JP3231244B2 - Method for producing spherical material made of inorganic material and apparatus for producing the same - Google Patents
Method for producing spherical material made of inorganic material and apparatus for producing the sameInfo
- Publication number
- JP3231244B2 JP3231244B2 JP21188396A JP21188396A JP3231244B2 JP 3231244 B2 JP3231244 B2 JP 3231244B2 JP 21188396 A JP21188396 A JP 21188396A JP 21188396 A JP21188396 A JP 21188396A JP 3231244 B2 JP3231244 B2 JP 3231244B2
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- raw material
- spherical
- falling
- melt
- material melt
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、無機材料製の球状
体の製造方法及びその製造装置に関し、特に半導体、超
電導体、磁性体、誘電体、合金、ガラス等の無機材料の
原料体を浮遊状態で溶融後落下チューブ内を自由落下さ
せながら表面張力の作用で球状体に凝固させる技術に関
し、無機材料製の球状体を比較的簡単に経済的に製造す
る技術に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a spherical body made of an inorganic material and an apparatus for manufacturing the same, and more particularly to a method for floating a raw material of an inorganic material such as a semiconductor, a superconductor, a magnetic material, a dielectric, an alloy, and glass. The present invention relates to a technique of solidifying a spherical body by the action of surface tension while freely falling in a falling tube after melting in a state, and a technique of relatively easily and economically manufacturing a spherical body made of an inorganic material.
【０００２】[0002]
【従来の技術】従来、微小重力環境下で種々の無機材料
を溶融させてから球状体に凝固させる実験が行われてき
た。そのなかには、球状結晶を作る実験も行われた。微
小重力環境下において、容器を用いない溶融方法とし
て、電磁浮遊加熱、静電浮遊や音波浮遊装置にハロゲン
ランプ等の放射光加熱炉を組み合わせた技術が用いられ
て来た。しかし、このような実験は地上ではなく、地球
周回軌道上の人工衛星やスペースシャトルを利用して長
時間の微小重力環境下で行われたので、多大の費用と時
間がかかるほか、実施上の制約もきびしく、実験回数は
限定される。従って、学術的研究や実験に限られ、上述
の無機材料の球状結晶を経済的に短時間に繰り返し大量
に生産するのには適していない。2. Description of the Related Art Conventionally, experiments have been conducted in which various inorganic materials are melted in a microgravity environment and then solidified into spherical bodies. Among them, experiments to make spherical crystals were also performed. In a microgravity environment, as a melting method without using a container, a technology in which a radiation heating furnace such as a halogen lamp is combined with an electromagnetic floating heating, electrostatic floating or sound wave floating device has been used. However, such experiments were conducted on a long-term microgravity environment using satellites or space shuttles in orbit around the earth instead of on the ground. The restrictions are severe, and the number of experiments is limited. Therefore, the method is limited to academic research and experiments, and is not suitable for repeatedly producing a large amount of the above-mentioned spherical crystal of an inorganic material economically in a short time.
【０００３】一方、１０秒以下の短時間の微小重力環境
は、従来の地上に設けたドロップチューブやショットタ
ワー方式の実験装置によって実現できることは公知であ
る。例えば、米国のＮＡＳＡのドロップチューブ式実験
装置においては、地上にドロップチューブが装備され、
その上端部のベルジャーに電磁浮遊加熱装置が交換可能
に装備され、種々の無機材料の試料を容器に入れずに電
磁浮遊加熱して溶融し、ドロップチューブの真空中を自
由落下させながら微小重力下に球状体に凝固させる。On the other hand, it is known that a short microgravity environment of less than 10 seconds can be realized by a conventional drop tube or shot tower type experimental apparatus provided on the ground. For example, a NASA drop tube type experimental device in the United States is equipped with a drop tube on the ground,
An electromagnetic floating heating device is replaceably mounted on the bell jar at the upper end of the bell jar, and various inorganic materials are melted by electromagnetic floating heating without putting them in a container, and fall under microgravity while falling freely in the vacuum of a drop tube. To solidify into a spherical body.
【０００４】また、ショットタワーを用いてシリコンの
球状結晶を作った例が発表されている〔「Development
and Evaluation of the Texas Instruments Solar Ener
gy System 」 16th IEEE PVSC Proceedings P.257 〜P.
260(1982) 〕。この発表論文によれば、ショットタワー
の上端に装備した小さなノズルから、シリコンの融液を
少量づつ噴射し、ショットタワー内の不活性ガス中を自
由落下させて、シリコンの球状結晶を製造する。米国特
許第4,021,323 号公報にも、前記と同様にショットタワ
ーの上端に装備した小さなノズルから、シリコンの融液
を少量づつ噴射し、ショットタワー内を自由落下させて
シリコンの球状結晶を製造する技術が記載されている。[0004] An example in which a spherical crystal of silicon is formed using a shot tower has been published ["Development".
and Evaluation of the Texas Instruments Solar Ener
gy System '' 16th IEEE PVSC Proceedings P.257 to P.257
260 (1982)]. According to the published paper, a small nozzle provided at the upper end of a shot tower injects a small amount of a silicon melt, and the silicon melt is allowed to fall freely into an inert gas in the shot tower to produce spherical silicon crystals. U.S. Pat.No. 4,021,323 also discloses a technique for producing a spherical silicon crystal by injecting a small amount of silicon melt from a small nozzle mounted on the upper end of a shot tower in the same manner as described above, and allowing the silicon melt to fall freely in the shot tower. Is described.
【０００５】[0005]
【発明が解決しようとする課題】前記のように、シリコ
ンの融液をノズルから噴射させてシリコンの球状結晶を
製造する場合には、ノズルからシリコン融液に不純物が
溶け込む可能性が高く、高純度のシリコン球状結晶を製
造するのに適していない。このことはシリコン以外の無
機材料製の球状結晶や球状体を製造する場合も同様であ
る。但し、ＮＡＳＡのドロップチューブ式実験装置のよ
うに、電磁浮遊加熱装置を適用すれば、シリコン融液を
容器に接触させないので、シリコン融液に不純物が溶け
込むことはない。As described above, when a silicon melt is jetted from a nozzle to produce a spherical silicon crystal, there is a high possibility that impurities will dissolve into the silicon melt from the nozzle. Not suitable for producing pure silicon spherical crystals. This is the same when manufacturing spherical crystals or spherical bodies made of an inorganic material other than silicon. However, when an electromagnetic floating heating device is applied as in the NASA drop tube type experimental device, the silicon melt is not brought into contact with the container, so that impurities do not dissolve into the silicon melt.
【０００６】他方、シリコンの融液を真空中又は不活性
ガス中を自由落下させて凝固させる場合、シリコン融液
の表面から放熱するためシリコン融液の表面側から凝固
が開始する。しかし、シリコンは凝固時に体積膨張する
ため、表面側よりも遅れて融液の内部が凝固するときシ
リコン融液の一部が表面側の一個所に膨出して尻尾状の
突起部が形成されるため、真球状のシリコン球状結晶を
形成できない。凝固時に体積収縮する無機材料の場合に
は、前記とは反対に、凝固した球状体の表面部に凹部が
形成される可能性がある。また、シリコン融液の表面側
が先に凝固すると、シリコン原料体に付着していた気泡
が球状体の内部に混入し易くなる。On the other hand, when the silicon melt is allowed to fall freely in a vacuum or an inert gas and solidified, solidification starts from the surface side of the silicon melt in order to radiate heat from the surface of the silicon melt. However, since silicon expands in volume at the time of solidification, when the inside of the melt solidifies later than the surface side, a part of the silicon melt swells at one place on the surface side to form a tail-like protrusion. Therefore, a true spherical silicon spherical crystal cannot be formed. In the case of an inorganic material that contracts in volume at the time of solidification, concavities may be formed on the surface of the solidified spherical body, on the contrary. Further, when the surface side of the silicon melt solidifies first, the air bubbles adhering to the silicon raw material easily mix into the spherical body.
【０００７】しかも、シリコン融液が表面側から凝固す
ることから、凝固後の球状結晶の内部歪みも大きくな
る。シリコンの球状結晶を製造する場合には、前記内部
歪みは別途焼鈍処理により除去できる。しかし、球状体
を形成後熱処理できない無機材料の場合には、球状体の
内部歪みを除去することが難しい。何れにしても、球状
結晶や球状体の品質を高める為には、球状結晶や球状体
の形成段階から内部歪みを極力小さくすることが望まし
い。Moreover, since the silicon melt solidifies from the surface side, the internal distortion of the solidified spherical crystal also increases. In the case of producing a silicon spherical crystal, the internal strain can be separately removed by annealing. However, in the case of an inorganic material that cannot be heat-treated after the formation of the sphere, it is difficult to remove the internal strain of the sphere. In any case, in order to improve the quality of the spherical crystal or the spherical body, it is desirable to minimize the internal strain from the stage of forming the spherical crystal or the spherical body.
【０００８】本発明の目的は、無機材料製の球状体を製
造する際に、球状体の表面の一部に尻尾状の突起部が形
成されるのを抑制でき、球状体の内部歪みを小さくする
ことができ、球状体の内部への気泡の混入を防止できる
ような球状体の製造方法及びその製造装置を提供するこ
とである。An object of the present invention is to suppress the formation of a tail-like projection on a part of the surface of a spherical body when manufacturing a spherical body made of an inorganic material, and to reduce internal distortion of the spherical body. It is an object of the present invention to provide a method of manufacturing a spherical body and a manufacturing apparatus for the same, which can prevent air bubbles from entering the inside of the spherical body.
【０００９】[0009]
【課題を解決するための手段】請求項１の無機材料製の
球状体の製造方法は、無機材料からなる原料体を浮遊力
発生手段により真空中又は所定のガス中に浮遊させた状
態で加熱手段により加熱して溶融させる第１工程と、次
に原料融液を鉛直姿勢にした落下チューブ内の真空中又
は所定のガス中を落下させながら融液状態のまま放熱さ
せる第２工程と、次に前記原料融液を前記落下チューブ
内の真空中又は所定のガス中を落下させながら、補助加
熱手段により原料融液の表面部を加熱する第３工程と、
次に前記原料融液を前記落下チューブ内の真空中又は所
定のガス中を落下させながら冷却して原料融液の表面張
力の作用で球状体に凝固させる第４工程と、次に前記球
状体を前記落下チューブの下端に臨む冷却液槽の冷却液
内に収容する第５工程とを備えたことを特徴とするもの
である。According to a first aspect of the present invention, there is provided a method of manufacturing a spherical body made of an inorganic material, wherein a raw material body made of an inorganic material is heated in a state of being floated in a vacuum or a predetermined gas by a buoyancy generating means. A first step in which the raw material melt is heated and melted by means, and a second step in which the raw material melt is radiated in a molten state while falling in a vacuum or a predetermined gas in a falling tube in a vertical position, and A third step of heating the surface portion of the raw material melt by auxiliary heating means while dropping the raw material melt in a vacuum or a predetermined gas in the drop tube;
Next, a fourth step in which the raw material melt is cooled while falling in a vacuum or a predetermined gas in the drop tube and solidified into a spherical body by the action of the surface tension of the raw material melt; And a fifth step of storing in a cooling liquid in a cooling liquid tank facing a lower end of the drop tube.
【００１０】前記浮遊力発生手段としては、電磁浮遊加
熱装置、静電浮遊装置、音波浮遊装置等を適用でき、前
記加熱手段としては、電磁浮遊加熱装置、赤外線ヒー
タ、電気ヒータ、レーザ光ヒータ、ハロゲンランプ等を
適用できる。所定のガスとしては、アルゴンガス、ヘリ
ウムガス、窒素ガス等の不活性ガス、または、酸素ガス
あるいは酸素ガスを含む窒素ガス等の酸化性ガスを適用
できる。無機材料は、半導体、超電導体、磁性体、誘電
体、合金、ガラス等の何れかの材料である。As the floating force generating means, an electromagnetic floating heating device, an electrostatic floating device, a sound wave floating device, etc. can be applied. As the heating means, an electromagnetic floating heating device, an infrared heater, an electric heater, a laser light heater, A halogen lamp or the like can be applied. As the predetermined gas, an inert gas such as an argon gas, a helium gas, or a nitrogen gas, or an oxidizing gas such as an oxygen gas or a nitrogen gas containing an oxygen gas can be used. The inorganic material is any material such as a semiconductor, a superconductor, a magnetic material, a dielectric, an alloy, and glass.
【００１１】最初の第１工程では、無機材料の微小な塊
状の原料体をパーツフィーダ等で浮遊力発生手段に供給
し、その浮遊力発生手段により原料体を真空中又は所定
のガス中に浮遊させた状態で加熱手段により加熱して溶
融させる。このように、原料体を浮遊状態にして溶融さ
せるため、原料融液が容器に接触することがないため、
原料融液に不純物が溶け込むことがない。次の第２工程
では、原料融液を鉛直姿勢にした落下チューブ内の真空
中又は所定のガス中を落下させながら融液状態のまま放
熱させる。In a first first step, a minute bulk raw material of an inorganic material is supplied to a buoyant force generating means by a parts feeder or the like, and the buoyant force generating means floats the raw material in a vacuum or a predetermined gas. In this state, it is heated and melted by a heating means. In this way, since the raw material is melted in a floating state, the raw material melt does not come into contact with the container,
Impurities do not dissolve in the raw material melt. In the next second step, the raw material melt is radiated in a molten state while falling in a vacuum or a predetermined gas in a falling tube in a vertical posture.
【００１２】原料融液を落下チューブ内を自由落下させ
るため、原料融液は微小重力状態に入り、原料融液の表
面張力の作用で球状になり、重力や熱対流の影響が無い
ため成分が均一に分布した融液となる。真空中を落下さ
せる場合、輻射により原料融液の表面から放熱し、所定
のガス中を落下させる場合、輻射と伝熱により原料融液
の表面から放熱する。前記原料融液の表面の凝固が発生
しない程度もしくは部分的にしか凝固が発生しない程度
に放熱させることにより、原料融液全体の温度低下を図
る。但し、原料融液の表面側から放熱するため、原料融
液の内部よりも表面部の方が低温になる。Since the raw material melt is allowed to fall freely in the falling tube, the raw material melt enters a microgravity state, and becomes spherical by the action of the surface tension of the raw material melt. The resulting melt is uniformly distributed. When falling in a vacuum, heat is radiated from the surface of the raw material melt by radiation, and when dropped in a predetermined gas, heat is radiated from the surface of the raw material melt by radiation and heat transfer. By radiating heat to such an extent that solidification of the surface of the raw material melt does not occur or only partially occurs, the temperature of the entire raw material melt is reduced. However, since the heat is radiated from the surface side of the raw material melt, the temperature of the surface portion becomes lower than that of the inside of the raw material melt.
【００１３】次の第３工程では、原料融液を落下チュー
ブ内の真空中又は所定のガス中を落下させながら、補助
加熱手段により原料融液の表面部を加熱する。この補助
加熱手段としては、表面部のみを加熱する為に、赤外線
ヒータを適用することが望ましく、原料融液の内部の温
度よりも表面部の温度が高くなるように加熱する。In the next third step, the surface portion of the raw material melt is heated by the auxiliary heating means while dropping the raw material melt in a vacuum or a predetermined gas in the falling tube. As this auxiliary heating means, it is desirable to apply an infrared heater in order to heat only the surface portion, and the heating is performed so that the temperature of the surface portion becomes higher than the temperature of the inside of the raw material melt.
【００１４】次の第４工程では、原料融液を、落下チュ
ーブ内の真空中又は所定のガス中を落下させながら冷却
して半導体融液の表面張力の作用で球状体に凝固させ
る。原料融液が、自由落下しながら凝固するため表面張
力の作用で球状を保持しつつ球状体に凝固する。このと
き、原料融液は表面部から放熱するけれども、原料融液
の内部の温度が表面部の温度と同等または表面部の温度
よりも低くなっているため、原料融液の内部から、或い
は、内部と表面部の両方から凝固が開始する。それ故、
凝固時に体積膨張する無機材料の場合でも球状体の表面
の一部に突起部が形成されるのを効果的に抑制すること
ができ、凝固時に体積収縮する無機材料の場合でも球状
体の表面の一部に凹部が形成されるのを効果的に抑制す
ることができ、球状体の内部歪みを小さくすることがで
きる。また、球状体内に気泡が混入しにくくなる。しか
も、凝固開始の起点となる種結晶の無い状態から凝固す
るため、過冷却状態での凝固が生じる。無機材料がガラ
スである場合、過冷却凝固により全く新しいガラスの球
状体となる。In the next fourth step, the raw material melt is cooled while falling in a vacuum or a predetermined gas in a drop tube and solidified into a spherical body by the action of the surface tension of the semiconductor melt. Since the raw material melt solidifies while falling freely, it solidifies into a spherical body while maintaining a spherical shape by the action of surface tension. At this time, although the raw material melt radiates heat from the surface portion, since the temperature inside the raw material melt is equal to or lower than the surface portion temperature, from the inside of the raw material melt, or Solidification starts from both the interior and the surface. Therefore,
Even in the case of an inorganic material that expands in volume during solidification, it is possible to effectively suppress the formation of projections on a part of the surface of the spherical body. The formation of a concave portion in a part can be effectively suppressed, and the internal distortion of the spherical body can be reduced. In addition, bubbles are less likely to be mixed into the spherical body. In addition, since the solidification is started from a state where there is no seed crystal serving as a starting point of solidification start, solidification occurs in a supercooled state. When the inorganic material is glass, a completely new glass sphere is formed by supercooling and solidification.
【００１５】特に、無機材料がシリコンである場合、シ
リコンは凝固するときには、体積膨張するため、原料融
液の表面部から凝固し始めると、原料融液の内部が凝固
する際に融液の一部が表面部に突出して突起部が形成さ
れることになるが、本発明では、そのような突起部が形
成されることはなく、仮に突起部が形成されるとしても
別途焼鈍処理の際に消滅する位の極く小さな突起部が形
成されるだけである。In particular, when the inorganic material is silicon, the volume of the silicon expands when it is solidified. Therefore, when the solidification starts from the surface of the raw material melt, one part of the melt is solidified when the inside of the raw material melt is solidified. The projections are formed by projecting the surface to the surface, but in the present invention, such projections are not formed, and even if the projections are formed, they are separately formed during annealing. Only a very small protrusion that disappears is formed.
【００１６】次の第５工程では、球状体を落下チューブ
の下端に臨む冷却液槽の冷却液内に収容する。この冷却
液としては、球状体に不純物を溶け込ませることのない
液体（例えば、シリコンオイル）を適用する。このよう
に落下してきた球状体を冷却液内に収容することで、緩
衝を図り球状体を十分に冷却することができる。In the next fifth step, the spherical body is stored in the cooling liquid in the cooling liquid tank facing the lower end of the falling tube. As the cooling liquid, a liquid (for example, silicon oil) that does not dissolve impurities into the spherical body is used. By containing the dropped spherical body in the cooling liquid, the spherical body can be sufficiently cooled by buffering.
【００１７】請求項２の無機材料製の球状体の製造方法
は、請求項１の発明において、前記無機材料がシリコン
であることを特徴とするものである。前記請求項１の欄
において説明したとおり、シリコン球状結晶の表面部に
突起が形成されるのを抑制でき、球状結晶の内部歪みを
小さくすることができる。The method of manufacturing a spherical body made of an inorganic material according to a second aspect is characterized in that, in the first aspect, the inorganic material is silicon. As described in the section of claim 1, the formation of projections on the surface of the silicon spherical crystal can be suppressed, and the internal strain of the spherical crystal can be reduced.
【００１８】請求項３の無機材料製の球状体の製造方法
は、相互に異なる種類の無機材料からなる複数の原料体
を、浮遊力発生手段により真空中又は所定のガス中に接
触状に浮遊させた状態で加熱手段により加熱して一体的
に溶融させる第１工程と、次に原料融液を鉛直姿勢にし
た落下チューブ内の真空中又は所定のガス中を落下させ
ながら融液状態のまま放熱させる第２工程と、次に前記
原料融液を前記落下チューブ内の真空中又は所定のガス
中を落下させながら、補助加熱手段により原料融液の表
面部を加熱する第３工程と、次に前記原料融液を前記落
下チューブ内の真空中又は所定のガス中を落下させなが
ら冷却して原料融液の表面張力の作用で球状体に凝固さ
せる第４工程と、次に前記球状体を前記落下チューブの
下端に臨む冷却液槽の冷却液内に収容する第５工程とを
備えたことを特徴とするものである。According to a third aspect of the present invention, there is provided a method of manufacturing a spherical body made of an inorganic material, wherein a plurality of raw materials made of different kinds of inorganic materials are floated in contact with each other in a vacuum or a predetermined gas by a floating force generating means. A first step in which the raw material melt is heated and melted integrally by the heating means in a state where the raw material melt is melted while falling in a vacuum or a predetermined gas in a falling tube in a vertical posture. A second step of radiating heat; and a third step of heating the surface of the raw material melt by auxiliary heating means while dropping the raw material melt in a vacuum or a predetermined gas in the drop tube, and A fourth step of cooling the raw material melt while falling in a vacuum or a predetermined gas in the drop tube and solidifying the raw material melt into a spherical body by the action of the surface tension of the raw material melt; and Coolant facing the lower end of the drop tube It is characterized in that a fifth step of receiving the coolant in.
【００１９】この製造方法は、基本的に請求項１の製造
方法と基本的に同様であるが、第１工程において、相互
に異なる種類の無機材料からなる複数の原料体を適用す
る点で異なっており、第２工程〜第５工程については、
請求項１と同様である。即ち、第１工程において相互に
異なる種類の無機材料からなる複数の原料体を、浮遊力
発生手段により真空中又は所定のガス中に接触状に浮遊
させた状態で加熱手段により加熱して一体的に溶融させ
る。複数の原料体の重量比率は、同一とは限らず適宜設
定される。前記無機材料、浮遊力発生手段、加熱手段に
ついては請求項１と同様であるので説明を省略する。こ
の製造方法によれば、複数の種類の異なる無機材料から
なる球状体であって成分が均一に分布した球状体を製造
することができ、球状体の表面部に突起部が形成される
のを抑制でき、球状体の内部歪みを小さくすることがで
きる。This manufacturing method is basically the same as the manufacturing method of claim 1, except that in the first step, a plurality of raw materials made of different kinds of inorganic materials are applied. For the second to fifth steps,
Same as claim 1. That is, in the first step, a plurality of raw materials made of inorganic materials different from each other are heated by the heating means in a state of being floated in a vacuum or a predetermined gas in a contact state by the buoyancy generating means, and are integrally formed. To be melted. The weight ratio of the plurality of raw materials is not necessarily the same, and may be appropriately set. The inorganic material, the buoyancy generating means, and the heating means are the same as those in the first aspect, and thus description thereof is omitted. According to this production method, it is possible to produce a spherical body composed of a plurality of types of different inorganic materials and in which the components are uniformly distributed, and that a projection is formed on the surface of the spherical body. It can be suppressed, and the internal strain of the spherical body can be reduced.
【００２０】請求項４の無機材料製の球状結晶の製造方
法は、請求項３の発明において、前記相互に異なる種類
の無機材料がシリコンとゲルマニウムであることを特徴
とするものである。シリコンとゲルマニウムは全率固溶
体を形成するので、組成比を任意に選択することによ
り、所望の混晶比を有するシリコン・ゲルマニウム混晶
半導体の球状結晶を製造することができる。A method of manufacturing a spherical crystal made of an inorganic material according to claim 4 is characterized in that, in the invention of claim 3, the different types of inorganic materials are silicon and germanium. Since silicon and germanium form a solid solution in all ratios, a spherical crystal of a silicon-germanium mixed crystal semiconductor having a desired mixed crystal ratio can be produced by arbitrarily selecting the composition ratio.
【００２１】請求項５の無機材料製の球状体の製造装置
は、無機材料からなる原料体を落下チューブ内の真空中
又は所定のガス中で浮遊状態で加熱し、その原料融液を
落下チューブ内を自由落下させながら凝固させて球状体
を製造する装置において、鉛直姿勢の落下チューブと、
前記落下チューブ内へその上端から原料体を供給する原
料体供給手段と、前記落下チューブの上端部又はその付
近内で原料体を浮遊させた状態で加熱して原料融液にす
る浮遊加熱手段と、前記浮遊加熱手段の下側に所定距離
以上離隔して配設され、落下チューブ内を落下中の原料
融液の表面部を加熱するアフターヒータとを備えたもの
である。According to a fifth aspect of the present invention, there is provided an apparatus for manufacturing a spherical body made of an inorganic material, wherein a raw material body made of an inorganic material is heated in a vacuum or a predetermined gas in a falling tube in a floating state, and the raw material melt is dropped into the falling tube. In a device that manufactures a spherical body by solidifying while freely falling inside, a falling tube with a vertical posture,
A raw material supply means for supplying a raw material from the upper end thereof into the drop tube, and a floating heating means for heating the raw material in a state of being floated at or near the upper end of the drop tube to produce a raw material melt; And an after-heater disposed below the floating heating means at a predetermined distance or more and heating a surface portion of the raw material melt falling in the drop tube.
【００２２】前記無機材料は、半導体、超電導体、磁性
体、合金、ガラス等の何れか１つの材料又は複数の材料
であり、原料体としては、１種類の材料の原料体、複数
の材料の原料体、１個の原料体、複数個の原料体等種々
形態の原料体を適用できる。所定のガスについては請求
項１と同様である。前記浮遊加熱手段としては、電磁浮
遊加熱装置、静電浮遊装置と加熱装置、音波浮遊装置と
加熱装置、の何れかを適用でき、前記加熱装置として
は、電気ヒータ、赤外線ヒータ、ハロゲンランプヒー
タ、レーザ光ヒータ等の種々の加熱手段を適用できる。
前記アフターヒータとしては、赤外線ヒータ、ハロゲン
ランプヒータ、レーザ光ヒータ、電気ヒータ等の種々の
ヒータを適用できる。The inorganic material is any one or a plurality of materials such as a semiconductor, a superconductor, a magnetic material, an alloy, and glass, and the raw material is a raw material of one kind of material, a raw material of a plurality of materials. Various types of raw materials such as a raw material, a single raw material, and a plurality of raw materials can be applied. The predetermined gas is the same as in claim 1. As the floating heating means, any of an electromagnetic floating heating device, an electrostatic floating device and a heating device, a sound wave floating device and a heating device can be applied, and as the heating device, an electric heater, an infrared heater, a halogen lamp heater, Various heating means such as a laser light heater can be applied.
Various heaters such as an infrared heater, a halogen lamp heater, a laser light heater, and an electric heater can be applied as the after heater.
【００２３】原料供給手段が落下チューブ内へその上端
から原料体を供給すると、浮遊加熱手段は、落下チュー
ブの上端部又はその付近内で原料体を浮遊させた状態で
加熱して原料融液にする。原料融液は浮遊状態であるの
で、容器に接触することがないから原料融液に不純物が
溶け込むことがない。アフターヒータは、浮遊加熱手段
の下側に所定距離以上離隔して配設されているため、原
料融液が落下チューブ内をアフターヒータのレベルまで
落下する間に原料融液が放射冷却等により放熱して、原
料融液の全体の温度が低下するものの、原料融液の内部
よりも表面部の方が低温になる。When the raw material supply means supplies the raw material into the falling tube from its upper end, the floating heating means heats the raw material in a floating state at or near the upper end of the falling tube to form a raw material melt. I do. Since the raw material melt is in a floating state, it does not come into contact with the container, so that no impurities are dissolved in the raw material melt. Since the after-heater is arranged at a predetermined distance or more below the floating heating means, the raw material melt is radiated by radiation cooling or the like while the raw material melt falls in the falling tube to the level of the after heater. Then, although the temperature of the entire raw material melt decreases, the temperature of the surface portion becomes lower than that of the inside of the raw material melt.
【００２４】次に、アフターヒータによりその原料融液
の表面部が加熱されるため、原料融液の内部よりも表面
部の方が高温になる。その原料融液がアフターヒータを
通過してから原料融液の落下中に原料融液の表面部から
放熱していくため、凝固点まで温度低下したとき、原料
融液の内部の温度が表面部の温度と同等又は表面部の温
度よりも低くなっているため、原料融液の内部から、或
いは、内部と表面部の両方から凝固が開始する。その結
果、請求項１に説明した作用と同様の作用を奏する。Next, since the surface portion of the raw material melt is heated by the after heater, the temperature of the surface portion becomes higher than that of the inside of the raw material melt. After the raw material melt passes through the after heater, heat is radiated from the surface of the raw material melt during the fall of the raw material melt. Since the temperature is equal to or lower than the temperature of the surface portion, solidification starts from inside the raw material melt or from both the inside and the surface portion. As a result, an operation similar to the operation described in claim 1 is achieved.
【００２５】請求項６の無機材料製の球状体の製造装置
は、請求項５の発明において、前記落下チューブ内を真
空ポンプを介して真空状態にする真空化手段を設けたも
のである。落下チューブ内を真空状態にして球状体を製
造する際には、真空化手段を作動させて落下チューブ内
を真空状態にする。In a sixth aspect of the present invention, there is provided the apparatus for producing a spherical body made of an inorganic material according to the fifth aspect of the present invention, further comprising a vacuuming means for evacuating the inside of the falling tube via a vacuum pump. When manufacturing a spherical body by evacuating the inside of the drop tube, the evacuation means is operated to bring the inside of the drop tube into a vacuum state.
【００２６】請求項７の無機材料製の球状体の製造装置
は、請求項６の発明において、無機材料の種類に応じた
所定のガスを落下チューブ内に供給するとともに、落下
チューブ内に原料融液の落下方向へほぼ同速で流れるガ
ス流を形成し且つ落下チューブ内に球状体の落下方向と
反対方向へ流れるガス流を形成するガス供給手段を設け
たものである。例えば、ガラス製の球状体や酸化物高温
超電導体製の球状体を製造するような場合には、真空化
手段を停止させ、酸化ガスまたは酸素ガスを含む窒素ガ
スを落下チューブ内に供給し、そのガス中で球状体を製
造することになる。その場合、ガス供給手段により、落
下チューブ内にガスを供給するとともに、落下チューブ
内に原料融液の落下方向へほぼ同速で流れるガス流を形
成し且つ落下チューブ内に球状体の落下方向と反対方向
へ流れるガス流を形成する。According to a seventh aspect of the present invention, in the apparatus for manufacturing a spherical body made of an inorganic material according to the sixth aspect of the present invention, a predetermined gas corresponding to the type of the inorganic material is supplied into the falling tube and the raw material is melted into the falling tube. A gas supply means for forming a gas flow flowing at substantially the same speed in the liquid drop direction and forming a gas flow flowing in a direction opposite to the drop direction of the spherical body in the drop tube is provided. For example, in the case of manufacturing a spherical body made of glass or a spherical body made of an oxide high-temperature superconductor, the vacuuming means is stopped, and a nitrogen gas containing an oxidizing gas or an oxygen gas is supplied into the drop tube, A spherical body will be produced in the gas. In this case, the gas is supplied into the falling tube by the gas supply means, and a gas flow is formed in the falling tube at substantially the same speed in the falling direction of the raw material melt. Form a gas flow that flows in the opposite direction.
【００２７】落下チューブ内で数１００〜２０００μｍ
程度の小径の原料融液は、極く短時間で凝固するが、凝
固前の原料融液の落下方向へほぼ同速で流れるガス流を
形成するため、ガス流から凝固中の原料融液に摩擦力が
殆ど作用せず、原料融液は真球状に凝固する。そして、
凝固後の球状体の落下方向と反対方向へ流れるガス流を
形成するため、ガス流と球状体との接触度合いが高くな
り、ガスと球状体との反応や球状体の冷却が促進され
る。Several hundred to 2,000 μm in a falling tube
Although the raw material melt having a small diameter is solidified in a very short time, it forms a gas flow that flows at almost the same speed in the falling direction of the raw material melt before solidification. The frictional force hardly acts, and the raw material melt solidifies into a true sphere. And
Since the gas flow that flows in the direction opposite to the falling direction of the spherical body after solidification is formed, the degree of contact between the gas flow and the spherical body is increased, and the reaction between the gas and the spherical body and the cooling of the spherical body are promoted.
【００２８】請求項８の無機材料製の球状体の製造装置
は、請求項７の発明において、前記落下チューブの下端
に臨み、その下端外へ落下した球状体を冷却液内に収容
する冷却液槽を設けたものである。落下チューブの下端
外へ落下した球状体を冷却液槽の冷却液内に収容するた
め、球状体が衝撃で損傷するのを防止するとともに、球
状体を冷却することができる。According to an eighth aspect of the present invention, there is provided an apparatus for manufacturing a spherical body made of an inorganic material according to the seventh aspect of the present invention, wherein the spherical body which faces the lower end of the drop tube and falls outside the lower end is accommodated in the coolant. A tank was provided. Since the spherical body that has fallen to the outside of the lower end of the falling tube is accommodated in the cooling liquid in the cooling liquid tank, the spherical body can be prevented from being damaged by impact, and the spherical body can be cooled.
【００２９】[0029]
【発明の実施の形態】以下、本発明の実施の形態につい
て図面を参照しながら説明する。最初に、本発明に適用
する無機材料製の球状体（直径数１００〜２０００μ
ｍ）を製造する球状体製造装置について説明する。図１
に示すように、球状体製造装置１は、直径５〜１０ｃｍ
で高さ約１４ｍの鉛直の落下チューブ１０と、落下チュ
ーブ１０の上端部の外側に配置した電磁浮遊加熱装置１
２と、アフターヒータとしての赤外線ヒータ１３（補助
加熱手段）と、落下チューブ１０の上端に原料体２ａを
１個ずつ供給する原料供給装置１１と、落下チューブ１
０の下端に連なる収容部１４内に収容されて落下チュー
ブ１０の下端に臨むシリコンオイル槽１５と、落下チュ
ーブ１０内の空気を吸引する真空ポンプ１６と、ガス供
給装置１７と、配管系及びバルブ類と、落下チューブ１
０内を落下中の原料融液２ｂや球状結晶２ｃ（球状体）
を撮影する高速度カメラ１８ａ〜１８ｃと、これらの機
器を制御する制御ユニット２０等で構成されている。
尚、工場の１階〜５階のフロア３ａ〜３ｅも図示してあ
る。Embodiments of the present invention will be described below with reference to the drawings. First, a spherical body made of an inorganic material (having a diameter of 100 to 2000 μm) applied to the present invention.
The spherical body manufacturing apparatus for manufacturing m) will be described. FIG.
As shown in the figure, the spherical body manufacturing apparatus 1 has a diameter of 5 to 10 cm.
And a vertical drop tube 10 having a height of about 14 m and an electromagnetic floating heating device 1 disposed outside the upper end of the drop tube 10
2, an infrared heater 13 (auxiliary heating means) as an after heater, a raw material supply device 11 for supplying the raw material 2a one by one to the upper end of the falling tube 10, and a falling tube 1
0, a silicon oil tank 15 housed in a housing 14 connected to the lower end of the fall tube 10 and facing the lower end of the drop tube 10, a vacuum pump 16 for sucking air in the fall tube 10, a gas supply device 17, a piping system and a valve Kind and falling tube 1
Raw material melt 2b and spherical crystal 2c (spherical body) falling inside 0
And high-speed cameras 18a to 18c for photographing images, and a control unit 20 for controlling these devices.
The floors 3a to 3e of the first to fifth floors of the factory are also shown.
【００３０】原料供給装置１１は、落下チューブ１０の
上端に接続された供給器２１と、多数の所定サイズの小
塊状の原料体２ａを収容し且つ供給器２１に１個ずつ供
給するパーツフィーダ２２とを備え、パーツフィーダ２
２は、原料体２ａを予熱するとともに原料体２ａの表面
の空気を抜気するように構成してある。供給器２１のケ
ース２３は、電磁開閉弁２４を有する吸引管２５で真空
ポンプ１６に接続され、ケース２３内の受入器２６は、
電磁開閉シャッター２７を有する通路２８でパーツフィ
ーダ２２に接続され、受入器２６の出口通路２９には電
磁開閉シャッター３０が設けられ、受入器２６には複数
の微小孔を介してケース２３内の真空が導入される。The raw material supply device 11 includes a supply device 21 connected to the upper end of the drop tube 10 and a parts feeder 22 for accommodating a large number of small-sized raw material bodies 2a of a predetermined size and supplying the raw material materials 2 to the supply device 21 one by one. And the parts feeder 2
Numeral 2 is configured to preheat the raw material body 2a and to bleed air from the surface of the raw material body 2a. The case 23 of the supply device 21 is connected to the vacuum pump 16 by a suction pipe 25 having an electromagnetic on-off valve 24, and a receiver 26 in the case 23
The part feeder 22 is connected to the parts feeder 22 through a passage 28 having an electromagnetic opening / closing shutter 27, an electromagnetic opening / closing shutter 30 is provided in an outlet passage 29 of the receiving device 26, and the receiving device 26 has a vacuum inside the case 23 through a plurality of minute holes. Is introduced.
【００３１】球状体製造装置１の稼働中には、電磁開閉
弁２４は開かれて供給器２１内は真空状態である。パー
ツフィーダ２２から供給器２１に１個の原料体２ａを供
給する場合、電磁開閉シャッター３０を閉じ、電磁開閉
シャッター２７を開いて受入器２６内に原料体２ａを供
給し、その後電磁開閉シャッター２７を閉じる。原料供
給装置１１は、所定時間（例えば、１秒）おきに１個の
原料体２ａを供給器２１へ供給可能になっている。During operation of the spherical body manufacturing apparatus 1, the electromagnetic on-off valve 24 is opened and the inside of the supply unit 21 is in a vacuum state. When supplying one raw material 2a from the parts feeder 22 to the supply device 21, the electromagnetic opening / closing shutter 30 is closed, the electromagnetic opening / closing shutter 27 is opened, and the raw material 2a is supplied into the receiving unit 26. Close. The raw material supply device 11 is capable of supplying one raw material body 2a to the supply unit 21 every predetermined time (for example, every one second).
【００３２】落下チューブ１０内の空気を吸引する吸引
管３３〜３５には、電磁開閉弁３６〜３８が装備されて
おり、これら吸引管３３〜３５は真空ポンプ１６に接続
されている。無機材料の種類によっては、落下チューブ
１０内に所定のガス（不活性ガス、酸化性ガス等）を流
すことができるように、ガス供給装置１７とそのガス供
給装置１７から延びるガス供給管３９が設けられ、ガス
供給管３９から分岐した分岐管３９ａは落下チューブ１
０の上段部に接続され、ガス供給管３９から分岐した分
岐管３９ｂは落下チューブ１０の下段部に接続され、ガ
ス供給管３９には電磁開閉弁４０が装備されている。落
下チューブ１０の中段部に接続されたガス排出管４１が
大気開放され、このガス排出管４１には電磁開閉弁４２
が装備されている。The suction pipes 33 to 35 for sucking the air in the drop tube 10 are equipped with electromagnetic on-off valves 36 to 38, and these suction pipes 33 to 35 are connected to the vacuum pump 16. Depending on the type of the inorganic material, the gas supply device 17 and the gas supply tube 39 extending from the gas supply device 17 are provided so that a predetermined gas (inert gas, oxidizing gas, or the like) can flow through the fall tube 10. The branch pipe 39a branched from the gas supply pipe 39 is provided
The branch pipe 39b branched from the gas supply pipe 39 is connected to the lower part of the drop tube 10, and the gas supply pipe 39 is equipped with an electromagnetic on-off valve 40. A gas exhaust pipe 41 connected to the middle part of the drop tube 10 is opened to the atmosphere.
Is equipped.
【００３３】ガス供給装置１７から所定のガスを供給す
る場合には、落下チューブ１０の上半部内ではガスは原
料融液２ｂと同方向へほぼ同速で流れるので、原料融液
２ｂにガスから摩擦力が作用しない。落下チューブ１０
の下半部内ではガスは球状結晶２ｃと反対側へ流れるの
で、球状結晶２ｃとガスとの接触度合いが高くなる。但
し、落下チューブ１０内を真空に維持する場合には、ガ
ス供給装置１７は停止し、電磁開閉弁４０，４２は閉じ
ている。When a predetermined gas is supplied from the gas supply device 17, the gas flows in the upper half portion of the drop tube 10 at substantially the same speed in the same direction as the raw material melt 2b. No frictional force acts. Drop tube 10
In the lower half part, the gas flows to the opposite side to the spherical crystal 2c, so that the degree of contact between the spherical crystal 2c and the gas increases. However, when the inside of the drop tube 10 is maintained at a vacuum, the gas supply device 17 is stopped, and the electromagnetic on-off valves 40 and 42 are closed.
【００３４】図２に示すように、電磁浮遊加熱装置１２
は、上部コイル４５と、下部コイル４６と、これらコイ
ル４５，４６に逆方向の等しい高周波電流を供給する高
周波電流発生装置１９（図１参照）等で構成され、上部
コイル４５で上向きの磁力線が発生し、下部コイル４６
で下向きの磁力線が発生し、原料体２ａが導体や半導体
の無機材料で構成されている場合、高周波数で変化する
磁力線により原料体２ａに誘導電流が発生し、原料体２
ａが上部コイル４５と下部コイル４６の中間位置（図示
の位置）にあるとき、誘導電流に磁力線から作用する上
向きの力と下向きの力とが均衡するため原料体２ａが浮
遊状態を保持し、誘導電流が原料体２ａ中を流れるとき
の発熱作用で原料体２ａが加熱される。As shown in FIG.
Is composed of an upper coil 45, a lower coil 46, a high-frequency current generator 19 (see FIG. 1) for supplying equal high-frequency currents to the coils 45 and 46 in opposite directions, and the like. Occurs and the lower coil 46
When the raw material body 2a is made of a conductor or semiconductor inorganic material, an induced current is generated in the raw material body 2a by the magnetic field lines changing at a high frequency, and the raw material body 2a
When a is at an intermediate position (position shown) between the upper coil 45 and the lower coil 46, the upward force and the downward force acting on the induced current from the lines of magnetic force are balanced, so that the raw material body 2a maintains a floating state, The raw material 2a is heated by the heat generation when the induced current flows through the raw material 2a.
【００３５】こうして、原料体２ａが加熱されて溶融し
原料融液２ｂになってから両コイル４５，４６への高周
波電流を遮断すると、原料融液２ｂが赤外線ヒータ１３
の方へ自由落下する。この自由落下により、原料融液２
ｂは、１０-5Ｇの微小重力状態になり、表面張力の作用
で真球状になる。In this way, when the raw material 2a is heated and melted to become the raw material melt 2b, and the high-frequency current to both coils 45 and 46 is cut off, the raw material melt 2b is
Free fall towards. By this free fall, the raw material melt 2
b is in a state of microgravity of 10 -5 G and becomes spherical due to the effect of surface tension.
【００３６】前記赤外線ヒータ１３は、原料融液２ｂの
表面部のみを少し加熱する為のものであり、電磁浮遊加
熱装置１２との間に球状体２ｃの大きさと材料とに応じ
て設定される所定距離以上離して落下チューブ１０の外
側に環状に配置され、高さ位置を微調節可能に取付けら
れている。この赤外線ヒータ１３は、赤外線放射セラミ
ックスからなる円筒状のヒータ本体４７を有し、このヒ
ータ本体４７へ供給する電流を制御することで、加熱能
力を精密に制御することができる。原料融液２ｂは、自
転しながら落下してくるため、赤外線ヒータ１３により
原料融液２ｂの表面部のみが一様に加熱される。尚、図
２には、電磁浮遊加熱装置１２と赤外線ヒータ１３で加
熱される原料体２ａ又は原料融液２ｂの全体のマクロ的
温度を図示してあり、温度Ｔｏは融解点（凝固点）であ
る。The infrared heater 13 serves to slightly heat only the surface of the raw material melt 2b, and is set in accordance with the size and material of the spherical body 2c with the electromagnetic floating heating device 12. It is annularly arranged outside the drop tube 10 at a predetermined distance or more, and is attached so that the height position can be finely adjusted. The infrared heater 13 has a cylindrical heater main body 47 made of infrared-emitting ceramics. By controlling the current supplied to the heater main body 47, the heating capability can be precisely controlled. Since the raw material melt 2b falls while rotating, only the surface portion of the raw material melt 2b is uniformly heated by the infrared heater 13. FIG. 2 shows the entire macro temperature of the raw material 2a or the raw material melt 2b heated by the electromagnetic floating heating device 12 and the infrared heater 13, and the temperature To is a melting point (solidification point). .
【００３７】次に、前記球状体製造装置１を用いて、無
機材料としてシリコンを適用し、シリコンの原料体２ａ
を供給して１個のシリコンの球状結晶２ｃを製造する方
法について説明する。先ず、最初の準備段階において、
電磁開閉弁４０，４２が閉じられ、電磁開閉弁２４，３
６〜３８が開かれ、真空ポンプ１６が作動されて、落下
チューブ１０内は所定の真空状態にされる。原料供給装
置１１の受入器２６には１個の原料体２ａが収容され、
赤外線ヒータ１３には予め設定された所定の電流が通電
される。Next, using the spherical body manufacturing apparatus 1, silicon is applied as an inorganic material to form a silicon raw material 2a.
Is supplied to produce one silicon spherical crystal 2c. First, in the first preparation stage,
The electromagnetic on / off valves 40 and 42 are closed, and the electromagnetic on / off valves 24 and 3 are closed.
6 to 38 are opened, the vacuum pump 16 is operated, and the inside of the drop tube 10 is brought into a predetermined vacuum state. One raw material body 2a is accommodated in the receiver 26 of the raw material supply device 11,
A predetermined current that is set in advance is supplied to the infrared heater 13.
【００３８】次に、電磁浮遊加熱装置１２に通電され、
電磁開閉シャッター３０が開かれて原料体２ａが落下チ
ューブ１０内に供給され、その原料体２ａは電磁浮遊加
熱装置１２により所定の微小時間の間浮遊状態に保持し
て加熱され、溶融して原料融液２ｂになる。このときの
原料融液２ｂの温度分布は、図３（ａ）に示すように、
原料融液２ｂの内部と表面部とがほぼ一様になる。Next, the electromagnetic floating heating device 12 is energized,
The electromagnetic opening / closing shutter 30 is opened and the raw material body 2a is supplied into the drop tube 10, and the raw material body 2a is heated while being held in a floating state by the electromagnetic floating heating device 12 for a predetermined minute time, melted, and melted. It becomes melt 2b. The temperature distribution of the raw material melt 2b at this time is, as shown in FIG.
The inside and the surface of the raw material melt 2b become substantially uniform.
【００３９】次に、電磁浮遊加熱装置１２への通電が遮
断されると、原料融液２ｂが落下チューブ１０の真空中
を落下し始める。最初原料融液２ｂの落下速度は低速で
あり、原料融液２ｂが赤外線ヒータ１３の上端のレベル
まで落下する微小時間の間に放射冷却されて放熱する。
このとき、原料融液２ｂの表面部から放熱するため、原
料融液２ｂの内部よりも表面部の方が低温になる（図３
（ｂ）の温度分布参照）。この落下開始後には、原料融
液２ｂは微小重力状態になるため、原料融液２ｂの表面
張力の作用で真球状になる。Next, when the power supply to the electromagnetic floating heating device 12 is stopped, the raw material melt 2b starts falling in the vacuum of the drop tube 10. Initially, the falling speed of the raw material melt 2b is low, and the raw material melt 2b is radiatively cooled and radiates heat in a minute time when the raw material melt 2b falls to the level at the upper end of the infrared heater 13.
At this time, since the heat is radiated from the surface portion of the raw material melt 2b, the temperature of the surface portion becomes lower than that of the inside of the raw material melt 2b (FIG. 3).
(Refer to the temperature distribution in (b)). After the start of the drop, the raw material melt 2b is in a state of microgravity, so that the raw material melt 2b becomes a truly spherical shape due to the surface tension of the raw material melt 2b.
【００４０】次に、落下チューブ１０内のうちの赤外線
ヒータ１３の内部を落下中に、原料融液２ｂの表面部の
みが加熱され、原料融液２ｂの温度分布は図３（ｃ）に
示すように、原料融液２ｂの内部よりも表面部の方が高
温になる。次に、落下チューブ１０の真空中を赤外線ヒ
ータ１３の下方へ落下しながら、原料融液２ｂは放射冷
却により放熱し、原料融液２ｂの表面張力の作用で真球
状の球状結晶２ｃに凝固する。Next, while falling inside the infrared heater 13 in the falling tube 10, only the surface portion of the raw material melt 2b is heated, and the temperature distribution of the raw material melt 2b is shown in FIG. As described above, the temperature of the surface portion becomes higher than that of the inside of the raw material melt 2b. Next, while falling in the vacuum of the drop tube 10 below the infrared heater 13, the raw material melt 2b radiates heat by radiative cooling and solidifies into a true spherical crystal 2c by the action of the surface tension of the raw material melt 2b. .
【００４１】前記赤外線ヒータ１３を通過後、放射冷却
が進行して、凝固点Ｔｏ近くまで温度低下した状態にお
ける原料融液２ｂの温度分布は、図３（ｄ）に実線又は
２点鎖線で示すようになる。即ち、図３（ｃ）に示す温
度分布状態から放射冷却により表面部から冷却される結
果、原料融液２ｂの内部と表面部の温度がほぼ一様にな
る。このように、図３（ｄ）に実線で示す温度分布の状
態から原料融液２ｂが凝固する場合には、原料融液２ｂ
の内部と表面の両方から同時進行的に凝固するので、シ
リコンの原料融液２ｂが凝固中に体積膨張しても、球状
結晶２ｃの表面部に突起部が形成されることがなく、球
状結晶２ｃの内部歪みも非常に小さくなる。また、図３
（ｄ）に２点鎖線で示す温度分布の状態から原料融液２
ｂが凝固する場合には、原料融液２ｂの内部から凝固が
開始し、表面部が遅れて凝固するため、球状結晶２ｃの
表面部に突起部が形成されることがなく、球状結晶２ｃ
の内部歪みも非常に小さくなる。After passing through the infrared heater 13, radiative cooling proceeds, and the temperature distribution of the raw material melt 2b in a state where the temperature has dropped to near the freezing point To is shown by a solid line or a two-dot chain line in FIG. become. That is, as a result of being cooled from the surface portion by the radiation cooling from the temperature distribution state shown in FIG. 3C, the temperature of the inside and the surface portion of the raw material melt 2b become substantially uniform. As described above, when the raw material melt 2b solidifies from the state of the temperature distribution shown by the solid line in FIG.
Solidification simultaneously from both the inside and the surface of the spherical crystal 2c, even if the silicon raw material melt 2b expands in volume during the solidification, no projection is formed on the surface of the spherical crystal 2c, and the spherical crystal 2c is solidified. The internal distortion of 2c is also very small. FIG.
From the state of the temperature distribution indicated by the two-dot chain line in FIG.
When b solidifies, solidification starts from the inside of the raw material melt 2b, and the surface is solidified with a delay, so that no projection is formed on the surface of the spherical crystal 2c and the spherical crystal 2c
Also has a very small internal distortion.
【００４２】その後、落下チューブ１０内のほぼ中段部
のレベルで凝固が完了した球状結晶２ｃは、シリコンオ
イル槽１５内のシリコンオイル内へ落下し、そこに収容
されて完全に冷却される。シリコンオイル内へ落下する
とき、シリコンオイルで緩衝されるため、球状結晶２ｃ
が損傷することがない。尚、多数の球状結晶２ｃを製造
後には図示外の開閉扉を開いてシリコンオイル槽１５が
外部へ取り出される。尚、前記のように球状結晶２ｃの
内部歪みが小さくなるものの、球状結晶２ｃの全体が単
結晶にならない場合には、別途焼鈍処理することで球状
結晶２ｃの全体を単結晶にすることができる。Thereafter, the spherical crystal 2c, which has been solidified almost at the level of the middle stage in the drop tube 10, falls into the silicon oil in the silicon oil tank 15, is stored therein, and is completely cooled. When falling into silicon oil, it is buffered by silicon oil, so spherical crystals 2c
Is not damaged. After manufacturing a large number of spherical crystals 2c, the open / close door (not shown) is opened and the silicon oil tank 15 is taken out. In addition, as described above, when the internal strain of the spherical crystal 2c is reduced, but the entire spherical crystal 2c does not become a single crystal, the entire spherical crystal 2c can be made into a single crystal by separately annealing. .
【００４３】以上説明した球状体製造装置１及び球状体
製造方法によれば、赤外線ヒータ１３を介して原料融液
２ｂの温度分布を図３（ｄ）のように均一化してから球
状結晶２ｃに凝固させるため、シリコンの原料融液２ｂ
が凝固する際に膨張しても、球状結晶２ｃの表面部に突
起部が形成されるのを確実に抑制し、突起部の無い真球
状の球状結晶２ｃを製造することができる。そして、仮
に突起部が形成されるとしても、非常に小さな焼鈍処理
の際に消滅する位の突起部が形成されるだけである。ま
た、原料融液２ｂの表面部が内部よりも先に凝固しない
ため、原料体２ａの表面に付着した気泡が球状結晶２ｃ
に混入しなくなる。また、原料融液２ｂは微小重力状態
下に凝固して球状結晶２ｃになるため、熱対流、浮力、
沈降の影響を受けることなく成分が均一に分布した球状
結晶２ｃとなる。また、原料融液２ｂが凝固する際に種
結晶の無い状態で凝固するため、過冷却状態から凝固す
ることになる。According to the spherical body manufacturing apparatus 1 and the spherical body manufacturing method described above, the temperature distribution of the raw material melt 2b is made uniform via the infrared heater 13 as shown in FIG. To solidify, silicon raw material melt 2b
Even if swells when solidified, the formation of projections on the surface of the spherical crystal 2c is reliably suppressed, and a spherical spherical crystal 2c having no projections can be manufactured. And even if a projection is formed, only a projection which disappears during a very small annealing process is formed. Further, since the surface portion of the raw material melt 2b does not solidify before the inside thereof, bubbles adhering to the surface of the raw material body 2a become spherical crystals 2c.
Will not be mixed in. In addition, since the raw material melt 2b solidifies under microgravity to form a spherical crystal 2c, thermal convection, buoyancy,
A spherical crystal 2c is obtained in which the components are uniformly distributed without being affected by sedimentation. Further, when the raw material melt 2b is solidified, it solidifies without a seed crystal, so that it solidifies from a supercooled state.
【００４４】前記落下チューブ１０の高さは約１４ｍで
あるので、原料融液２ｂの落下時間は約１．７秒間であ
り、この約１．７秒の間に凝固できるサイズの球状結晶
２ｃを製造することができる。但し、落下チューブ１０
の長さを一層大きくすれば、一層大きな球状結晶２ｃを
製造することができる。尚、前記の例は、シリコンの球
状結晶２ｃを製造する場合を例として説明したが、シリ
コンに限らず、種々の無機材料（半導体、超電導体、誘
電体、磁性体、合金、ガラス等）であって誘導加熱可能
な無機材料製の球状結晶や球状体を製造することができ
る。そして、凝固の際に体積収縮する無機材料の場合に
も、球状体２ｃの表面部に凹部が形成されず、真球状の
球状体になる。しかも、原料供給装置１１は所定時間お
きに原料体２ａを落下チューブ１０内へ供給できるよう
に構成してあるため、無機材料製の球状結晶や球状体を
能率的に量産することができる。Since the height of the drop tube 10 is about 14 m, the falling time of the raw material melt 2 b is about 1.7 seconds, and the spherical crystal 2 c having a size that can be solidified in about 1.7 seconds. Can be manufactured. However, the falling tube 10
If the length is further increased, a larger spherical crystal 2c can be manufactured. In the above-described example, the case of manufacturing the silicon spherical crystal 2c has been described as an example. However, the present invention is not limited to silicon, and various inorganic materials (semiconductor, superconductor, dielectric, magnetic material, alloy, glass, etc.) Thus, a spherical crystal or a spherical body made of an inorganic material that can be induction-heated can be produced. Then, even in the case of an inorganic material that contracts in volume during solidification, no concave portion is formed on the surface of the spherical body 2c, and the spherical body 2c becomes a true spherical body. In addition, since the raw material supply device 11 is configured to supply the raw material 2a into the falling tube 10 at predetermined time intervals, it is possible to efficiently mass-produce spherical crystals and spherical bodies made of an inorganic material.
【００４５】ガラス製または酸化物高温超電導体（例え
ば、ＹＢａ2 Ｃｕ3 Ｏ2 ）製の球状体を製造するような
場合には、真空ポンプ１６を停止し、電磁開閉弁２４，
３６〜３８を閉じ、電磁開閉弁４０，４２を開き、ガス
供給装置１７から、酸素ガスまたは酸素ガスを含む窒素
ガスを落下チューブ１０に供給し、そのガス中で原料体
を加熱溶融させ、そのガス中を原料融液２ｂを自由落下
させつつ凝固させる。また、球状結晶２ｃの表面部に種
類の異なる無機材料をドーピングするような場合には、
ガス供給装置１７から供給する不活性ガスとともにドー
ピングの為の無機材料のガスを落下チューブ１０内へ供
給し、そのガス中で原料体を加熱溶融させ、そのガス中
を原料融液２ｂを自由落下させつつ凝固させることもで
きる。When manufacturing a spherical body made of glass or an oxide high-temperature superconductor (for example, YBa 2 Cu 3 O 2 ), the vacuum pump 16 is stopped and the electromagnetic on-off valve 24,
36 to 38 are closed, the electromagnetic on / off valves 40 and 42 are opened, and oxygen gas or nitrogen gas containing oxygen gas is supplied from the gas supply device 17 to the drop tube 10, and the raw material is heated and melted in the gas. The raw material melt 2b is solidified while falling freely in the gas. In the case of doping the surface portion of the spherical crystal 2c with a different kind of inorganic material,
A gas of an inorganic material for doping is supplied into the drop tube 10 together with the inert gas supplied from the gas supply device 17, the raw material is heated and melted in the gas, and the raw material melt 2b falls freely in the gas. It can be coagulated while it is being made.
【００４６】絶縁体の無機材料（例えば、ガラス）の場
合には、電磁浮遊加熱装置１２により誘導加熱すること
ができないので、電磁浮遊加熱装置１２の代わりに、静
電浮遊装置と加熱装置、又は音波浮遊装置と加熱装置を
適用すればよい。尚、その加熱装置としては、電気ヒー
タ、赤外線ヒータ、ハロゲンランプヒータ、レーザ光ヒ
ータ等の種々の加熱手段を適用可能である。他方、無機
材料の種類と関係無しに、前記赤外線ヒータ１３の代わ
りに、電気ヒータ、ハロゲンランプヒータ、レーザ光ヒ
ータ等の種々のヒータを適用可能である。In the case of an insulating inorganic material (eg, glass), induction heating cannot be performed by the electromagnetic floating heating device 12, and therefore, instead of the electromagnetic floating heating device 12, an electrostatic floating device and a heating device, or What is necessary is just to apply a sound wave floating device and a heating device. As the heating device, various heating means such as an electric heater, an infrared heater, a halogen lamp heater, and a laser beam heater can be applied. On the other hand, various heaters such as an electric heater, a halogen lamp heater, and a laser beam heater can be applied instead of the infrared heater 13 regardless of the type of the inorganic material.
【００４７】次に、前記の実施形態を部分的に変更した
別実施形態について説明する。図４に示すように、この
無機材料製の球状体製造装置１Ａは、２種類の異なる無
機材料製の原料体２ａ，２Ａを落下チューブ１０内に供
給し、電磁浮遊加熱装置１２により一体的に溶融して２
種類の無機材料製からなる球状結晶や球状体を製造する
装置である。原料供給装置１１Ａ以外の構成は、前記実
施形態のものと同様であるので、同一の構成要素に同一
符号を付して説明を省略する。Next, another embodiment in which the above embodiment is partially modified will be described. As shown in FIG. 4, an apparatus 1A for manufacturing a sphere made of an inorganic material supplies two kinds of raw materials 2a and 2A made of an inorganic material into a drop tube 10 and integrally uses an electromagnetic floating heating device 12. Melted 2
It is an apparatus for producing spherical crystals and spherical bodies made of various kinds of inorganic materials. The configuration other than the raw material supply device 11A is the same as that of the above-described embodiment.
【００４８】原料供給装置１１Ａは、パーツフィーダ２
２の他に、パーツフィーダ２２Ａを有し、このパーツフ
ィーダ２２Ａは電磁開閉シャッター２７Ａを有する通路
２８Ａを介して供給器２１の受入器２６に接続され、こ
のパーツフィーダ２２Ａからも受入器２６に原料体２Ａ
を供給可能に構成してある。パーツフィーダ２２からは
シリコンの原料体２ａが受入器２６に供給され、パーツ
フィーダ２２Ａからはゲルマニウムの原料体２Ａが受入
器２６に供給される。但し、原料体２ａと原料体２Ａは
所定の組成比となるように夫々の重量が設定されてい
る。The raw material supply device 11A includes a parts feeder 2
In addition to the parts feeder 22A, the parts feeder 22A is connected to the receiver 26 of the feeder 21 through a passage 28A having an electromagnetic opening / closing shutter 27A. Body 2A
Can be supplied. The raw material body 2a of silicon is supplied to the receiver 26 from the parts feeder 22, and the raw material body 2A of germanium is supplied to the receiver 26 from the parts feeder 22A. However, the weights of the raw material 2a and the raw material 2A are set so as to have a predetermined composition ratio.
【００４９】シリコンとゲルマニウムとからなるＰ形又
はＮ形半導体の球状結晶を製造する場合、受入器２６に
１個のシリコンの原料体２ａと１個のゲルマニウムの原
料体２Ａとを収容後、前記実施形態と同様に、原料体２
ａ，２Ａを電磁浮遊加熱装置１２に供給して接触状に浮
遊させた状態で加熱して一体的に溶融させて原料融液と
する。それ以降は前記実施形態と同様である。このよう
にして、シリコンとゲルマニウムを混合した混晶半導体
の球状結晶を製造することができる。尚、シリコンとゲ
ルマニウムに限らず、種々の無機材料のうち２種類の無
機材料からなる球状結晶や球状体を製造することができ
る。尚、２つのパーツフィーダ２２，２２Ａに限らず、
３つ以上のパーツフィーダを設け、３種類以上の無機材
料からなる球状結晶や球状体を製造することもできる。In the case of producing a spherical crystal of a P-type or N-type semiconductor comprising silicon and germanium, one silicon raw material 2a and one germanium raw material 2A are accommodated in the receiver 26, and As in the embodiment, the raw material body 2
The raw materials a and 2A are supplied to the electromagnetic floating heating device 12 and are heated and melted integrally in a state of floating in a contact state to obtain a raw material melt. Subsequent steps are the same as in the above embodiment. In this manner, a mixed crystal semiconductor spherical crystal in which silicon and germanium are mixed can be manufactured. In addition, not only silicon and germanium but also spherical crystals and spherical bodies made of two kinds of inorganic materials among various inorganic materials can be manufactured. In addition, it is not limited to the two parts feeders 22 and 22A,
By providing three or more parts feeders, a spherical crystal or a spherical body made of three or more kinds of inorganic materials can be manufactured.
【００５０】[0050]
【発明の効果】請求項１の発明によれば、第１工程〜第
５工程により、原料体を浮遊させた状態で溶融し、落下
チューブ内を自由落下させながら凝固させて球状体にす
るので、不純物を含まない球状体、熱対流や浮力や沈降
の影響無しに、成分が均一に分布した無機材料製の球状
体（球状結晶を含む）を製造することができる。また、
第２工程と第３工程とを経て原料融液を凝固させること
により、原料融液の内部から、或いは、内部と表面部の
両方から凝固を開始させて、球状体の表面の一部に突起
部や凹部が形成されるのを効果的に抑制することができ
るうえ、球状体の内部歪みを小さくすることができる。
また、原料体の表面に付着していた気泡が球状体の内部
に混入するのを防止することもできる。According to the first aspect of the present invention, in the first to fifth steps, the raw material is melted in a floating state and solidified into a spherical body while freely falling in the falling tube. It is possible to produce spherical bodies (including spherical crystals) made of an inorganic material in which components are uniformly distributed without the influence of thermal convection, buoyancy, and sedimentation. Also,
By solidifying the raw material melt through the second step and the third step, solidification is started from the inside of the raw material melt or from both the inside and the surface portion, and a projection is formed on a part of the surface of the spherical body. The formation of the portions and the concave portions can be effectively suppressed, and the internal distortion of the spherical body can be reduced.
Further, it is possible to prevent bubbles adhering to the surface of the raw material from being mixed into the spherical body.
【００５１】請求項２の発明によれば、請求項１と同様
の効果を奏する他、無機材料がシリコンであるので、シ
リコンの球状結晶を製造することができ、その球状結晶
の表面部に突起部が形成されるのを抑制して、真球状の
球状結晶にすることができ、球状結晶の内部歪みを小さ
くすることができる。According to the second aspect of the invention, in addition to the same effect as the first aspect, since the inorganic material is silicon, it is possible to produce a spherical crystal of silicon, and a projection is formed on the surface of the spherical crystal. The formation of a portion can be suppressed to make a true spherical spherical crystal, and the internal strain of the spherical crystal can be reduced.
【００５２】請求項３の発明によれば、請求項１と同様
の効果を奏する他、複数の種類の異なる無機材料からな
る球状体（球状結晶を含む）であって成分が均一に分布
した球状体を製造することができ、球状体の表面部に突
起部や凹部が形成されるのを抑制でき、球状体の内部歪
みを小さくすることができる。According to the third aspect of the present invention, in addition to the same effects as those of the first aspect, a spherical body (including a spherical crystal) made of a plurality of different inorganic materials, in which components are uniformly distributed, is provided. The body can be manufactured, the formation of projections and recesses on the surface of the spherical body can be suppressed, and the internal distortion of the spherical body can be reduced.
【００５３】請求項４の無機材料製の球状結晶の製造方
法は、請求項３と同様の効果を奏するが、前記相互に異
なる種類の無機材料がシリコンとゲルマニウムであるの
で、シリコン・ゲルマニウムの混晶半導体の球状結晶を
製造することができる。The method for producing a spherical crystal made of an inorganic material according to the fourth aspect has the same effect as that of the third aspect. However, since the mutually different types of inorganic materials are silicon and germanium, a mixture of silicon and germanium is obtained. Spherical semiconductor crystals can be produced.
【００５４】請求項５の無機材料製の球状体の製造装置
によれば、落下チューブと、原料体供給手段と、浮遊加
熱手段と、浮遊加熱手段の下側に所定距離以上離隔して
配設され落下チューブ内を落下中の原料融液の表面部を
加熱するアフターヒータとを備えているため、請求項１
と同様に、表面部に突起部や凹部が無く真球状で、内部
歪みが小さく、気泡の混入の無い無機材料製の球状体を
連続的に能率的に安価に量産することができる。According to the apparatus for manufacturing a spherical body made of an inorganic material according to the fifth aspect, the drop tube, the raw material supply means, the floating heating means, and the lower side of the floating heating means are arranged at a predetermined distance or more. An after-heater for heating a surface portion of the raw material melt falling in the falling tube.
Similarly to the above, a spherical body made of an inorganic material, which is a true sphere with no protrusions or recesses on its surface, has small internal distortion, and contains no air bubbles, can be continuously mass-produced efficiently and inexpensively.
【００５５】請求項６の無機材料製の球状体の製造装置
によれば、請求項５と同様の効果を奏するが、落下チュ
ーブ内を真空状態にする真空化手段を設けたので、落下
チューブ内を真空状態にして球状体を製造することがで
きる。According to the apparatus for manufacturing a spherical body made of an inorganic material according to the sixth aspect, the same effect as that of the fifth aspect can be obtained, but the vacuuming means for evacuating the inside of the falling tube is provided, so that the inside of the falling tube is provided. In a vacuum to produce a spherical body.
【００５６】請求項７の無機材料製の球状体の製造装置
によれば、請求項６と同様の効果を奏するが、無機材料
の種類に応じた所定のガスを落下チューブ内に供給する
とともに、落下チューブ内に原料融液の落下方向へほぼ
同速で流れるガス流を形成し且つ落下チューブ内に球状
体の落下方向と反対方向へ流れるガス流を形成するガス
供給手段を設けたので、落下チューブ内に所定のガスを
供給して供給体を製造する場合に、ガス流から凝固中の
原料融液に摩擦力が殆ど作用せず、原料融液は真球状に
凝固する。そして、ガス流と凝固後の球状体との接触度
合いが高くなり、ガスと球状体との反応や球状体の冷却
が促進される。According to the apparatus for manufacturing a spherical body made of an inorganic material according to the seventh aspect, the same effect as that of the sixth aspect is obtained, but a predetermined gas corresponding to the type of the inorganic material is supplied into the falling tube. Since the gas supply means for forming a gas flow flowing at substantially the same speed in the falling direction of the raw material melt in the falling tube and forming a gas flow flowing in the direction opposite to the falling direction of the spherical body in the falling tube is provided. When a predetermined gas is supplied into the tube to produce a supply body, little frictional force acts on the raw material melt being solidified from the gas flow, and the raw material melt solidifies in a true spherical shape. Then, the degree of contact between the gas flow and the solidified spherical body is increased, and the reaction between the gas and the spherical body and the cooling of the spherical body are promoted.
【００５７】請求項８の無機材料製の球状体の製造装置
によれば、請求項７と同様の効果を奏するが、落下チュ
ーブの下端に臨み、その下端外へ落下した球状体を冷却
液内に収容する冷却液槽を設けたので、球状体が衝撃で
損傷するのを防止するとともに、球状体を冷却すること
ができる。According to the apparatus for manufacturing a spherical body made of an inorganic material according to the eighth aspect, the same effect as that of the seventh aspect can be obtained, but the spherical body which faces the lower end of the falling tube and falls outside the lower end is filled in the cooling liquid. Since the cooling liquid tank accommodated in the sphere is provided, it is possible to prevent the sphere from being damaged by impact and to cool the sphere.
【図１】本発明の実施形態に係る無機材料製の球状体製
造装置の全体構成図である。FIG. 1 is an overall configuration diagram of an apparatus for manufacturing a spherical body made of an inorganic material according to an embodiment of the present invention.
【図２】前記製造装置の電磁浮遊加熱装置と赤外線ヒー
タの構成図である。FIG. 2 is a configuration diagram of an electromagnetic floating heating device and an infrared heater of the manufacturing apparatus.
【図３】（ａ）は電磁浮遊加熱後の原料融液の温度分布
図、（ｂ）は赤外線ヒータ直前の原料融液の温度分布
図、（ｃ）は赤外線ヒータで加熱後の原料融液の温度分
布図、（ｄ）は凝固直前の原料融液の温度分布図であ
る。3 (a) is a temperature distribution diagram of the raw material melt after electromagnetic floating heating, (b) is a temperature distribution diagram of the raw material melt immediately before the infrared heater, and (c) is a raw material melt heated by the infrared heater (D) is a temperature distribution diagram of the raw material melt immediately before solidification.
【図４】別実施形態に係る無機材料製の球状体製造装置
の全体構成図である。FIG. 4 is an overall configuration diagram of an apparatus for manufacturing a spherical body made of an inorganic material according to another embodiment.
１，１Ａ 球状体製造装置 ２ａ，２Ａ 原料体 ２ｂ 原料融液 ２ｃ 球状結晶（球状体） １０ 落下チューブ １１ 原料供給装置 １２ 電磁浮遊加熱装置（浮遊力発生手
段、加熱手段、浮遊加熱手段） １３ 赤外線ヒータ（補助加熱手段、アフ
ターヒータ） １６ 真空ポンプ １７ ガス供給装置1, 1A spherical body manufacturing apparatus 2a, 2A raw material body 2b raw material melt 2c spherical crystal (spherical body) 10 drop tube 11 raw material supply device 12 electromagnetic floating heating device (floating force generating means, heating means, floating heating means) 13 infrared rays Heater (auxiliary heating means, after heater) 16 Vacuum pump 17 Gas supply device
Claims (8)
段により真空中又は所定のガス中に浮遊させた状態で加
熱手段により加熱して溶融させる第１工程と、 次に原料融液を鉛直姿勢にした落下チューブ内の真空中
又は所定のガス中を落下させながら融液状態のまま放熱
させる第２工程と、 次に前記原料融液を前記落下チューブ内の真空中又は所
定のガス中を落下させながら、補助加熱手段により原料
融液の表面部を加熱する第３工程と、 次に前記原料融液を前記落下チューブ内の真空中又は所
定のガス中を落下させながら冷却して原料融液の表面張
力の作用で球状体に凝固させる第４工程と、 次に前記球状体を前記落下チューブの下端に臨む冷却液
槽の冷却液内に収容する第５工程と、 を備えたことを特徴とする無機材料製の球状体の製造方
法。1. A first step of heating and melting a raw material body made of an inorganic material by a heating means in a state of being floated in a vacuum or a predetermined gas by a buoyancy force generating means; A second step of radiating heat in a molten state while dropping in a vacuum or a predetermined gas in a falling tube in a posture, and then passing the raw material melt in a vacuum or a predetermined gas in the falling tube. A third step of heating the surface portion of the raw material melt by the auxiliary heating means while dropping, and then cooling the raw material melt while dropping it in a vacuum or a predetermined gas in the falling tube to melt the raw material melt. A fourth step of solidifying into a spherical body by the action of the surface tension of the liquid; and a fifth step of storing the spherical body in a cooling liquid in a cooling liquid tank facing a lower end of the drop tube. Manufacture of spherical material made of inorganic material Method.
徴とする請求項１に記載の無機材料製の球状体の製造方
法。2. The method for producing a spherical body made of an inorganic material according to claim 1, wherein the inorganic material is silicon.
数の原料体を、浮遊力発生手段により真空中又は所定の
ガス中に接触状に浮遊させた状態で加熱手段により加熱
して一体的に溶融させる第１工程と、 次に原料融液を鉛直姿勢にした落下チューブ内の真空中
又は所定のガス中を落下させながら融液状態のまま放熱
させる第２工程と、 次に前記原料融液を前記落下チューブ内の真空中又は所
定のガス中を落下させながら、補助加熱手段により原料
融液の表面部を加熱する第３工程と、 次に前記原料融液を前記落下チューブ内の真空中又は所
定のガス中を落下させながら冷却して原料融液の表面張
力の作用で球状体に凝固させる第４工程と、 次に前記球状体を前記落下チューブの下端に臨む冷却液
槽の冷却液内に収容する第５工程と、 を備えたことを特徴とする無機材料製の球状体の製造方
法。3. A plurality of raw materials made of different kinds of inorganic materials are heated by a heating means in a state of being floated in a vacuum or a predetermined gas in a contact state by a buoyancy force generating means to integrally form the raw materials. A first step of melting; and a second step of releasing the raw material melt in a molten state while falling in a vacuum or a predetermined gas in a falling tube in a vertical position, and then releasing the raw material melt. A third step of heating the surface portion of the raw material melt by auxiliary heating means while dropping the raw material melt in a vacuum or a predetermined gas in the drop tube; Or a fourth step of cooling while dropping in a predetermined gas to solidify into a spherical body by the action of the surface tension of the raw material melt, and then a cooling liquid in a cooling liquid tank facing the lower end of the falling tube. 5th process to be accommodated in Method of producing an inorganic material made of spherical bodies, characterized in that the.
コンとゲルマニウムであることを特徴とする請求項３に
記載の無機材料製の球状体の製造方法。4. The method according to claim 3, wherein the different types of inorganic materials are silicon and germanium.
内の真空中又は所定のガス中で浮遊状態で加熱し、その
原料融液を落下チューブ内を自由落下させながら凝固さ
せて球状体を製造する装置において、 鉛直姿勢の落下チューブと、 前記落下チューブ内へその上端から原料体を供給する原
料体供給手段と、 前記落下チューブの上端部又はその付近内で原料体を浮
遊させた状態で加熱して原料融液にする浮遊加熱手段
と、 前記浮遊加熱手段の下側に所定距離以上離隔して配設さ
れ、落下チューブ内を落下中の原料融液の表面部を加熱
するアフターヒータと、 を備えたことを特徴とする無機材料製の球状体の製造装
置。5. A spherical body is produced by heating a raw material body made of an inorganic material in a floating state in a vacuum or a predetermined gas in a falling tube and solidifying the raw material melt while freely falling in the falling tube. A falling tube having a vertical posture, a raw material supply means for supplying a raw material into the falling tube from an upper end thereof, and heating the raw material in a state of being floated at or near the upper end of the falling tube. A floating heating means for converting the raw material melt into a raw material melt, and an after heater disposed at a predetermined distance or less below the floating heating means and heating a surface portion of the raw material melt falling in the falling tube, An apparatus for producing a spherical body made of an inorganic material, comprising:
て真空状態にする真空化手段を設けたことを特徴とする
請求項５に記載の無機材料製の球状体の製造装置。6. The apparatus for producing a spherical body made of an inorganic material according to claim 5, wherein a vacuuming means for evacuating the inside of the drop tube via a vacuum pump is provided.
下チューブ内に供給するとともに、落下チューブ内に原
料融液の落下方向へほぼ同速で流れるガス流を形成し且
つ落下チューブ内に球状体の落下方向と反対方向へ流れ
るガス流を形成するガス供給手段を設けたことを特徴と
する請求項６に記載の無機材料製の球状体の製造装置。7. A predetermined gas corresponding to the type of the inorganic material is supplied into the drop tube, and a gas flow that flows at substantially the same speed in the dropping direction of the raw material melt is formed in the drop tube. The apparatus for producing a spherical body made of an inorganic material according to claim 6, further comprising gas supply means for forming a gas flow flowing in a direction opposite to the direction in which the spherical body falls.
端外へ落下した球状体を冷却液内に収容する冷却液槽を
設けたことを特徴とする請求項７に記載の無機材料製の
球状体の製造装置。8. A spherical ball made of an inorganic material according to claim 7, wherein a cooling liquid tank which faces a lower end of said falling tube and accommodates a spherical body dropped to the outside of the lower end in a cooling liquid is provided. Body manufacturing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21188396A JP3231244B2 (en) | 1996-07-22 | 1996-07-22 | Method for producing spherical material made of inorganic material and apparatus for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21188396A JP3231244B2 (en) | 1996-07-22 | 1996-07-22 | Method for producing spherical material made of inorganic material and apparatus for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1033969A JPH1033969A (en) | 1998-02-10 |
| JP3231244B2 true JP3231244B2 (en) | 2001-11-19 |
Family
ID=16613213
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21188396A Expired - Fee Related JP3231244B2 (en) | 1996-07-22 | 1996-07-22 | Method for producing spherical material made of inorganic material and apparatus for producing the same |
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| JP (1) | JP3231244B2 (en) |
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| US7387400B2 (en) | 2003-04-21 | 2008-06-17 | Kyosemi Corporation | Light-emitting device with spherical photoelectric converting element |
| ATE425574T1 (en) | 2003-06-09 | 2009-03-15 | Kyosemi Corp | GENERATOR SYSTEM |
| CA2537777C (en) | 2003-10-24 | 2011-08-02 | Kyosemi Corporation | Light receiving or emitting modular sheet and production method thereof |
| WO2006123403A1 (en) * | 2005-05-17 | 2006-11-23 | Kyosemi Corporation | Granular crystal production apparatus |
| WO2007141836A1 (en) | 2006-06-02 | 2007-12-13 | Hitachi, Ltd. | Method for manufacturing inlet for ic tag |
| JP6424301B2 (en) * | 2014-02-24 | 2018-11-14 | 竹田 眞司 | Method of manufacturing an efficient solar power generation device |
-
1996
- 1996-07-22 JP JP21188396A patent/JP3231244B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8237045B2 (en) | 2004-03-12 | 2012-08-07 | Kyosemi Corporation | Laminated solar battery |
| US9159856B2 (en) | 2004-03-12 | 2015-10-13 | Kyosemi Corporation | Laminated solar battery |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH1033969A (en) | 1998-02-10 |
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