JP2013177280A - Sapphire single crystal growth apparatus - Google Patents

Sapphire single crystal growth apparatus Download PDF

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JP2013177280A
JP2013177280A JP2012042890A JP2012042890A JP2013177280A JP 2013177280 A JP2013177280 A JP 2013177280A JP 2012042890 A JP2012042890 A JP 2012042890A JP 2012042890 A JP2012042890 A JP 2012042890A JP 2013177280 A JP2013177280 A JP 2013177280A
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crucible
sapphire
single crystal
heat retaining
retaining member
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Kenji Hori
健次 堀
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Kyocera Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a sapphire single crystal growth apparatus capable of preventing impurities from mixing into a sapphire single crystal grown by the Czochralski method, and capable of suppressing the generation of bubbles or the like in the sapphire single crystal.SOLUTION: A gas supply means 60 makes a noble gas to flow along a shaft 12a from a lower side opening 17A of a heat insulation member 17, toward a gap of a crucible 10 and the heat insulation member 17, thereby forming a flow of the noble gas passing an upper side opening 17B and flowing out from the gap after the gas flows through the side of the crucible 10 from the side of the shaft 12a.

Description

本発明は、サファイア単結晶育成装置に関する。   The present invention relates to a sapphire single crystal growing apparatus.

サファイア単結晶の育成方法として、坩堝を高温に加熱して、この坩堝に投入したサファイア原料を溶融し、坩堝内のサファイア原料融液の液面に上方からサファイア種結晶を接触させた後に上昇させることで、サファイア種結晶に連なる長尺の単結晶体を育成する、いわゆるチョクラルスキー法と呼ばれる単結晶育成方法が、従来から実施されている。   As a method for growing a sapphire single crystal, the crucible is heated to a high temperature, the sapphire raw material charged in the crucible is melted, and the sapphire seed crystal is brought into contact with the liquid surface of the sapphire raw material melt in the crucible from above and then raised. Thus, a so-called Czochralski method for growing a single crystal continuous with a sapphire seed crystal has been conventionally practiced.

チョクラルスキー法によるサファイア単結晶育成では、坩堝の周囲に保温部材が配置され、その周囲に高周波電流が流される誘導コイルが配されており、この誘導コイルに高周波電流を流すことにより生じる誘導加熱によって坩堝が発熱し、坩堝内のサファイア原料が溶融される。チョクラルスキー法では、サファイア種結晶の上昇に伴い、このサファイア原料融液から引き上げられるようにサファイア単結晶体が成長する。   In sapphire single crystal growth by the Czochralski method, a heat insulating member is arranged around the crucible, and an induction coil through which high-frequency current flows is arranged, and induction heating generated by flowing high-frequency current through the induction coil As a result, the crucible generates heat and the sapphire material in the crucible is melted. In the Czochralski method, as the sapphire seed crystal rises, a sapphire single crystal grows so as to be pulled up from the sapphire raw material melt.

例えば特許文献１には、従来のサファイア単結晶の育成装置の一例が開示されている。従来のサファイア単結晶の育成装置では、放熱による坩堝の温度低下を抑制するため、および、引き上げ中のサファイア単結晶からの過度な放熱を抑制するために、坩堝と誘導コイルとの間に、例えばジルコニア等のセラミックスやカーボンからなる耐熱性の保温部材が配置されている。   For example, Patent Document 1 discloses an example of a conventional sapphire single crystal growth apparatus. In a conventional sapphire single crystal growth apparatus, in order to suppress the temperature drop of the crucible due to heat dissipation, and to suppress excessive heat dissipation from the sapphire single crystal being pulled, between the crucible and the induction coil, for example, A heat-resistant heat retaining member made of ceramics such as zirconia or carbon is disposed.

特開２００５−１９３４号公報Japanese Patent Laid-Open No. 2005-1934

サファイア単結晶の育成では、サファイア原料を溶融させるために、坩堝は２０００℃以上の高温に加熱される。坩堝を効率的に保温するためにジルコニア等のセラミックスからなる保温部材をこの坩堝に近接して配置した場合には、この保温部材も２０００℃近くの温度まで熱せられることになる。このように高温に熱せられた場合、保温部材から、少量ではあるがアウトガスが発生することがあった。また、溶融された高温のアルミナ原料からも酸素ガスが放出され、この酸素ガスがジルコニア等からなる保温部材の表面の金属原子と反応し、金属酸化物となって脱粒して、坩堝周辺の雰囲気に放出されることもあった。これらアウトガスや脱粒した微粒子等のパーティクルが坩堝内の溶融サファイア原料に混入すると、サファイア単結晶内の不純物やサファイア単結晶内に発生する気泡の原因となっていた。本発明は、かかる問題点を解決するためになされた発明である。   In growing the sapphire single crystal, the crucible is heated to a high temperature of 2000 ° C. or higher in order to melt the sapphire raw material. When a heat retaining member made of ceramics such as zirconia is disposed in the vicinity of the crucible in order to efficiently retain the temperature of the crucible, the heat retaining member is also heated to a temperature close to 2000 ° C. When heated to a high temperature in this way, outgas may be generated from the heat retaining member although the amount is small. Also, oxygen gas is released from the molten high-temperature alumina raw material, and this oxygen gas reacts with the metal atoms on the surface of the heat insulating member made of zirconia or the like, and becomes a metal oxide, which is granulated, and the atmosphere around the crucible Was sometimes released. When particles such as outgas and shed particles are mixed into the molten sapphire raw material in the crucible, impurities in the sapphire single crystal and bubbles generated in the sapphire single crystal are caused. The present invention has been made to solve such problems.

本発明は、サファイア原料融液を保持する坩堝と、該坩堝の下方に配置されて当接した、該坩堝を保持する坩堝保持部材と、サファイア種結晶を保持して上下動し、前記坩堝内の前記サファイア原料融液に前記サファイア種結晶を接触させた後に上昇させることで、該サファイア種結晶に連続したサファイア単結晶体を引き上げるための引き上げ機構と、前記坩堝保持部材が挿通した下側開口、および前記引き上げ機構によって上下動する前記サファイア種結晶が通過する上側開口を有する、前記坩堝の周囲を囲む保温部材と、高周波電流が流れることで前記坩堝を発熱させてサファイア原料を溶融させ、前記坩堝内に前記サファイア原料融液を保持させるための、前記保温部材を介して前記坩堝の周囲に配置された誘導コイルと、前記坩堝の周辺部分に希ガスを供給するためのガス供給手段とを備えたサファイア単結晶育成装置であって、前記坩堝保持部材は、前記保温部材の前記下側開口に挿通された、前記坩堝の外径よりも小さい外径を有する軸体と、該軸体の上端部に設けられた、前記軸体の外径よりも大きく、かつ前記坩堝の外径よりも小さい外径を有する、前記坩堝が載置された坩堝載置体とを備え、前記ガス供給手段は、前記保温部材の前記下側開口から、前記軸体に沿って前記坩堝と前記保温部材との間隙に向けて前記希ガスを流すことで、前記軸体の側面から前記坩堝の側面を流れた後に前記上側開口を通過して前記間隙から流出する前記希ガスの流れを形成するサファイア単結晶育成装置を提供する。   The present invention provides a crucible for holding a sapphire raw material melt, a crucible holding member for holding the crucible disposed below and in contact with the crucible, a sapphire seed crystal, and moving up and down, The sapphire source melt is brought into contact with the sapphire seed crystal and then lifted to raise a sapphire single crystal continuous sapphire single crystal, and a lower opening through which the crucible holding member is inserted. And a heat retaining member surrounding the crucible having an upper opening through which the sapphire seed crystal that moves up and down by the pulling mechanism passes, and the crucible is heated by high-frequency current flowing to melt the sapphire raw material, An induction coil arranged around the crucible via the heat retaining member for holding the sapphire raw material melt in the crucible, and the crucible A sapphire single crystal growth apparatus comprising a gas supply means for supplying a rare gas to a peripheral portion, wherein the crucible holding member is inserted into the lower opening of the heat retaining member, and the outer diameter of the crucible A shaft body having a smaller outer diameter, and the crucible having an outer diameter larger than the outer diameter of the shaft body and smaller than the outer diameter of the crucible provided at an upper end portion of the shaft body are mounted. And the gas supply means flows the rare gas from the lower opening of the heat retaining member toward the gap between the crucible and the heat retaining member along the shaft body. Thus, there is provided a sapphire single crystal growth apparatus that forms the flow of the rare gas that flows from the side surface of the shaft body through the upper opening and then flows out of the gap.

本発明のサファイア単結晶育成装置によれば、保温部材の下側開口から、坩堝と保温部材との間隙に向けて希ガスを流すことで、坩堝の側面を流れた後に保温部材の上側開口を通過して間隙から流出する希ガスの流れを形成することから、保温部材から放出されたアウトガスや保温部材から脱粒した微粒子を、坩堝と保温部材との間隙から坩堝の上方へと排出することができ、育成したサファイア単結晶への不純物の混入や、サファイア単結晶内の気泡等の発生を抑制することができる。   According to the sapphire single crystal growth apparatus of the present invention, by flowing a rare gas from the lower opening of the heat retaining member toward the gap between the crucible and the heat retaining member, the upper opening of the heat retaining member is opened after flowing through the side surface of the crucible. Since the flow of the rare gas that passes through and flows out of the gap is formed, the outgas discharged from the heat retaining member and the fine particles that have fallen from the heat retaining member can be discharged from the gap between the crucible and the heat retaining member to the upper side of the crucible. It is possible to suppress the mixing of impurities into the grown sapphire single crystal and the generation of bubbles in the sapphire single crystal.

本発明のサファイア単結晶育成装置の一実施形態の例の構成を示す概略構成図である。It is a schematic block diagram which shows the structure of the example of one Embodiment of the sapphire single crystal growth apparatus of this invention. 図１に示すサファイア単結晶育成装置が備える、保温部材を拡大して示す断面図である。It is sectional drawing which expands and shows the heat retention member with which the sapphire single crystal growth apparatus shown in FIG. 1 is provided. 本発明のサファイア単結晶育成装置の他の実施形態について説明する図である。It is a figure explaining other embodiment of the sapphire single crystal growth apparatus of this invention.

以下、本発明のサファイア単結晶育成装置の一実施形態について説明する。図１は、本発明のサファイア単結晶育成装置１（以下、育成装置１ともいう。）の概略構成図である。   Hereinafter, an embodiment of the sapphire single crystal growing apparatus of the present invention will be described. FIG. 1 is a schematic configuration diagram of a sapphire single crystal growing apparatus 1 (hereinafter also referred to as a growing apparatus 1) of the present invention.

育成装置１は、坩堝１０、坩堝１０の下方に配置されて坩堝１０に当接した、坩堝１０を保持する坩堝保持部材１２と、育成室１６、保温部材１７、保温材部１７を介して坩堝１０の側壁１０ａを囲むように配置された誘導コイル３２、この誘導コイル３２に交流電流を流すための高周波電源３０、結晶引き上げ手段４０（以降、単に引き上げ手段４０ともいう）、ガス供給手段６０、排気手段７０、坩堝回転機構８０、および制御部５０を有して構成されている。   The growing apparatus 1 includes a crucible 10, a crucible holding member 12 that is disposed below the crucible 10 and is in contact with the crucible 10 and holds the crucible 10, a growing chamber 16, a heat insulating member 17, and a heat insulating material part 17. An induction coil 32 disposed so as to surround the side wall 10a, a high-frequency power source 30 for supplying an alternating current to the induction coil 32, a crystal pulling means 40 (hereinafter also simply referred to as pulling means 40), a gas supply means 60, The exhaust means 70, the crucible rotation mechanism 80, and the control part 50 are comprised.

保温部材１７は、坩堝保持部材１２が挿通した下側開口１７Ａ、および引き上げ手段４０によって上下動するサファイア種結晶１３が通過する上側開口１７Ｂを有する。引き上げ手段４０、高周波電源３０、ガス供給手段６０、排気手段７０、および坩堝回転機構８０には、制御部５０が接続されている。制御部５０は、ＣＰＵとメモリとを備えた例えば公知のコンピュータからなり、制御部５０が、育成装置１全体の動作を制御する。   The heat retaining member 17 has a lower opening 17A through which the crucible holding member 12 is inserted, and an upper opening 17B through which the sapphire seed crystal 13 moving up and down by the pulling means 40 passes. A controller 50 is connected to the pulling means 40, the high frequency power supply 30, the gas supply means 60, the exhaust means 70, and the crucible rotating mechanism 80. The control part 50 consists of a well-known computer provided with CPU and memory, for example, and the control part 50 controls operation | movement of the cultivation apparatus 1 whole.

坩堝１０は、例えばイリジウム（Ｉｒ）からなる、側壁１０ａの断面が円環状の容器体である。この坩堝１０には、サファイア単結晶の原料である酸化アルミニウム粉末が投入され、さらに、坩堝１０自体の発熱によって、この酸化アルミニウムが溶融されてなるサファイア原料融液が保持される。   The crucible 10 is a container body made of, for example, iridium (Ir) and having an annular cross section of the side wall 10a. The crucible 10 is charged with aluminum oxide powder which is a raw material of sapphire single crystal, and further, the sapphire raw material melt obtained by melting the aluminum oxide is held by the heat generated by the crucible 10 itself.

誘導コイル３２は例えば銅からなり、高周波電源３０に接続されている。誘導コイル３
２は、坩堝１０の周囲に配置されており、高周波電源３０から高周波電圧が印加されて高周波電流が流れる。誘導コイル３２の高周波電流に起因した電磁界によって、坩堝１０の表面に渦電流が流れ、坩堝１０が発熱する。 The induction coil 32 is made of copper, for example, and is connected to the high frequency power supply 30. Induction coil 3
2 is arranged around the crucible 10, and a high frequency voltage is applied from the high frequency power supply 30 to flow a high frequency current. An eddy current flows on the surface of the crucible 10 by the electromagnetic field caused by the high-frequency current of the induction coil 32, and the crucible 10 generates heat.

保温部材１７は、坩堝１０の周囲を囲むように配置された、横断面が円環状の部材であり、例えばジルコニアを主成分としたセラミックスからなる。保温部材１７は上側開口１７Ｂを有し、この上側開口１７Ｂに引き上げ手段４０の引き上げ軸４２が挿通されている。引き上げ軸４２も、例えばジルコニアを主成分としたセラミックスからなる。サファイア単結晶の育成の際、引き上げ軸４２の下端には、サファイア単結晶育成の基点となる、サファイア種結晶１３（以降、種結晶１３ともいう）が保持される。種結晶１３は、高純度のサファイア単結晶体である。   The heat retaining member 17 is a member having an annular cross section disposed so as to surround the crucible 10 and is made of, for example, ceramics mainly composed of zirconia. The heat retaining member 17 has an upper opening 17B, and a lifting shaft 42 of the lifting means 40 is inserted into the upper opening 17B. The pulling shaft 42 is also made of ceramics mainly composed of zirconia, for example. At the time of growing the sapphire single crystal, a sapphire seed crystal 13 (hereinafter also referred to as a seed crystal 13) serving as a base point for sapphire single crystal growth is held at the lower end of the pulling shaft 42. The seed crystal 13 is a high-purity sapphire single crystal.

結晶引き上げ部４０は、引き上げ軸４２と、この引き上げ軸４２を図中の上下方向に移動させる、引き上げ機構部４４とを備えて構成されている。引き上げ機構部４４は、図示しないモーター等の動力源と、この動力源によって駆動して引き上げ軸４２を上下方向に移動させる図示しない機構部とを有している。サファイア単結晶育成の際、種結晶１３は引き上げ軸４２の先端（図１中の下端）に保持されて、坩堝１０の開口１１から、先端に種結晶１３が取り付けられた引き上げ軸４２が坩堝１０内に挿入され、坩堝１０に貯留されたサファイア原料融液の液面に種結晶１３が接触する。引き上げ軸４２は、坩堝１０の開口１１の中心を通る中心軸Ｃに対応する位置に配置されており、種結晶１３の一部が中心軸Ｃに対応する位置に浸漬されて、種結晶１３とサファイア原料融液とが接触する。   The crystal pulling portion 40 includes a pulling shaft 42 and a pulling mechanism portion 44 that moves the pulling shaft 42 in the vertical direction in the drawing. The lifting mechanism 44 has a power source such as a motor (not shown) and a mechanism (not shown) that is driven by the power source to move the lifting shaft 42 in the vertical direction. When growing the sapphire single crystal, the seed crystal 13 is held at the tip of the pull-up shaft 42 (the lower end in FIG. 1), and the pull-up shaft 42 with the seed crystal 13 attached to the tip is provided from the opening 11 of the crucible 10. The seed crystal 13 comes into contact with the liquid surface of the sapphire raw material melt inserted in the crucible 10. The pulling shaft 42 is disposed at a position corresponding to the central axis C passing through the center of the opening 11 of the crucible 10, and a part of the seed crystal 13 is immersed in a position corresponding to the central axis C. Contact with the sapphire material melt.

保温部材１７はまた、下側開口１７Ａを有し、この下側開口１７Ａに坩堝保持部材１２が挿通されている。坩堝保持部材１２は、保温部材１７の下側開口１７Ａに挿通された、坩堝１０の外径よりも小さい外径を有する軸体１２ａと、軸体１２ａの上端部に設けられた、軸体１２ａの外径よりも大きく、かつ坩堝１０の外径よりも小さい外径を有する、坩堝１０が載置された坩堝載置体１２ｂとを備えている。軸体１２ａおよび坩堝載置体１２ｂも、例えばジルコニアを主成分としたセラミックスからなる。坩堝保持部材１２の軸体１２ａは、坩堝回転機構８０に接続されている。坩堝回転機構８はモータ等の駆動手段を備えており、軸体１２ａと坩堝載置体１２ｂとを、軸体１２ａの中心軸周りに回転させることで、坩堝１０を回転させる。軸体１２の中心軸に一致する仮想線Ｃは、下側開口１７Ａの中心および上側開口１７Ｂの中心を通過する。このように、坩堝保持部材１２は、坩堝載置体１２ｂに坩堝１０が載置された状態で、坩堝１０ととともに軸体１２の中心軸周りに回転する。   The heat retaining member 17 also has a lower opening 17A, and the crucible holding member 12 is inserted into the lower opening 17A. The crucible holding member 12 is inserted into the lower opening 17A of the heat retaining member 17 and has a shaft body 12a having an outer diameter smaller than the outer diameter of the crucible 10, and a shaft body 12a provided at the upper end of the shaft body 12a. A crucible mounting body 12b on which the crucible 10 is mounted, which has an outer diameter larger than the outer diameter of the crucible 10 and smaller than the outer diameter of the crucible 10. The shaft body 12a and the crucible mounting body 12b are also made of ceramics mainly composed of zirconia, for example. The shaft body 12 a of the crucible holding member 12 is connected to the crucible rotation mechanism 80. The crucible rotating mechanism 8 includes driving means such as a motor, and rotates the crucible 10 by rotating the shaft body 12a and the crucible mounting body 12b around the central axis of the shaft body 12a. An imaginary line C coinciding with the central axis of the shaft body 12 passes through the center of the lower opening 17A and the center of the upper opening 17B. Thus, the crucible holding member 12 rotates around the central axis of the shaft body 12 together with the crucible 10 in a state where the crucible 10 is placed on the crucible placing body 12b.

このように坩堝１０は周囲を保温部材１７によって囲まれており、坩堝１０、保温部材１７、誘導コイル３２は、金属製の筐体からなる育成室１６内に配置されている。ガス供給手段６０は、図示しないガスボンベ、ガス流量計を備えており、ガス配管６２を介して、育成室１６内に希ガスを流入させる。本実施形態では、ガス供給手段６０にはアルゴン（Ａｒ）ガスボンベを備えており、ガス供給管６２を介して育成室１６内にアルゴン（Ａｒ）ガスが送られる。また、排気部７０は、例えば図示しない排気ポンプ等を備えている。排気部７０は、排気管７２を介して育成室１６に接続されており、育成室１６内の気体を排気管７２を介して排気する。   As described above, the crucible 10 is surrounded by the heat retaining member 17, and the crucible 10, the heat retaining member 17, and the induction coil 32 are disposed in the growth chamber 16 formed of a metal casing. The gas supply means 60 includes a gas cylinder and a gas flow meter (not shown), and allows a rare gas to flow into the growth chamber 16 via the gas pipe 62. In this embodiment, the gas supply means 60 is provided with an argon (Ar) gas cylinder, and argon (Ar) gas is sent into the growth chamber 16 through the gas supply pipe 62. The exhaust unit 70 includes, for example, an exhaust pump (not shown). The exhaust unit 70 is connected to the growth chamber 16 via the exhaust pipe 72, and exhausts the gas in the growth chamber 16 via the exhaust pipe 72.

ガス供給管６２の流出口６２ａは複数あり、流出口６２ａの少なくとも１つが、保温部材１７の下側開口１７Ａの近傍において、この下側開口１７Ａと対向するように配置されている。ガス供給手段６０は、保温部材１７の下側開口１７Ａから、軸体１２ａに沿って坩堝１０と保温部材１７との間隙に向けて希ガス（本実施形態ではアルゴンガス）を流す。また、排気管７２の吸入口７２ａは、保温部材１７の上側開口１７Ｂの近傍において、上側開口１７Ｂと対向するように配置されている。ガス供給手段６０は、流出口６２ａから希ガスを流出させ、軸体１２ａの側面から坩堝１０の側面を流れた後に上側開口１７Ｂを通過して間隙から流出する、希ガスの流れを形成する。   The gas supply pipe 62 has a plurality of outlets 62a, and at least one of the outlets 62a is disposed in the vicinity of the lower opening 17A of the heat retaining member 17 so as to face the lower opening 17A. The gas supply means 60 allows a rare gas (argon gas in the present embodiment) to flow from the lower opening 17A of the heat retaining member 17 toward the gap between the crucible 10 and the heat retaining member 17 along the shaft body 12a. Further, the suction port 72a of the exhaust pipe 72 is arranged in the vicinity of the upper opening 17B of the heat retaining member 17 so as to face the upper opening 17B. The gas supply means 60 causes a rare gas to flow out from the outlet 62a, and forms a flow of the rare gas that flows through the side surface of the crucible 10 from the side surface of the shaft body 12a and then flows out from the gap through the upper opening 17B.

サファイア原料を溶融させるために、坩堝を２０００℃以上の高温に加熱すると、ジルコニア等のセラミックスからなる保温部材１７も、２０００℃近くの高温となる。高温に熱せられた保温部材１７からは、少量ではあるがアウトガスが発生したり、溶融された高温のアルミナ原料から酸素ガスが放出されることで、この酸素ガスがジルコニア等のセラミックスの表面の金属原子と反応し、酸化物となって脱粒し、坩堝１０の周辺雰囲気に放出される場合もある。育成装置１では、軸体１２ａおよび坩堝載置体１２ｂの側面から坩堝１０の側面を流れた後に上側開口１７Ｂを通過して間隙から流出する希ガスの流れによって、これらアウトガスや、脱粒した微粒子等のパーティクルは、上側開口１７Ｂを通過して間隙から排出され、上側開口１７Ｂ近傍の吸入口７２ａを通って排気部７０によって排気される。育成装置１では、保温部材１７からのアウトガスや脱粒した微粒子等のパーティクルに起因する、成長したサファイア単結晶内への不純物の混入や、サファイア単結晶内の気泡の発生を抑制することができる。   When the crucible is heated to a high temperature of 2000 ° C. or higher in order to melt the sapphire raw material, the heat retaining member 17 made of ceramics such as zirconia also has a high temperature of about 2000 ° C. A small amount of outgas is generated from the heat retaining member 17 heated to a high temperature, or oxygen gas is released from the molten high temperature alumina raw material, so that this oxygen gas becomes a metal on the surface of ceramics such as zirconia. In some cases, it reacts with atoms, becomes an oxide, sheds, and is released to the atmosphere around the crucible 10. In the growth apparatus 1, these outgases, deagglomerated fine particles, etc. are generated by the flow of the rare gas that flows from the side surface of the crucible 10 from the side surface of the shaft body 12 a and the crucible mounting body 12 b and then passes through the upper opening 17 B and flows out from the gap. The particles pass through the upper opening 17B and are discharged from the gap, and are exhausted by the exhaust unit 70 through the suction port 72a in the vicinity of the upper opening 17B. In the growth apparatus 1, it is possible to suppress the entry of impurities into the grown sapphire single crystal and the generation of bubbles in the sapphire single crystal due to particles such as outgas from the heat retaining member 17 and deagglomerated fine particles.

なお、育成装置１では、軸体１２ａの中心軸に一致する仮想線Ｃが、下側開口１７Ａの中心および上側開口１７Ｂの中心を通過するとともに、下側開口１７Ａの内径および上側開口１７Ｂの内径が、坩堝１０の外径よりも小さくなっている。例えば、下側開口１７Ａの内径の大きさを、坩堝１０近傍部分での保温部材１７の内径と同様の大きさとした場合や、軸体１２ａと下側開口１２Ａの中心位置がすれて、軸体１２ａと下側開口１２Ａの内周面との離間距離が部分的に大きい場合など、下側開口１７Ａの近傍において乱流が生じやすい。また、上側開口１７Ｂを比較的大きくした場合なども、この上側開口１７Ｂの近傍において乱流が発生し易い。本実施形態では、軸体１２ａの中心軸に一致する仮想線Ｃが、下側開口１７Ａの中心および上側開口１７Ｂの中心を通過するとともに、下側開口１７Ａの内径および上側開口１７Ｂの内径が、坩堝１０の外径よりも小さいので、下側開口１７Ａや上側開口１７Ｂの近傍における乱流の発生を抑制している。   In the growth apparatus 1, an imaginary line C that coincides with the central axis of the shaft body 12a passes through the center of the lower opening 17A and the center of the upper opening 17B, and the inner diameter of the lower opening 17A and the inner diameter of the upper opening 17B. However, it is smaller than the outer diameter of the crucible 10. For example, when the size of the inner diameter of the lower opening 17A is the same as the inner diameter of the heat retaining member 17 in the vicinity of the crucible 10, the center position of the shaft body 12a and the lower opening 12A is offset, Turbulence is likely to occur in the vicinity of the lower opening 17A, such as when the separation distance between 12a and the inner peripheral surface of the lower opening 12A is partially large. Further, even when the upper opening 17B is made relatively large, turbulence is likely to occur near the upper opening 17B. In the present embodiment, an imaginary line C that coincides with the central axis of the shaft body 12a passes through the center of the lower opening 17A and the center of the upper opening 17B, and the inner diameter of the lower opening 17A and the inner diameter of the upper opening 17B are Since it is smaller than the outer diameter of the crucible 10, the occurrence of turbulent flow in the vicinity of the lower opening 17A and the upper opening 17B is suppressed.

図２は、育成装置１が備える保温部材１７の例を拡大して示す断面図である。保温部材１７は、それぞれが貫通孔を有する、複数の部分保温部材１９ａ〜１９ｆが積み上げられて構成されている。部分保温部材１９ａ〜１９ｂは、ジルコニア原料粉末を加圧成型してなる生成型体を焼成した後、研磨等によって高精度に成型する、公知のセラミック部材製造工程を経て製造することができる。   FIG. 2 is an enlarged cross-sectional view showing an example of the heat retaining member 17 included in the growing apparatus 1. The heat retaining member 17 is configured by stacking a plurality of partial heat retaining members 19a to 19f each having a through hole. The partial heat retaining members 19a to 19b can be manufactured through a known ceramic member manufacturing process in which a formed body formed by press-molding zirconia raw material powder is fired and then molded with high accuracy by polishing or the like.

また、図１に示すように、保温部材１７の内周面の断面線は、下側開口１７Ａから上側開口１７Ｂに向けて、滑らかな曲線状とされている。保温部材１７の内周面に顕著な段差があれば、その段差部分で希ガスの流れに剥離が生じて乱流が発生し易い。本実施形態では、このような、保温部材１７の内周面の段差における乱流の発生を抑制している。なお、図３は、サファイア単結晶育成装置の他の実施形態の例について説明する図である。図３において、図１と対応する部材については、図１と同じ図および符号を用いて示している。希ガスの流れが十分に小さい場合など、保温部材１７の内周面における希ガスの乱流が十分に無視できる場合など、保温部材１７の内周面の断面線を必ずしも滑らかな曲線状とする必要はなく、図３に示すように段差状としてもよい。図３に示す例では、保温部材１７の内周面を高精度に成型・研磨する必要がないので、育成装置１が比較的安価に構成できる。   Moreover, as shown in FIG. 1, the cross-sectional line of the inner peripheral surface of the heat retaining member 17 has a smooth curved shape from the lower opening 17A toward the upper opening 17B. If there is a notable step on the inner peripheral surface of the heat retaining member 17, turbulence is likely to occur due to separation of the rare gas flow at the step. In the present embodiment, the occurrence of such turbulent flow at the step on the inner peripheral surface of the heat retaining member 17 is suppressed. In addition, FIG. 3 is a figure explaining the example of other embodiment of a sapphire single crystal growth apparatus. In FIG. 3, members corresponding to those in FIG. 1 are shown using the same drawings and symbols as in FIG. 1. When the flow of the rare gas is sufficiently small, or when the turbulent flow of the rare gas on the inner peripheral surface of the heat retaining member 17 is sufficiently negligible, the cross-sectional line of the inner peripheral surface of the heat retaining member 17 is not necessarily a smooth curved line. It is not necessary, and may be stepped as shown in FIG. In the example shown in FIG. 3, since it is not necessary to mold and polish the inner peripheral surface of the heat retaining member 17 with high accuracy, the growing device 1 can be configured at a relatively low cost.

また、坩堝載置体１２ｂが、坩堝１０の外形に対して大きく張り出している場合などは、この張り出した部分において希ガスの流れの剥離が生じやすい。坩堝載置体１２ｂの外径を、坩堝１０の外径よりも小さくすることで、乱流の発生を抑制している。また、図１に示すように、坩堝１０が載置された坩堝載置体１２ｂの表面の断面線も、保温部材１７の内周面の断面線と同様に滑らかな曲線状とされている。これにより、坩堝載置体１２ｂ近傍部分での乱流の発生を抑制している。   In addition, when the crucible mounting body 12b is greatly extended with respect to the outer shape of the crucible 10, the separation of the rare gas flow is likely to occur at the protruding portion. Generation | occurrence | production of a turbulent flow is suppressed by making the outer diameter of the crucible mounting body 12b smaller than the outer diameter of the crucible 10. FIG. Further, as shown in FIG. 1, the cross-sectional line of the surface of the crucible mounting body 12 b on which the crucible 10 is mounted is also a smooth curved line like the cross-sectional line of the inner peripheral surface of the heat retaining member 17. Thereby, generation | occurrence | production of the turbulent flow in the crucible mounting body 12b vicinity part is suppressed.

また、坩堝保持部材１２は、坩堝載置体１２ｂに坩堝１０が載置された状態で、坩堝１０ととともに軸体１２ａの中心軸周りに回転する。この回転に伴って、ガス供給管６２の流出口６２ａから流出した希ガスは、軸体１２ａの表面にひきずられるように流れ、坩堝１０と保温部材１７との間隙に形成される希ガスの流れに、軸体１２ａの中心軸周りに回転する速度成分が付加される。これにより、坩堝１０と保温部材１７との間隙において、坩堝１０の周方向全体にわたって、軸体１２ａの側面から坩堝１０の側面を流れた後に上側開口１７Ｂを通過して間隙から流出する、希ガスの流れを形成することができる。   The crucible holding member 12 rotates around the central axis of the shaft body 12a together with the crucible 10 in a state where the crucible 10 is placed on the crucible placing body 12b. Along with this rotation, the rare gas flowing out from the outlet 62 a of the gas supply pipe 62 flows so as to be dragged to the surface of the shaft body 12 a, and the flow of the rare gas formed in the gap between the crucible 10 and the heat retaining member 17. In addition, a speed component rotating around the central axis of the shaft body 12a is added. Thereby, in the gap between the crucible 10 and the heat retaining member 17, the rare gas that flows through the side surface of the crucible 10 from the side surface of the shaft body 12 a over the entire circumferential direction of the crucible 10 and then flows out from the gap through the upper opening 17 </ b> B. Flow can be formed.

サファイア単結晶育成装置１におけるサファイア単結晶の育成では、まず坩堝１０内に、サファイア単結晶の原料である酸化アルミニウム粉末が投入される。次に、排気部７０によって、ガス排気管７２を介して育成室１６内の気体を排気した後、ガス供給手段６０により、ガス供給管６２を介して育成室１６内に継続してアルゴンガスを供給しながら、排気部７０によって排気を継続する。この際、坩堝回転機構８０によって、軸体１２ａの中心軸周りの回転が継続して実施される。   In the growth of the sapphire single crystal in the sapphire single crystal growth apparatus 1, first, aluminum oxide powder that is a raw material of the sapphire single crystal is put into the crucible 10. Next, after exhausting the gas in the growth chamber 16 through the gas exhaust pipe 72 by the exhaust unit 70, argon gas is continuously supplied into the growth chamber 16 through the gas supply pipe 62 by the gas supply means 60. While supplying, the exhaust unit 70 continues the exhaust. At this time, the crucible rotating mechanism 80 continues to rotate around the central axis of the shaft body 12a.

ガス供給管６２の流出口６２ａの少なくとも１つは、保温部材１７の下側開口１７Ａの近傍において、この下側開口１７Ａと対向するように配置されており、排気管７２の吸入口７２ａは、保温部材１７の上側開口１７Ｂの近傍において、上側開口１７Ｂと対向するように配置されている。ガス供給手段６０による希ガスの供給および排気手段７０による排気によって、軸体１２ａの側面から坩堝１０の側面を流れた後に上側開口１７Ｂを通過して間隙から流出する、希ガスの流れが形成される。以降、このガス供給手段６０による希ガスの供給、および排気手段７０による排気を継続し、上記希ガスの流れをサファイア単結晶の育成が終了するまで、継続して実施する。   At least one of the outlets 62a of the gas supply pipe 62 is disposed in the vicinity of the lower opening 17A of the heat retaining member 17 so as to face the lower opening 17A. In the vicinity of the upper opening 17B of the heat retaining member 17, it is arranged so as to face the upper opening 17B. By the supply of the rare gas by the gas supply means 60 and the exhaust by the exhaust means 70, a flow of the rare gas is formed which flows from the side surface of the shaft body 12a through the side surface of the crucible 10 and then flows out of the gap through the upper opening 17B. The Thereafter, the supply of the rare gas by the gas supply means 60 and the exhaust by the exhaust means 70 are continued, and the flow of the rare gas is continued until the growth of the sapphire single crystal is completed.

育成室１６がアルゴンガス雰囲気となり、軸体１２ａの側面から坩堝１０の側面を流れた後に上側開口１７Ｂを通過して間隙から流出する希ガスの流れが形成された状態で、高周波電源３０によって誘導コイル３２に高周波電流を流し、坩堝１０の側壁を発熱させる。坩堝１０が発熱して高温となることで、坩堝１０内のサファイア単結晶原料が溶融し、溶融したサファイア単結晶原料（サファイア原料融液）が坩堝１０によって保持された状態となる。   Induced by the high-frequency power source 30 in a state where the growth chamber 16 is in an argon gas atmosphere and a flow of a rare gas flowing from the side surface of the shaft body 12a through the side surface of the crucible 10 and then passing through the upper opening 17B and flowing out of the gap is formed. A high-frequency current is passed through the coil 32 to heat the side wall of the crucible 10. When the crucible 10 generates heat and becomes high temperature, the sapphire single crystal raw material in the crucible 10 is melted, and the molten sapphire single crystal raw material (sapphire raw material melt) is held in the crucible 10.

このように、サファイア原料融液が坩堝１０に保持された状態で、坩堝１０内のサファイア原料融液の液面に、種結晶１３が接触させられる。種結晶１３は、引き上げ軸４２の先端に保持されて、坩堝１０の開口１１から、先端に種結晶１３が取り付けられた引き上げ軸４２が坩堝１０内に挿入されて、坩堝１０の溶融原料の液面に種結晶１３が接触する。引き上げ軸４２は、坩堝１０の開口１１の中心を通る中心軸Ｃに対応する位置に配置されており、種結晶１３の一部が中心軸Ｃに対応する位置においてサファイア原料融液に接触する。   In this way, the seed crystal 13 is brought into contact with the liquid surface of the sapphire raw material melt in the crucible 10 while the sapphire raw material melt is held in the crucible 10. The seed crystal 13 is held at the tip of the pulling shaft 42, and the pulling shaft 42 with the seed crystal 13 attached to the tip is inserted into the crucible 10 from the opening 11 of the crucible 10, so The seed crystal 13 contacts the surface. The pulling shaft 42 is disposed at a position corresponding to the central axis C passing through the center of the opening 11 of the crucible 10, and a part of the seed crystal 13 contacts the sapphire raw material melt at a position corresponding to the central axis C.

種結晶１３をサファイア原料融液に接触させた後、引き上げ軸４２は、中心軸Ｃを中心に回転しながら種結晶１３を上方に上昇させる。これにより、種結晶１３を起点に、溶融原料の単結晶（サファイア単結晶体１５）が上方に引き上げられるように成長する。   After bringing the seed crystal 13 into contact with the sapphire raw material melt, the pulling shaft 42 raises the seed crystal 13 upward while rotating about the central axis C. Thereby, starting from the seed crystal 13, the single crystal (sapphire single crystal 15) of the melting raw material is grown so as to be pulled upward.

サファイアのように、赤外線や可視光に対して比較的高い透過率を有する結晶では、結晶の内部を輻射熱が伝熱し易く、サファイア単結晶体１５を伝わって坩堝１０内のサファイア原料融液から逃げる熱量が比較的大きい。サファイア単結晶を引き上げ法によって成長させる場合に、坩堝１０の周辺は、比較的温度が低下し易い。坩堝１０の周辺の温度低
下を抑制するには、保温部材１７を坩堝１０になるべく近接して配置したり、坩堝１０の周囲を全体的になるべく広く包むように、保温部材１７を大きくするといった手段が考えられる。しかしながら、このように保温部材１７を坩堝１０に近接させたり、保温部材１７を大きくした場合、上述した保温部材１７から発生するアウトガスやパーティクルが多くなり易く、また、坩堝１０に保持されたサファイア原料融液に、パーティクル等が入り易くなってしまう。 In a crystal having a relatively high transmittance with respect to infrared rays and visible light, such as sapphire, the radiant heat is easily transferred inside the crystal, and it escapes from the sapphire raw material melt in the crucible 10 through the sapphire single crystal body 15. The amount of heat is relatively large. When the sapphire single crystal is grown by the pulling method, the temperature around the crucible 10 is relatively easy to decrease. In order to suppress the temperature drop around the crucible 10, there are means such as arranging the heat retaining member 17 as close as possible to the crucible 10 or enlarging the heat retaining member 17 so as to wrap the entire periphery of the crucible 10 as widely as possible. Conceivable. However, when the heat retaining member 17 is brought close to the crucible 10 or the heat retaining member 17 is enlarged as described above, the outgas and particles generated from the heat retaining member 17 described above tend to increase, and the sapphire raw material retained in the crucible 10 Particles and the like are likely to enter the melt.

本実施形態では、保温部材１７を配置して、坩堝１０の周辺の温度低下を抑制しつつ、間隙に形成する希ガスの流れによって、サファイア単結晶体への不純物の混入や気泡の発生を抑制している。このため本発明によれば、保温部材１７を大きくしたり、坩堝１０と保温部材１７との間隙を狭くしても、サファイア原料融液内へのパーティクル等の混入が少ないので、保温部材１７を大きく、かつ坩堝１０との距離を近くして、坩堝１０周辺の温度低下を保温部材１７によって効果的に抑制することができる。本発明によれば、例えばアフターヒータ部材や、輻射熱の拡散を抑制する反射鏡等の機構を設けることなく、保温部材１７のみの比較的安価な構成で、坩堝１０周囲の温度低下を十分に抑制することができる。   In the present embodiment, the heat retaining member 17 is arranged to suppress the decrease in temperature around the crucible 10 and suppress the introduction of impurities and bubbles in the sapphire single crystal by the flow of the rare gas formed in the gap. doing. For this reason, according to the present invention, even if the heat retaining member 17 is enlarged or the gap between the crucible 10 and the heat retaining member 17 is narrowed, particles are not mixed into the sapphire raw material melt. The temperature reduction around the crucible 10 can be effectively suppressed by the heat retaining member 17 with a large distance from the crucible 10. According to the present invention, for example, an after-heater member or a reflecting mirror that suppresses the diffusion of radiant heat is not provided, and a temperature reduction around the crucible 10 is sufficiently suppressed with a relatively inexpensive configuration including only the heat retaining member 17. can do.

以上、本発明の実施形態について説明したが、本発明は上述の各種実施形態に限定されるものでなく、本発明の要旨を逸脱しない範囲において、各種の改良および変更を行なってもよいのはもちろんである。   As mentioned above, although embodiment of this invention was described, this invention is not limited to the above-mentioned various embodiment, In the range which does not deviate from the summary of this invention, it is possible to perform various improvements and changes. Of course.

１ サファイア単結晶育成装置
８ 坩堝回転機構
１０ 坩堝
１２ 坩堝保持部材
１２ａ 軸体
１２ｂ 坩堝載置体
１３ 種結晶
１６ 育成室
１７ 保温部材
１７Ａ 下側開口
１７Ｂ 上側開口
３０ 高周波電源
３２ 誘導コイル
４０ 結晶引き上げ機構
５０ 制御部
６０ ガス供給手段
７０ 排気手段
８０ 坩堝回転機構 DESCRIPTION OF SYMBOLS 1 Sapphire single crystal growth apparatus 8 Crucible rotating mechanism 10 Crucible 12 Crucible holding member 12a Shaft body 12b Crucible mounting body 13 Seed crystal 16 Growth chamber 17 Heat retaining member 17A Lower opening 17B Upper opening 30 High frequency power supply 32 Inductive coil 40 Crystal pulling mechanism 50 Control Unit 60 Gas Supply Unit 70 Exhaust Unit 80 Crucible Rotating Mechanism

Claims (3)

サファイア原料融液を保持する坩堝と、
該坩堝の下方に配置されて当接した、該坩堝を保持する坩堝保持部材と、
サファイア種結晶を保持して上下動し、前記坩堝内の前記サファイア原料融液に前記サファイア種結晶を接触させた後に上昇させることで、該サファイア種結晶に連続したサファイア単結晶体を引き上げるための引き上げ機構と、
前記坩堝保持部材が挿通した下側開口、および前記引き上げ機構によって上下動する前記サファイア種結晶が通過する上側開口を有する、前記坩堝の周囲を囲む保温部材と、
高周波電流が流れることで前記坩堝を発熱させてサファイア原料を溶融させ、前記坩堝内に前記サファイア原料融液を保持させるための、前記保温部材を介して前記坩堝の周囲に配置された誘導コイルと、
前記坩堝の周辺部分に希ガスを供給するためのガス供給手段とを備えたサファイア単結晶育成装置であって、
前記坩堝保持部材は、前記保温部材の前記下側開口に挿通された、前記坩堝の外径よりも小さい外径を有する軸体と、該軸体の上端部に設けられた、前記軸体の外径よりも大きく、かつ前記坩堝の外径よりも小さい外径を有する、前記坩堝が載置された坩堝載置体とを備え、
前記ガス供給手段は、前記保温部材の前記下側開口から、前記軸体に沿って前記坩堝と前記保温部材との間隙に向けて前記希ガスを流すことで、前記軸体の側面から前記坩堝の側面を流れた後に前記上側開口を通過して前記間隙から流出する前記希ガスの流れを形成することを特徴とするサファイア単結晶育成装置。 A crucible holding a sapphire raw material melt;
A crucible holding member for holding the crucible, disposed below and in contact with the crucible;
Holding the sapphire seed crystal and moving up and down to raise the sapphire single crystal continuous to the sapphire seed crystal by raising the sapphire seed crystal after contacting the sapphire raw material melt in the crucible A lifting mechanism;
A heat retaining member surrounding the periphery of the crucible, having a lower opening through which the crucible holding member is inserted, and an upper opening through which the sapphire seed crystal moving up and down by the lifting mechanism passes;
An induction coil disposed around the crucible via the heat retaining member for heating the crucible by flowing a high-frequency current to melt the sapphire raw material and holding the sapphire raw material melt in the crucible; ,
A sapphire single crystal growth apparatus comprising a gas supply means for supplying a rare gas to a peripheral portion of the crucible,
The crucible holding member is inserted into the lower opening of the heat retaining member, and has a shaft body having an outer diameter smaller than the outer diameter of the crucible, and an upper end portion of the shaft body. A crucible mounting body on which the crucible is mounted, having an outer diameter larger than the outer diameter and smaller than the outer diameter of the crucible,
The gas supply means causes the rare gas to flow from the lower opening of the heat retaining member toward the gap between the crucible and the heat retaining member along the shaft body, so that the crucible is formed from a side surface of the shaft body. An apparatus for growing a sapphire single crystal that forms a flow of the rare gas that flows through the upper opening and then flows out of the gap after flowing through the side surface of the sapphire. 前記軸体の中心軸に一致する仮想線が、前記下側開口の中心および前記上側開口の中心を通過するとともに、前記下側開口の内径および前記上側開口の内径が、前記坩堝の外径よりも小さいことを特徴とする請求項１記載のサファイア単結晶育成装置。   An imaginary line that coincides with the central axis of the shaft passes through the center of the lower opening and the center of the upper opening, and the inner diameter of the lower opening and the inner diameter of the upper opening are larger than the outer diameter of the crucible. The sapphire single crystal growing apparatus according to claim 1, wherein the sapphire single crystal growing apparatus is also small. 前記坩堝保持部材は、前記坩堝載置体に前記坩堝が載置された状態で、該坩堝ととともに前記軸体の中心軸周りに回転することを特徴とする請求項１または２記載のサファイア単結晶育成装置。

3. The sapphire unit according to claim 1, wherein the crucible holding member rotates around a central axis of the shaft body together with the crucible in a state where the crucible is placed on the crucible placing body. Crystal growth device.

JP2012042890A 2012-02-29 2012-02-29 Sapphire single crystal growth apparatus Pending JP2013177280A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018095511A (en) * 2016-12-13 2018-06-21 住友金属鉱山株式会社 Hot zone structure of high frequency induction heating furnace, and rearing method of oxide single crystal using hot zone structure
CN116949562A (en) * 2023-09-19 2023-10-27 内蒙古晶环电子材料有限公司 Sapphire crystal growth furnace
CN117488402A (en) * 2024-01-02 2024-02-02 内蒙古晶环电子材料有限公司 Temperature regulation and control method of sapphire crystal growth furnace
CN117552110A (en) * 2024-01-02 2024-02-13 内蒙古晶环电子材料有限公司 Heat preservation structure and crystal growth furnace

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018095511A (en) * 2016-12-13 2018-06-21 住友金属鉱山株式会社 Hot zone structure of high frequency induction heating furnace, and rearing method of oxide single crystal using hot zone structure
CN116949562A (en) * 2023-09-19 2023-10-27 内蒙古晶环电子材料有限公司 Sapphire crystal growth furnace
CN116949562B (en) * 2023-09-19 2024-02-13 内蒙古晶环电子材料有限公司 Sapphire crystal growth furnace
CN117488402A (en) * 2024-01-02 2024-02-02 内蒙古晶环电子材料有限公司 Temperature regulation and control method of sapphire crystal growth furnace
CN117552110A (en) * 2024-01-02 2024-02-13 内蒙古晶环电子材料有限公司 Heat preservation structure and crystal growth furnace

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