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.

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：US07455822B2

公开(公告)日：2008-11-25

申请号：US10490584

申请日：2003-07-22

申请人： Jiro Kondo ,  Masaki Okajima ,  Shinji Tokumaru ,  Hitoshi Dohnomae

发明人： Jiro Kondo ,  Masaki Okajima ,  Shinji Tokumaru ,  Hitoshi Dohnomae

IPC分类号： C01B33/02

CPC分类号： C01B33/021

摘要： A process for production of Si, characterized by adding an oxide, hydroxide, carbonate or fluoride of an alkali metal element, or an oxide, hydroxide, carbonate or fluoride of an alkaline earth metal element, or two or more of such compounds, to solid SiO in a total molar amount of from 1/20 to 1000 times with respect to the moles of solid SiO, heating the mixture at between the melting point of Si and 2000° C. to induce a chemical reaction which produces Si and separating and recovering the Si from the reaction by-product, for the purpose of inexpensively and efficiently producing Si from various forms of solid SiO with no industrial value produced from Si production steps and the like.

摘要翻译： 一种制备Si的方法，其特征在于将碱金属元素的氧化物，氢氧化物，碳酸盐或氟化物，或碱土金属元素的氧化物，氢氧化物，碳酸盐或氟化物，或两种或更多种这些化合物加入到固体 SiO的总摩尔量相对于固体SiO的摩尔数为1/20至1000倍，在Si的熔点和2000℃之间加热混合物以引起产生Si的化学反应并分离和回收 来自反应副产物的Si，目的是从Si生产步骤等产生的没有工业价值的各种形式的固体SiO低成本和有效地生产Si。

公开(公告)号：US06395249B1

公开(公告)日：2002-05-28

申请号：US09582383

申请日：2000-06-23

申请人： Jiro Kondo ,  Haruo Shimada ,  Shinji Tokumaru ,  Ryuji Watanabe ,  Atsushi Nogami ,  Akihito Kiyose

发明人： Jiro Kondo ,  Haruo Shimada ,  Shinji Tokumaru ,  Ryuji Watanabe ,  Atsushi Nogami ,  Akihito Kiyose

IPC分类号： C01B33037

CPC分类号： C01B33/039 ,  B01J7/00 ,  B01J12/02 ,  B01J19/0013 ,  B01J2219/00087 ,  B01J2219/00141 ,  B01J2219/00159 ,  B01J2219/00164 ,  B01J2219/00184 ,  C01B33/021 ,  C01B33/027 ,  C01B33/037

摘要： It is possible to produce high purity Si by heating solid SiO at a temperature of at least 1000° C. and lower than 1730° C., for a disproportionation reaction in which the SiO solid is decomposed to liquid or solid Si and solid SiO2, and the produced Si is separated from the SiO2 and/or SiO. The SiO solid can be obtained by a process whereby a starting mixture of carbon C, silicon Si or ferrosilicon, or a combination thereof, with SiO2 is heated to generate SiO gas-containing gas, and the SiO-containing gas is cooled to produce SiO solid.

摘要翻译： 通过在至少1000℃且低于1730℃的温度下加热固体SiO，可以通过将SiO固体分解为液体或固体Si和固体SiO 2的歧化反应来生产高纯度Si， 并且所产生的Si与SiO 2和/或SiO 2分离。 通过将碳C，硅Si或硅铁的起始混合物或其组合与SiO 2的起始混合物加热以产生含有SiO气体的气体，可以获得SiO固体，并且将含SiO的气体冷却以产生SiO 固体。

公开(公告)号：US07662356B2

公开(公告)日：2010-02-16

申请号：US11883280

申请日：2006-02-09

申请人： Shinji Tokumaru ,  Kensuke Okazawa ,  Jirou Kondou ,  Masaki Okajima

发明人： Shinji Tokumaru ,  Kensuke Okazawa ,  Jirou Kondou ,  Masaki Okajima

IPC分类号： C01B33/02 ,  C01B33/07

CPC分类号： C01B33/037

摘要： The present invention provides a method of refining low purity Si by a slag, in particular removing B, which suppresses wear of the reaction vessel due to the slag and produces high purity Si used for solar battery materials etc. at a low cost, comprising adding SiO2 and an alkali oxide or alkali carbonate as a slag material into molten Si to form a slag during which adding one or more types of materials among materials the same as the reaction vessel material used or ingredients included in the reaction vessel material into the slag so as to remove the impurities in the molten Si.

摘要翻译： 本发明提供一种通过炉渣精炼低纯度Si的方法，特别是除去B，其抑制了由于炉渣引起的反应容器的磨损，并以低成本产生用于太阳能电池材料等的高纯度Si，包括加入 SiO 2和碱金属氧化物或碱金属碳酸盐作为炉渣材料，形成熔融Si以形成炉渣，在炉渣中添加一种或多种类型的材料，与所使用的反应容器材料相同的材料或包含在反应容器材料中的成分进入炉渣 以去除熔融Si中的杂质。

公开(公告)号：US20080145294A1

公开(公告)日：2008-06-19

申请号：US11883280

申请日：2006-02-09

申请人： Shinji Tokumaru ,  Kensuke Okazawa ,  Jirou Kondou ,  Masaki Okajima

发明人： Shinji Tokumaru ,  Kensuke Okazawa ,  Jirou Kondou ,  Masaki Okajima

IPC分类号： C01B33/023

CPC分类号： C01B33/037

摘要： The present invention provides a method of refining low purity Si by a slag, in particular removing B, which suppresses wear of the reaction vessel due to the slag and produces high purity Si used for solar battery materials etc. at a low cost, comprising adding SiO2 and an alkali oxide or alkali carbonate as a slag material into molten Si to form a slag during which adding one or more types of materials among materials the same as the reaction vessel material used or ingredients included in the reaction vessel material into the slag so as to remove the impurities in the molten Si.

摘要翻译： 本发明提供一种通过炉渣精炼低纯度Si的方法，特别是除去B，其抑制了由于炉渣引起的反应容器的磨损，并以低成本产生用于太阳能电池材料等的高纯度Si，包括加入 SiO 2和作为炉渣的碱金属氧化物或碱金属碳酸盐混合成熔融Si以形成炉渣，在炉渣中添加与所使用的反应容器材料相同的材料中的一种或多种材料， 将反应容器的材料倒入炉渣中以除去熔融Si中的杂质。

公开(公告)号：US08038973B2

公开(公告)日：2011-10-18

申请号：US12086041

申请日：2006-07-20

申请人： Nobuaki Ito ,  Kensuke Okazawa ,  Shinji Tokumaru ,  Masaki Okajima

发明人： Nobuaki Ito ,  Kensuke Okazawa ,  Shinji Tokumaru ,  Masaki Okajima

IPC分类号： C01B33/023 ,  B01J19/12

CPC分类号： C01B33/037

摘要： The present invention provides a high purity silicon production system and production method suitable for using inexpensive metallurgical grade metal silicon as a material and using the slag refining method to produce high purity silicon with a purity of 6N or more suitable for solar battery applications, in particular, high purity silicon with a boron content of at least not more than 0.3 mass ppm, inexpensively on an industrial scale, that is, a high purity silicon production system and production method using the slag refining method wherein a direct electromagnetic induction heating means having the function of directly heating the molten silicon in the crucible by electromagnetic induction is arranged outside the outside wall surface of the above crucible and the crucible is formed by an oxidation resistant material at least at a region where the molten silicon contacts the crucible inside wall surface at the time of not powering the direct electromagnetic induction heating means.

摘要翻译： 本发明提供了一种适用于廉价的冶金级金属硅作为材料的高纯度硅生产系统和生产方法，并且使用炉渣精炼方法生产出适合于太阳能电池应用的纯度为6N或更高的高纯度硅，特别是 硼含量至少为0.3质量ppm以下的高纯度硅，以工业规模廉价，即高纯硅生产系统和使用渣精炼方法的生产方法，其中直接电磁感应加热装置具有 通过电磁感应直接加热坩埚中的熔融硅的功能被布置在上述坩埚的外壁表面的外侧，坩埚至少在熔融硅与坩埚内壁表面接触的区域由抗氧化材料形成 没有为直接电磁感应加热装置供电的时间。

公开(公告)号：US20090155158A1

公开(公告)日：2009-06-18

申请号：US12086041

申请日：2006-07-20

申请人： Nobuaki Ito ,  Kensuke Okazawa ,  Shinji Tokumaru ,  Masaki Okajima

发明人： Nobuaki Ito ,  Kensuke Okazawa ,  Shinji Tokumaru ,  Masaki Okajima

IPC分类号： C01B33/02 ,  B01J19/00

CPC分类号： C01B33/037

摘要： The present invention provides a high purity silicon production system and production method suitable for using inexpensive metallurgical grade metal silicon as a material and using the slag refining method to produce high purity silicon with a purity of 6N or more suitable for solar battery applications, in particular, high purity silicon with a boron content of at least not more than 0.3 mass ppm, inexpensively on an industrial scale, that is, a high purity silicon production system and production method using the slag refining method wherein a direct electromagnetic induction heating means having the function of directly heating the molten silicon in the crucible by electromagnetic induction is arranged outside the outside wall surface of the above crucible and the crucible is formed by an oxidation resistant material at least at a region where the molten silicon contacts the crucible inside wall surface at the time of not powering the direct electromagnetic induction heating means.

摘要翻译： 本发明提供了一种适用于廉价的冶金级金属硅作为材料的高纯度硅生产系统和生产方法，并且使用炉渣精炼方法生产出适合于太阳能电池应用的纯度为6N或更高的高纯度硅，特别是 硼含量至少为0.3质量ppm以下的高纯度硅，以工业规模廉价，即高纯硅生产系统和使用渣精炼方法的生产方法，其中直接电磁感应加热装置具有 通过电磁感应直接加热坩埚中的熔融硅的功能被布置在上述坩埚的外壁表面的外侧，坩埚至少在熔融硅与坩埚内壁表面接触的区域由抗氧化材料形成 没有为直接电磁感应加热装置供电的时间。

公开(公告)号：US5523166A

公开(公告)日：1996-06-04

申请号：US375195

申请日：1995-01-18

申请人： Shinji Tokumaru ,  Misao Hashimoto ,  Tomomi Murata

发明人： Shinji Tokumaru ,  Misao Hashimoto ,  Tomomi Murata

IPC分类号： C23C14/06 ,  C23C14/08 ,  C23C14/10 ,  C23C14/34 ,  C23C14/35 ,  C23C14/46 ,  B32B9/00

CPC分类号： C23C14/3435 ,  C23C14/0641 ,  C23C14/081 ,  C23C14/083 ,  C23C14/088 ,  C23C14/10 ,  C23C14/3492 ,  C23C14/35 ,  C23C14/46

摘要： A dense insulating thin film having a remarkably improved insulating property can be formed by a process comprising a first step of forming a first portion of an insulating thin film on a substrate by a sputtering process without exposing the substrate to a plasma or while irradiating the substrate with low energy particles and a second step of forming a second portion of the insulating thin film on the first portion while exposing the substrate to a plasma or while irradiating the substrate with high energy particles, thereby forming said insulating thin film on the substrate. The insulating property in terms of the dielectric breakdown voltage is 100 V or more as determined in a film thickness of 1 .mu.m or less and an area of 20 mm.sup.2.

摘要翻译： 可以通过包括以下步骤形成具有显着提高的绝缘性能的致密绝缘薄膜：第一步骤，通过溅射工艺在衬底上形成绝缘薄膜的第一部分，而不将衬底暴露于等离子体或同时照射衬底 并且在第一部分上形成绝缘薄膜的第二部分，同时将衬底暴露于等离子体或者同时用高能粒子照射衬底，从而在衬底上形成所述绝缘薄膜。 在介电击穿电压方面的绝缘性在膜厚为1μm以下，面积为20mm 2的情况下为100V以上。