公开(公告)号：US20150028268A1

公开(公告)日：2015-01-29

申请号：US14383321

申请日：2012-03-08

申请人： Shinji Tokumaru ,  Masataka HIiyoshi ,  Jiro Kondo ,  Hitoshi Dohnomae ,  Yutaka Kishida ,  Shigeru Nakazawa ,  Kozo Onoue

发明人： Shinji Tokumaru ,  Masataka HIiyoshi ,  Jiro Kondo ,  Hitoshi Dohnomae ,  Yutaka Kishida ,  Shigeru Nakazawa ,  Kozo Onoue

IPC分类号： C01B33/037 ,  H01L31/0288

CPC分类号： C01B33/037 ,  C01B33/021 ,  C30B11/002 ,  C30B11/007 ,  C30B13/10 ,  C30B21/00 ,  C30B29/06 ,  H01L31/0288

摘要： Provided are a method for manufacturing a highly pure silicon by unidirectional solidification of molten silicon, that can inexpensively and industrially easily manufacture highly pure silicon that has a low oxygen concentration and low carbon concentration and is suitable for applications such as manufacturing solar cells; highly pure silicon obtained by this method and silicon raw material for manufacturing highly pure silicon. A method for manufacturing highly pure silicon using molten silicon containing 100 to 1000 ppmw of carbon and 0.5 to 2000 ppmw of germanium as the raw material when manufacturing highly pure silicon by unidirectionally solidifying molten silicon raw material in a casting container, the highly pure silicon obtained by this method, and the silicon raw material for manufacturing the highly pure silicon.

摘要翻译： 提供一种通过熔融硅的单向凝固来制造高纯度硅的方法，其可以廉价和工业上容易地制造具有低氧浓度和低碳浓度的高纯度硅，并且适用于制造太阳能电池的应用; 通过该方法获得的高纯度硅和用于制造高纯度硅的硅原料。 通过在铸造容器中单独固化熔融硅原料制造高纯度硅时，使用含有100〜1000ppmw碳和0.5〜2000ppmw的锗作为原料的熔融硅制造高纯硅的方法，得到高纯硅 通过该方法和用于制造高纯度硅的硅原料。

公开(公告)号：US07582160B2

公开(公告)日：2009-09-01

申请号：US11451989

申请日：2006-06-13

申请人： Yutaka Kishida ,  Seiki Takebayashi ,  Teruyuki Tamaki

发明人： Yutaka Kishida ,  Seiki Takebayashi ,  Teruyuki Tamaki

IPC分类号： C30B15/00

CPC分类号： C30B15/00 ,  C30B29/06 ,  Y10S117/916

摘要： In silicon single crystal growth by the Czochralski method using a quartz crucible, a silicon single crystals with a uniform distribution of oxygen concentration can be produced in high yield without being affected by changes of crystal diameter and initial amount of melt feedstock. The oxygen concentration is adjusted by estimating oxygen concentration during growth on the basis of a relationship among three parameters: crucible rotation rate (Ω), crucible temperature (T), and the ratio (β) of contact area of molten silicon with the inner wall of the crucible and with atmospheric gas, and by associating the temperature (T) with the ratio (β) by the function 1/β×Exp(−E/T) where E is the dissolution energy (E) of quartz into molten silicon to control at least one of the rotation rate (Ω) and temperature (T) to conform the estimated oxygen concentration to a target concentration.

摘要翻译： 在使用石英坩埚的切克劳斯基法的硅单晶生长中，可以高产率地产生具有均匀氧浓度分布的硅单晶，而不受晶体直径变化和熔融原料初始量的影响。 通过根据三个参数之间的关系来估计生长期间的氧浓度来调节氧浓度：坩埚旋转速率（Omega），坩埚温度（T）和熔融硅与内壁的接触面积的比（β） 并且通过将温度（T）与比率（β）与功能1 / betaxExp（-E / T）相关联，其中E是石英溶解能量（E）到熔融硅中以控制 旋转速率（Omega）和温度（T）中的至少一个使估计的氧浓度与目标浓度一致。

公开(公告)号：US06899759B2

公开(公告)日：2005-05-31

申请号：US10283683

申请日：2002-10-30

申请人： Yutaka Kishida ,  Teruyuki Tamaki ,  Seiki Takebayashi ,  Wataru Ohashi

发明人： Yutaka Kishida ,  Teruyuki Tamaki ,  Seiki Takebayashi ,  Wataru Ohashi

IPC分类号： C30B29/06 ,  C30B15/00 ,  C30B15/20 ,  C30B15/30

CPC分类号： C30B29/06 ,  C30B15/30 ,  Y10T117/1068 ,  Y10T117/1072

摘要： A single crystal production method based on the Czochralski method comprises controlling a number of crucible rotations and crystal rotations so that a number of vibrations for driving a melt, determined on the basis of the number of crucible and crystal rotations during a single crystal growing procedure, is outside a range from 95% to 105% of a number of sloshing resonance vibrations of the melt. In another embodiment, the method comprises controlling a number of rotations of a crystal and crucible, so that when a number of vibrations for driving a melt, determined by the number of crucible and crystal rotations during a single crystal growing procedure, is within a range from 95% to 105% of a number of sloshing resonance vibrations of the melt, the number of vibrations of the melt due to sloshing does not exceed 2000 times during a period when the number of vibrations is within that range.

摘要翻译： 基于切克劳斯基法的单晶制造方法包括：控制多个坩埚旋转和晶体旋转，使得在单晶生长过程中，基于坩埚的数量和晶体旋转确定的用于驱动熔体的多个振动， 在熔融物的共振振动的数量的95％至105％的范围之外。 在另一个实施例中，该方法包括控制晶体和坩埚的旋转次数，使得当在单晶生长过程期间由坩埚的数量和晶体旋转确定的用于驱动熔体的多个振动在一定范围内 熔体共振振动数量的95％至105％时，在振动次数在该范围内的期间，由于晃动引起的熔体振动次数不超过2000次。

公开(公告)号：US10370253B2

公开(公告)日：2019-08-06

申请号：US14381150

申请日：2012-03-09

申请人： Yutaka Kishida ,  Hitoshi Dohnomae

发明人： Yutaka Kishida ,  Hitoshi Dohnomae

IPC分类号： C01B33/037 ,  B01J6/00

摘要： Provided is a silicon refining device that is used when industrially producing silicon of high purity by vacuum melting, has a high P removal rate and thus high productivity, and is a practical device cost-wise with a simple and cheap device configuration. This silicon refining device comprises, in a decompression vessel provided with a vacuum pump, a crucible that contains a metal silicon material, a heating device that heats the crucible, and a molten metal surface thermal insulation member that covers the upper portion of silicon molten metal and has an exhaust opening with an opening area that is smaller than the silicon molten metal surface area. The molten metal surface thermal insulation member comprises a laminated insulation material with a multilayer structure in which three or more laminates are laminated at predetermined intervals from each other, and which exhibits a radiant heat insulating function based on the multilayer structure.

公开(公告)号：US20150033798A1

公开(公告)日：2015-02-05

申请号：US14381150

申请日：2012-03-09

申请人： Yutaka Kishida ,  Hitoshi Dohnomae

发明人： Yutaka Kishida ,  Hitoshi Dohnomae

IPC分类号： C01B33/037

CPC分类号： C01B33/037 ,  B01J6/007 ,  B01J2219/00155

摘要： Provided is a silicon refining device that is used when industrially producing silicon of high purity by vacuum melting, has a high P removal rate and thus high productivity, and is a practical device cost-wise with a simple and cheap device configuration. This silicon refining device comprises, in a decompression vessel provided with a vacuum pump, a crucible that contains a metal silicon material, a heating device that heats the crucible, and a molten metal surface thermal insulation member that covers the upper portion of silicon molten metal and has an exhaust opening with an opening area that is smaller than the silicon molten metal surface area. The molten metal surface thermal insulation member comprises a laminated insulation material with a multilayer structure in which three or more laminates are laminated at predetermined intervals from each other, and which exhibits a radiant heat insulating function based on the multilayer structure.

摘要翻译： 本发明提供一种在通过真空熔融工业生产高纯度硅的硅精炼装置中，具有高P去除率和高生产率的硅精炼装置，并且成本低廉的装置结构是实用的装置。 该硅精制装置在具有真空泵的减压容器中包括含有金属硅材料的坩埚，加热坩埚的加热装置和覆盖硅熔融金属上部的熔融金属表面保温部件 并且具有开口面积小于硅熔融金属表面积的排气口。 熔融金属表面绝热构件包括具有多层结构的层压绝缘材料，其中三个或更多个层叠体以预定间隔彼此层叠，并且基于多层结构呈现辐射绝热功能。

公开(公告)号：US06200384B1

公开(公告)日：2001-03-13

申请号：US09361245

申请日：1999-07-27

申请人： Yutaka Kishida ,  Wataru Ohashi ,  Teruyuki Tamaki ,  Seiki Takebayashi

发明人： Yutaka Kishida ,  Wataru Ohashi ,  Teruyuki Tamaki ,  Seiki Takebayashi

IPC分类号： C30B1522

CPC分类号： C30B29/06 ,  C30B15/305 ,  Y10S117/917

摘要： In the growth of a large silicon single crystal weighing not less than 100 kg by the Czokralski method resorting to application of a magnetic field, a crucible, not less than 0.7 m in inside diameter is used, and a cusped magnetic field which manifests a maximum intensity of not more than 1000 gausses on the inner wall of the crucible is applied.

摘要翻译： 在通过施加磁场的Czokralski方法生长重量不小于100kg的大型硅单晶时，使用内径不小于0.7μm的坩埚和表现出最大值的尖细磁场 应用坩埚内壁上不超过1000高斯的强度。

公开(公告)号：US20150082942A1

公开(公告)日：2015-03-26

申请号：US14374941

申请日：2012-02-06

申请人： Yutaka Kishida ,  Hitoshi Dohnomae ,  Jiro Kondo ,  Kiyoshi Goto ,  Wataru Ohashi

发明人： Yutaka Kishida ,  Hitoshi Dohnomae ,  Jiro Kondo ,  Kiyoshi Goto ,  Wataru Ohashi

IPC分类号： F27B14/14 ,  C22B9/02 ,  B01D1/02 ,  F27B14/04 ,  F27B14/06 ,  C22B9/04 ,  F27D99/00

CPC分类号： F27B14/14 ,  B01D1/02 ,  C01B33/037 ,  C22B9/02 ,  C22B9/04 ,  F27B14/04 ,  F27B14/06 ,  F27B2014/045 ,  F27D99/0006 ,  F27D2099/0008

摘要： An objective of the present invention is, in refining a metal or a semiconductor melt, without impairing refining efficiency, to alleviate wear and tear commensurate with unevenness in a crucible caused by instability in melt flow, and to allow safe operation over long periods of time such that leakages from the crucible do not occur. Provided is a metal or semiconductor melt refining method, in which, by using an AC resistance heating heater as a crucible heating method, the melt is heat retained and mixed by a rotating magnetic field which is generated by the resistance heating heater. The metal or semiconductor melt refinement method and a vacuum refinement device which is optimal for the refinement method are characterized in that, in order that a fluid instability does not occur in the boundary between the melt and the bottom face of the crucible when the melt is rotated by the rotating magnetic field, with a kinematic viscosity coefficient of the melt designated ν (m2/sec), the radius of the fluid surface of the melt designated R (m), and the rotational angular velocity of the melt designated Ω (rad/sec), the operation is carried out such that the value of a Reynolds number (Re) which is defined as Re=R×(Ω/ν)̂(1/2) does not exceed 600.

摘要翻译： 本发明的目的是在不损害精炼效率的同时，在精炼金属或半导体熔体的同时，减轻由熔体流动不稳定引起的坩埚中的不均匀度的磨损和撕裂，并允许长时间的安全运行 从而不会发生坩埚的泄漏。 提供一种金属或半导体熔融精炼方法，其中通过使用交流电阻加热器作为坩埚加热方法，通过由电阻加热器产生的旋转磁场将熔体热保持并混合。 金属或半导体熔体精制方法和对精制方法最佳的真空精制装置的特征在于，为了在熔体与坩埚的底面之间的边界处不会发生流体不稳定性，当熔体是 通过旋转磁场旋转，熔体的运动粘度系数指定为ngr; （m2 / sec），指定为R（m）的熔体的流体表面的半径以及指定为＆OHgr的熔体的旋转角速度; （rad / sec），进行操作，使得被定义为Re = R×（＆OHgr; /＆ngr;）（1/2）的雷诺数（Re）的值不超过600。

公开(公告)号：US07195668B2

公开(公告)日：2007-03-27

申请号：US11020858

申请日：2004-12-22

申请人： Yutaka Kishida ,  Teruyuki Tamaki

发明人： Yutaka Kishida ,  Teruyuki Tamaki

IPC分类号： C30B15/20

CPC分类号： C30B15/10 ,  Y10S117/90 ,  Y10T117/10 ,  Y10T117/1068

摘要： A crucible for the growth of single crystals by the Czochralski method which can enhance the productivity, yield and quality of crystal and a single crystal growing method, wherein the crucible has an inner bottom surface, the profile of which has at least one raised portion symmetrical about the rotary axis of the crucible wherein the periphery of the raised portion is positioned at a distance of from 0.4 to 1.2 times the radius of crystal to be grown from the rotary axis and the height of the raised portion is generally not smaller than 7% and greater than 100% of the radius of crystal to be grown.

摘要翻译： 一种用于通过切克劳斯基法生长单晶的坩埚，其可以提高晶体的生产率，产率和质量以及单晶生长方法，其中坩埚具有内底表面，其内廓具有至少一个凸起部分对称 关于坩埚的旋转轴线，其中凸起部分的周边位于离旋转轴线生长的晶体半径的0.4至1.2倍的距离处，并且凸起部分的高度通常不小于7％ 并且大于待生长的晶体半径的100％。

公开(公告)号：US20060283378A1

公开(公告)日：2006-12-21

申请号：US11451989

申请日：2006-06-13

申请人： Yutaka Kishida ,  Seiki Takebayashi ,  Teruyuki Tamaki

发明人： Yutaka Kishida ,  Seiki Takebayashi ,  Teruyuki Tamaki

IPC分类号： C30B15/00 ,  C30B21/06 ,  C30B27/02 ,  C30B28/10 ,  C30B30/04

CPC分类号： C30B15/00 ,  C30B29/06 ,  Y10S117/916

摘要： In silicon single crystal growth by the Czochralski method using a quartz crucible, a silicon single crystals with a uniform distribution of oxygen concentration can be produced in high yield without being affected by changes of crystal diameter and initial amount of melt feedstock. The oxygen concentration is adjusted by estimating oxygen concentration during growth on the basis of a relationship among three parameters: crucible rotation rate (Ω), crucible temperature (T), and the ratio (β) of contact area of molten silicon with the inner wall of the crucible and with atmospheric gas, and by associating the temperature (T) with the ratio (β) by the function 1/β×Exp(−E/T) where E is the dissolution energy (E) of quartz into molten silicon to control at least one of the rotation rate (Ω) and temperature (T) to conform the estimated oxygen concentration to a target concentration.

公开(公告)号：US10167199B2

公开(公告)日：2019-01-01

申请号：US14383321

申请日：2012-03-08

申请人： Shinji Tokumaru ,  Masataka Hiyoshi ,  Jiro Kondo ,  Hitoshi Dohnomae ,  Yutaka Kishida ,  Shigeru Nakazawa ,  Kozo Onoue

发明人： Shinji Tokumaru ,  Masataka Hiyoshi ,  Jiro Kondo ,  Hitoshi Dohnomae ,  Yutaka Kishida ,  Shigeru Nakazawa ,  Kozo Onoue

IPC分类号： C01B33/021 ,  C30B21/00 ,  C01B33/037 ,  C30B29/06 ,  C30B11/00 ,  H01L31/0288 ,  C30B13/10

摘要： Provided are: a method for manufacturing a highly pure silicon by unidirectional solidification of molten silicon, that can inexpensively and industrially easily manufacture highly pure silicon that has a low oxygen concentration and low carbon concentration and is suitable for applications such as manufacturing solar cells; highly pure silicon obtained by this method; and silicon raw material for manufacturing highly pure silicon. A method for manufacturing highly pure silicon using molten silicon containing 100 to 1000 ppmw of carbon and 0.5 to 2000 ppmw of germanium as the raw material when manufacturing highly pure silicon by unidirectionally solidifying molten silicon raw material in a casting container, the highly pure silicon obtained by this method, and the silicon raw material for manufacturing the highly pure silicon.