JP2006273685A - Single crystal producing apparatus - Google Patents
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本発明は、原料融液の液面に種結晶を接触させながら引き上げて単結晶を成長させる単結晶製造装置に関し、特に、高純度の大きな単結晶を育成することが可能な単結晶製造装置に関する。 The present invention relates to a single crystal manufacturing apparatus that grows a single crystal by pulling a seed crystal in contact with a liquid surface of a raw material melt, and particularly relates to a single crystal manufacturing apparatus that can grow a large single crystal with high purity. .
単結晶の製造方法の１つとして、原料を収容したルツボをコイルで加熱し、その熱でルツボ内の原料を溶解することにより得られた融液に種結晶を接触および回転させながら種結晶を引き上げることにより種結晶に単結晶を成長させるチョクラルスキー法（Czochralski：ＣＺ法）がある。 As one method for producing a single crystal, a crucible containing a raw material is heated with a coil, and the seed crystal is brought into contact with and rotated by a melt obtained by melting the raw material in the crucible with the heat. There is a Czochralski method (CZ method) in which a single crystal is grown on a seed crystal by pulling up.
しかし、上記したチョクラルスキー法では、原料融液が加熱によってルツボ内での対流にともなって原料およびルツボに含まれる不純物、あるいはルツボを構成する元素が原料融液中に溶け出して表面に浮上し、中心付近に不純物として浮遊する現象が生じる。この不純物を放置したままにすると、成長界面に介在し、単結晶を成長させる際の障害になり、高純度の大きな単結晶を得ることができないため、少なくとも種結晶の直下には介在させないようにする必要がある。 However, in the Czochralski method described above, the raw material melt is heated to cause convection in the crucible, and the impurities contained in the raw material and the crucible, or the elements constituting the crucible, dissolve into the raw material melt and float on the surface. However, a phenomenon of floating as an impurity near the center occurs. If this impurity is left unattended, it will intervene at the growth interface, which will hinder the growth of a single crystal, and a large single crystal with high purity cannot be obtained. There is a need to.
融液面の不純物を成長界面に介在させない方法として、例えば、パージチューブ法があり、ガス等を不純物に吹きかけて吹き飛ばす方法が知られている（例えば、非特許文献１参照。）。 As a method for preventing impurities on the melt surface from interposing on the growth interface, for example, there is a purge tube method, and a method is known in which a gas or the like is blown off and blown away (see, for example, Non-Patent Document 1).
しかし、従来の単結晶製造方法によれば、パージチューブ法によって成長界面から吹き飛ばしても、ルツボ外へは除去できないので、対流にともなって再び成長界面に現れる恐れがあるため、完全な解決にはならない。 However, according to the conventional single crystal manufacturing method, even if it blows off from the growth interface by the purge tube method, it cannot be removed out of the crucible, so it may appear again at the growth interface due to convection. Don't be.
従って、本発明の目的は、高純度の大きな単結晶を育成することが可能な単結晶製造装置を提供することにある。 Accordingly, an object of the present invention is to provide a single crystal production apparatus capable of growing a large single crystal with high purity.
本発明は、上記目的を達成するため、ルツボに収納した原料を加熱することにより溶融した融液の液面に種結晶を接触させながら引き上げて単結晶を成長させる単結晶製造装置において、前記融液の表面に浮遊する不純物を除去する不純物除去手段を設けたことを特徴とする単結晶製造装置を提供する。 In order to achieve the above object, the present invention provides a single crystal production apparatus for growing a single crystal by pulling a seed crystal in contact with a liquid surface of a melt melted by heating a raw material stored in a crucible. Provided is a single crystal manufacturing apparatus provided with an impurity removing means for removing impurities floating on the surface of a liquid.
この構成によれば、融液の表面に浮遊する不純物を除去するため、種結晶は、不純物の少ない融液と接触する。そのため、高純度の単結晶を成長させることができる。 According to this configuration, in order to remove impurities floating on the surface of the melt, the seed crystal comes into contact with the melt with less impurities. Therefore, a high-purity single crystal can be grown.
前記不純物除去手段は、前記不純物を表面に付着させる不純物除去部材と、前記不純物除去部材を前記融液面に対して接触および退避させる駆動手段とを備えることが好ましい。 The impurity removing unit preferably includes an impurity removing member that attaches the impurity to the surface, and a driving unit that contacts and retracts the impurity removing member with respect to the melt surface.
前記不純物除去部材は、前記不純物をすくい取る不純物除去部を有することが好ましい。 The impurity removing member preferably has an impurity removing portion that scoops up the impurities.
前記不純物除去部材は、前記種結晶に同心円状に配置され、下端が前記融液面に接触する略円筒形であることが好ましい。 The impurity removing member is preferably concentric with the seed crystal and has a substantially cylindrical shape whose lower end is in contact with the melt surface.
前記不純物除去部材は、前記原料と同じ材料、あるいは前記原料の融点より高い融点を有する材料で構成されることが好ましい。 The impurity removing member is preferably made of the same material as the raw material or a material having a melting point higher than the melting point of the raw material.
前記不純物除去手段は、前記種結晶に同心円状に配置され、下端が前記融液面に接触する円筒形の不純物除去部材と、前記融液面の液面下降に応じて前記融液面との接触を保持したまま前記不純物除去部材を下降させる駆動手段とを備えることが好ましい。 The impurity removing means is arranged concentrically with the seed crystal, and has a cylindrical impurity removing member whose lower end is in contact with the melt surface, and the melt surface in response to a drop in the melt surface. It is preferable to include a driving unit that lowers the impurity removing member while maintaining contact.
本発明に係る単結晶製造装置によれば、高純度の大きな単結晶を育成することができる。 According to the single crystal manufacturing apparatus according to the present invention, a large single crystal with high purity can be grown.
［第１の実施の形態］
（単結晶製造装置）
図１は、本発明の第１の実施の形態に係る単結晶製造装置を示す。この単結晶製造装置１は、側面に覗き窓１０ａを有し上部に形成されたガス供給口１０ｂからＡｒ等の不活性ガスが充填され、内部をＡｒ雰囲気にされたチャンバー１０と、チャンバー１０内に設置され、セラミック等からなる断熱部１１と、断熱部１１と同軸状に配置された高周波コイル１２と、原料、例えば、β−Ｇａ２Ｏ３の融液１３が満たされる凹部を有するルツボ１４と、ルツボ１４上に退避可能に配設されるとともに原料と同一材料で構成された不純物除去部材１５と、不純物除去部材１５を吊り下げるワイヤ１６と、ワイヤ１６がチャンバー１０の外部に引き出されるように挿通されるとともにチャンバー１０の天井部１０ｂに回動可能に取り付けられたパイプによる回動軸１７と、ルツボ１４の上方に配設された、例えば、β−Ｇａ２Ｏ３単結晶からなる種結晶１８と、種結晶１８を保持する種結晶ロッド１９と、高周波コイル１２を駆動する高周波電源２０と、種結晶ロッド１９に取り付けられて単結晶の重量を測定するロードセル２１と、ロードセル２１の出力に基づいて高周波電源２０を制御する制御部２２とを有する。回動軸１７は、所定の曲率を有する曲げ部１７ａが形成されている。不純物除去部材１５、ワイヤ１６、および回動軸１７により、不純物除去手段を形成している。
[First Embodiment]
(Single crystal manufacturing equipment)
FIG. 1 shows a single crystal manufacturing apparatus according to a first embodiment of the present invention. This single crystal manufacturing apparatus 1 includes a chamber 10 having a viewing window 10a on its side surface and filled with an inert gas such as Ar from a gas supply port 10b formed on the upper side, and the inside of the chamber 10 having an Ar atmosphere. And a crucible 14 having a recess filled with a raw material, for example, a melt 13 of β-Ga 2 O 3 , a heat insulating part 11 made of ceramic or the like, a high-frequency coil 12 arranged coaxially with the heat insulating part 11, and the like. An impurity removing member 15 that is removably disposed on the crucible 14 and made of the same material as the raw material, a wire 16 that suspends the impurity removing member 15, and a wire 16 that is pulled out of the chamber 10. Is disposed above the crucible 14 and a pivot shaft 17 that is inserted into the ceiling portion 10b of the chamber 10 and is pivotally attached to the ceiling portion 10b of the chamber 10. a seed crystal 18 made of β-Ga 2 O 3 single crystal, a seed crystal rod 19 for holding a seed crystal 18, the weight of the high-frequency power source 20 for driving the high-frequency coil 12, mounted on the seed crystal rod 19 monocrystal And a control unit 22 for controlling the high-frequency power source 20 based on the output of the load cell 21. The rotating shaft 17 is formed with a bent portion 17a having a predetermined curvature. Impurity removing means is formed by the impurity removing member 15, the wire 16, and the rotating shaft 17.
断熱部１１は、その上部に凹部１１ａが形成され、その凹部１１ａにルツボ１４が載置される。ルツボ１４は、Ｉｒ、黒鉛、モリブデン等を用いてもよい。ルツボ１４は、耐熱性、耐酸性を考慮するとＩｒが好ましい。 As for the heat insulation part 11, the recessed part 11a is formed in the upper part, and the crucible 14 is mounted in the recessed part 11a. The crucible 14 may be made of Ir, graphite, molybdenum or the like. The crucible 14 is preferably Ir in consideration of heat resistance and acid resistance.
不純物除去部材１５は、原料が、例えば、β−Ｇａ２Ｏ３である場合、β−Ｇａ２Ｏ３の原料粉を圧縮・焼結して形成される。また、β−Ｇａ２Ｏ３より融点の高い材料、例えば、サファイアにより形成してもよい。 When the raw material is, for example, β-Ga 2 O 3 , the impurity removing member 15 is formed by compressing and sintering the raw material powder of β-Ga 2 O 3 . Further, a material having higher melting point than β-Ga 2 O 3, for example, may be formed by sapphire.
（不純物の除去動作）
図２は回動軸１７の配置を示し、図３は不純物の発生状況を示す。また、図４は、不純物除去部材による不純物の除去工程を示す。なお、図３においては、図を簡略にするため、高周波コイル１２の図示を省略している。図１〜図４を参照して不純物の除去動作を説明する。
(Removal of impurities)
FIG. 2 shows the arrangement of the rotating shaft 17, and FIG. 3 shows the state of generation of impurities. FIG. 4 shows an impurity removal process by the impurity removal member. In FIG. 3, the high-frequency coil 12 is not shown in order to simplify the drawing. The impurity removal operation will be described with reference to FIGS.
図１において、作業者は、ルツボ１４に所定の原料を入れたあと、単結晶製造装置１の電源をオンにし、高周波電源２０から高周波コイル１２に高周波電力を供給し、ルツボ１４の側壁を介して原料を加熱して融解させ、融液１３を生成する。作業者は、所定の時間が経過した時点で、覗き窓１０ａから不純物の発生状況を観察する。 In FIG. 1, the operator puts a predetermined raw material in the crucible 14, turns on the power of the single crystal manufacturing apparatus 1, supplies high-frequency power from the high-frequency power supply 20 to the high-frequency coil 12, and passes through the side wall of the crucible 14. The raw material is heated and melted to produce the melt 13. The operator observes the state of generation of impurities from the viewing window 10a when a predetermined time has elapsed.
ここで、図３を参照して不純物の発生原理を説明する。図３の（ａ），（ｂ）に示すように、ルツボ１４では、高周波コイル１２の加熱によって融液１３に矢印Ａで示すように外側から中心に向かって対流が生じている。この対流によって融液１３の表面の中心部には、不純物２３が浮遊しながら滞留する。 Here, the principle of impurity generation will be described with reference to FIG. As shown in FIGS. 3A and 3B, in the crucible 14, convection is generated in the melt 13 from the outside toward the center as indicated by an arrow A due to the heating of the high-frequency coil 12. Due to this convection, the impurity 23 stays in the center of the surface of the melt 13 while floating.
図３のように不純物２３が浮遊していた場合、作業者は、図示せぬ手段により回動軸１７を回動させ、不純物除去部材１５をルツボ１４の中心部上に位置決めする。ついで、不純物除去部材１５を降下させ、図４に示すように、不純物除去部材１５の下面を不純物２３に接触させる。作業者は、ワイヤ１６を操作しながら、不純物２３を沈下させるか、不純物除去部材１５の下面に付着させて融液１３と不純物２３とを不純物除去部材１５とともに上昇させて融液１３を凝固させて不純物２３を不純物除去部材１５に付着させ、あるいは両方を行って融液面に浮遊する不純物２３を除去する。除去後、回動軸１７をチャンバー１０の内壁方向へ回動させ、種結晶１８に接触しない位置に退避させる。次に、種結晶１８を回転させながら下降させ、下面を融液１３に接触させた後、単結晶を育成する。 When the impurity 23 is floating as shown in FIG. 3, the operator rotates the rotating shaft 17 by means not shown to position the impurity removing member 15 on the center portion of the crucible 14. Next, the impurity removing member 15 is lowered, and the lower surface of the impurity removing member 15 is brought into contact with the impurity 23 as shown in FIG. The operator operates the wire 16 to sink the impurities 23 or attach them to the lower surface of the impurity removing member 15 to raise the melt 13 and the impurities 23 together with the impurity removing member 15 to solidify the melt 13. The impurities 23 are adhered to the impurity removing member 15 or both are performed to remove the impurities 23 floating on the melt surface. After the removal, the pivot shaft 17 is pivoted toward the inner wall of the chamber 10 and retracted to a position where it does not contact the seed crystal 18. Next, the seed crystal 18 is lowered while being rotated, the lower surface is brought into contact with the melt 13, and then a single crystal is grown.
単結晶は、一定の速度で引き上げられて円錐状に育成させられ、次いで、引上げ速度を変えられ、大径の単結晶を育成させられる。この成長が行われている間、ロードセル２１からは重量信号が出力されており、この重量信号に基づいて、制御部２２は単結晶が所望の径になるようにフィードバック制御を実行する。 The single crystal is pulled up at a constant speed and grown in a conical shape, and then the pulling speed is changed to grow a large-diameter single crystal. While this growth is being performed, a weight signal is output from the load cell 21, and based on this weight signal, the control unit 22 performs feedback control so that the single crystal has a desired diameter.
（第１の実施の形態の効果）
この第１の実施の形態によれば、以下の効果を奏する。
（イ）不純物除去部材１５によって不純物２３をルツボ１４の外に除去することができるため、高純度の大きな単結晶を育成することができる。
（ロ）従来の単結晶製造装置に不純物除去部材１５、ワイヤ１６、および回動軸１７を追加するのみでよいため、構成を簡単にすることができるとともに、単結晶製造装置のコストアップを防止することができる。
（ハ）原料と不純物除去部材１５とは、同一の材料で形成されるため、不純物除去部材１５が融解しても、不純物が増加することがない。
（ニ）不純物除去部材１５を原料の融点より高い融点を有する材料で形成する場合、不純物除去部材１５は、融液１３により融解されないため、原料融液中に不純物として溶け出さない。
（ホ）回動軸１７は、所定の曲率を有する曲げ部１７ａを設けているため、ワイヤが曲げ部１７で引っ掛からなくなるので、不純物除去部材１５の操作が容易になる。
(Effects of the first embodiment)
According to the first embodiment, the following effects are obtained.
(A) Since the impurities 23 can be removed out of the crucible 14 by the impurity removing member 15, a large single crystal with high purity can be grown.
(B) Since only the impurity removing member 15, the wire 16, and the rotating shaft 17 need be added to the conventional single crystal manufacturing apparatus, the configuration can be simplified and the cost of the single crystal manufacturing apparatus can be prevented from increasing. can do.
(C) Since the raw material and the impurity removing member 15 are formed of the same material, the impurities do not increase even if the impurity removing member 15 is melted.
(D) When the impurity removing member 15 is formed of a material having a melting point higher than that of the raw material, the impurity removing member 15 is not melted by the melt 13 and therefore does not dissolve out as impurities in the raw material melt.
(E) Since the rotating shaft 17 is provided with the bent portion 17a having a predetermined curvature, the wire is not caught by the bent portion 17, so that the operation of the impurity removing member 15 is facilitated.
なお、第１の実施の形態では、不純物除去部材１５の下面に不純物２３を付着させる除去方法を説明したが、他の方法として、不純物除去部材１５を下降させて融液１３とともに不純物２３を付着させ、融液１３の温度降下に基づく結晶化によって不純物除去部材１５の表面に不純物２３を固化させた後、不純物除去部材１５を上昇させることにより融液１３から不純物２３を除去するようにしても良い。 In the first embodiment, the removal method of attaching the impurity 23 to the lower surface of the impurity removal member 15 has been described. However, as another method, the impurity removal member 15 is lowered to attach the impurity 23 together with the melt 13. Then, after the impurities 23 are solidified on the surface of the impurity removing member 15 by crystallization based on the temperature drop of the melt 13, the impurities 23 are removed from the melt 13 by raising the impurity removing member 15. good.
［第２の実施の形態］
図５は、本発明の第２の実施の形態に係る単結晶製造装置の不純物除去部材を示す。この不純物除去部材１５は、原料と同等またはそれ以上の融点をもつ１本のワイヤを円形の不純物除去部１５ａと、これに直角に伸び、上端がワイヤ１６に結合された直線部１５ｂとを有する形状にしたものであり、その他の単結晶製造装置１の構成は、第１の実施の形態と同様である。
[Second Embodiment]
FIG. 5 shows an impurity removing member of a single crystal manufacturing apparatus according to the second embodiment of the present invention. The impurity removing member 15 has a circular impurity removing portion 15 a made of one wire having a melting point equal to or higher than that of the raw material, and a straight portion 15 b extending perpendicularly to the wire and having an upper end coupled to the wire 16. The other configuration of the single crystal manufacturing apparatus 1 is the same as that of the first embodiment.
第１の実施の形態と同様に、不純物２３を除去する必要が生じたとき、覗き窓１０ａを通して融液面を観察しながらワイヤ１６を操作して不純物除去部材１５を降下し、不純物２３をすくい上げるように不純物除去部材１５を動かすことにより、不純物２３はこの不純物２３に付着している融液１３の表面張力によって不純物除去部１５ａを覆うように付着する。不純物２３を付着させた後の不純物除去部材１５の操作は、第１の実施の形態と同様である。 Similar to the first embodiment, when it becomes necessary to remove the impurities 23, the wire 16 is operated while observing the melt surface through the viewing window 10a to lower the impurity removing member 15 and scoop up the impurities 23. By moving the impurity removing member 15 as described above, the impurity 23 is attached so as to cover the impurity removing portion 15 a by the surface tension of the melt 13 attached to the impurity 23. The operation of the impurity removing member 15 after the impurities 23 are attached is the same as in the first embodiment.
（第２の実施の形態の効果）
この第２の実施の形態によれば、不純物除去部材１５を有するため、単結晶の育成前に不純物を除去するので、高純度で大径の単結晶を育成することができるほか、不純物除去部材１５を非常に簡単に構成できるため、第１の実施の形態の単結晶製造装置１に比べ、さらに低価格化が可能になる。
(Effect of the second embodiment)
According to the second embodiment, since the impurity removing member 15 is provided, the impurities are removed before the single crystal is grown. Therefore, the single crystal having a high purity and a large diameter can be grown, and the impurity removing member. Since 15 can be configured very easily, the cost can be further reduced as compared with the single crystal manufacturing apparatus 1 of the first embodiment.
［第３の実施の形態］
図６は、本発明の第３の実施の形態に係る単結晶製造装置の不純物除去部材を示す。この不純物除去部材１５は、第２の実施の形態において、不純物除去部１５ａを原料と同等またはそれ以上の融点をもつ金属製の網部１５ｃと、この網部１５ｃを保持するとともに直線部１５ｂに連結された円形の支持部１５ｄとを有する構成に特徴があり、その他の構成は第２の実施の形態と同様である。なお、網部１５ｃに代えて、凹面に加工した円板に複数の孔を設けた構成の部材を用いてもよい。
[Third Embodiment]
FIG. 6 shows an impurity removing member of a single crystal manufacturing apparatus according to the third embodiment of the present invention. In the second embodiment, the impurity removing member 15 has a metal net portion 15c having a melting point equal to or higher than that of the raw material, and the net portion 15c and the straight portion 15b. The structure having the connected circular support portions 15d is characterized, and the other structure is the same as that of the second embodiment. Instead of the net portion 15c, a member having a configuration in which a plurality of holes are provided in a disk processed into a concave surface may be used.
（第３の実施の形態の効果）
この第３の実施の形態によれば、第２の実施の形態に比べ、網部１５ｃを設けたため、不純物の除去効果を高めることができる。この不純物除去部材１５は、融液１３の温度で融解しないため、これ自身が不純物になることはない。また、不純物除去部材１５により単結晶の育成前に不純物を除去するので、高純度で大径の単結晶を育成することができる。
(Effect of the third embodiment)
According to the third embodiment, since the mesh portion 15c is provided as compared with the second embodiment, the effect of removing impurities can be enhanced. Since the impurity removing member 15 does not melt at the temperature of the melt 13, it does not become an impurity itself. Further, since the impurities are removed by the impurity removing member 15 before the single crystal is grown, a single crystal having a high purity and a large diameter can be grown.
［第４の実施の形態］
図７は、本発明の第４の実施の形態に係る単結晶製造装置の主要部を示す。また、図８は、図７において種結晶を降下させた状態を示し、図９は、不純物除去部材の引き上げ工程を示す。
[Fourth Embodiment]
FIG. 7 shows a main part of a single crystal manufacturing apparatus according to the fourth embodiment of the present invention. 8 shows a state where the seed crystal is lowered in FIG. 7, and FIG. 9 shows a step of pulling up the impurity removing member.
本実施の形態は、第１の実施の形態において、不純物除去部材１５に代えて、種結晶１８に対して同心円状に配置される円筒型の不純物除去部２４を備えたものであり、その他の構成は第１の実施の形態と同様である。不純物除去部材２４は、原料と同等または原料よりも融点の高い材料で形成する。 In the present embodiment, instead of the impurity removing member 15 in the first embodiment, a cylindrical impurity removing portion 24 arranged concentrically with respect to the seed crystal 18 is provided. The configuration is the same as in the first embodiment. The impurity removing member 24 is formed of a material equivalent to the raw material or having a higher melting point than the raw material.
この第４の実施の形態によれば、融液１３が形成された時点で、不純物除去部材２４を融液１３の液面上に降下させる。融液１３は、高周波コイル１２による加熱で矢印Ａに示す対流が生じており、対流にともなって外側から内側に流れる不純物２３は、不純物除去部材２４の外周面の下端に付着する。したがって、成長界面には不純物２３は侵入しない。この状態で、図８のように、種結晶ロッド１９を降下させ、融液１３の液面に接触させる。単結晶が成長した時点で、図９のように、不純物除去部材２４を融液１３の液面から引き上げる。これにより、単結晶２５の径が大きくなっても、不純物除去部材２４が邪魔になることがない。 According to the fourth embodiment, when the melt 13 is formed, the impurity removing member 24 is lowered onto the liquid surface of the melt 13. In the melt 13, the convection indicated by the arrow A is generated by heating by the high-frequency coil 12, and the impurity 23 flowing from the outside to the inside along with the convection adheres to the lower end of the outer peripheral surface of the impurity removing member 24. Therefore, the impurity 23 does not enter the growth interface. In this state, the seed crystal rod 19 is lowered and brought into contact with the liquid surface of the melt 13 as shown in FIG. When the single crystal grows, the impurity removing member 24 is pulled up from the liquid surface of the melt 13 as shown in FIG. Thereby, even if the diameter of the single crystal 25 becomes large, the impurity removing member 24 does not get in the way.
（第４の実施の形態の効果）
この第４の実施の形態によれば、前記各実施の形態に比べ、不純物の除去効果を高めることができる。また、不純物除去部材２４を有するために高純度で大径の単結晶を育成することができる。
(Effect of the fourth embodiment)
According to the fourth embodiment, the effect of removing impurities can be enhanced as compared with the above embodiments. In addition, since the impurity removing member 24 is provided, a single crystal having a high purity and a large diameter can be grown.
［第５の実施の形態］
図１０は、本発明の第５の実施の形態に係る単結晶製造装置の主要部を示す。本実施の形態は、第４の実施の形態において、不純物除去部材２４に代えて、星形の断面形状を有する不純物除去部材２６を用いたものであり、その他の構成は第４の実施の形態と同様である。なお、不純物除去部材２６は、その外周部分に不純物を付着させるなどにより、不純物を除去する。
[Fifth Embodiment]
FIG. 10 shows a main part of a single crystal manufacturing apparatus according to the fifth embodiment of the present invention. In this embodiment, an impurity removing member 26 having a star-shaped cross section is used in place of the impurity removing member 24 in the fourth embodiment, and other configurations are the same as those in the fourth embodiment. It is the same. The impurity removing member 26 removes impurities by attaching impurities to the outer peripheral portion thereof.
（第５の実施の形態の効果）
この第５の実施の形態によれば、第４の実施の形態に比べ、外周面がルツボ１４の内周面に接触して不純物除去部材２６の内径方向への動きを規制するため、不純物除去部材２６と接触することなく単結晶２５を成長させることができる。
(Effect of 5th Embodiment)
According to the fifth embodiment, as compared with the fourth embodiment, the outer peripheral surface is in contact with the inner peripheral surface of the crucible 14 and restricts the movement of the impurity removing member 26 in the inner diameter direction. The single crystal 25 can be grown without contacting the member 26.
［第６の実施の形態］
図１１は、本発明の第６の実施の形態に係る単結晶製造装置を示す。なお、図１１においては、主要部のみを図示している。本実施の形態は、第４の実施の形態において、不純物除去部材２４を融液１３の液面の減少に同調して下降させるようにしたものであり、その他の構成は第４の実施の形態と同様である。
[Sixth Embodiment]
FIG. 11 shows a single crystal manufacturing apparatus according to the sixth embodiment of the present invention. In FIG. 11, only the main part is shown. In the fourth embodiment, the impurity removing member 24 is lowered in synchronization with the decrease in the liquid level of the melt 13 in the fourth embodiment, and other configurations are the fourth embodiment. It is the same.
不純物除去部材２４は、その上端が昇降動作をする図示しない駆動機構に取り付けられており、この駆動機構は制御部２２によって制御される。制御部２２は、ロードセル２１から出力される重量信号に基づいて融液１３の液面の減量度合いを算出し、その算出量に応じて前記駆動機構を動作させ、不純物除去部材２４を追従下降させる制御を実行する。なお、不純物除去部材２４と駆動機構により、不純物除去手段を形成している。 The impurity removing member 24 is attached to a driving mechanism (not shown) whose upper end moves up and down, and this driving mechanism is controlled by the control unit 22. Based on the weight signal output from the load cell 21, the control unit 22 calculates the degree of decrease in the liquid level of the melt 13, operates the drive mechanism in accordance with the calculated amount, and lowers the impurity removal member 24 by following it. Execute control. The impurity removing member 24 and the driving mechanism form impurity removing means.
種結晶１８が、融液１３の液面に接触した当初は、図１１の（ａ）のように、融液は十分に満たされている。しかし、単結晶２５の成長が進むと、融液１３の液面は、図１１の（ｂ）のように、図１１の（ａ）の高さからｈだけ低下する。この過程において、制御部２２は、ロードセル２１からの重量信号に基づいて前記駆動機構を動作させ、図１１の（ｂ）のように不純物除去部材２４を下降させる。 When the seed crystal 18 comes into contact with the liquid surface of the melt 13, the melt is sufficiently filled as shown in FIG. However, as the growth of the single crystal 25 proceeds, the liquid level of the melt 13 decreases by h from the height of FIG. 11A as shown in FIG. In this process, the control unit 22 operates the drive mechanism based on the weight signal from the load cell 21 and lowers the impurity removing member 24 as shown in FIG.
（第６の実施の形態の効果）
この第６の実施の形態によれば、融液１３の液面変化に追従して不純物除去部材２４を降下させることができるため、液面が下がった状態においても不純物を除去できる。従って、第４の実施の形態よりも不純物の除去量を多くすることができる。
(Effect of 6th Embodiment)
According to the sixth embodiment, since the impurity removing member 24 can be lowered following the change in the liquid level of the melt 13, the impurities can be removed even when the liquid level is lowered. Therefore, the amount of impurities removed can be increased as compared with the fourth embodiment.
［他の実施の形態］
なお、本発明は、上記各実施の形態に限定されず、その要旨を変更しない範囲内で種々な変形が可能である。例えば、図７に示すような円筒形の不純物除去部材の外周にルツボ１４の内周面に伸びる腕を複数設けてもよい。これにより、ルツボ１４の内径方向の動きを規制することができる。
[Other embodiments]
The present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the scope of the invention. For example, a plurality of arms extending to the inner peripheral surface of the crucible 14 may be provided on the outer periphery of a cylindrical impurity removing member as shown in FIG. Thereby, the movement of the crucible 14 in the inner diameter direction can be restricted.
また、不純物除去部材１５は、融点の差が１００℃以内であれば、融液との短時間の接触では融解しないため、不純物除去部材の融点が、原料の融点よりも低くてもよい。 Moreover, since the impurity removal member 15 does not melt in a short time contact with the melt if the difference in melting point is within 100 ° C., the impurity removal member 15 may have a melting point lower than that of the raw material.
１…単結晶製造装置、１０…チャンバー、１０ａ…覗き窓、１０ｂ…ガス供給口、１１…断熱部、１１ａ…凹部、１２…高周波コイル、１３…融液、１４…ルツボ、１５…不純物除去部材、１５ａ…不純物除去部、１５ｂ…直線部、１５ｃ…網部、１５ｄ…支持部、１６…ワイヤ、１７…回動軸、１８…種結晶、１９…種結晶ロッド、２０…高周波電源、２１…ロードセル、２２…制御部、２３…不純物、２４…不純物除去部材、２５…単結晶、２６…不純物除去部材 DESCRIPTION OF SYMBOLS 1 ... Single crystal manufacturing apparatus, 10 ... Chamber, 10a ... Viewing window, 10b ... Gas supply port, 11 ... Heat insulation part, 11a ... Recessed part, 12 ... High frequency coil, 13 ... Melt, 14 ... Crucible, 15 ... Impurity removal member 15a ... impurity removing portion, 15b ... straight portion, 15c ... net portion, 15d ... support portion, 16 ... wire, 17 ... rotating shaft, 18 ... seed crystal, 19 ... seed crystal rod, 20 ... high frequency power source, 21 ... Load cell, 22 ... control unit, 23 ... impurity, 24 ... impurity removing member, 25 ... single crystal, 26 ... impurity removing member
Claims (6)
前記融液の表面に浮遊する不純物を除去する不純物除去手段を設けたことを特徴とする単結晶製造装置。 In a single crystal manufacturing apparatus that grows a single crystal by pulling the seed crystal in contact with the melt surface melted by heating the raw material stored in the crucible,
An apparatus for producing a single crystal, comprising an impurity removing means for removing impurities floating on the surface of the melt.
前記不純物除去部材を前記融液面に対して接触および退避させる駆動手段とを備えることを特徴とする請求項１に記載の単結晶製造装置。 The impurity removing means includes an impurity removing member that adheres the impurities to the surface;
The single crystal manufacturing apparatus according to claim 1, further comprising driving means for bringing the impurity removing member into contact with and withdrawing from the melt surface.
前記融液面の液面下降に応じて前記融液面との接触を保持したまま前記不純物除去部材を下降させる駆動手段とを備えることを特徴とする請求項１に記載の単結晶製造装置。 The impurity removing means is arranged concentrically with the seed crystal, and a cylindrical impurity removing member whose lower end is in contact with the melt surface;
2. The single crystal manufacturing apparatus according to claim 1, further comprising: a driving unit that lowers the impurity removing member while maintaining contact with the melt surface as the melt surface descends. 3.
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| WO2013080576A1 (en) * | 2011-12-01 | 2013-06-06 | シャープ株式会社 | Metal manufacturing method, and product of same |
| CN103147119A (en) * | 2013-03-21 | 2013-06-12 | 北京雷生强式科技有限责任公司 | Preparation method and growth equipment of magnesium fluoride crystal |
| CN114232070A (en) * | 2021-11-05 | 2022-03-25 | 浙江大学杭州国际科创中心 | Double-cavity structure and method for growing gallium oxide crystal by Czochralski method |
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| KR20230106211A (en) | 2022-01-05 | 2023-07-13 | (주)금강쿼츠 | Single crystal manufacturing apparatus |
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| WO2013080576A1 (en) * | 2011-12-01 | 2013-06-06 | シャープ株式会社 | Metal manufacturing method, and product of same |
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