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公开(公告)号：EP3168190A1
公开(公告)日：2017-05-17
申请号：EP15818302.0
申请日：2015-07-02
IPC分类号： C01B33/107
CPC分类号： C01B33/10794 , B01D3/14 , C01B33/107 , C01B33/1071 , C01B33/10789
摘要： First, at least one of silanol and a siloxane compound is generated in a chlorosilane (S101). In the step, for example, an inert gas having a moisture concentration of 0.5 to 2.5 ppm is brought into contact with the chlorosilane to dissolve the moisture, and at least one of silanol and a siloxane compound is generated through a hydration reaction of a moiety of the chlorosilane. Next, a boron-containing compound contained in the chlorosilane is reacted with the silanol or the siloxane compound, thereby converting the boron-containing compound to a boron oxide (S102). Through the step (S102), the boron-containing compound being a low boiling point compound is converted to a boron oxide being a high boiling point compound, and therefore the difference in boiling point from the boiling point of chlorosilane becomes larger to make later separation easy.
摘要翻译： 首先，在氯硅烷中生成硅烷醇和硅氧烷化合物中的至少一种（S101）。 在该工序中，例如使水分浓度为0.5〜2.5ppm的惰性气体与氯硅烷接触而溶解水分，通过水分子反应生成硅烷醇和硅氧烷化合物中的至少一种 的氯硅烷。 接着，使氯硅烷中含有的含硼化合物与硅烷醇或硅氧烷化合物反应，将含硼化合物转化为氧化硼（S102）。 通过步骤（S102），将作为低沸点化合物的含硼化合物转化为高沸点化合物即氧化硼，因此与氯硅烷的沸点的沸点差变大，以后分离 简单。
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2.发明公开METHOD FOR PRODUCING POLYCRYSTALLINE SILICON ROD, POLYCRYSTALLINE SILICON ROD, AND POLYCRYSTALLINE SILICON MASS 审中-公开用于生产多晶硅棒，多晶硅BAR和多晶硅MASS
公开(公告)号：EP3153468A1
公开(公告)日：2017-04-12
申请号：EP15803978.4
申请日：2015-05-27
IPC分类号： C01B33/035 , C30B29/06
CPC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.
摘要翻译： 多晶硅棒是由西门子法（S101）合成。 多晶硅棒从上方覆盖有塑料袋，其内表面已被清洗后，并在塑料袋坐落在反应器中（S103），多晶硅棒被除去的反应器（S104），和热 密封，并存储在状态（S105）包围。 。根据本发明，步骤通常视为基本,:例如洗涤，蚀刻，和水洗涤，并不总是必要的，并且氟离子，硝酸根离子，和二氧化氮离子残留在表面上。因此所述浓度可以分别是以下 0.2等于0.1ppbw。 此外，通过用塑料袋覆盖，所述金属污染水平显着降低。 更完了，当处理gemäß在本发明中进行，表面污染难以进行即使多晶硅棒被存储很长一段时间。
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3.发明公开POLYCRYSTALLINE SILICON ROD, METHOD FOR PRODUCING POLYCRYSTALLINE SILICON ROD, AND MONOCRYSTALLINE SILICON 审中-公开POLYKRISTALLINER SILICIUMSTAB，VERFAHREN ZUR HERSTELLUNG DES POLYKRISTALLINEN SILICIUMSTABS UND MONOKRISTALLINES SILICIUM
公开(公告)号：EP3141525A1
公开(公告)日：2017-03-15
申请号：EP15788993.2
申请日：2015-04-24
IPC分类号： C01B33/035 , C30B29/06
CPC分类号： C30B13/08 , C01B33/035 , C30B15/02 , C30B29/06
摘要： In the present invention, once a polycrystalline silicon rod is grown by the Siemens process, the polycrystalline silicon rod is heat-treated within a temperature range from 750°C to 900°C to relieve residual stress in the crystal. According to the experiment of the present inventors, residual stress can be relieved satisfactorily by heat treatment at the above-described low temperature, and in addition, metal contamination cannot be induced and the physical properties of the polycrystalline silicon rod cannot be changed. The above heat treatment can be conducted inside a furnace used to grow the polycrystalline silicon rod, and can also be conducted outside a furnace used to grow the polycrystalline silicon rod. According to the present invention, a polycrystalline silicon rod with residual stress (σ) of not more than +20 MPa evaluated by a 26-sin 2 Ψ diagram can be obtained.
摘要翻译： 在本发明中，一旦通过西门子工艺生长多晶硅棒，多晶硅棒在750℃至900℃的温度范围内进行热处理，以减轻晶体中的残余应力。 根据本发明人的实验，通过在上述低温下的热处理可以令人满意地消除残余应力，另外不能引起金属污染，并且多晶硅棒的物理性质不能改变。 上述热处理可以在用于生长多晶硅棒的炉内进行，也可以在用于生长多晶硅棒的炉子的外部进行。 根据本发明，可以获得具有不超过+ 20MPa的残余应力（×）的多晶硅棒，其通过26-sin 2图进行评估。
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4.发明公开METHOD FOR EVALUATING CRYSTAL GRAIN SIZE DISTRIBUTION OF POLYCRYSTALLINE SILICON 审中-公开评估过程结晶粒径分布多晶硅
公开(公告)号：EP3015853A1
公开(公告)日：2016-05-04
申请号：EP14817826.2
申请日：2014-06-03
发明人： MIYAO, Shuichi , NETSU, Shigeyoshi
IPC分类号： G01N23/207 , C01B33/02 , C30B29/06
CPC分类号： G01N23/207 , C01B33/02 , C30B13/00 , C30B15/00 , C30B29/06 , G01N2223/3306 , G01N2223/606
摘要： The method comprises following steps; a collected disk sample (20) is disposed at a position where Bragg reflection from a Miller index plane is detected; the disk sample (20) is rotated in-plane about the center thereof by a rotation angle φ so that an X-ray irradiation region defined by a slit φ-scans the principal plane of the disk sample (20); a chart showing the dependence of intensity of the Bragg reflection on the rotation angle(φ) of the disk sample (20) is determined; the amount of change per a unit rotation angle of diffraction intensity of a baseline of the φ scan chart is determined as a first derivative value; skewness in the normal distribution of the absolute value of the amount of change is calculated; and the skewness is used as an evaluation index of the crystal grain size distribution to select polycrystalline silicon.
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5.发明公开METHOD FOR EVALUATING CRYSTALLINITY OF POLYCRYSTALLINE SILICON 审中-公开VERFAHREN ZUR BEWERTUNG DERKRISTALLINITÄTVON POLYKRISTALLINEM SILICIUM
公开(公告)号：EP3012620A1
公开(公告)日：2016-04-27
申请号：EP14813733.4
申请日：2014-06-03
发明人： MIYAO, Shuichi , NETSU, Shigeyoshi
IPC分类号： G01N23/207 , C30B29/06 , C01B33/02
CPC分类号： G01N23/207 , C01B33/02 , C01P2002/70 , C30B13/00 , C30B15/00 , C30B29/06 , C30B35/007
摘要： The method for evaluating crystallinity of polycrystalline silicon includes: disposing a collected plate sample (20) at a position where Bragg reflection from a first Miller index plane 1 k 1 l 1 > is detected; rotating the plate sample (20) in-plane about the center thereof by a rotation angle φ so that an X-ray irradiation region defined by a slit φ-scans a principal plane of the plate sample (20); determining a chart showing the dependence of intensity of the Bragg reflection from the Miller index plane on the rotation angle (φ) of the plate sample (20); determining a diffraction intensity value (I B 1 ) of a baseline from the chart; similarly determining a diffraction intensity value (I B 2 ) of a baseline from a φ scan chart obtained from a second Miller index plane 2 k 2 1 2 >; and using size relation between the I B 1 value and the I B 2 value as an evaluation index of the crystallinity of polycrystalline silicon.
摘要翻译： 评价多晶硅的结晶性的方法包括：将收集的板样品（20）设置在检测来自第一米勒分度平面
的布拉格反射的位置; 使平板样品（20）的中心绕其中心旋转旋转角度Æ，使得由狭缝Æ扫描的X射线照射区域扫描板样品（20）的主平面; 确定显示来自米勒分度平面 的布拉格反射强度对板样品（20）的旋转角（Æ）的依赖性的图表; 从图表确定基线的衍射强度值（I B 1）; 类似地根据从第二米勒分度平面 获得的Æ扫描图确定基线的衍射强度值（I B 2）; 并且使用I B 1值和I B 2值之间的尺寸关系作为多晶硅的结晶度的评价指标。 -
公开(公告)号：EP3260415B1
公开(公告)日：2020-03-11
申请号：EP15882516.6
申请日：2015-12-10
发明人： MIYAO, Shuichi , NETSU, Shigeyoshi
IPC分类号： C01B33/035 , C01B33/02 , C30B29/06
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7.发明公开POLYCRYSTALLINE SILICON ROD, PRODUCTION METHOD THEREFOR, AND FZ SILICON SINGLE CRYSTAL 审中-公开多晶硅棒及其生产方法和FZ硅单晶
公开(公告)号：EP3260415A1
公开(公告)日：2017-12-27
申请号：EP15882516.6
申请日：2015-12-10
发明人： MIYAO, Shuichi , NETSU, Shigeyoshi
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 (S p /S t ) between an area S p of a peak part appearing in the diffraction chart and a total area S t of the diffraction chart is calculated.
摘要翻译： 从多晶硅棒的中心（r = 0）到R / 3的区域采样具有与多晶硅棒的径向垂直的截面作为主表面的板状样品。 然后，将样品设置在检测来自（111）米勒指数平面的布拉格反射的位置。 以样品的中心作为旋转中心进行样品的旋转角度为φ的面内旋转，使得由狭缝限定的X射线照射区域在样品的主表面上进行φ扫描以获得 衍射图表示来自（111）米勒指数平面的布拉格反射强度对样品的旋转角度的依赖性。 计算出现在衍射图中的峰值部分的面积Sp与衍射图的总面积St之间的比（Sp / St）。
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8.发明公开
公开(公告)号：EP3159680A1
公开(公告)日：2017-04-26
申请号：EP15809419.3
申请日：2015-06-17
发明人： MIYAO, Shuichi , NETSU, Shigeyoshi
IPC分类号： G01N23/207 , C01B33/035
CPC分类号： C01B33/035 , G01K11/30 , G01N23/207 , G01N2223/60
摘要： An average diffraction intensity ratio (y = (h 1 , k 1 , l 1 )/(h 2 , k 2 , l 2 )) for a rotation angle (ϕ) is obtained from a first diffraction chart and a second diffraction chart, and a surface temperature during deposition is calculated based on this average diffraction intensity ratio. Based on data on the surface temperature of a polycrystalline silicon rod calculated and supplied current and applied voltage during the deposition of the polycrystalline silicon rod, the supplied current and the applied voltage when newly manufacturing a polycrystalline silicon rod is controlled to control a surface temperature during the deposition process. By using such a temperature control method, it is also possible to control the difference ΔT (= T c - T s ) between the center temperature T c and the surface temperature T s of a polycrystalline silicon rod during a deposition process to control the value of residual stress in the polycrystalline silicon rod.
摘要翻译： 对于旋转角度的平均衍射强度比（Y =（H 1，K 1升1）/（H 2，K 2，L 2））（O）由第一衍射图和第二衍射图获得， 和沉积期间的表面温度基于此平均衍射强度比被计算。 基于计算出的多晶硅棒的表面温度数据和所述多晶硅棒的沉积过程中提供的电流和施加电压时，所提供的电流，并且当新制造的多晶硅棒的施加电压被控制期间控制表面温度 在沉积过程。 通过使用搜索温度控制方法，因此有可能以控制差“T（= T C - T的多个）在沉积过程期间以控制中心温度T c和多晶硅棒的表面温度Ts之间 在多晶硅棒的残余应力的值。
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公开(公告)号：EP2862840B1
公开(公告)日：2017-01-25
申请号：EP13804452.4
申请日：2013-06-13
IPC分类号： C01B33/03 , G01N33/00 , C01B33/035 , H01L21/02 , H01L21/66
CPC分类号： H01L22/10 , C01B33/03 , C01B33/035 , G01N33/00 , G01N2033/0095 , H01L21/02532 , H01L21/02595 , H01L21/0262
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10.发明公开
公开(公告)号：EP3613704A1
公开(公告)日：2020-02-26
申请号：EP19196058.2
申请日：2015-04-24
IPC分类号： C01B33/035 , C30B29/06 , C30B33/02 , C30B13/08 , C30B15/02
摘要： In the present invention, once a polycrystalline silicon rod is grown by the Siemens process, the polycrystalline silicon rod is heat-treated within a temperature range from 750°C to 900°C to relieve residual stress in the crystal. According to the experiment of the present inventors, residual stress can be relieved satisfactorily by heat treatment at the above-described low temperature, and in addition, metal contamination cannot be induced and the physical properties of the polycrystalline silicon rod cannot be changed. The above heat treatment can be conducted inside a furnace used to grow the polycrystalline silicon rod, and can also be conducted outside a furnace used to grow the polycrystalline silicon rod. According to the present invention, a polycrystalline silicon rod with residual stress (σ) of not more than +20 MPa evaluated by a 2θ-sin 2 Ψ diagram can be obtained.
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