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1. 发明授权

US11242620B2 Polycrystalline silicon rod and method for producing polycrystalline silicon rod 有权
公开(公告)号：US11242620B2
公开(公告)日：2022-02-08
申请号：US16026818
申请日：2018-07-03
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Naruhiro Hoshino , Tetsuro Okada , Shigeyoshi Netsu , Masahiko Ishida
IPC分类号： C01B33/035 , C30B35/00 , C23C16/24 , C30B29/06 , C23C16/44 , C30B13/00
摘要： To provide polycrystalline silicon suitable as a raw material for production of single-crystalline silicon. A D/L value is set within the range of less than 0.40 when multiple pairs of silicon cores are placed in a reaction furnace in production of a polycrystalline silicon rod having a diameter of 150 mm or more by deposition according to a chemical vapor deposition process and it is assumed that the average value of the final diameter of the polycrystalline silicon rod is defined as D (mm) and the mutual interval between the multiple pairs of silicon cores is defined as L (mm).

2. 发明授权

US11167994B2 Polycrystalline silicon rod, processing method for polycrystalline silicon rod, method for evaluating polycrystalline silicon rod, and method for producing FZ single crystal silicon 有权
公开(公告)号：US11167994B2
公开(公告)日：2021-11-09
申请号：US17012418
申请日：2020-09-04
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu , Junichi Okada
IPC分类号： C30B13/00 , C01B33/02 , C01B33/035 , C30B29/06 , C30B35/00 , C30B13/30 , G01N23/20 , G01N23/207
摘要： For evaluating a polycrystalline silicon rod to be used as a raw material for production of FZ Si single crystals, novel evaluation values (values of characteristics×amount of crystals) including the amount of crystals grown in the growth direction (radial direction) are defined and the homogeneity in crystal characteristics in the growth direction (radial direction) is evaluated. Specifically, the homogeneity of the polycrystalline rod is evaluated by sampling a plurality of specimen plates each having, as a principal plane thereof, a cross-section perpendicular to a radial direction of the polycrystalline rod grown by a Siemens method at equal intervals in the radial direction, determining values of characteristics of the crystals of the specimen plates by measurements, and by using evaluation values obtained by multiplying amounts of the crystals (relative amounts of the crystals) at sites where the specimen plates have been sampled by the values of the crystal characteristics.

3. 发明申请

US20180002180A1 POLYCRYSTALLINE SILICON ROD, PRODUCTION METHOD THEREFOR, AND FZ SILICON SINGLE CRYSTAL 审中-公开
公开(公告)号：US20180002180A1
公开(公告)日：2018-01-04
申请号：US15548569
申请日：2015-12-10
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu
IPC分类号： C01B33/035 , C30B28/14 , C30B13/00 , C30B29/06 , C23C16/24
CPC分类号： C01B33/035 , C01B33/02 , C23C16/24 , C30B13/00 , C30B28/14 , C30B29/06
摘要： A plate-shaped sample with a cross-section perpendicular to a radial direction of a polycrystalline silicon rod as a principal surface is sampled from a region from a center (r=0) of the polycrystalline silicon rod to R/3. Then, the sample is disposed at a position at which a Bragg reflection from a (111) Miller index plane is detected. In-plane rotation with a rotational angle φ on the sample is performed with a center of the sample as a rotational center such that an X-ray irradiation region defined by a slit performs φ-scanning on the principal surface of the sample to obtain a diffraction chart indicating dependency of a Bragg reflection intensity from the (111) Miller index plane on a rotational angle of the sample. A ratio (Sp/St) between an area Sp of a peak part appearing in the diffraction chart and a total area St of the diffraction chart is calculated.

4. 发明授权

US10377636B2 Method for producing polycrystalline silicon rod, polycrystalline silicon rod, and polycrystalline silicon mass 有权
公开(公告)号：US10377636B2
公开(公告)日：2019-08-13
申请号：US15309218
申请日：2015-05-27
申请人： SHIN-ETSU CHEMICAL CO., LTD.
发明人： Shuichi Miyao , Junichi Okada , Shigeyoshi Netsu
IPC分类号： C01B33/035 , C30B29/06
摘要： A polycrystalline silicon rod is synthesized by the Siemens method (S101). After the polycrystalline silicon rod is covered from above with a plastic bag whose inner surface has been washed, and housed in the plastic bag in a reactor (S103), the polycrystalline silicon rod is removed out of the reactor (S104), and heat-sealed and stored in an enclosed state (S105). According to the present invention, steps conventionally considered as essential, such as washing, etching, and water washing, are not always necessary, and therefore the concentrations of fluorine ions, nitrate ions, and nitrogen dioxide ions remaining on the surface can each be less than 0.2 ppbw. In addition, by covering with the plastic bag, the metal contamination levels decrease significantly. Moreover, when the handling according to the present invention is performed, surface contamination hardly proceeds even if the polycrystalline silicon rod is stored for a long period.

5. 发明授权

US10066320B2 Polycrystalline silicon, FZ single crystal silicon, and method for producing the same 有权
公开(公告)号：US10066320B2
公开(公告)日：2018-09-04
申请号：US15432171
申请日：2017-02-14
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu
IPC分类号： C30B29/06 , C30B28/14 , C30B13/08 , C23C16/24
摘要： When FZ single crystal silicon is produced from polycrystalline silicon, which is synthesized by the Siemens method followed by being subjected to thermal treatment and includes crystal grains having a Miller index plane or as a principal plane and grown by the thermal treatment, and in which the X-ray diffraction intensity from either of the Miller index planes and after the thermal treatment is 1.5 times or less the X-ray diffraction intensity before the thermal treatment, as raw material, disappearance of crystal lines in the step of forming an FZ single crystal is markedly prevented.

6. 发明申请

US20180105950A1 POLYCRYSTALLINE SILICON INGOT, POLYCRYSTALLINE SILICON BAR, AND METHOD FOR PRODUCING SINGLE CRYSTAL SILICON 审中-公开
公开(公告)号：US20180105950A1
公开(公告)日：2018-04-19
申请号：US15785895
申请日：2017-10-17
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu , Naruhiro Hoshino , Tetsuro Okada
IPC分类号： C30B13/34 , C30B29/06
摘要： A polycrystalline silicon ingot having a value of Te−Ts, ΔT, of 50° C. or less, wherein Ts and Te are the onset temperature and the completion temperature of melting, respectively, when the temperature is increased at a rate of 60° C./minute or less in the temperature range of 1400° C. or more is used as the production raw material for single crystal silicon. The present invention provides a polycrystalline silicon ingot or polycrystalline silicon rod suitable for stably producing single crystal silicon.

7. 发明授权

US09355918B2 Method for producing high-purity polycrystalline silicon 有权
标题翻译：高纯多晶硅生产方法
公开(公告)号：US09355918B2
公开(公告)日：2016-05-31
申请号：US14407255
申请日：2013-06-13
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Kazunori Funazaki , Kazuomi Sato , Shuichi Miyao
IPC分类号： G01R31/26 , H01L21/66 , C01B33/03 , C01B33/035 , G01N33/00 , H01L21/02
CPC分类号： H01L22/10 , C01B33/03 , C01B33/035 , G01N33/00 , G01N2033/0095 , H01L21/02532 , H01L21/02595 , H01L21/0262
摘要： The present invention provides technology for realizing higher purification of a polycrystalline silicon. First, trichlorosilane is prepared as a sample (S101) and then the carbon-containing impurities content in the trichlorosilane is analyzed by GC/MS-SIM method (S102). The quality of the trichlorosilane is determined based on the analysis results (S103) and the trichlorosilane determined to be a good material (S103: Yes) is used as the raw material for producing a high-purity polycrystalline silicon by CVD method (104). In case, the trichlorosilane determined to be a bad material (S103: No) is not used as the raw material for producing a polycrystalline silicon. When the impurities analysis by GC/MS-SIM method is performed using, as a separation column, a column having a non-polar column and a medium-polar column connected in series with each other, it is possible to simultaneously perform both of the separation of chlorosilanes and hydrocarbons and the separation of chlorosilanes and methylsilanes.
摘要翻译：本发明提供了实现多晶硅更高纯化的技术。首先，作为样品制备三氯硅烷（S101），然后通过GC / MS-SIM法分析三氯硅烷中的含碳杂质含量（S102）。基于分析结果确定三氯硅烷的质量（S103），将通过CVD法制造高纯度多晶硅的原料（104）用作为高质量的三氯硅烷（S103：是）。判定为不良物质的三氯硅烷（S103：否）不用作多晶硅的制造原料。当通过GC / MS-SIM方法进行杂质分析时，使用具有非极性列和中极性列的列作为分离柱进行串联连接，可以同时进行分离氯硅烷和烃类以及氯硅烷和甲基硅烷的分离。

8. 发明授权

US10800659B2 Polycrystalline silicon rod, processing method for polycrystalline silicon rod, method for evaluating polycrystalline silicon rod, and method for producing FZ single crystal silicon 有权
公开(公告)号：US10800659B2
公开(公告)日：2020-10-13
申请号：US15537968
申请日：2015-12-09
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu , Junichi Okada
IPC分类号： C01B33/02 , C01B33/035 , C30B29/06 , C30B35/00 , C30B13/30 , G01N23/20 , G01N23/207 , C30B13/00
摘要： For evaluating a polycrystalline silicon rod to be used as a raw material for production of FZ Si single crystals, novel evaluation values (values of characteristics×amount of crystals) including the amount of crystals grown in the growth direction (radial direction) are defined and the homogeneity in crystal characteristics in the growth direction (radial direction) is evaluated. Specifically, the homogeneity of the polycrystalline rod is evaluated by sampling a plurality of specimen plates each having, as a principal plane thereof, a cross-section perpendicular to a radial direction of the polycrystalline rod grown by a Siemens method at equal intervals in the radial direction, determining values of characteristics of the crystals of the specimen plates by measurements, and by using evaluation values obtained by multiplying amounts of the crystals (relative amounts of the crystals) at sites where the specimen plates have been sampled by the values of the crystal characteristics.

9. 发明授权

US10343922B2 Polycrystalline silicon rod, production method therefor, and FZ silicon single crystal 有权
公开(公告)号：US10343922B2
公开(公告)日：2019-07-09
申请号：US15548569
申请日：2015-12-10
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Shigeyoshi Netsu
IPC分类号： C01B33/02 , C01B33/035 , G01N23/20 , C30B29/06 , C23C16/24 , C30B13/00 , C30B28/14
摘要： A plate-shaped sample with a cross-section perpendicular to a radial direction of a polycrystalline silicon rod as a principal surface is sampled from a region from a center (r=0) of the polycrystalline silicon rod to R/3. Then, the sample is disposed at a position at which a Bragg reflection from a (111) Miller index plane is detected. In-plane rotation with a rotational angle φ on the sample is performed with a center of the sample as a rotational center such that an X-ray irradiation region defined by a slit performs φ-scanning on the principal surface of the sample to obtain a diffraction chart indicating dependency of a Bragg reflection intensity from the (111) Miller index plane on a rotational angle of the sample. A ratio (Sp/St) between an area Sp of a peak part appearing in the diffraction chart and a total area St of the diffraction chart is calculated.

10. 发明申请

US20190017193A1 POLYCRYSTALLINE SILICON ROD AND METHOD FOR PRODUCING POLYCRYSTALLINE SILICON ROD 审中-公开
公开(公告)号：US20190017193A1
公开(公告)日：2019-01-17
申请号：US16026818
申请日：2018-07-03
申请人： Shin-Etsu Chemical Co., Ltd.
发明人： Shuichi Miyao , Naruhiro Hoshino , Tetsuro Okada , Shigeyoshi Netsu , Masahiko Ishida
IPC分类号： C30B35/00 , C30B29/06 , C23C16/24
摘要： To provide polycrystalline silicon suitable as a raw material for production of single-crystalline silicon. A D/L value is set within the range of less than 0.40 when multiple pairs of silicon cores are placed in a reaction furnace in production of a polycrystalline silicon rod having a diameter of 150 mm or more by deposition according to a chemical vapor deposition process and it is assumed that the average value of the final diameter of the polycrystalline silicon rod is defined as D (mm) and the mutual interval between the multiple pairs of silicon cores is defined as L (mm).

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