公开(公告)号：US09017482B2

公开(公告)日：2015-04-28

申请号：US13496060

申请日：2010-07-20

申请人： Shigeyoshi Netsu ,  Kyoji Oguro ,  Takaaki Shimizu ,  Yasushi Kurosawa ,  Fumitaka Kume

发明人： Shigeyoshi Netsu ,  Kyoji Oguro ,  Takaaki Shimizu ,  Yasushi Kurosawa ,  Fumitaka Kume

IPC分类号： C01B33/035 ,  B01J19/02 ,  C23C16/44 ,  C23C16/54 ,  C23C16/24 ,  C23C16/52

CPC分类号： H01L21/02595 ,  B01J19/02 ,  B01J2219/0236 ,  C01B33/035 ,  C23C16/24 ,  C23C16/4411 ,  C23C16/463 ,  C23C16/52 ,  H01L21/02532 ,  H01L21/02636 ,  Y02P20/124 ,  Y02P20/129

摘要： The present invention provides a technique by which heat can be efficiently recovered from a coolant used to cool a reactor, and contamination with dopant impurities from an inner wall of a reactor when polycrystalline silicon is deposited within the reactor can be reduced to produce high-purity polycrystalline silicon. With the use of hot water 15 having a temperature higher than a standard boiling point as a coolant fed to the reactor 10, the temperature of the reactor inner wall is kept at a temperature of not more than 370° C. Additionally, the pressure of the hot water 15 to be recovered is reduced by a pressure control section provided in a coolant tank 20 to generate steam. Thereby, a part of the hot water is taken out as steam to the outside, and reused as a heating source for another application.

摘要翻译： 本发明提供了一种技术，通过该技术可以降低用于冷却反应器的冷却剂的热量，并且可以减少在反应器内沉积多晶硅时来自反应器的内壁的掺杂剂杂质的污染，以产生高纯度 多晶硅。 通过使用温度高于标准沸点的热水15作为供给到反应器10的冷却剂，反应器内壁的温度保持在不高于370℃的温度。另外， 通过设置在冷却剂罐20中的压力控制部来减少要回收的热水15，以产生蒸汽。 因此，一部分热水作为蒸汽被取出到外部，并且再次用作另一种应用的加热源。

公开(公告)号：US20120207662A1

公开(公告)日：2012-08-16

申请号：US13496060

申请日：2010-07-20

申请人： Shigeyoshi Netsu ,  Kyoji Oguro ,  Takaaki Shimizu ,  Yasushi Kurosawa ,  Fumitaka Kume

发明人： Shigeyoshi Netsu ,  Kyoji Oguro ,  Takaaki Shimizu ,  Yasushi Kurosawa ,  Fumitaka Kume

IPC分类号： C01B33/027 ,  B01J19/00

CPC分类号： H01L21/02595 ,  B01J19/02 ,  B01J2219/0236 ,  C01B33/035 ,  C23C16/24 ,  C23C16/4411 ,  C23C16/463 ,  C23C16/52 ,  H01L21/02532 ,  H01L21/02636 ,  Y02P20/124 ,  Y02P20/129

摘要： The present invention provides a technique by which heat can be efficiently recovered from a coolant used to cool a reactor, and contamination with dopant impurities from an inner wall of a reactor when polycrystalline silicon is deposited within the reactor can be reduced to produce high-purity polycrystalline silicon. With the use of hot water 15 having a temperature higher than a standard boiling point as a coolant fed to the reactor 10, the temperature of the reactor inner wall is kept at a temperature of not more than 370° C. Additionally, the pressure of the hot water 15 to be recovered is reduced by a pressure control section provided in a coolant tank 20 to generate steam. Thereby, a part of the hot water is taken out as steam to the outside, and reused as a heating source for another application.

摘要翻译： 本发明提供了一种技术，通过该技术可以降低用于冷却反应器的冷却剂的热量，并且可以减少在反应器内沉积多晶硅时来自反应器的内壁的掺杂剂杂质的污染，以产生高纯度 多晶硅。 通过使用温度高于标准沸点的热水15作为供给到反应器10的冷却剂，反应器内壁的温度保持在不高于370℃的温度。另外， 通过设置在冷却剂罐20中的压力控制部来减少要回收的热水15，以产生蒸汽。 因此，一部分热水作为蒸汽被取出到外部，并且再次用作另一种应用的加热源。

公开(公告)号：US20090060817A1

公开(公告)日：2009-03-05

申请号：US12190151

申请日：2008-08-12

申请人： Takaaki SHIMIZU ,  Kyoji Oguro

发明人： Takaaki SHIMIZU ,  Kyoji Oguro

IPC分类号： C01B33/107

CPC分类号： C01B33/1071 ,  C23C16/24 ,  C23C16/4412 ,  C23C16/45593

摘要： A by-product mixture produced in a process for producing polycrystalline silicon is made to react with chlorine to form tetrachlorosilane (STC) distillate in a chlorination reaction vessel, and the tetrachlorosilane (STC) distillate is made to react with hydrogen in a hydrogenation reaction vessel to be converted into trichlorosilane (TCS). In the chlorination step, methyl chlorosilanes having boiling points close to TCS are hyper-chlorinated to be converted into hyper-chlorinated methyl chlorosilanes having higher boiling points, which facilitates the hyper-chlorinated methyl chlorosilanes to be separated into high concentration, and inhibits carbon from contaminating the polycrystalline silicon. A donor/acceptor eliminator is provided in the circulation cycle for producing TCS, and accordingly there is no need to take out a by-product produced in the process for producing TCS to the outside of the system, which can highly purify the TCS.

摘要翻译： 在多晶硅的制造方法中制造的副产物混合物与氯反应，在氯化反应容器中形成四氯硅烷（STC）馏出物，使四氯硅烷（STC）馏出物在氢化反应容器中与氢反应 转化为三氯硅烷（TCS）。 在氯化步骤中，沸点接近TCS的甲基氯硅烷被高氯化转化为沸点高的高氯甲基氯硅烷，有利于将高氯甲基氯硅烷分离成高浓度，并抑制碳 污染多晶硅。 在生产TCS的循环循环中提供了供体/受体消除器，因此不需要在系统外部将TCS生产过程中产生的副产物取出，这可以高度净化TCS。

公开(公告)号：US20090057129A1

公开(公告)日：2009-03-05

申请号：US12135487

申请日：2008-06-09

申请人： Takaaki Shimizu ,  Kyoji Oguro

发明人： Takaaki Shimizu ,  Kyoji Oguro

IPC分类号： B01D3/34

CPC分类号： C01B33/1071 ,  C01B33/035 ,  C01B33/10778

摘要： A hydrogenation reaction vessel makes STC-containing substance react with hydrogen to convert the substance into TCS. A low boils removal column separates a chlorosilane distillate discharged from a hydrogenation reaction vessel into TCS and a mixture distillate containing hyper-hydrogenated chlorosilane, and circulates the mixture distillate containing hyper-hydrogenated chlorosilane to the hydrogenation reaction vessel. The mixture distillate containing the hyper-hydrogenated chlorosilane separated in the low boils removal column is circulatingly supplied to the hydrogenation reaction vessel. Accordingly, low boils by-product conventionally wasted is circulated and recycled in the process, which results in enhancing a yield of TCS production.

摘要翻译： 加氢反应容器使含STC的物质与氢反应，将物质转化为TCS。 低沸点去除塔将从氢化反应容器排出的氯硅烷馏出物分离成TCS和含有高氢氯硅烷的混合物馏出物，并将含有高氢化氯硅烷的混合物馏出物循环到氢化反应容器中。 将含有在低沸点去除塔中分离的高氢化氯硅烷的混合物馏出物循环供给到氢化反应器。 因此，通常浪费的低沸点副产物在该过程中循环和循环，这导致提高TCS生产的产率。

公开(公告)号：US5693189A

公开(公告)日：1997-12-02

申请号：US508561

申请日：1995-07-28

申请人： Kyoji Oguro ,  Yasushi Kurosawa

发明人： Kyoji Oguro ,  Yasushi Kurosawa

IPC分类号： C30B25/14 ,  B01J4/00 ,  C03B19/14 ,  C23C16/44 ,  C23C16/448 ,  C23C16/52 ,  H01L21/205 ,  B01D3/42

CPC分类号： C23C16/4482 ,  B01J4/008 ,  C03B19/1415 ,  C23C16/52

摘要： The mixed gas of a liquid raw material is stably supplied to not only one reactor but also a plurality of reactors as maintained with high purity at a fixed concentration. A method to supply a liquid raw material gas by the steps of storing a liquid raw material 31 in a bubbling tank 13 with maintaining the stored liquid raw material at a controlled temperature, bubbling a carrier gas 41 through the liquid raw material 31 thereby evaporating the liquid raw material and simultaneously generating a mixed gas composed of the carrier gas 41 and the liquid raw material 31, subjecting the mixed gas to a condensation treatment, and returning the liquefied liquid raw material 31 to the bubbling tank 13 and meanwhile supplying the mixed gas escaped from the liquefaction to a reactor(s), which method is characterized in that the condensation treatment of the mixed gas is carried out with the pressure and temperature thereof controlled at fixed levels, thereby the concentration of the mixed gas supplied to a reactor(s) is kept at a fixed level.

摘要翻译： 液体原料的混合气体不仅稳定地供给至一个反应器，而且以固定浓度保持高纯度的多个反应器。 通过以下步骤供给液体原料气体的方法：将液体原料31储存在发泡罐13中，同时将储存的液体原料保持在受控温度，使载气41通过液体原料31鼓泡，从而蒸发 同时产生由载气41和液体原料31构成的混合气体，使混合气体进行冷凝处理，并将液化液原料31返回到发泡槽13，同时供给混合气体 该方法的特征在于，将混合气体的压缩和温度控制在固定水平，由此将供给到反应器的混合气体的浓度（ s）保持在一个固定的水平。

公开(公告)号：US20090060822A1

公开(公告)日：2009-03-05

申请号：US12190229

申请日：2008-08-12

申请人： Takaaki Shimizu ,  Kyoji Oguro ,  Takeshi Aoyama

发明人： Takaaki Shimizu ,  Kyoji Oguro ,  Takeshi Aoyama

IPC分类号： H01L21/205

CPC分类号： C23C16/24 ,  C01B33/03 ,  C01B33/1071 ,  C01B33/10721 ,  C23C16/4412 ,  C23C16/45593

摘要： A by-product mixture produced when polycrystalline silicon is deposited on a base material in a CVD reactor is made to react with chlorine to form a tetrachlorosilane (STC) effluent in a chlorination reaction vessel, and the tetrachlorosilane (STC) distillate is made to react with hydrogen in a hydrogenation reaction vessel to be converted into trichlorosilane (TCS). In the chlorination step, poly-silane contained in the above described by-product mixture can be efficiently recycled as a raw material for producing the polycrystalline silicon, which can enhance a yield of the production process. In addition, in the chlorination step, methyl chlorosilanes having boiling points close to TCS are hyper-chlorinated to be converted into hyper-chlorinated methyl chlorosilanes having higher boiling points, which facilitates the hyper-chlorinated methyl chlorosilanes to be separated into high concentration, and reduces carbon contamination of the polycrystalline silicon.

摘要翻译： 将多晶硅沉积在CVD反应器中的基材上产生的副产物混合物与氯反应，在氯化反应容器中形成四氯硅烷（STC）流出物，并使四氯硅烷（STC）馏出物反应 在氢化反应容器中用氢气转化为三氯硅烷（TCS）。 在氯化工序中，上述副产物混合物中含有的聚硅烷可以作为制造多晶硅的原料被有效地再循环，从而可提高生产工艺的产率。 此外，在氯化工序中，沸点接近TCS的甲基氯硅烷被高氯化转化为沸点较高的高氯甲基氯硅烷，有利于高氯化甲基氯硅烷分离成高浓度， 减少多晶硅的碳污染。

公开(公告)号：US20090060820A1

公开(公告)日：2009-03-05

申请号：US12203395

申请日：2008-09-03

申请人： Takaaki Shimizu ,  Kyoji Oguro

发明人： Takaaki Shimizu ,  Kyoji Oguro

IPC分类号： C01B33/107 ,  C23C16/22

CPC分类号： C01B33/03 ,  C01B33/035 ,  C01B33/1071

摘要： The present invention includes a step of separating an effluent produced in a hydrogenation step of making tetrachlorosilane (STC) react with hydrogen into trichlorosilane (TCS), into a chlorosilane fraction containing a hydrocarbon and a TCS fraction, and a chlorination step of making the chlorosilane fraction containing the hydrocarbon react with chlorine to form STC and a substance containing a chlorinated hydrocarbon, wherein the effluent containing STC produced in the chlorination step is circulated to the hydrogenation step. In the chlorination step, the chlorosilane fraction containing a hydrocarbon (capable of containing hyper-hydrogenated chlorosilanes) having a boiling point close to TCS is hyper-chlorinated to be converted and acquire a higher boiling point, which facilitates the hyper-chlorinated chlorosilanes and the hyper-chlorinated hydrocarbons to be separated into high concentration, and increases the purity of TCS to be finally obtained.

摘要翻译： 本发明包括将制备四氯硅烷（STC）的氢化步骤中产生的流出物与氢气反应成三氯硅烷（TCS）的步骤，分离成含有烃和TCS馏分的氯硅烷部分，以及制备氯硅烷 含有烃的馏分与氯反应形成STC和含有氯化烃的物质，其中在氯化步骤中产生的含有STC的流出物循环到氢化步骤。 在氯化步骤中，含有沸点接近TCS的烃（能够含有高氢氯硅烷）的氯代硅烷馏分被高氯化转化并获得较高的沸点，这有助于高氯代氯代硅烷和 将高氯化烃分离成高浓度，并提高最终获得的TCS的纯度。

公开(公告)号：US08293076B2

公开(公告)日：2012-10-23

申请号：US12135487

申请日：2008-06-09

申请人： Takaaki Shimizu ,  Kyoji Oguro

发明人： Takaaki Shimizu ,  Kyoji Oguro

IPC分类号： B01D3/34

CPC分类号： C01B33/1071 ,  C01B33/035 ,  C01B33/10778

摘要： Methods for producing trichlorosilane, including: reacting a tetrachlorosilane containing substance with hydrogen at a temperature of 400° C. to 1,200° C. to obtain a mixture including silane, monochlorosilane, dichlorosilane, and trichlorosilane; removing impurities which are electrically active in a semiconductor crystal from the mixture; separating the trichlorosilane from the silane, monochlorosilane and dichlorosilane to obtain purified trichlorosilane; and circulating the silane, monochlorosilane and dichlorosilane obtained from the separating step into the reacting step.

摘要翻译： 制备三氯硅烷的方法包括：使含四氯硅烷的物质与氢气在400℃至1200℃的温度下反应，得到包括硅烷，一氯硅烷，二氯硅烷和三氯硅烷的混合物; 从混合物中除去在半导体晶体中具有电活性的杂质; 从硅烷，一氯硅烷和二氯硅烷中分离出三氯硅烷，得到纯化的三氯硅烷; 并将从分离步骤获得的硅烷，一氯硅烷和二氯硅烷循环进入反应步骤。

公开(公告)号：US07790132B2

公开(公告)日：2010-09-07

申请号：US12203395

申请日：2008-09-03

申请人： Takaaki Shimizu ,  Kyoji Oguro

发明人： Takaaki Shimizu ,  Kyoji Oguro

IPC分类号： C01B33/107 ,  C01B33/023 ,  B01D53/44 ,  B01D53/72

CPC分类号： C01B33/03 ,  C01B33/035 ,  C01B33/1071

摘要： The present invention includes a step of separating an effluent produced in a hydrogenation step of making tetrachlorosilane (STC) react with hydrogen into trichlorosilane (TCS), into a chlorosilane fraction containing a hydrocarbon and a TCS fraction, and a chlorination step of making the chlorosilane fraction containing the hydrocarbon react with chlorine to form STC and a substance containing a chlorinated hydrocarbon, wherein the effluent containing STC produced in the chlorination step is circulated to the hydrogenation step. In the chlorination step, the chlorosilane fraction containing a hydrocarbon (capable of containing hyper-hydrogenated chlorosilanes) having a boiling point close to TCS is hyper-chlorinated to be converted and acquire a higher boiling point, which facilitates the hyper-chlorinated chlorosilanes and the hyper-chlorinated hydrocarbons to be separated into high concentration, and increases the purity of TCS to be finally obtained.

摘要翻译： 本发明包括将制备四氯硅烷（STC）的氢化步骤中产生的流出物与氢气反应到三氯硅烷（TCS）中的流出物分离成含有烃和TCS馏分的氯硅烷馏分和制备氯硅烷的氯化步骤的步骤 含有烃的馏分与氯反应形成STC和含有氯化烃的物质，其中在氯化步骤中产生的含有STC的流出物循环到氢化步骤。 在氯化步骤中，含有沸点接近TCS的烃（能够含有高氢氯硅烷）的氯代硅烷馏分被高氯化转化并获得较高的沸点，这有助于高氯代氯代硅烷和 将高氯化烃分离成高浓度，并提高最终获得的TCS的纯度。

公开(公告)号：US07691357B2

公开(公告)日：2010-04-06

申请号：US12190229

申请日：2008-08-12

申请人： Takaaki Shimizu ,  Kyoji Oguro ,  Takeshi Aoyama

发明人： Takaaki Shimizu ,  Kyoji Oguro ,  Takeshi Aoyama

IPC分类号： C01B33/08 ,  C07F7/00

CPC分类号： C23C16/24 ,  C01B33/03 ,  C01B33/1071 ,  C01B33/10721 ,  C23C16/4412 ,  C23C16/45593

摘要： A by-product mixture produced when polycrystalline silicon is deposited on a base material in a CVD reactor is made to react with chlorine to form a tetrachlorosilane (STC) effluent in a chlorination reaction vessel, and the tetrachlorosilane (STC) distillate is made to react with hydrogen in a hydrogenation reaction vessel to be converted into trichlorosilane (TCS). In the chlorination step, poly-silane contained in the above described by-product mixture can be efficiently recycled as a raw material for producing the polycrystalline silicon, which can enhance a yield of the production process. In addition, in the chlorination step, methyl chlorosilanes having boiling points close to TCS are hyper-chlorinated to be converted into hyper-chlorinated methyl chlorosilanes having higher boiling points, which facilitates the hyper-chlorinated methyl chlorosilanes to be separated into high concentration, and reduces carbon contamination of the polycrystalline silicon.

摘要翻译： 将多晶硅沉积在CVD反应器中的基材上产生的副产物混合物与氯反应，在氯化反应容器中形成四氯硅烷（STC）流出物，并使四氯硅烷（STC）馏出物反应 在氢化反应容器中用氢气转化为三氯硅烷（TCS）。 在氯化工序中，上述副产物混合物中含有的聚硅烷可以作为制造多晶硅的原料被有效地再循环，从而可提高生产工艺的产率。 此外，在氯化工序中，沸点接近TCS的甲基氯硅烷被高氯化转化为沸点较高的高氯甲基氯硅烷，有利于将高氯甲基氯代硅烷分离成高浓度， 减少多晶硅的碳污染。