provided. Here, the annular body 16 and the partition part 17 have thermal conductivity, and the annular body 16 and the partition part 17 can be made of, for example, a material containing graphite. In this case, the partition portion 17 can sufficiently heat the raw material 6 facing the opening 16 a inside the annular body 16. For this reason, compared with the case where a heat conductor does not have a partition part, it becomes possible to make the heating nonuniformity in the surface 6a of the raw material 6 smaller. Accordingly, the growth rate of the single crystal 15 is further stabilized as compared with the case where the heat conductor does not have the partition portion, and as a result, the growth rate of the single crystal 15 is further decreased as the single crystal 15 grows. Sufficiently suppressed. In addition, although the partition part 17 has completely crossed the opening part 16a, it is also possible to replace the partition part 17 with an extending part that extends from the inner peripheral surface of the annular body 16 and does not completely cross the opening part 16a. It is.

また熱伝導体は、図５に示す熱伝導体１１Ｃのように、環状体１６と、環状体１６の内側の開口部１６ａを仕切る網１８を設けてなるものであってもよい。ここで、網１８は複数の仕切り部１７を交差させることによって構成される。この場合、環状体１６の内側に網１８が設けられていることで、原料６の昇華ガスの通路を十分に確保しながら原料６の表面６ａにおける加熱ムラを極めて小さくすることが可能である。従って、熱伝導体が網１８を有しない場合に比べて、単結晶１５の成長速度がより安定化され、その結果、単結晶１５が成長するにつれて単結晶１５の成長速度が低下することがより十分に抑制される。   Further, the thermal conductor may be provided with an annular body 16 and a net 18 that partitions the opening 16a inside the annular body 16 as in the thermal conductor 11C shown in FIG. Here, the net 18 is configured by crossing a plurality of partition portions 17. In this case, by providing the net 18 inside the annular body 16, it is possible to extremely reduce the heating unevenness on the surface 6 a of the raw material 6 while sufficiently securing the passage of the sublimation gas of the raw material 6. Therefore, the growth rate of the single crystal 15 is further stabilized as compared with the case where the heat conductor does not have the network 18, and as a result, the growth rate of the single crystal 15 is decreased as the single crystal 15 grows. Sufficiently suppressed.

なお、熱伝導体は、図６に示す熱伝導体１１Ｄのように、環状体１６のみからなるものでもよい。この場合でも、ルツボ８の内壁面８ａ近傍の原料６のみならず、原料６の中央部付近の原料６をも加熱することは可能である。   The heat conductor may be composed only of the annular body 16 as in the heat conductor 11D shown in FIG. Even in this case, it is possible to heat not only the raw material 6 in the vicinity of the inner wall surface 8 a of the crucible 8 but also the raw material 6 in the vicinity of the center of the raw material 6.

また上記実施形態では、棒状部材１２の先端に傾き防止部１４が設けられているが、傾き防止部１４が設けられる代わりに、ルツボ８の内壁面８ａに、ルツボ８の上下方向に沿って形成される溝を設け、その溝に沿って棒状部材１２の先端が動くようにされてもよい。この場合でも、熱伝導体１１の傾きを抑制することは可能である。   Further, in the above embodiment, the tilt preventing portion 14 is provided at the tip of the rod-shaped member 12, but instead of being provided with the tilt preventing portion 14, it is formed on the inner wall surface 8 a of the crucible 8 along the vertical direction of the crucible 8. A groove may be provided, and the tip of the rod-shaped member 12 may be moved along the groove. Even in this case, it is possible to suppress the inclination of the heat conductor 11.

また上記実施形態では、ルツボ８及び熱伝導体１１Ａは、高周波コイル３により誘導加熱によって発熱しているが、高周波コイル３は必ずしも必要ではない。例えば抵抗加熱によってルツボ８及び熱伝導体８を発熱させることも可能である。   Moreover, in the said embodiment, although the crucible 8 and the heat conductor 11A are heat-generating by the induction heating with the high frequency coil 3, the high frequency coil 3 is not necessarily required. For example, the crucible 8 and the heat conductor 8 can be heated by resistance heating.

さらに上記実施形態では、製造装置１００は、結晶成長部１のほか、収容部２、高周波コイル３を備えているが、結晶成長部１のみで構成されてもよい。   Furthermore, in the above-described embodiment, the manufacturing apparatus 100 includes the accommodating unit 2 and the high-frequency coil 3 in addition to the crystal growing unit 1, but may be configured by only the crystal growing unit 1.

以下、本発明の内容を、実施例を挙げてより具体的に説明するが、本発明は下記の実施例に限定されるものではない。   Hereinafter, the content of the present invention will be described more specifically with reference to examples. However, the present invention is not limited to the following examples.

（実施例１）
図１に示す製造装置を用いて、以下のようにしてＳｉＣ単結晶を製造した。即ち、まずグラファイト製のルツボを用意した。そして、ルツボ内に、原料であるＳｉＣ粉末を収納した。そして、乳棒を用いて、原料の表面を平坦化した。 Example 1
Using the manufacturing apparatus shown in FIG. 1, a SiC single crystal was manufactured as follows. First, a graphite crucible was prepared. And the SiC powder which is a raw material was accommodated in the crucible. And the surface of the raw material was planarized using the pestle.

一方、以下のようにして熱伝導体を用意した。即ち、まず円柱状の３つの棒状部材の片端同士を、グラファイト製の接合部に接合した。このとき、３つの棒状部材が３回対象形になるように接合した。即ち３つの棒状部材が接合部から放射状に且つ互いのなす角が１２０°となるように接合した。また３つの棒状部材はグラファイトで構成した。そして、３つの棒状部材のもう片端には楕円板を、３つの棒状部材が形成する平面の法線と楕円板の長軸方向とが一致し且つ棒状部材の中心軸線が楕円板の中心を通るように接合した。こうして熱伝導体を作製した。   On the other hand, a heat conductor was prepared as follows. That is, first, the ends of three cylindrical rod-shaped members were joined to a graphite joint. At this time, it joined so that three rod-shaped members might become a target shape 3 times. That is, the three rod-shaped members were joined so as to radiate from the joint and the angle between them was 120 °. The three rod members were made of graphite. An elliptical plate is provided at the other end of the three rod-shaped members, and the normal line of the plane formed by the three rod-shaped members coincides with the major axis direction of the elliptical plate, and the central axis of the rod-shaped member passes through the center of the elliptical plate. Were joined. Thus, a heat conductor was produced.

その後、上記のようにして得られた熱伝導体を、原料の表面上に配置した。このとき、楕円板を原料に差し込むように配置することにより棒状部材を原料の表面に接触させた。   Thereafter, the heat conductor obtained as described above was disposed on the surface of the raw material. At this time, the rod-shaped member was brought into contact with the surface of the raw material by arranging the elliptical plate so as to be inserted into the raw material.

一方、蓋体の表面には、接着剤によって、種結晶を固定した。このとき、種結晶としては、６Ｈ−ＳｉＣ（０００１）を用いた。   On the other hand, a seed crystal was fixed to the surface of the lid with an adhesive. At this time, 6H—SiC (0001) was used as a seed crystal.

そして、種結晶をルツボの内側に向けるようにしてルツボ８を蓋体９で密閉し、結晶成長部１を得た。この結晶成長部１を収容部２内に設置した。   Then, the crucible 8 was sealed with the lid 9 so that the seed crystal was directed to the inside of the crucible, and the crystal growth portion 1 was obtained. This crystal growth part 1 was installed in the accommodating part 2.

そして、収容部２内を、真空ポンプを用いて真空引きした。その後、ガス導入口４から収容部２に不活性ガスとしてアルゴンガスを導入するとともに、ガス排出口５から収容部２内のガスを排出させた。こうしてルツボ８の内部を、約１０Ｔｏｒｒのアルゴンガス雰囲気となるようにした。   And the inside of the accommodating part 2 was evacuated using the vacuum pump. Thereafter, argon gas was introduced as an inert gas from the gas inlet 4 into the container 2 and the gas in the container 2 was discharged from the gas outlet 5. Thus, the inside of the crucible 8 was made to have an argon gas atmosphere of about 10 Torr.

次に、高周波コイル３に高周波磁場を印加してルツボ及び熱伝導体を発熱させ、ＳｉＣ粉末を加熱した。このとき、原料の温度は約２３５０℃とし、種結晶の温度は約２２５０℃とした。こうして蓋体に固定した種結晶に原料の昇華ガスを再結晶させ、１０時間にわたってＳｉＣ単結晶を成長させた。   Next, a high frequency magnetic field was applied to the high frequency coil 3 to heat the crucible and the heat conductor, and the SiC powder was heated. At this time, the temperature of the raw material was about 2350 ° C., and the temperature of the seed crystal was about 2250 ° C. The raw material sublimation gas was recrystallized in the seed crystal thus fixed to the lid, and a SiC single crystal was grown for 10 hours.

（比較例１）
熱伝導体として、実施例１の熱伝導体に代えて、グラファイト製の円柱状の棒状部材を用い、この棒状部材を、ルツボに原料を収容する前にルツボの底面の中心に固定したこと以外は実施例１と同様にしてＳｉＣ単結晶を成長させた。 (Comparative Example 1)
As a heat conductor, instead of the heat conductor of Example 1, a graphite columnar rod-shaped member was used, and this rod-shaped member was fixed to the center of the bottom surface of the crucible before containing the raw material in the crucible. Grown a SiC single crystal in the same manner as in Example 1.

（比較例２）
熱伝導体を配置しなかったこと以外は実施例１と同様にしてＳｉＣ単結晶を成長させた。 (Comparative Example 2)
A SiC single crystal was grown in the same manner as in Example 1 except that no heat conductor was disposed.

（実施例２）
図１に示す製造装置を用いて、以下のようにしてＡｌＮ単結晶を製造した。即ち、まずルツボ８を用意した。ここで、ルツボとしては、グラファイト製の本体部の内面を窒化タングステンで被覆したものを用いた。そして、ルツボ８内に、原料であるＡｌＮ粉末を収納した。そして、実施例１と同様にして原料の表面を平坦化した。 (Example 2)
Using the manufacturing apparatus shown in FIG. 1, an AlN single crystal was manufactured as follows. That is, first, the crucible 8 was prepared. Here, as the crucible, a graphite body whose inner surface was coated with tungsten nitride was used. And the AlN powder which is a raw material was accommodated in the crucible 8. And the surface of the raw material was planarized like Example 1.

一方、以下のようにして熱伝導体を用意した。即ち、まず断面形状が長方形となる円環状体を用意し、この円環状体に、その内側の開口部を仕切る網を設けた。このとき、円環状体も網も、窒化タングステンで被覆したグラファイトで構成した。こうして熱伝導体を作製した。   On the other hand, a heat conductor was prepared as follows. That is, first, an annular body having a rectangular cross-sectional shape was prepared, and a net for partitioning the opening inside the annular body was provided. At this time, both the torus and the net were made of graphite coated with tungsten nitride. Thus, a heat conductor was produced.

その後、上記のようにして得られた熱伝導体を、原料の表面上に配置した。このとき、熱伝導体は、網が原料の表面に対向するように原料の表面上に配置した。   Thereafter, the heat conductor obtained as described above was disposed on the surface of the raw material. At this time, the heat conductor was arranged on the surface of the raw material so that the net faced the surface of the raw material.

一方、蓋体の表面には、接着剤によって、種結晶を固定した。このとき、種結晶としては、６Ｈ−ＳｉＣ（０００１）を用いた。   On the other hand, a seed crystal was fixed to the surface of the lid with an adhesive. At this time, 6H—SiC (0001) was used as a seed crystal.

そして、種結晶をルツボ８の内側に向けるようにしてルツボ８を蓋体９で密閉し、成長容器７を得た。この成長容器７を、収容部２内に設置した。   Then, the crucible 8 was sealed with the lid 9 so that the seed crystal was directed to the inside of the crucible 8 to obtain a growth vessel 7. The growth vessel 7 was installed in the storage unit 2.

そして、収容部２内を、真空ポンプを用いて真空引きした。その後、ガス導入口４から収容部２に不活性ガスとして窒素ガスを導入するとともに、ガス排出口５から収容部２内のガスを排出させた。こうしてルツボ８の内部を、100Ｔｏｒｒの窒素ガス雰囲気となるようにした。   And the inside of the accommodating part 2 was evacuated using the vacuum pump. Thereafter, nitrogen gas was introduced as an inert gas from the gas introduction port 4 into the accommodation unit 2, and the gas in the accommodation unit 2 was discharged from the gas discharge port 5. Thus, the inside of the crucible 8 was set to a nitrogen gas atmosphere of 100 Torr.

次に、高周波コイル３に高周波磁場を印加してルツボ及び熱伝導体を発熱させ、ＡｌＮ粉末を加熱した。このとき、原料の温度は2050℃とし、種結晶の温度は2000℃とした。こうして蓋体に固定した種結晶に原料の昇華ガスを再結晶させ、１００時間にわたってＡｌＮ単結晶を成長させた。   Next, a high frequency magnetic field was applied to the high frequency coil 3 to heat the crucible and the heat conductor, and the AlN powder was heated. At this time, the temperature of the raw material was 2050 ° C., and the temperature of the seed crystal was 2000 ° C. The seed sublimation gas was recrystallized in the seed crystal thus fixed to the lid, and an AlN single crystal was grown for 100 hours.

（比較例３）
熱伝導体として、実施例２の熱伝導体に代えて、グラファイト製の円柱状の棒状部材を用い、この棒状部材を、ルツボに原料を収容する前にルツボの底面の中心に固定したこと以外は実施例２と同様にしてＡｌＮ単結晶を成長させた。 (Comparative Example 3)
As a heat conductor, instead of the heat conductor of Example 2, a graphite columnar rod-shaped member was used, and this rod-shaped member was fixed to the center of the bottom surface of the crucible before containing the raw material in the crucible. Grown an AlN single crystal in the same manner as in Example 2.

（比較例４）
熱伝導体を配置しなかったこと以外は実施例２と同様にしてＳｉＣ単結晶を成長させた。 (Comparative Example 4)
A SiC single crystal was grown in the same manner as in Example 2 except that no heat conductor was disposed.

［成長速度］
実施例１及び比較例１〜２において、結晶成長時間が１，２，５及び１０時間のときにそれぞれ、マイクロメータを用いて単結晶の厚さを測定し、下記式：
成長速度（μｍ／ｈ）＝単結晶の厚さ（μｍ）／結晶成長時間（ｈ）
に基づいて成長速度を算出した。そして、結晶成長時間と成長速度との関係を求めた。結果を図７に示す。なお、図７においては、実施例１、比較例１及び２における比較を容易にするため、実施例１、比較例１及び比較例２の各々において結晶成長時間が１時間であるときの成長速度を１とし、規格化してある。 [Growth speed]
In Example 1 and Comparative Examples 1 and 2, when the crystal growth time was 1, 2, 5 and 10 hours, respectively, the thickness of the single crystal was measured using a micrometer, and the following formula:
Growth rate (μm / h) = single crystal thickness (μm) / crystal growth time (h)
Based on the above, the growth rate was calculated. And the relationship between crystal growth time and growth rate was calculated | required. The results are shown in FIG. In FIG. 7, in order to facilitate comparison in Example 1 and Comparative Examples 1 and 2, the growth rate when the crystal growth time is 1 hour in each of Example 1, Comparative Example 1 and Comparative Example 2. 1 is standardized.

また実施例２及び比較例３〜４において、結晶成長時間が１０，２０，５０及び１００時間のときにそれぞれ、実施例１の場合と同様にして単結晶の厚さを測定し、上記式に基づいて成長速度を算出した。そして、結晶成長時間と成長速度との関係を求めた、結果を図８に示す。なお、図８においては、実施例２、比較例３及び４における比較を容易にするため、実施例２、比較例３及び比較例４の各々において結晶成長時間が１０時間であるときの成長速度を１とし、規格化してある。   In Example 2 and Comparative Examples 3 to 4, when the crystal growth time was 10, 20, 50 and 100 hours, the thickness of the single crystal was measured in the same manner as in Example 1, and the above formula was obtained. Based on this, the growth rate was calculated. And the result of having calculated | required the relationship between crystal growth time and growth rate is shown in FIG. In FIG. 8, in order to facilitate comparison in Example 2 and Comparative Examples 3 and 4, the growth rate when the crystal growth time is 10 hours in each of Example 2, Comparative Example 3 and Comparative Example 4. 1 is standardized.

図７に示す結果より、実施例１では、結晶成長時間が長くなっても成長速度の低下が極めて小さいことが分かった。これに対し、比較例１，２では、結晶成長時間が長くなるにつれて成長速度が大きく低下していくことが分かった。   From the results shown in FIG. 7, it was found that in Example 1, the decrease in growth rate was extremely small even when the crystal growth time was increased. On the other hand, in Comparative Examples 1 and 2, it was found that the growth rate greatly decreased as the crystal growth time increased.

また図８に示す結果より、実施例２では、結晶成長時間が長くなっても成長速度の低下が極めて小さいことが分かった。これに対し、比較例３，４では、結晶成長時間が長くなるにつれて成長速度が大きく低下していくことが分かった。   Further, from the results shown in FIG. 8, it was found that in Example 2, the decrease in the growth rate was extremely small even when the crystal growth time was long. On the other hand, in Comparative Examples 3 and 4, it was found that the growth rate greatly decreased as the crystal growth time increased.

以上より、本発明の単結晶の製造方法によれば、単結晶の製造装置を大型化せずに単結晶の製造効率を向上させることができることが確認された。   From the above, it was confirmed that according to the method for producing a single crystal of the present invention, the production efficiency of the single crystal can be improved without increasing the size of the single crystal production apparatus.

３…高周波コイル（加熱装置）
６…原料
６ａ…原料の表面
８…ルツボ
９…蓋体
１０…種結晶
１１Ａ…熱伝導体
１２…棒状部材
１５…単結晶
１６…環状体
１６ａ…開口部
１７…仕切部
１８…網
１００…単結晶の製造装置 3. High frequency coil (heating device)
6 ... Raw material 6a ... Raw material surface 8 ... Crucible 9 ... Lid 10 ... Seed crystal 11A ... Thermal conductor 12 ... Rod-like member 15 ... Single crystal 16 ... Ring 16a ... Opening 17 ... Partition 18 ... Net 100 ... Single Crystal manufacturing equipment

Claims (6)

ルツボ内に収容した昇華性の原料の表面上に熱伝導体を配置する熱伝導体配置工程と、
前記ルツボ及び前記熱伝導体を加熱して前記原料を昇華させ、前記熱伝導体を下降させながら、昇華した前記原料のガスを、前記ルツボを密閉する蓋体に固定した種結晶に付着させて再結晶させ、単結晶を成長させる成長工程と、
を含むことを特徴とする単結晶の製造方法。 A heat conductor arranging step of arranging a heat conductor on the surface of the sublimable raw material contained in the crucible;
The crucible and the heat conductor are heated to sublimate the raw material, and the sublimated gas of the raw material is attached to a seed crystal fixed to a lid that seals the crucible while lowering the heat conductor. A growth step of recrystallizing and growing a single crystal;
A method for producing a single crystal, comprising: 前記熱伝導体が環状体を有し、
前記熱伝導体配置工程において、前記熱伝導体は、前記環状体の内側の開口部を前記原料の表面に対向させるように配置される、請求項１に記載の単結晶の製造方法。 The thermal conductor has an annular body;
2. The method for producing a single crystal according to claim 1, wherein, in the thermal conductor arrangement step, the thermal conductor is arranged so that an opening inside the annular body faces a surface of the raw material. 前記熱伝導体が、前記環状体の内側の開口部を仕切る少なくとも１つの仕切り部をさらに有する請求項２に記載の単結晶の製造方法。   The method for producing a single crystal according to claim 2, wherein the heat conductor further includes at least one partition portion that partitions an opening inside the annular body. 前記熱伝導体が、前記環状体の内周面から延び且つ前記開口部を完全には横切らない少なくとも１つの延出部をさらに有する請求項２に記載の単結晶の製造方法。   3. The method for producing a single crystal according to claim 2, wherein the heat conductor further includes at least one extending portion that extends from an inner peripheral surface of the annular body and does not completely cross the opening. 前記熱伝導体が、複数の棒状部材の一端を接合部に接合してなるものであり、
前記熱伝導体配置工程において、前記熱伝導体は、前記複数の棒状部材が前記原料の表面に接触するように配置される、請求項１に記載の単結晶の製造方法。 The heat conductor is formed by joining one end of a plurality of rod-shaped members to a joint portion,
2. The method for producing a single crystal according to claim 1, wherein, in the thermal conductor arranging step, the thermal conductor is arranged such that the plurality of rod-shaped members are in contact with the surface of the raw material. 昇華性の原料が収容されるルツボと、
前記原料の上に配置される熱伝導体と、
前記ルツボ及び前記熱伝導体を加熱する加熱装置と、
前記ルツボを密閉し、種結晶を固定するための蓋体と、
を備えることを特徴とする単結晶の製造装置。 A crucible containing a sublimable raw material;
A heat conductor disposed on the raw material;
A heating device for heating the crucible and the heat conductor;
A lid for sealing the crucible and fixing the seed crystal;
An apparatus for producing a single crystal, comprising:
JP2010268056A 2010-12-01 2010-12-01 Apparatus and method for manufacturing single crystal Pending JP2012116709A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115595656A (en) * 2022-10-14 2023-01-13 武汉大学（Cn） Device for growing aluminum nitride crystal by sublimation method

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JPH0558774A (en) * 1991-09-03 1993-03-09 Sanyo Electric Co Ltd Vessel for silicone carbide single crystal growing device
JPH11199396A (en) * 1998-01-19 1999-07-27 Sumitomo Electric Ind Ltd Synthesis of sic single crystal
JP2006069851A (en) * 2004-09-02 2006-03-16 Bridgestone Corp Method and device for manufacturing silicon carbide single crystal
JP2007076928A (en) * 2005-09-12 2007-03-29 Matsushita Electric Ind Co Ltd Method and device for manufacturing single crystal
JP2008290903A (en) * 2007-05-24 2008-12-04 Denso Corp Method and apparatus for producing silicon carbide single crystal

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JPH0558774A (en) * 1991-09-03 1993-03-09 Sanyo Electric Co Ltd Vessel for silicone carbide single crystal growing device
JPH11199396A (en) * 1998-01-19 1999-07-27 Sumitomo Electric Ind Ltd Synthesis of sic single crystal
JP2006069851A (en) * 2004-09-02 2006-03-16 Bridgestone Corp Method and device for manufacturing silicon carbide single crystal
JP2007076928A (en) * 2005-09-12 2007-03-29 Matsushita Electric Ind Co Ltd Method and device for manufacturing single crystal
JP2008290903A (en) * 2007-05-24 2008-12-04 Denso Corp Method and apparatus for producing silicon carbide single crystal

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115595656A (en) * 2022-10-14 2023-01-13 武汉大学（Cn） Device for growing aluminum nitride crystal by sublimation method

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